Clarus 500 GC Hardware Guide

Clarus 500 GC Hardware Guide
Clarus 500 GC
Hardware Guide
Release History
Part Number
Release
Publication Date
09936591
B
August 2002
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton
Connecticut 06484-4794
U.S.A.
Or emailed to: [email protected]
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer
makes no warranty of any kind with regard to this document, including, but not
limited to, the implied warranties of merchantability and fitness for a particular
purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential
damages in connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form
whatsoever or translated into any language without the prior, written permission of
PerkinElmer, Inc.
Copyright © 2002 PerkinElmer, Inc.
Produced in the USA.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically
marked as such, are protected by law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.
e-ssentials is a trademark of PerkinElmer, Inc.
Table of Contents
Chapter 1 Introduction
About This Manual...................................................................................... 1-3
Conventions Used in this Manual................................................................ 1-5
Electromagnetic Compatibility (EMC) ....................................................... 1-6
Warning Signs on the Instrument ................................................................ 1-8
Chapter 2 Safety Practices
Chapter Overview........................................................................................ 2-3
Precautions .................................................................................................. 2-5
Environmental Conditions........................................................................... 2-6
Electrical Safety .......................................................................................... 2-8
Moving the Clarus 500 GC........................................................................ 2-11
ECD Radioactive Hazards......................................................................... 2-12
Safe Handling of Gases ............................................................................. 2-16
Hazardous Chemicals ................................................................................ 2-20
Definitions in Warning for Hazardous Chemicals .................................... 2-21
Chapter 3 System Description
Overview of the Clarus 500 GC .................................................................. 3-4
About the Touch Screen .............................................................................. 3-7
Chapter 4 Before You Install a Column
Column Installation Information ................................................................. 4-4
Protecting Your Column.............................................................................. 4-6
Chapter 5 Installing a Packed Column
Summary ..................................................................................................... 5-4
Materials and Tools Required ..................................................................... 5-5
Packed Column Injector Overview ............................................................. 5-6
Chapter 6 Installing a Capilliary Column
Summary ..................................................................................................... 6-4
Materials and Tools Required ..................................................................... 6-5
Step A: Turn the Heaters Off: ..................................................................... 6-7
Step B: Connect the Column to the Injector:............................................... 6-8
Step C: Set the Carrier Gas ................................................................... 6-59
Step D
Leak Test All New Connections: ............................................. 6-78
Step E: Condition the Column and the Mechanical Joint
Between the Pre-column and Column:...................................................... 6-81
Step F:
Connect the Column to the Detector:....................................... 6-86
Step G: Leak Test All New Connections: ............................................. 6-91
Step H: Set up the Split Mode for a CAP or PSS Injector: .................. 6-92
PSS and POC Operating Hints: ................................................................. 6-93
Calculating a Capillary Column Split Ratio .............................................. 6-96
Chapter 7 PreVent
Overview ..................................................................................................... 7-3
Installing PreVent on an Injector................................................................. 7-5
Installing PreVent on a Detector ............................................................... 7-27
Installing PreVent on a TurboMass MS Detector ..................................... 7-45
PreVent Operating Techniques.................................................................. 7-71
Chapter 8 PPC Fundamentals
Introduction ................................................................................................. 8-3
Carrier Gas Control ..................................................................................... 8-5
Detector Gas Flow Control........................................................................ 8-30
Auxiliary Pressure and Flow Control ........................................................ 8-34
PPC Tips and Techniques.......................................................................... 8-38
Chapter 9 Maintenance
Autosampler Maintenance........................................................................... 9-4
Changing a Syringe ..................................................................................... 9-5
Installing a Syringe.................................................................................... 9-10
Replacing the Vial-Locator Mechanism.................................................... 9-11
Syringe Maintenance ................................................................................. 9-13
Injector Maintenance ................................................................................. 9-14
Changing the Charcoal Trap or Replacing Charcoal on
the Split/Splitless CAP and PSS Injectors................................................. 9-36
ECD Maintenance ..................................................................................... 9-40
FID Maintenance ....................................................................................... 9-49
PID Maintenance ....................................................................................... 9-56
ElCD Maintenance .................................................................................... 9-62
NPD Maintenance ..................................................................................... 9-67
FPD Maintenance ...................................................................................... 9-82
PPC Maintenance ...................................................................................... 9-97
Practical Hints ......................................................................................... 9-101
Chapter 10 Troubleshooting
Error Messages .......................................................................................... 10-4
GC Troubleshooting .................................................................................. 10-9
ElCD Troubleshooting ............................................................................ 10-12
Appendix 1
Nuclear Regulatory Commission Regulations ......................................... A1-1
Appendix 11
Ionization Potential
Index
A2-1
Introduction
1
Introduction
1-2
Clarus 500 GC Hardware Guide
About This Manual
This hardware guide is divided into following chapters:
Chapter 1 Introduction
This chapter contains a brief introduction on the instrument, the conventions and
warnings used in the manual.
Chapter 2 Safety Practices
Important safety information for the Clarus 500 GC is provided in this chapter.
Chapter 3 System Description
This chapter contains information on the components of the instrument, how it
works and instrument specifications.
Chapter 4 Before You Install a Column
This chapter contains general information regarding column installation and the
basic procedures you should know in order to install a column.
Chapter 5 Installing a Packed Column
This chapter contains procedures for connecting a packed column to the packed
column injector and setting the carrier gas flow using PPC and/or manual
pneumatics.
Chapter 6 Installing a Capillary Column
This chapter contains procedures for connecting a capillary column to a Capillary
Injector (CAP); a Programmed Split/Splitless Capillary Injector (PSS); and a
Programmed On-Column Capillary Injector (POC). It also describes how to set
the gas flows using PPC and/or manual pneumatics.
1-3
Introduction
Chapter 7 PreVent
PreVent is an enhanced capillary inlet system for the Clarus 500 GC that uses
columns with an inside diameter (i.d.) between 0.25 mm and 0.53 mm.
Chapter 8 PPC Fundamentals
This chapter describes the fundamentals of Programmable Pneumatic Control
(PPC) and how to use PPC to control your injectors.
Chapter 9 Maintenance
Maintenance and cleaning procedures for the various components of your
instrument are provided.
Chapter 10 Troubleshooting
Performance checks, troubleshooting information, software and system error
messages along with practical hints for running for the instrument are provided.
Appendix I: U.S. Nuclear Regulations
Regulations from the Nuclear Regulatory Commission.
Appendix II: Ionization Potential
Ionization potentials for representative compounds.
1-4
Clarus 500 GC Hardware Guide
Conventions Used in this Manual
Normal text is used to provide information and instructions.
Bold text refers to button or tab page that is displayed on the touch screen.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
Notes, cautions and warnings
Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.
NOTE: A note indicates additional, significant information that is provided with some
procedures.
CAUTION
We use the term CAUTION to inform you about situations that
could result in serious damage to the instrument or other
equipment. Details about these circumstances are in a box like
this one.
We use the term WARNING to inform you about situations that
could result in personal injury to yourself or other persons.
Details about these circumstances are in a box like this one.
WARNING
Customer Service
PerkinElmer Instruments
710 Bridgeport Avenue
Shelton, CT 06484-4794 U.S.A
Tel: 1 (800) 762-4000 or (203) 762-4000
Internet: http://www.perkinelmer.com
1-5
Introduction
Electromagnetic Compatibility (EMC)
United States (FCC)
This product is classified as a digital device used exclusively as industrial,
commercial, or medical test equipment. It is exempt from the technical standards
specified in Part 15 of the FCC Rules and Regulations, based on Section 15.103
(c).
European Union
All information concerning EMC standards will be in the Declaration of
Conformity and these standards will change as the European Union adds new
requirements.
European Union Industrial Environment
The 230 V/50 Hz. Clarus GC has been manufactured for use in the European
Union and is intended for the industrial environment. The instrument is to be
connected to a mains power network supplied from a high or medium-voltage
transformer dedicated for the supply of an installation feeding a manufacturing or
similar plant.
Industrial environments are characterized by the existence of one or more of the
following conditions:
-industrial, scientific and medical (ISM) apparatus are present
-heavy inductive or capacitive loads are frequently switched
-currents and associated magnetic fields are high
These are the major contributors to the industrial electromagnetic environment
and as such distinguish the industrial from other environments. The instrument is
not intended for connection to a public mains network supplying residential,
commercial and light-industrial locations.
Susceptibility to RF Interference
With the exception of the Flame Ionization Detector (FID), an RF field strength
of 10 V/m between 80 MHz. and 1000 MHz. with 80% modulation at 1 kHz.
may cause a deflection on the chromatographic detector baseline that exceeds its
1-6
Clarus 500 GC Hardware Guide
normal pattern. This implies that if a transmitting device, such as a walkie-talkie
carried by a security guard, is use near the detector, a spike or peak on the
chromatographic baseline may occur. If you are concerned that such an event
may occur, PerkinElmer recommends that walkie-talkie restriction notices be
posted in the vicinity. Cell phones, beepers, and other similar devices operate in
a much higher frequency range and do not cause interference.
1-7
Introduction
Warning Signs on the Instrument
Alternating current.
Protective conductor terminal.
Off position of the main power source.
On position of the main power source.
1-8
Clarus 500 GC Hardware Guide
Warning, hot surface
Warning, risk of electric shock.
Warning (refer to accompanying documents).
1-9
Introduction
Label locations on instrument
1-10
Safety Practices
2
Safety Practices
2-2
Clarus 500 GC Hardware Guide
Chapter Overview
This chapter describes the general safety practices and precautions that must be
observed when operating the Clarus 500 GC.
This advice is intended to supplement, not supersede, the normal safety codes in
the user's country. It is also a supplement to the PerkinElmer standard Safety and
Health Policy. The information provided does not cover every safety procedure
that should be practiced. Ultimately, maintenance of a safe laboratory
environment is the responsibility of the analyst and the analyst's organization.
Please consult all manuals supplied with the Clarus 500 GC and accessories
before you start working with the instrument. Carefully read the safety
information in this chapter and in the other manuals supplied. When setting up
the instrument or performing analyses or maintenance procedures, strictly follow
the instructions provided. The Clarus 500 GC should be used in accordance with
the instructions provided in this manual. If used otherwise, the protection
provided by the instrument may be impaired.
Generic Warnings
Before installing or operating the Clarus 500 GC, read the following information
concerning hazards and potential hazards. You should ensure that anyone
involved with installation and/or operation of the Clarus 500 GC is
knowledgeable in both general safety practices for the laboratory and safety
practices for the Clarus 500 GC. Get advice from your safety engineer, industrial
hygienist, environmental engineer, or safety manager before you install or use
this instrument.
Heated Zones
Heated zones should be treated with caution, for example, injector caps and
detectors. Avoid physical contact with the injector caps. The detector cover may
get hot, especially if flame ionization detectors are operated at high temperatures.
As a general rule, allow heated zones to cool before attempting to work in the
oven, injector, or detector areas.
2-3
Safety Practices
CAUTION
THERMAL RUNAWAY PROTECTION: The Clarus 500 GC
software shuts down the instrument if any heated zone exceeds 470 °C.
Should this occur, the following error message is displayed:
INSTRUMENT SHUTDOWN
xxx THERM RUNAWAY where xxx is the heated zone
Call your PerkinElmer Representative.
Instrument shutdown also occurs if there is a PRT (Platinum
Resistance Thermometer) or MPU (Micro Processor Unit) failure. In
these cases the following error message is displayed:
INSTRUMENT SHUTDOWN
xxx PRT ERROR where xxx is the failed zone.
Call your PerkinElmer Representative.
2-4
Clarus 500 GC Hardware Guide
Precautions
Be sure that all instrument operators read and understand
the precautions listed below. It is advisable to post a copy of
the precautions near or on the instrument shelf.
WARNING
The following precautions must be observed when using the Clarus 500 GC:
•
Be sure that the power line voltage of the Clarus 500 GC corresponds to the
voltage used in your laboratory.
•
Never remove the side panels of the Clarus 500 GC without shutting down
the instrument and disconnecting the instrument power cord from line
power.
•
Do not immerse the purge gas exit line in a liquid, as the liquid may be
drawn back into the sample holder.
•
Only high quality purge gases should be used with the Clarus 500 GC.
Minimum purity of 99.995% is recommended. A high quality filter-dryer
accessory is recommended for the removal of any moisture from the purge
gases.
2-5
Safety Practices
Environmental Conditions
Operating Conditions
CAUTION
The Clarus 500 GC is designed for indoor use only.
Do not operate in a Cold Room or a refrigerated area. The Clarus
500 GC operates most efficiently under the following conditions:
CAUTION
•
Ambient temperature is 10 °C to 35 °C (50 °F to
95 °F). The GC will operate safely between 5 °C and 40 °C (41
°F and 104 °F).
•
Ambient relative humidity is 20% to 80% non-condensing.
•
Operating altitude is in the range of 0 to 2 000 m.
The Clarus 500 GC is not designed for operation in an explosive
environment.
WARNING
Installation Category
The Clarus 500 GC is able to withstand transient overvoltage according to
Installation Category II as defined in IEC 1010-1.
Pollution Degree
The Clarus 500 GC will operate safely in environments that contain
nonconductive foreign matter up to Pollution Degree 2 in IEC 1010-1.
2-6
Clarus 500 GC Hardware Guide
Clarus 500 GC Touch Screen
For optimum performance, the Clarus 500 GC’s touch screen may require
periodic re-calibration. The interval between re-calibration may be affected by
exposure to combined heat and humidity conditions (ambient conditions between
30 °C / 50% RH and 35 °C / 80% RH).
Storage Conditions
The Clarus 500 GC may be stored under the following conditions:
•
ambient temperature is -20 °C to +60 °C (-4 to 140 °F)
•
ambient relative humidity is 20 to 80%, non-condensing
•
altitude is in the range 0 to 12 000 m.
General Laboratory Safety
Your laboratory should have all equipment ordinarily required for the safety of
individuals working with chemicals (fire extinguishers, first-aid equipment,
safety shower and eye-wash fountain, spill cleanup equipment, etc.).
2-7
Safety Practices
Electrical Safety
The Clarus 500 GC contains high voltage. To prevent the risk of shock, unplug
the line cord from the AC outlet and wait at least one minute before opening or
removing any instrument panels.
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
CAUTION
This unit contains protective circuitry. Contact PerkinElmer
Service before performing any AC line tests.
WARNING
Connect the GC to an AC line power outlet that has a protective
ground connection. To ensure satisfactory and safe operation of
the GC, it is essential that the protective ground conductor (the
green/yellow lead) of the line power cord is connected to a true
electrical ground. Any interruption of the protective ground
conductor, inside or outside the GC, or disconnection of the
protective ground terminal may impair the protection provided by
the GC.
Do not operate the GC with any covers or parts removed.
WARNING
2-8
Clarus 500 GC Hardware Guide
WARNING
To avoid electrical shock, disconnect the power cord from the
AC outlet before servicing. Servicing on the GC is to be
performed only by a PerkinElmer service representative or
similarly trained and authorized person.
Do not attempt to make adjustments, replacements or repairs to
this GC except as described in the user documentation.
WARNING
WARNING
CAUTION
For protection against fire hazard, only replace fuses with the
same type and rating. Servicing on the GC is to be
performed only by a PerkinElmer service representative or
similarly trained and authorized person.
To ensure adequate cooling of the instrument electronics, do not obstruct
the gap at the base of the GC, and leave at least a 6-inch clearance
between instruments.
Ensure that the power cord is correctly wired and that the ground leads of all
electrical units (for example, recorders, integrators) are connected together via
the circuit ground to earth. Use only three-prong outlets with common earth
ground connections.
Servicing of incoming AC line components in your laboratory should be
performed only by a licensed electrician.
2-9
Safety Practices
WARNING
Lethal voltages are present at certain areas within the
instrument. Installation and internal maintenance of the
instrument should only be performed by a PerkinElmer service
engineer or similarly authorized and trained person. When the
instrument is connected to line power, opening the instrument
covers is likely to expose live parts. Even when the power switch is
off, high voltages can still be present. Capacitors inside the
instrument may still be charged even if the instrument has been
disconnected from all voltage sources.
The instrument must be correctly connected to a suitable electrical supply. The
supply must have a correctly installed protective conductor (earth ground) and
must be installed or checked by a qualified electrician before connecting the
instrument.
WARNING
Any interruption of the protective conductor (earth ground) inside or
outside the instrument or disconnection of the protective conductor
terminal is likely to make the instrument dangerous. Intentional
interruption is prohibited.
When working with the instrument:
•
Disconnect the instrument from all voltage sources before opening it for any
adjustment, replacement, maintenance, or repair. If afterwards, the opened
instrument must be operated for further adjustment, maintenance, or repair,
this must only be done by a PerkinElmer Service engineer.
•
Whenever it is possible that the instrument is no longer electrically safe for
use, make the instrument inoperative and secure it against any unauthorized
or unintentional operation. The electrical safety of the instrument is likely to
be impaired if, for example, the instrument shows visible damage, has been
subjected to prolonged storage under unfavorable conditions, or has been
subjected to severe stress during transportation.
2-10
Clarus 500 GC Hardware Guide
Moving the Clarus 500 GC
The Clarus 500 GC weighs 53.5 kg (118 lb). Improper lifting can cause injury to
the back. If the instrument must be moved, we recommend that at least two
people carefully lift the instrument in order to move it.
2-11
Safety Practices
ECD Radioactive Hazards
To assure that removable radioactive contamination on the external parts of the
ECD remains at a safe level, the United States Nuclear Regulatory Commission
requires that:
WARNING
•
The ECD must be wipe tested at least once every six months.
•
A record of the results must be maintained for NRC inspection.
United States Government Regulations for ECDs
NOTE: To repair an Electron Capture Detector cell requires a specific license issued by
the U.S. Nuclear Regulatory Commission (NRC) and/or in some states by the
equivalent state agency. For further information on obtaining a license, contact
the Customer Service Department at PerkinElmer, Shelton, Connecticut, or the
NRC Material Branch, Office of Nuclear Materials, Safety and Safeguards,
Washington, DC 20555.
All USNRC regulations can be obtained through the internet at
www.nrc.gov/reading-rm/
NOTE: These instructions are for ECD cell purchasers who are not specifically licensed
to handle radioactive materials.
The Clarus 500 GC Electron Capture Detector model (Part No. N610-0063)
contains a maximum of 15 mCi of Nickel 63 (Ni 63), a radioactive material.
Your possession and use of this detector is governed by 10 C.F.R. Section 31.5
which is reproduced in Appendix I. Under the provisions of that regulation you
are deemed a "General Licensee."
Your possession and use of the detector cell may also be regulated by the state
where you are located. The requirements of state regulatory agencies are
substantially similar to those contained in NRC regulation 10 C.F.R. Section
31.5, but they may differ in some respects. It is suggested that you procure a copy
of the regulations of your particular state. (Supplement 2 in Appendix I contains
a list of the "Agreement States" which have been granted authority by the U.S.
Nuclear Regulatory Commission to regulate the possession and use of radioactive
material.)
2-12
Clarus 500 GC Hardware Guide
It is required that you be familiar with regulation 10 C.F.R. Section 31.5
(Appendix 1 in the Hardware Guide 0993-6590). Following are summaries of its
requirements.
Labels
Do not remove any of the labels attached to the ECD cell or any of the labels
attached to your Clarus 500 Gas Chromatograph that refer to the ECD cell.
Follow all instructions and abide by all precautions provided by the labels and in
user instruction manuals referred to by the labels.
2-13
Safety Practices
Leak Testing
You are obligated under U.S. federal and state regulations to make certain that
the ECD cell is wipe-tested for leakage of radioactive materials at intervals of no
longer than six months, and that the analysis of these wipe tests is conducted by a
person specifically licensed to do so, either by the U.S. Nuclear Regulatory
Commission or by an Agreement State. The analyses can be performed by the
firm listed below:
National Leak Test Center
P.O. Box 486
North Tonawanda, New York 14120
ECD Cell Failure or Damage
If a leak test detects more than 0.005 µCi (microcurie) of removable radioactive
material on the surface of an ECD cell, or if the cell itself is damaged in such a
way as to indicate that it may no longer adequately shield the radioactive material
inside, you must immediately suspend operation of your chromatograph until the
cell has been repaired or disposed of by a person specifically licensed to do so.
Any such incident must be reported by you to the Regional Office, Inspection
and Enforcement, U.S. Nuclear Regulatory Commission.
Reporting Radiation Incidents, Theft or Loss
Please read Regulation 10 C.F.R. Section 20.2201 and 20.2202. These describe
your duties should the radioactive material (Ni 63) in the ECD cell be lost, stolen,
or released, or should any person be exposed to radiation.
Other ECD Requirements
Regulation 10 C.F.R. Section 31.5 (see Appendix I) does not permit you to
abandon the ECD cell or export it. It may not be transferred except to a person
specifically licensed to receive it. Within thirty days of such a transfer, you must
report to the Director of Nuclear Material Safety and Safeguards, U.S. Nuclear
Regulatory Commission, Washington, D.C. 20555, the name and address of the
2-14
Clarus 500 GC Hardware Guide
transferee. However, no report is needed to transfer a defective ECD cell to
PerkinElmer in order to obtain a replacement.
You may transfer the ECD cell to another general licensee, like yourself, only
when it remains at the same location to which it was shipped by PerkinElmer.
Give the transferee a copy of these instructions and the regulations in Appendix I,
and report to the commission as required in Regulation C.F.R. Section 31.5.
NEVER DISMANTLE THE ECD CELL!!
You can remove the ECD cell from the GC for repair.
WARNING
United Kingdom Regulations
In the U.K., registration is required under the Radioactive Substances Act of
1960, for anyone keeping or using radioactive materials. Application should be
made to any one of the following governing bodies:
ENGLAND
Department of the Environment
Queen Anne's Chambers
Tothill Street
London, SW1H 9J4
SCOTLAND Scottish Development Department
21 Hill Street
Edinburgh, EH2 3J4
WALES
Welsh Office
Cathay's Park
Cardiff, CF1 3NG
NORTHERN Ministry of Development
IRELAND
Parliament Building
Storemont
Belfast, Northern Ireland
2-15
Safety Practices
Safe Handling of Gases
When using hydrogen, either as the combustion gas for a flame ionization
detector or as a carrier gas, special care must be taken to avoid buildup of
explosive hydrogen/air mixtures. Ensure that all hydrogen line couplings are
leak-free and do not allow hydrogen to vent within the oven.
Ventilation
Adequate ventilation must be provided, particularly if a liquid nitrogen or carbon
dioxide subambient accessory is in constant use. When analyzing hazardous
compounds, such as pesticides, it may be necessary to arrange for venting of
detector effluent into a fume hood.
Using Hydrogen
WARNING
Flame Ionization Detectors (FID) and Flame Photometric
Detectors (FPD) use hydrogen as fuel. If the hydrogen is turned
on without a column attached to the injector and detector fittings
inside the oven, hydrogen could diffuse into the oven creating the
possibility of an explosion. To avoid possible injury, DO NOT
TURN ON THE HYDROGEN UNLESS A COLUMN IS
ATTACHED AND ALL JOINTS HAVE BEEN LEAK TESTED.
Before disconnecting a column, make certain that the hydrogen has
been turned OFF.
If two FIDs or FPDs are installed and only one has a column
attached to it, make certain that you cap off the unused detector
inlet fitting with a 1/8-inch stainless steel plug (Part No. N9300061).
2-16
Clarus 500 GC Hardware Guide
WARNING
Contact the gas supplier for a material safety data sheet
(MSDS) containing detailed information on the potential
hazards associated with the gas. Carefully use, store, and handle
compressed gases in cylinders. Gas cylinders can be hazardous
if they are mishandled.
NOTE: The permanent installation of gas supplies is the responsibility of the user and
should conform to local safety and building codes.
If liquid nitrogen is used, the gas cylinder must be fitted with an over-pressure
regulator which will vent the cylinder as necessary to prevent it from becoming a
safety hazard.
Consult the following references for more detailed information and additional
guidelines about gas cyclinders.
•
Compressed Gas Association (USA), "Safe Handling of Compressed Gases
in Containers," pamphlet no. P-1, 1984.
•
Compressed Gas Association (USA), "The Inert Gases – Argon, Nitrogen
and Helium," pamphlet no. P-9, 1992.
Identification of Gas Cylinders
•
Legibly mark cylinders to identify their contents. Use the chemical name or
commercially accepted name for the gas.
Storing Gas Cylinders
Review the following precautions with the customer to ensure the safe use and
storage of gas cylinders.
•
Cylinders should be stored in accordance with the regulations and standards
applicable to the customer’s locality, state, and country.
2-17
Safety Practices
•
When cylinders are stored indoors in storage rooms, the storage room
should be well ventilated and dry. Ensure that the ventilation is adequate to
prevent the formation of dangerous accumulations of gas. This is
particularly important in small or confined areas.
•
Do not store cylinders near elevators, gangways, or in locations where
heavy moving objects may strike or fall against them.
•
Use and store cylinders away from exits and exit routes.
•
Locate cylinders away from heat sources, including heat lamps. Compressed
gas cylinders should not be subjected to temperatures above 52 °C (126 °F).
•
It is recommended that gas cylinders be stored and placed outside the
laboratory and connected to the instrument through copper lines.
Handling of Gas Cylinders
•
Do not allow ignition sources in the storage area and keep cylinders away
from readily ignitable substances such as gasoline or waste, or combustibles
in bulk, including oil.
•
Store cylinders standing upright, fastened securely to an immovable
bulkhead or permanent wall.
•
When storing cylinders outdoors, they should be stored above ground on a
suitable floor and protected against temperature extremes (including the
direct rays of the sun).
•
Arrange gas hoses where they will not be damaged or stepped on and where
things will not be dropped on them.
•
Take care not to kink or stress the gas lines. For safety, cylinders should be
firmly clamped in position.
2-18
Clarus 500 GC Hardware Guide
•
If it becomes necessary to move the cylinders, do so with a suitable hand
truck after insuring that the container cap is secured and the cylinder is
properly fastened to the hand truck.
•
Use only regulators, tubing and hose connectors approved by an appropriate
regulatory agency.
•
Do not refill cylinders.
•
Check the condition of pipes, hoses and connectors regularly. Perform gas
leak tests at all joints and seals of the gas system regularly, using an
approved gas leak detection system.
•
When the equipment is turned off, close all gas cylinder valves tightly at the
cylinder. Bleed the remainder of the line before turning the exhaust vent off.
2-19
Safety Practices
Hazardous Chemicals
Before using samples, you should be thoroughly familiar with all hazards and
safe handling practices. Observe the manufacturer’s recommendations for use,
storage and disposal. These recommendations are normally provided in the
Material Safety Data Sheets (MSDS) supplied with the solvents.
Be aware that the chemicals that you use in conjunction with the GC may be
hazardous. DO NOT store, handle, or work with any chemicals or hazardous
materials unless you have received appropriate safety training and have read and
understood all related Material Safety Data Sheets (MSDS). MSDSs provide
information on physical characteristics, precautions, first aid, spill clean up and
disposal procedures. Familiarize yourself with the information and precautions
contained in these documents before attempting to store, use or dispose of the
reagents. Comply with all federal, state, and local laws related to chemical
storage, handling, and disposal.
You must work under a suitable hood when handling and mixing certain
chemicals. The room in which you work must have proper ventilation and a
waste collection system. Always wear appropriate safety attire (full-length
laboratory coat, protective glasses, gloves, etc.), as indicated on Material Safety
Data Sheets.
WARNING
2-20
Some chemicals used with this GC may be hazardous or may
become hazardous after completion of an analysis. The responsible
body (for example, the Lab Manager) must take the necessary
precautions to ensure that the GC operators and the surrounding
workplace are not exposed to hazardous levels of toxic substances
(chemical or biological) as defined in the applicable Material Safety
Data Sheets (MSDS) or OSHA, ACGIH, or COSHH documents.
Venting for fumes and disposal of waste must be in accordance with
all national, state and local health and safety regulations and laws.
Clarus 500 GC Hardware Guide
Definitions in Warning for Hazardous
Chemicals
Responsible body. “Individual or group responsible for the use and maintenance
of equipment, and for ensuring that operators are adequately trained.” [per IEC
1010-1].
Operator. “Person operating equipment for its intended purpose.”
[per IEC 1010-1].
OSHA:
Occupational Safety and Health Administration (United States)
ACGIH:
American Conference of Governmental Industrial Hygienists
COSHH:
Control of Substances Hazardous to Health (United Kingdom)
2-21
Safety Practices
2-22
System Description
3
System Description
3-2
Clarus 500 GC Hardware Guide
The Clarus 500 Gas Chromatograph is a dual-channel, temperatureprogrammable stand-alone gas chromatograph (GC). It is available in many
configurations, such as with or without, an autosampler, programmable
pneumatic control (PPC), and a variety of injector/detector combinations to
provide you with total GC flexibility. The Clarus 500 GC is microprocessor
controlled. You use the touch screen to operate this instrument.
Figure 3-1. The Clarus 500 GC.
3-3
System Description
Overview of the Clarus 500 GC
Your Clarus 500 GC may have none, one, or two of the following detectors
installed:
●
Flame Ionization (FID)
●
Electrolytic Conductivity (ElCD)
●
Electron Capture (ECD)
●
Nitrogen Phosphorus (NPD)
●
Thermal Conductivity (TCD)
●
Flame Photometric (FPD)
●
Photoionization (PID)
The FID, ECD, TCD, NPD, or FPD may be installed in either the front or the rear
detector position. But only one PID or PID/ElCD Series can be installed and it
must be installed only in the rear position (Channel 2).
Each installed detector has one analog output which may be attached to either an
integrator or recorder. Signals may be routed under instrument control.
Either none, one, or two packed column injectors; none, one, or two capillary
column injectors; or one of each injector type may be installed. Capillary column
injectors consist of the conventional split/splitless injector (CAP), a temperatureprogrammed split/splitless injector (PSS), and a temperature programmed oncolumn injector (POC).
Up to two gas sampling valves may be installed.
The Clarus 500 GC is sold in two versions, the manual pneumatics version and
the programmable pneumatic control (PPC) version (fully automated pneumatic
control).
In the Manual Pneumatics Version of the Clarus 500 GC, the carrier gas and
detector gas controls are built into the pneumatics control panel on the Clarus
500 GC. The carrier gas controls are used to set the flow for packed and POC
injectors and the pressure for CAP and PSS injectors. The detector gas controls
3-4
Clarus 500 GC Hardware Guide
are used to set the hydrogen and air for FID, NPD, and FPD; and hydrogen for
EICD; reference for TCD; and make-up gas for the ECD and PID. The following
figure is an example of a dual-channel pneumatics control panel with Channel 1
containing a capillary injector and a FID and Channel 2 containing a packed
injector and an ECD.
For each channel, the injector-pneumatic controls are on the left and the detectorpneumatic controls are on the right.
Figure 3-2. Example of a dual-channel pneumatics control panel in the
manual pneumatics version of the Clarus 500 GC.
Channel 1 designates an injector/detector combination installed in the front
position of the instrument, whereas Channel 2 designates a injector/detector
combination installed in the rear position.
In the PPC Version of the Clarus 500 GC, the carrier gas and detector gases are
monitored and controlled by the microprocessor, thereby producing a fully
automated system that is capable of managing all pneumatic functions within the
gas chromatograph. In this case, the panel of Figure 3-2 would be blank. You
can also have combinations of PPC and manual pneumatics injectors and
detectors. For example, you many have a PPC injector and a manual pneumatics
detector setup in the Clarus 500 GC.
The Clarus 500 GC can store up to five GC methods. Methods can be generated,
copied, deleted, edited, set up, and printed.
3-5
System Description
The autosampler can run up to 15 injections per vial from as many as 82 vials
and one priority vial using one or two autosampler programs. In the latter case, a
different GC method can be used by each program if desired. The autosampler
operates in one of two program modes, single or multi.
Real-time digital readouts are provided to simplify setting carrier gas pressures
and flows, if flow readout or PPC is installed. An additional digital readout can
be displayed to show the detector output (in mV).
3-6
Clarus 500 GC Hardware Guide
About the Touch Screen
You control the Clarus 500 GC by the touch screen. The touch screen is your link
to the software. It is designed to provide the easiest access to the most
frequently-used features. The touch screen allows quick access to settings and
functions, such as the Oven program and Ignite button.
The System Status screen provides access to all heated zones. The icons
represent configured components. These icons will guide you through the
application.
The System Status screen provides you with one-click access to the oven
settings. For detailed information on the touch screen see the Clarus 500 User
Guide (0993- 6625A).
Figure 3-3. The Clarus 500 GC System Status screen on the touch screen.
3-7
System Description
3-8
Before You Install a
Column
4
Before You Install a Column
4-2
Clarus 500 GC Hardware Guide
WARNING
At the moment you turn on the Clarus 500 GC, the oven,
injector(s), and detector(s) begin to heat up rapidly. To avoid
injury while installing a column, all heaters should be turned
off and their respective zones allowed to cool before touching
the injector septum caps or any of the fittings inside the oven.
This chapter contains general column installation information, and the following
procedures:
•
Installing your column
•
Protecting your column
4-3
Before You Install a Column
Column Installation Information
Injector and Detector Fittings
Columns are installed inside the oven. The injector fittings are on the left side
and the detector fittings are on the right side of the oven ceiling. Figure 4-1
shows a capillary injector fitting in the front position and a packed injector fitting
in the rear position.
Before installing a column, make certain the oven is OFF
(by opening the oven door), the oven fan has stopped, and
the oven is cool.
WARNING
Figure 4-1. Injector and detector fittings.
Column Hangers
Capillary columns are supported on column hangers. The left and right sides of
the oven walls each have two rectangular slots into which column hangers are
4-4
Clarus 500 GC Hardware Guide
inserted. The two rear slots are used to install a column hanger in the rear
position. The two front slots are used to install a column in the front position.
To install a column hanger, simply insert one end into the left slot and the other
end into the right slot. If you are installing two capillary columns, install the rear
hanger and the rear column before installing the front hanger and the front
column.
Figure 4-2. A column hanger installed in the oven rear position.
4-5
Before You Install a Column
Protecting Your Column
The Clarus 500 GC provides a means for protecting your column(s) from
overheating. It does this by not allowing the oven to heat up beyond the Oven
Maximum Temperature Limit (OMTL), a value that you set in the active method.
You should set the OMTL equal to or less than the maximum permissible
operating temperature recommended in the specifications for your column. If you
are installing two columns, use the lower of the two permissible maximum
operating temperatures.
To protect the column, the OMTL value (that you enter) works in conjunction
with the Oven Temperature specified in the Active Method. Should you (or
someone else) attempt to set an Oven Temperature in the Active Method to a
value greater than the OMTL, the system displays an error message and will not
allow you to continue until an appropriate new oven temperature is set.
To set the oven temperature:
1. Go to the System Status screen and touch the oven icon:
4-6
Clarus 500 GC Hardware Guide
2. Touch the field you need to update. It will appear black and then using the
plus and minus buttons input the correct oven temperatures and time.
4-7
Before You Install a Column
For information on turning the heaters and detectors on and off see the Clarus
500 Users Guide (0993-6625) chapter on the Active Method.
4-8
Installing a Packed
Column
5
Installing a Packed Column
5-2
Clarus 500 GC Hardware Guide
This chapter describes procedures for installing a packed column and setting the
carrier gas flow in either the programmed pressure controlled (PPC) version of
the Clarus 500 GC or the manual pneumatics version. After installing a packed
column as described in this chapter, you should set up the detector(s) to be used
with this injector.
5-3
Installing a Packed Column
Summary
The following steps summarize how to install a new packed column and get it
ready for use:
•
Step 1: Turn off the heaters.
•
Step 2: Set the carrier gas flow.
•
Step 3: Attach one end of the column to the packed injector.
•
Step 4: Leak test.
•
Step 5: Condition the column
•
Step 6: Attach the other end of the column to the detector.
•
Step 7: Leak test the column/detector connection.
NOTE: A new packed column should not be used until it is conditioned overnight with
carrier gas flowing through the column. Do not connect the column to the
detector during the conditioning process.
5-4
Clarus 500 GC Hardware Guide
Materials and Tools Required
•
Two 7/16-inch open end wrenches when a normal 1/8-inch column is
being installed. Two 9/16-inch open end wrenches will be required in
addition if a 1/4-inch column is being installed.
•
Two 1/8-inch to 1/4-inch adapters (Part No 0008-0100) if a 1/4-inch
column is being installed.
•
A flow meter or the optional flow readout.
•
A packed column of your choice.
•
A leak test solution or an electronic leak tester.
5-5
Installing a Packed Column
Packed Column Injector Overview
The packed column injector consists of a septum cap, needle guide, quartz
injector liner, and the injector body. This injector is used with 1/8-inch or 1/4inch glass or metal packed columns. In addition, by installing the 530 Micron
Wide-Bore Adapter Kit (Part No N612-0001) you can convert the injector to
accept wide-bore capillary columns.
5-6
Clarus 500 GC Hardware Guide
Figure 5-1. Packed Column Injector.
About the Wide-Bore Adapter
If you are operating in the off-column mode at above optimum flow rates (>10
mL/min), you may not need to install the wide-bore quartz injector liner.
Depending on your sample or solvent, the solvent profile (tail) may be acceptable
for your application with the standard liner (the illustration at the left in
Figure 5-2) and the addition of the adapter fitting (Part No N610-0083).
5-7
Installing a Packed Column
However, if the solvent profile is not acceptable, install the wide-bore quartz
injector liner.
The off-column or on-column flash vaporization mode of operation is
determined by the position of the hourglass portion of the wide-bore quartz
injector liner in the packed column injector. When installed correctly, this liner
produces improved solvent profiles, especially at optimum flow rates. For
complete installation instructions, refer to the Installation Instructions: 530
Micron Wide-Bore Adapter Kit for the AutoSystem GC and Clarus 500 GC (Part
No 0993-8661).
Insert the wide-bore quartz injector liner (Part No N612-1003) into the packed
column injector with the hourglass portion in the correct position for your desired
mode of operation. Figure 5-2 shows a cross section of a packed column injector
containing a standard liner and a cross section of a packed column injector
containing a wide-bore quartz injector liner installed in the off-column position
and the on-column position.
For off-column flash vaporization (hourglass end first):
To avoid contaminating the quartz wool, wear vinyl, powder-free disposable
gloves (the same type used to perform maintenance on TurboMass). Take a small
piece of quartz wool and twist it into an elongated shape so that you can insert it
into the liner. Then using a 1/16-inch rod (Part No N610-T100), push the quartz
wool into the liner. Loosely pack some quartz wool in the top portion of the liner
to wipe the syringe needle upon injection. Insert the wide-bore quartz injector
liner into the packed column injector with the hourglass end first.
Or
For on-column flash vaporization (hourglass end last):
Insert the wide-bore quartz injector liner into the packed column injector with the
hourglass end of the liner last. Do not pack the wide-bore quartz injector liner
with silanized quartz wool. You must use a 0.47-mm O.D. syringe in this mode.
If you are using the autosampler, install a 0.47-mm O.D. syringe and use the
“SLOW" injection mode. If the Clarus 500 GC software is Rev. 1.6 or lower, use
the “ON-COL" injection mode.
5-8
Clarus 500 GC Hardware Guide
Figure 5-2. Cross sections of three packed injector configurations with a
wide-bore column.
5-9
Installing a Packed Column
Step 1: Turn off the Heaters
WARNING
The moment the Clarus 500 GC is turned on, the oven, injector(s), and
detector(s) begin to heat up rapidly. To avoid burns and injury while
installing a column, all heaters should be turned off and their
respective zones allowed to cool before touching the injector septum
caps or any of the fittings inside the oven.
NOTE: See the Clarus 500 GC Users Guide for detailed procedures for turning heaters
off and on.
NOTE: It is recommended that you remove the injector liner shipped with the packed
injector and pack it with a small amount of silanized glass wool before
performing analyses. Please refer to the Maintenance chapter later in this
manual.
Step 2: Set the Carrier Gas Flow
This step describes how to set the carrier gas using PPC and manual pneumatics
modules. Refer to the procedure that describes your system, PPC or manual
pneumatics.
Step 2A: Setting the Carrier Gas Using PPC Modules
Step 2B: Setting the Carrier Gas Using Manual Pneumatics
5-10
Clarus 500 GC Hardware Guide
Step 2A: Setting the Carrier Gas Using PPC Modules
1.
Turn on the carrier gas at the tank.
2.
Adjust the line pressure between 60 to 90 psig.
3.
From the System Status screen select either A or B injector (the example
here shows the B injector ready for setting the carrier gas).
5-11
Installing a Packed Column
4.
In the following window touch the Program screen under the Carrier Gas
field.
5.
Using the plus and minus buttons enter the desired values.
5-12
Clarus 500 GC Hardware Guide
Step 2B: Setting the Carrier Gas Using Manual
Pneumatics
The following two procedures describe how to set the carrier gas flow for manual
pneumatics modules:
• Setting the Carrier Gas Flow Using the Optional Flow Readout.
•
Setting the Carrier Gas Flow Using a Soap Bubble or Electronic Flowmeter.
Setting the Carrier Gas Flow Using the Optional Flow Readout
1.
Turn on the carrier gas at the tank.
2.
Adjust the line pressure to 90 psig.
3.
From the System Status screen select either A or B injector (the example
here shows the A injector ready for setting the carrier gas).
5-13
Installing a Packed Column
4.
Using the plus and minus buttons enter the desired values.
5.
Adjust the flow by turning the flow control knob (see below)
counterclockwise to increase the flow, clockwise to decrease the flow,
until the actual flow displayed equals the set point value.
5-14
Clarus 500 GC Hardware Guide
Figure 5-3. Packed Injector and POC controls.
Setting the Carrier Gas Flow Using a Soap Bubble or Electronic
Flowmeter
The procedure below assumes that you know how to measure carrier gas flow
using a soap bubble or electronic flowmeter and the built-in stopwatch. If you
need instructions, please read “Using Tools,” in the Clarus 500 GC Users Guide
(0993-6625) before proceeding.
1. Locate the packed injector fitting inside the oven.
5-15
Installing a Packed Column
Figure 5-4. A packed injector fitting.
5-16
Clarus 500 GC Hardware Guide
2. Attach a soap bubble flowmeter to the packed injector fitting.
3. Turn on the carrier gas at the tank and adjust the line pressure to 90 psig.
4. From the System Status Screen select the Tools button and then select
Utilities from the drop down menu
.
5-17
Installing a Packed Column
5. In the Utilities window select the Stopwatch icon.
6. Using the plus and minus buttons enter the appropriate values and press Start.
5-18
Clarus 500 GC Hardware Guide
7. Start the carrier gas flowing by turning the flow controller knob
counterclockwise and measure the flow.
NOTE: For best accuracy, use a soap bubble flowmeter volume that gives a reading of at
least 30 seconds.
8. Adjust the flow to the desired set point by repeatedly measuring the flow and
turning the flow controller knob counterclockwise to increase the flow,
clockwise to decrease the flow, until the desired flow is obtained.
9. Disconnect the soap bubble flow meter before proceeding to the next step.
Step 3: Connect One End of the Column to the
Packed Injector
NOTE: If you are installing a 1/4-inch column, attach a 1/8-inch to 1/4-inch adapter to
the packed injector fitting before continuing. Finger tighten the adapter, then
5-19
Installing a Packed Column
while holding the packed injector fitting steady with a 7/16-inch wrench, tighten
the adapter with a 9/16-inch wrench.
1.
Insert one end of the column into the packed injector fitting until it
bottoms, then finger tighten the column nut onto the packed injector
fitting (see below).
Figure 5-3. Packed column connected to a packed injector fitting.
2.
While holding the packed injector fitting with one 7/16-inch wrench,
tighten the column nut an additional 1/8 to 1/4 turn with the other
wrench.
NOTE: Do not overtighten column nuts. Overtightening causes permanent damage to
the fittings.
Step 4: Leak Test
Test the connection to the packed injector fitting for leaks using a 50/50 mixture
of isopropanol/water or an electronic leak detector. To avoid contaminating the
system, DO NOT use a soap solution for leak testing. Tighten all leaking
connections.
5-20
Clarus 500 GC Hardware Guide
Step 5: Condition the Column
This section contains a suggested temperature program for conditioning a
column. The program starts off by holding the oven temperature at a medium
value for 10 minutes, gradually increasing the oven temperature at a fixed rate
(5 °C/min) to the column operating temperature, then holding that temperature
overnight with the carrier gas flowing.
CAUTION
The temperatures shown in the following examples should only be
used as guidelines. Please refer to the column manufacturer's
operating instructions for specific temperature recommendations.
To condition the column:
1. Close the oven door go to the System Status screen and touch the oven icon.
5-21
Installing a Packed Column
2. Using the plus and minus buttons input the initial oven temperature to a set
point of 50.
3. Enter a TIME of 10.
4. To add another program step, enter a RATE of 5 (°C/min).
5. Using the plus minus buttons enter for TEMP 2, enter a set point 25 °C to 50
°C above your planned analytical operating temperature. For example, enter
a set point of 150.
6. Set Time 2 to 999.
5-22
Clarus 500 GC Hardware Guide
CAUTION
To avoid damaging the column, do not enter a temperature higher
than the maximum operating temperature specified by the column
manufacturer.
7. In the above screen set, using the plus minus buttons set an Injection
Temperature about 50 °C higher than the TEMP 2 setting. See the chapter
“Active Method” in the Clarus 500 GC Users Guide for information on
setting TEMP 2.
8. Turn Detector Temperature off and run the system overnight.
9. The next morning go to the System Status screen and select the oven icon.
5-23
Installing a Packed Column
10. Reset the oven temperature set point to that specified for TEMP 1 at the
beginning of the temperature program.
11. Open the oven door and allow the oven to cool until the oven fan goes off.
This occurs when the oven cools down to 40 °C.
NOTE: Condition a new column before using it in an analysis. Once it is conditioned,
you will not need to recondition it.
Step 6: Attach the Other End of the Column to the
Detector
1. Insert the free end of the column into the detector fitting, then finger
tighten the column nut onto the detector fitting.
Figure 5-5. Packed column attached to the rear detector fitting.
5-24
Clarus 500 GC Hardware Guide
2. While holding the detector fitting with one of the 7/16-inch wrenches,
tighten the column nut an additional 1/8 to 1/4 turn with the other
wrench.
CAUTION
Make certain that no part of the column touches the bottom or sides
of the oven once it is installed.
NOTE: If you are installing a 1/4-inch column, attach a 1/8-inch to 1/4-inch adapter to
the detector fitting before continuing. Finger tighten the adapter, then while
holding the detector fitting steady with a 7/16-inch wrench, tighten the adapter
with a 9/16-inch wrench.
If you are attaching the end of a column to an ElCD:
Locate the ElCD Shipping Kit (Part No N610-0189) and then follow this
procedure.
1. Remove the 1/16-inch adapter from the ElCD.
2. Insert the 1/4 inch glass adapter (Part No N610-1445) through the nut
(Part No N610-1434) that you removed from the 1/16-inch adapter and
ferrule (Part No 0992-0140). Then insert the adapter into the ElCD
and tighten the nut enough to provide a leak-free seal.
3. If you are installing a 1/4-inch column, attach the free end of the ElCD
adapter to a 1/4-inch to 1/4-inch union (Part No 0990-1434). Then
attach the column to the union.
NOTE: If you are installing a 1/8-inch column, first connect the 1/8-inch to ¼-inch union
(Part No. 0990-3472) in place of the ¼-inch union
4. While holding the detector fitting steady with an appropriate wrench,
tighten the column nut with another appropriate wrench.
5-25
Installing a Packed Column
Figure 5-6. Removing the 1/16-inch ElCD adapter and installing the
1/4-inch adapter.
Step 7: Leak Test the Column/Detector Connection
The following procedures describe leak testing the column to detector
connections.
Using Manual Pneumatics
With the carrier gas still flowing from the overnight conditioning, test the
column/detector connection for leaks using a 50/50 mixture of isopropanol/water
or use an electronic leak detector. To prevent contaminating the system, DO
5-26
Clarus 500 GC Hardware Guide
NOT use a soap solution for leak testing. Tighten the connection if a leak is
found.
Set up the detector to be used with this column (see The Clarus 500 GC Users
Guide, Active Method chapter for information on setting up detectors).
Using PPC Pneumatics
1. From the System Status screen select either A or B injector (the example here
shows the B packed injector ready for setting the carrier gas). In this
example, touch the Channel B packed injector icon
.
5-27
Installing a Packed Column
2. In the following window touch the Program screen under the Carrier Gas
field.
5-28
Clarus 500 GC Hardware Guide
3. Using the plus and minus buttons enter pressure 0.1 to 100 psig for minimum
and maximum.
The Clarus 500 GC monitors the column head pressure with a carrier-gas massflow controller in use. After selecting the carrier-gas Flow mode in
configuration, you enter the minimum and maximum values. If the inlet pressure
drops below or rises above the set limits for more than one consecutive minute,
an error message will appear: Carrier (with specific carrier number) unable to
maintain pressure.
NOTE: Refer to the Clarus 500 GC Users Guide (0993-6625) for minimal and maximum
values.
You should correct the leak; the most common area of a leak is the injector
septum. Clear the message by touching the OK button before continuing to use
the GC. This will stop an autosampler program from continuing.
If you do not make any entries, leak checking will not be done. If you are
temperature programming, then the maximum value you enter must be above the
column head pressure at the highest oven temperature. You can just enter a value
for the minimum and leave the maximum blank. See the Clarus 500 Users Guide
(0995-6625) for more information.
5-29
Installing a Packed Column
5-30
Installing a Capillary
Column
6
Installing a Capillary Column
6-2
Clarus 500 GC Hardware Guide
This chapter describes how to install a capillary column in the following three
injectors:
•
Capillary Split/Splitless (CAP)
•
Programmed Split/Splitless (PSS)
•
Programmed On-Column (POC)
The information in this chapter is presented as one sequential procedure (Steps A
through I) for all three injectors (CAP, PSS, and POC) with the following
procedural steps common to all three injectors:
•
Setting carrier gas flow using PPC modules and/or manual pneumatics
NOTE: For a thorough understanding of PPC, refer to Chapter 8, “PPC
Fundamentals.”
•
Leak testing
•
Conditioning the column
•
Attaching the column to the detector and leak checking
NOTE: If you are analyzing reactive compounds, appropriately deactivate injector liners
and wool for your sample type.
CAUTION
All three capillary injectors; CAP, PSS, and POC use a 1/16-inch
fitting for the column connection. This fitting is fragile. To preserve
the integrity of the fitting, carefully connect the column nut to
prevent cross-threading the fitting and/or overtightening the nut on
the fitting. You can also preserve the integrity of the fitting by
allowing the injector to cool before connecting a nut.
6-3
Installing a Capillary Column
Summary
The following steps summarize how to install a capillary column and get it ready
for use:
A.
Turn the heaters off.
B.
Connect the column to the CAP, PSS, or POC injector.
1.
2.
3.
C.
Split/Splitless (CAP) injector
Programmed Split/Splitless (PSS) injector
Programmed On-Column (POC) injector
Set the carrier gas. (Set the pressure for the CAP and the PSS, or the flow
for the POC, using the optional flow readout or a flowmeter.)
1.
2.
Setting carrier gas for PPC module
Setting carrier gas for Manual Pneumatics
D.
Leak test all new connections.
E.
Condition the column (to the manufacturers specifications) and the
mechanical joint between the column and pre-column.
F.
Connect the column to the detector.
G.
Leak test all new connections.
6-4
Clarus 500 GC Hardware Guide
Materials and Tools Required
1
•
1/8-inch x 1.0-mm graphite ferrules (Part No. 0990-3394) for 0.53-mm
i.d. columns
•
1/16-inch x 0.8-mm graphite ferrules (Part No 0992-0141)1 for 0.53-mm
i.d. columns
•
Two 7/16-inch open end wrenches
•
Two 1/4-inch open end wrenches
•
One 1/8-inch graphite ferrule (Part No 0990-3981)1 for 0.32/0.25-mm i.d.
columns
•
One 1/8-inch column nut (Part No 0990-3453)
•
One 1/16-inch graphite ferrule (Part No 0990-3700)1 for 0.32/0.25-mm
i.d. columns
•
One 1/16-inch column nut (Part No 0990-3392)1
•
One screwdriver (Part No. 0990-7273)1
•
Deactivated 0.53-mm i.d. fused silica (Part No. N610-1724)
•
Fused-silica universal connector (Part No. N930-2149)
•
Capillary column of your choice
•
White-out or felt-tip marker
•
Scribe for cutting columns (Part No. N930-1376)
(Pointed scribes are not recommended.)
•
Leak-test solution or electronic leak tester
Shipped in the Clarus 500 GC Shipping Kit.
6-5
Installing a Capillary Column
Figure 6-1. Examples of required fittings.
6-6
Clarus 500 GC Hardware Guide
Step A: Turn the Heaters Off:
CAUTION
The moment the Clarus 500 GC is turned on, the oven, injector(s),
and detector(s) begin to heat up rapidly. To avoid injury while
installing a column, all heaters should be turned off and their
respective zones allowed too cool before touching the injector
septum caps or any of the fittings inside the oven.
CAUTION
Before you install a column, follow the detailed procedures for
turning heaters off and on, in Chapter 4 of this manual “Before
You Install a Column.” If you have not read this chapter, please do
so before proceeding
6-7
Installing a Capillary Column
Step B: Connect the Column to the Injector:
This step contains a separate procedure that describes how to connect a column
to each of the following three Clarus 500 GC injectors:
Step B1:
Connect the Column to the Split/Splitless (CAP) Injector.
Step B2:
Connect the Column to the Programmed Split/Splitless (PSS)
Injector.
Step B3:
Connect the Column to the Programmed On-Column (POC)
Injector.
Proceed to the page that contains the procedure for your injector.
Step B1:
Connect the Column to the Split/Splitless
(CAP) Injector
Overview
The Split/Splitless injector (CAP) consists of a septum purge assembly and the
injector body. Carrier gas enters the injector body at the point just above the Oring and flows through the quartz liner past the column tip.
6-8
Clarus 500 GC Hardware Guide
Figure 6-2. Cutaway view of the Split/Splitless injector (CAP).
About the Injector Liners
The CAP injector uses the following two quartz liners:
•
Narrow-bore (2-mm i.d.) liner (Part No. N612-1002).
•
Wide-bore (4-mm i.d.) liner (Part No. N612-1001).
6-9
Installing a Capillary Column
The narrow-bore liner is generally used for splitless injections and the wide-bore
liner is generally used for split injections. Due to its small internal volume (0.3
mL), the amount of sample injected into the narrow-bore liner should be limited
to about 0.5 µL. This prevents the solvent expansion upon injection from
overfilling the liner with vapor.
To wipe the syringe needle, we recommend packing a small amount of quartz
wool in the top portion of all liner types or injection modes (for example, split or
splitless). Each liner should be packed with the quartz wool as described later in
this chapter.
Splitless Injections
In the splitless injection mode, the narrow-bore quartz liner is typically used
without quartz wool. The narrow-bore decreases the sample residence time in the
liner, making it useful for trace analysis with smaller sample volumes (0.5 µL or
less). By closing the split vent, most of the sample mixture enters the column.
Then, opening the split vent clears the inlet of residual solvent.
For splitless injection volumes over 0.5 µL, the wide-bore liner with an internal
volume of 1.25 mL should be used. However, the amount of sample should be
limited to a maximum of 2 µL for hydrocarbon solvents and less than that for
high-expansion solvents such as water or CH2Cl2. Refer to Table 6-1 for
examples of gas volumes formed upon sample injection for selected solvents.
If the wide-bore liner is used for splitless injection, the splitless sampling time
(vent-on time) should be at least one minute or more. Also, lower initial oven
temperatures may be required to produce good solute resolution in the first few
minutes after the solvent peak. The wide-bore liner should be used with columns
having an i.d. of 0.32 mm or greater.
6-10
Clarus 500 GC Hardware Guide
Table 6-1. Gas Volumes Formed Upon Sample Injection
(Injector 250 °C, Inlet Pressure 10 psig)
Solvent
Methylene Chloride
Methanol
Water
Volume Injected (µL)
Gas Volume Generated (µL)
1
333
2
571
1
475
2
768
1
823
2
1166
Split Injections
In the split injection mode, the wide-bore quartz liner is packed with quartz wool
to ensure thorough mixing of the sample and carrier gas before they encounter
the column tip. The split vent is open at the time of injection so that a fraction of
the sample mixture enters the column while the remainder is routed out through
the split vent.
About the Pneumatics Control
The injector pneumatics consist of either a PPC (programmable pneumatic
controlled) version or a manual pneumatics (flow control valves and pressure
regulators) version.
In the PPC version, the pneumatics consist of PPC modules that regulate the
inlet flow and pressure of the gases using software controlled by an Clarus 500
GC method.
In the manual pneumatics version, the pneumatics consist of a pressure
regulator with an inline pressure transducer for screen readout of the current
pressure and a needle valve to control the split vent.
6-11
Installing a Capillary Column
CAUTION
The CAP injector is shipped with the wide-bore liner installed without
quartz wool packing. Before using the injector, remove the liner and
pack it with quartz wool. If you are using the injector in the splitless
mode, you may want to install the narrow-bore liner.
Connecting a Column to the Cap Injector
The following five steps describe how to connect a column to the CAP injector:
Step 1. Remove the CAP injector liner.
Step 2. Select an appropriate CAP injector liner.
Step 3. Pack the CAP injector liner with quartz wool.
Step 4. Reinstall the liner in the CAP injector.
Step 5. Connect a column to the CAP injector.
Step 1. Remove the CAP Injector Liner.
To remove a CAP injector liner:
1. Ensure that the injector heater has been turned off.
Allow the injector to cool until it is slightly warm to the touch. Cooling
the injector to too-low a temperature (less than 80 °C) will make it
difficult to remove the injector liner.
2. Remove the septum cap.
6-12
Clarus 500 GC Hardware Guide
Figure 6-3. Removing the septum cap.
3. Remove the injector cover.
Figure 6-4. Removing the injector cover.
4. Loosen the threaded collar by using the spanner (Part No. N610-1359)
provided, then remove the threaded collar.
6-13
Installing a Capillary Column
Figure 6-5. Loosening the threaded collar.
5. Replace the septum cap on the injector.
6. Pull the septum cap upwards to remove the septum purge assembly.
Figure 6-6. Removing the septum purge assembly.
The carrier gas inlet line is coiled to allow you to pull the septum purge
assembly over to the side and gain access to the liner.
6-14
Clarus 500 GC Hardware Guide
7. Ensure that the CAP injector liner is cool, then twist the CAP injector
liner-removal tool (Part No. 0250-6534, see Figure 6-8) onto the
injector liner. Remove the injector liner by lifting it up and out of the
injector.
The CAP liner must be cool (no hotter than 100 °C) or the linerremoval tool will melt! The end of the CAP liner-removal tool may
flare out with use. If this happens, cut off the flared end with a razor
blade or scissors.
Figure 6-7. CAP injector liner-removal tool (Part No. 0250-6534).
Figure 6-8. Removing a capillary injector liner.
6-15
Installing a Capillary Column
CAUTION
If the O-ring adheres to the injector body, use a small screwdriver to loosen
the O-ring so that you can remove the liner and O-ring. Be careful not to
scratch the barrel where the O-ring seals. Discard this O-ring and install a
new O-ring.
NOTE: If the liner breaks inside the CAP injector, it can be removed by first removing
the column. Then using a 9/16-inch wrench, remove the 1/4-inch injector fitting
inside the oven. The liner should fall out. If the liner is stuck, you can push it out
from the top or bottom.
Step 2. Select an Appropriate CAP Injector Liner.
Select the appropriate injector liner for your application. The following two
injector liners are available for the CAP injector:
•
4-mm i.d. and 6-mm o.d. CAP injector wide-bore liner (Part No. N6121001)
•
2-mm i.d. and 6-mm o.d. CAP injector narrow-bore liner (Part No. N6121002)
The narrow-bore liner is generally used for a splitless injection, and the widebore liner is generally used for a split injection. Due to the small internal volume
(0.3 mL) of the narrow-bore liner, you can prevent overfilling the liner with
vapor (caused by solvent expansion upon injection) by limiting the amount of
sample injected to 0.5 µL.
The wide-bore liner is used for splitless injection volumes over 0.5 µl since its
internal volume is 1.25 mL. The sample size should be limited to a maximum of
2 µL for hydrocarbon solvents and less than that for high-expansion solvents,
such as water or CH2Cl2. Refer to Table 6-1.
If the wide-bore liner is used for splitless injection, the splitless sampling time
(vent-on time) should be more than one minute. Also, lower initial oven
temperatures may be required to give good resolution in the first few minutes
6-16
Clarus 500 GC Hardware Guide
after the solvent peak. The wide-bore liner should be used with columns having
an i.d. of 0.32 mm or greater.
Step 3. Pack the CAP Injector Liner with Quartz Wool.
To wipe the syringe needle, we recommend packing a small amount of quartz
wool in the top portion of the liner regardless of the liner type or injector mode
used (for example, split or splitless). This packing assures that reproducible
volumes are injected because it wipes the syringe needle every time the needle is
inserted.
Remove the liner and replace the quartz wool packing on a regular basis,
particularly if your samples contain nonvolatile components that could build up
on the wool. This could cause adsorption of peaks of interest, tailing, and loss of
sensitivity. Remove the wool with a small hook on the end of a thin wire, or blow
it out using compressed air.
NOTE: To avoid contaminating the quartz wool when packing the injection liner, wear
vinyl, powder-free, disposable.
Packing CAP Injector Liner for Split Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then using a 1/16-inch rod (Part No. N610-T100),
push the quartz wool into the liner. Pack the wool tightly2 from the dimple
upwards (about one inch [2.5 cm]). Loosely pack quartz wool in the top portion
of the liner to wipe the syringe needle upon injection.
Packing a CAP Injector Liner for Splitless Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then using a 1/16-inch rod (Part No. N610-T100),
push the quartz wool into the liner. Pack a one-inch piece (2.5 cm) of quartz wool
loosely below the top ground portion of the liner (see Figure 6-11). The sample is
2
The recovery of high molecular weight components (e.g., C40) may be improved if the liner is
loosely packed.
6-17
Installing a Capillary Column
then injected into the wool, thereby preventing the delivery of sample beyond the
column. The wool also wipes the syringe needle upon injection.
Figure 6-9. CAP injector liners packed with quartz wool.
Step 4. Reinstall the Liner in the CAP Injector.
To reinstall the liner:
6-18
1.
Install a new O-ring near the ground portion of the liner.
2.
Insert the liner in the injector body.
3.
Place the septum purge assembly over the liner.
4.
Press the septum purge assembly down to correctly position the
liner in the injector.
5.
Replace the threaded collar and tighten the assembly using the
spanner (Part No. N610-1359).
Clarus 500 GC Hardware Guide
Step 5. Connect a Column to the CAP Injector.
CAUTION
This injector terminates in a 1/16-inch fitting. This fitting is fragile. To
preserve the integrity of the fitting, carefully connect the nut to prevent
cross-threading the fitting and/or overtightening the nut on the fitting. You
can also preserve the integrity of the fitting by allowing the injector to
cool before connecting a nut.
To connect a column:
1.
Insert a 1/16-inch column nut (Part No. 0990-3392) and 1/16-inch
graphite ferrule (0.8 mm i.d., Part No. 0992-0141 or 0.5 mm i.d., Part
No. 0990-3700) over one end of the column as shown below:
Figure 6-10.
Narrow-bore capillary column, nut, and ferrule on the
injector end of a column.
NOTE: Verify that the tapered end of the ferrule is facing towards the nut as shown
above.
2.
Cut off about 1 cm (3/8 inch) from the column end using a wafer scribe
(Part No. N930-1376, pkg. of 10 scribes). Break off the tubing at the
score mark so that the break is clean and square. Examine the cut with a
magnifying glass and compare it to the examples shown in the following
figure:
6-19
Installing a Capillary Column
Figure 6-11. Example of a good cut and bad cuts.
3.
6-20
To automatically calculate the position of the column nut on the column
so that the back of the nut is the correct distance from the end of the
column, go to the system Status Screen and touch the Tools button.
Clarus 500 GC Hardware Guide
4. Touch Utilities from the drop down menu. The following screen appears.
5. In the Utilities screen touch the Column Length Calc icon
.
6-21
Installing a Capillary Column
6. Using the drop down menu touch the type of detector and injector you are
using. Select whether you want the calculation in mm or inches. The proper
distance will be calculated automatically.
7. Using typewriter "white-out" or a felt-tipped pen, make a mark on the column
just beyond the back edge of the column nut (see Figure 6-10).
CAUTION
To avoid contaminating the system, make certain that the nut and
ferrule do not contact the mark on the column.
8. Locate the capillary injector fitting inside the oven.
6-22
Clarus 500 GC Hardware Guide
Figure 6-12. Capillary injector fitting inside the oven.
9. Insert the column into the capillary injector fitting. Then hand-tighten the
column nut onto the capillary injector fitting. Insert the column into the
capillary injector fitting until the mark is aligned with the back of the nut.
10. Using two 1/4-inch wrenches, tighten the column nut only until the column
cannot be pulled out of the fitting.
CAUTION
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
6-23
Installing a Capillary Column
Figure 6-13. Capillary column attached to capillary injector fitting.
Step B2
Connect the Column to the Programmed
Split/Splitless (PSS) Injector:
Overview
The Programmed Split/Splitless injector (PSS) consists of a septum purge
assembly and the injector body. Carrier gas enters the injector at a point just
above the O-ring and flows through the quartz liner past the column tip.
6-24
Clarus 500 GC Hardware Guide
Figure 6-14. Cutaway view of the Programmed Split/Splitless injector
(PSS).
About the Injector Liners
The PSS injector uses the following three quartz liners:
•
2.0-mm i.d. (wide-bore) liner (Part No. N612-1004)
•
1-mm i.d. (narrow-bore) liner (Part No. N612-1006)
•
hourglass liner (N610-1539)
6-25
Installing a Capillary Column
In general, for split or splitless injections, use the 2-mm or 1-mm i.d. liner and
operate the PSS in the inlet-programmed mode. For on-column operation, use the
hourglass liner and the oven program mode. The 2-mm i.d. liner should be
packed with quartz wool as described in this chapter and used for either split or
splitless operation. The 1-mm i.d. liner may give better resolution of the earlyeluting peaks in the split or splitless mode and it is better for labile compounds;
however, it should be used for those samples with early-eluting peaks for which
additional solute trapping focusing cannot be obtained by lowering the initial
oven temperature or by using a column with a thicker stationary phase film.
To wipe the syringe needle, in all liner types (wide-bore or narrow-bore) or
injection modes (split or splitless), we recommend packing a small amount of
quartz wool in the top portion of the liner.
The sample is injected into the PSS injector at a "cool" temperature. The injector
temperature is then programmed to increase. This is useful for samples that are
thermally labile and/or have a wide molecular weight range. The PSS injector
can also be used in a programmed on-column mode by replacing the quartz liner
with the hourglass liner and closing the split vent flow.
CAUTION
6-26
The PSS can be used in the "hot" split or splitless mode.
This, however, is not recommended for use with the 1 mm
i.d. liner; it could cause solvent flashback in the injector.
This mode should be used with caution depending upon the
solvent and temperatures you choose. See Table 6-1.
Clarus 500 GC Hardware Guide
CAUTION
When using the PSS in the on-column mode with the
autosampler, you must use a special syringe that has a
needle o.d. of 0.47 mm (Part No. N610-1253 or N6101380). Refer the Active Method Chapter in the Clarus 500
Users Guide, “Controlling the Autosampler,” for more
detail. You must use only the "Norm" injection speed with
this syringe in the on-column mode. The "Fast" injection
speed will bend this thin needle; the "Slow" injection
speed may produce double peaks due to the momentary
stoppage of column flow during the longer injection. You
can achieve better precision in the on-column mode when
sample volumes of 1.0 µL or greater are injected.
Split Injections
In the split mode, the wide-bore quartz liner is packed with quartz wool to insure
thorough mixing of the sample and carrier gas before they reach the column tip.
The split vent is open at the time of injection so that a fraction of the sample
mixture enters the column while the remainder is routed out through the split
vent.
Splitless Injections
In the splitless mode, the narrow-bore quartz liner is typically used without
tightly packed quartz wool for mixing. Instead, a small amount of quartz wool in
the center is recommended. This is useful for trace analysis with smaller sample
volumes (less than 1 µL). By closing the split vent, most of the sample mixture
enters the column, then the split vent is opened to clear the injector inlet of
residual solvent.
Solvent Purge Injections
In applications where the sample is in a trace concentration and has a high
molecular weight, this sample can be injected into the PSS with the vent open
and the starting temperature near the boiling point of the solvent. In this way,
only the solvent is purged out through the vent, then the vent is closed and the
injector temperature is programmed up to elute the peaks of interest onto the
6-27
Installing a Capillary Column
column. This technique allows larger quantities of sample to enter the column
without large solvent effects.
About the Pneumatics Control
The PSS pneumatics consist of either a PPC (programmable pneumatics
controlled) version or a manual pneumatics version.
In the PPC version, the pneumatics consist of PPC modules that regulate the
inlet flow and pressure of the gases using software controlled by an Clarus 500
GC method.
In the manual pneumatics version, the pneumatics consist of a pressure
regulator with an inline pressure transducer for screen readout of the current
pressure and a needle valve to control the split vent.
CAUTION
The PSS injector is shipped with the wide-bore liner
installed but without the quartz wool packing. Before using
the injector, remove the liner and pack it with quartz wool.
Connect a column to the programmed split/splitless injector in either one of the
following two modes:
•
Split/Splitless Mode
•
On-Column Mode using the hourglass liner
Connect the Column to the PSS Injector
The following five steps summarize how to connect a column to the PSS injector
in the split/splitless mode:
Step 1. Remove the PSS injector liner.
Step 2. Select an appropriate PSS injector liner.
6-28
Clarus 500 GC Hardware Guide
Step 3. Pack the PSS injector liner with quartz wool.
Step 4. Reinstall the liner in the PSS injector.
Step 5. Connect a column to the PSS injector.
Step 1. Remove the PSS Injector Liner.
To remove the PSS injector liner:
1.
Ensure that the injector heater has been turned off.
Allow the injector to cool until it is slightly warm to the touch. Cooling the
injector to too low a temperature (less than 80 °C) will make it difficult to
remove the injector liner.
2.
Figure 6-15.
3.
Remove the septum cap.
Removing the septum cap.
Remove the injector cover.
6-29
Installing a Capillary Column
Figure 6-16. Removing the injector cover.
4.
Loosen the threaded collar by using the spanner (Part No. N6101359) provided, then remove the threaded collar.
Figure 6-17. Loosening the threaded collar.
5.
6-30
Replace the septum cap on the injector.
Clarus 500 GC Hardware Guide
6.
Pull the septum cap upwards to remove the septum purge
assembly.
Figure 6-18. Removing the septum purge assembly.
The carrier gas inlet line is coiled to allow you to pull the septum
purge assembly over to the side and gain access to the liner.
7.
Ensure that the PSS injector liner is cool, then insert the end of
the PSS liner-removal tool (Part No. 0250-6247) over the end of
the injector liner that is shipped with PSS injector. Remove the
liner by lifting it up and out of the injector.
The PSS liner must be cool (no hotter than 100 °C) or the
liner-removal tool will melt! The end of the PSS liner-removal
tool may flare out with use. If this happens, cut off the flared end
with a razor blade or scissors.
6-31
Installing a Capillary Column
CAUTION
Figure 6-19.
The PSS injector does not have a removable fitting at the bottom
of the assembly. Be very careful when removing this liner to
prevent breaking it. As the injector cools, the O-ring adheres to
the metal base of the injector body. Use a small screwdriver to
loosen the O-ring, then remove the liner and O-ring. Be careful
not to scratch the barrel where the O-ring seals. Replace the Oring with a new O-ring when you replace the liner.
Removing a PSS injector liner.
Step 2. Select an Appropriate PSS Injector Liner.
The PSS injector uses the following three liners:
•
6-32
2-mm i.d. PSS injector wide-bore liner (Part No. N612-1004)
Clarus 500 GC Hardware Guide
•
1-mm i.d. PSS injector narrow-bore liner (Part No. N612-1006)
•
PSS injector on-column (hourglass) liner (Part No. N610-1539)
The PSS injector is operated in the inlet-programmed mode for split or splitless
injection with either the 2-mm or 1-mm i.d. liner. If used in the “hot” split or
splitless mode, the 2-mm i.d. liner should be used. It is recommended that you do
not inject more than approximately 0.5 µL in the “Hot” mode. Refer to Table 6-1.
For PSS on-column operation, use the hourglass liner and the oven-program
mode. The 2-mm i.d. PSS liner that is used for either split or splitless operation
should be packed with quartz wool as described in this chapter. The 1-mm i.d.
PSS liner may give better early-eluting peak resolution in the split or splitless
mode. This liner should be used for samples with early-eluting peaks that cannot
be resolved by additional solute trapping/focusing (by lowering the initial oven
temperature or by using a column with a thicker stationary-phase film).
Step 3. Pack the PSS Injector Liner with Quartz Wool.
CAUTION
Never pack the hourglass liner with wool.
To wipe the syringe needle, we recommend packing a small amount of quartz
wool in the top portion of the liner regardless of the liner type (wide-bore or
narrow-bore but never the hourglass ) or injector mode (split or splitless). Quartz
wool assures that reproducible volumes are injected by wiping the syringe needle
every time it is inserted. Remove the liner and replace the quartz wool on a
regular basis, particularly if your samples contain nonvolatile components that
could build up on the wool. This could cause adsorption of peaks of interest,
tailing, and loss of sensitivity. Remove the wool with a small hook on the end of
a thin wire, or blow it out using compressed air.
6-33
Installing a Capillary Column
Figure 6-20. PSS liners packed with quartz wool.
Packing a PSS Injector Liner for the Splitless Mode
CAUTION
To prevent contaminating the quartz wool when packing the
injection liner, wear vinyl, powder-free, disposable gloves (for
example, the same type of gloves used to perform maintenance
on TurboMass).
Take a small piece of quartz wool and twist it into an elongated shape
so that you can insert it into the liner. Then using a 1/16-inch o.d. rod
(Part No. N610-T100), push the quartz wool into the liner. Pack a 2.5-cm (oneinch) piece of quartz wool loosely below the top ground portion of the liner (see
Figure 6-21). The sample is then injected into the wool, thereby preventing the
6-34
Clarus 500 GC Hardware Guide
delivery of sample beyond the column. The wool also wipes the syringe needle
upon injection.
NOTE: The narrow-bore liner is more difficult to pack because of its small i.d. However,
there is a dimple in the middle of the liner to hold the wool in place. Do not pack
the wool too tightly!
When the narrow-bore liner is installed, use a 5-cm needle-length syringe when
making manual injections.
Packing PSS Injector Liner for the Split Mode
CAUTION
To prevent contaminating the quartz wool when packing the
injection liner, wear vinyl, powder-free, disposable gloves.
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then using a 1/16-inch o.d. rod (Part No. N610-T100),
push the quartz wool into the liner. Pack the wool tightly3 from the dimple
upwards (about one inch [2.5 cm]). Loosely pack quartz wool in the top portion
of the liner to wipe the syringe needle upon injection.
NOTE: As you can see in Figure 6-20, each liner has an O-ring installed on the part
furthest away from the dimple on the PSS injector liner. If the O-ring has
adhered to the liner, you may not be able to easily remove the liner. Use a small
screwdriver to dislodge the O-ring before removing the liner and O-ring. Be
careful not to scratch the barrel where the O-ring seals.
Step 4: Reinstall the Liner in the PSS Injector.
To reinstall the liner:
3
The recovery of high molecular weight components (e.g., C40) may be improved if the liner is
loosely packed.
6-35
Installing a Capillary Column
1.
Install a new O-ring on the top portion of the liner.
2.
Insert the liner in the injector body.
3.
Place the septum purge assembly over the liner.
4.
Press the septum purge assembly down to correctly position the
liner in the injector.
Make sure that you tightly secure the septum purge assembly to the injector base
with the spanner.
Step 5. Connect a Column to the PSS Injector.
To connect a column:
1. Insert a 1/16-inch column nut (Part No. 0990-3392) and 1/16-inch
graphite ferrule (0.8 mm i.d., Part No. 0992-0141 or 0.5 mm i.d., Part
No. 0990-3700) over one end of the column as shown below:
CAUTION
6-36
This injector terminates in a 1/16-inch fitting. This fitting is
fragile. To preserve the integrity of the fitting, carefully
connect the nut to prevent cross-threading the fitting and/or
overtightening the nut on the fitting. You can also preserve
the integrity of the fitting by allowing the injector to cool
before connecting a nut.
Clarus 500 GC Hardware Guide
Figure 6-21.
Column, nut, and ferrule on the injector end of a narrowbore capillary column.
NOTE: Make certain that the tapered end of the ferrule (in Figure 6-21) is facing
towards the nut.
2.
Cut off about 1 cm (3/8 inch) from the column end using a wafer scribe
(Part No. N930-1376, pkg. of 10 scribes). Break off the tubing at the
score mark so that the break is clean and square. Examine the cut with a
magnifying glass and compare it to Figure 6-22.
Figure 6-22.
Example of a good cut and bad cuts.
3.
Position the column nut on the column so that the back of the nut is 3.8
cm to 4.4 cm (1 1/2 to 1 3/4 inches) from the end of the column.
4.
Using typewriter "white-out" or a felt tipped pen, make a mark on the
column just beyond the back edge of the column nut (see Figure 6-23).
6-37
Installing a Capillary Column
CAUTION
Figure 6-23.
To avoid contaminating the system, make certain that the
nut and ferrule do not come into contact with the mark
on the column.
Capillary column attached to PSS injector fitting.
Connect the Column to the PSS Injector in the OnColumn Mode Using the Hourglass Liner
The on-column mode is not recommended for use with columns having an
internal diameter of 0.1 mm. This is due to the flow differences between the precolumn (0.53 mm i.d.) and the column.
The following three steps summarize how to connect a column to the PSS
injector in the on-column mode:
Step 1. Remove the PSS split/splitless injector liner.
Step 2. Install the hourglass liner in the PSS injector.
6-38
Clarus 500 GC Hardware Guide
Step 3. Connect a column to the PSS injector.
Step 1. Remove the PSS Split/Splitless Injector Liner.
To remove the PSS injector liner:
1.
Ensure that the injector heater has been turned off.
Allow the injector to cool until it is slightly warm to the touch. Cooling
the injector to too low a temperature (less than 80 °C) will make it
difficult to remove the injector liner.
2.
Remove the septum cap.
Figure 6-24.
3.
Removing the septum cap.
Remove the injector cover.
6-39
Installing a Capillary Column
Figure 6-25.
4.
Removing the injector cover.
Loosen the threaded collar using the spanner (Part No. N610-1359)
provided, then remove the threaded collar.
Figure 6-26.
Loosening the threaded collar.
5.
Replace the septum cap on the injector.
6.
Pull the septum cap upwards to remove the septum purge assembly.
6-40
Clarus 500 GC Hardware Guide
Figure 6-27.
Removing the septum purge assembly.
The carrier gas inlet line is coiled to allow you to pull the septum purge
assembly over to the side and gain access to the liner.
7.
Ensure that the liner is cool, then insert the end of the PSS liner-removal
tool (Part No. 0250-6247) over the end of the wide-bore or narrow-bore
PSS injector liner. Remove the liner by lifting it up. Gently probe the Oring if it sticks to the injector body.
The PSS liner must be cool (no hotter than 100 °C) or the tubing will
melt! The end of the PSS liner-removal tool may flare out with use. If
this happens, cut off the flared end with a razor blade or scissors.
6-41
Installing a Capillary Column
Figure 6-28.
Removing an injector liner.
Step 2. Install the Hourglass Liner in the PSS Injector.
To install the hourglass liner:
1.
Replace the existing liner with the hourglass liner. Install the liner with
the hourglass end closest to the septum and use a new O-ring.
Figure 6-29.
6-42
Hourglass liner (Part No. N610-1539).
Clarus 500 GC Hardware Guide
2.
Replace the septum purge assembly removed previously. DO
NOT secure it with the collar at this time.
We recommend the following procedure to connect a column and pre-column to
the universal connector. You may find that changing the order of the steps is
more convenient for you. However, the critical concerns are:
•
Making straight, clean, even cuts on the column/pre-column.
•
Wetting the ends of the column/pre-column.
•
Wetting the fused-silica universal connector/hourglass needle guide.
•
GENTLY twisting the column/pre-column into the hourglass fused-silica
universal connector.
•
Conditioning the mechanical joint (this is critical).
In the on-column mode, you will install a column (0.53 mm i.d.) or a deactivated
fused silica pre-column (0.53 mm i.d.) in the injector body. This will enable the
sample to be deposited directly into the column or the pre-column.
Step 3. Connect a Column to the PSS Injector
To connect a column to the PSS in the on-column mode using the hourglass liner:
1.
Insert a 1/16-inch column nut (Part No. 0990-3392) and 1/16inch graphite ferrule (Part No. 0992-0141) over the other end of
the 0.53-mm i.d. column or pre-column as shown below:
6-43
Installing a Capillary Column
CAUTION
Figure 6-30.
CAUTION
2.
6-44
If you are using a 0.53-mm i.d. column, insert it directly into
the injector. If you are using a column with an i.d. less than
0.53 mm, insert a one-meter piece of deactivated 0.53-mm
i.d. fused silica (pre-column) into the injector. This precolumn will also serve as a retention gap. In addition, the
long length of this tubing will enable you to change columns
and still have enough of the pre-column to make numerous
new column connections. Connect a column to the end of
this pre-column (in the oven) with a universal connector
(Part No. N930-2149).
Column, Nut, and Ferrule on the injector end of a narrowbore capillary column.
Ensure that the tapered end of the ferrule is facing towards
the nut as shown above.
We have found that graphite/Vespel ferrules used to connect
the column to the injector fitting loosen after the injector
temperature cycles several times. Use graphite ferrules to
eliminate this problem.
Cut off about 1 cm (3/8 inch) from the column end using a wafer
scribe (Part No. N930-1376, pkg. of 10 scribes) or other column
Clarus 500 GC Hardware Guide
cutting tool. Break off the tubing at the score mark so that the
break is clean and square. If you are using a 0.53-mm i.d. precolumn, make a clean square cut on both ends. Examine the cut
with a magnifying glass and compare it to the following figure:
CAUTION
A clean, square cut is especially critical to produce a leak-free
seal in the fused-silica universal connector.
Figure 6-31.
3.
Example of a good cut and bad cuts.
Locate the PSS injector fitting inside the oven.
Figure 6-32.
PSS injector fitting in the column oven.
6-45
Installing a Capillary Column
4.
Insert the 0.53-mm i.d. column or pre-column into the PSS
injector fitting. Tighten the column nut so the column/precolumn can still be moved but with some resistance.
5.
Push the column/pre-column up into the injector until it can not
go any further.
You may notice the septum purge assembly move upward.
6.
Mark the column with typewriter "white out" just below the
column nut.
7.
Push the septum purge assembly down into position, place the
threaded collar on the assembly, and tighten the threaded collar
with the spanner provided.
Figure 6-33.
8.
6-46
Replacing the septum purge assembly.
Using a 1/4-inch wrench, tighten the fitting until the column
cannot be pulled out of the fitting.
Clarus 500 GC Hardware Guide
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
CAUTION
9.
Replace the septum cap but do not tighten it. Manually insert the
0.47-mm o.d. syringe needle into the 0.53-mm i.d. column/precolumn. With the syringe still inserted in the injector, tighten the
septum cap completely. This aligns the column and septum cap to
ensure a smooth movement of the syringe through the septum cap
and into the 0.53-mm i.d. column/pre-column.
10.
If your column i.d. is smaller than 0.53 mm, connect your column
to the 0.53-mm i.d. pre-column as follows:
a)
Make a clean, even cut on the end of your column and
examine it with a magnifying glass.
b)
Drop some solvent (for example, methanol) into both sides
of the fused-silica universal connector (Part No. N9302149, package of 5).
c)
Wet a tissue with solvent and wipe the end of the column.
d)
Insert the column end into the universal connector and
gently twist it. The column should seal in the universal
connector.
11.
Wet a tissue with solvent (for example, methanol) and wipe the
end of the pre-column.
12.
Carefully push the universal connector, with the attached
column, up into the end of the pre-column. Gently twist the
universal connector to seal the connection between pre-column
and universal connector. This connection is called the
mechanical joint.
6-47
Installing a Capillary Column
Figure 6-34. Connecting a column and universal connector to the precolumn to create the mechanical joint.
6-48
Clarus 500 GC Hardware Guide
Typically the split vent is closed in this mode of operation.
CAUTION
Condition the mechanical joint between the pre-column and
column prior to making any analytical runs. Condition the
joint by slowly temperature programming the oven up to 200
°C and holding it at 200 °C for one hour. Do not exceed the
recommended temperature of your column. This can be
incorporated when you condition the column, see Step E in
this Chapter.
If you replace the column, do not reuse the universal
connector. Cut the column and pre-column from the
universal connector. Replace the universal connector with a
new one. The pre-column ought to be long enough so that
you can reuse it.
If you replace the pre-column, it will also require some
conditioning. If the entire installation is new, the column
conditioning procedure will condition the pre-column, the
column, and the mechanical joint. If you are just replacing
the pre-column, you can condition it and the mechanical joint
by the above procedure. If a high background persists with a
fresh pre-column, condition the pre-column by only
increasing the injector temperature for one hour.
CAUTION
When using the PSS injector in the on-column mode or with
the autosampler, you must use a special syringe that has a
needle o.d. of 0.47 mm (Part No. N610-1253 or N610-1380).
Refer to Chapter 9 for more details. You must use only the
"Norm" injection speed with this syringe when you are in the
on-column mode. The "Fast" injection speed will bend this
thin needle and the "Slow" injection speed may produce peak
break up or distorted peaks. You can achieve better precision
in the on-column mode when sample volumes of 1.0 µL or
greater are injected.
6-49
Installing a Capillary Column
Step B3
Connect the Column to the Programmed
On-Column Injector (POC) :
Overview
The Programmed On-Column injector (POC) consists of an hourglass adapter, a
deactivated 0.53-mm i.d. fused-silica pre-column, and a fused-silica universal
connector. The sample is injected into the POC at a “cool" temperature; the
injector temperature is then programmed to increase. This is helpful for samples
that are thermally labile and/or of a wide molecular weight range. This injector is
used only for trace analysis or diluted solutions.
CAUTION
6-50
Only use a syringe that has a 0.47-mm o.d. needle (Part No.
N610-1380) with this injector.
Clarus 500 GC Hardware Guide
Figure 6-35. Cutaway view of a Programmed On-Column injector (POC).
About the Pneumatics Control
The POC pneumatics consist of a PPC (programmable pneumatics controlled)
version and a manual pneumatics version.
In the PPC version, the pneumatics consist of PPC modules that regulate the
inlet flow and pressure of the gases using software controlled by an Clarus 500
GC method.
6-51
Installing a Capillary Column
In the manual pneumatics version, the pneumatics consist of a flow controller
with an inline pressure transducer for screen readout of the current flow.
CAUTION
This injector terminates in a 1/16-inch fitting. When
connecting a nut to this fitting, take special care not to
crossthread the fitting or overtighten the nut..
On-column injection is not recommended for columns with an internal diameter
of 0.1 mm. This is because of flow differences between the pre-column (0.53
mm) and the column.
CAUTION
If you have ordered the POC without the flow readout
option, measure the carrier gas flow before connecting
the column to the POC. Proceed to: C2 Setting the
Carrier Gas for manual pneumatics and follow the
procedure "Set the Carrier Gas Flow for a POC injector
using the Soap Bubble Flowmeter" in this Chapter now!
We recommend that you use the following procedure to connect a column and
pre-column with the universal connector. You may find that changing the order
of the steps is more convenient for you. However, the critical concerns are:
•
Making straight, clean, even cuts on the column/pre-column.
•
Wetting the ends of the column/pre-column with solvent.
•
Wetting the universal connector/hourglass needle guide with solvent.
•
GENTLY twisting the column/pre-column into the hourglass universal
connector.
•
Conditioning the mechanical joint (this is critical).
6-52
Clarus 500 GC Hardware Guide
To connect a column to the programmed on-column injector (POC):
1.
Figure 6-36.
2.
Figure 6-37.
3.
Figure 6-38.
Remove the septum cap.
Removing a septum cap.
Remove the septum shield (Part No. N610-1702) with the large
end of the liner-removal tool (Part No. N610-0102).
Liner-removal tool (Part No. N610-0102).
Remove the hourglass needle guide (Part No. N610-1703) with a
pair of small pliers or tweezers.
Hourglass needle guide.
6-53
Installing a Capillary Column
CAUTION
4.
Figure 6-39.
CAUTION
6-54
If you are using a 0.53-mm i.d. column, insert it directly into the
injector. If you are using a column with an i.d. of less than 0.53
mm, insert a one-meter piece of deactivated 0.53-mm i.d. fused
silica into the injector to act as a pre-column. This pre-column
will also serve as a retention gap. In addition, the long length of
this tubing will enable you to change columns and still have
enough of the pre-column to make numerous new column
connections. Connect a column to the end of this pre-column (in
the oven) with a universal connector (Part No. N930-2149).
Insert the column nut (Part No. 0990-3392) and ferrule (Part No.
0992-0141) on the end of the column/pre-column.
Column, nut, and ferrule on the injector end of a narrowbore capillary column.
We have found that graphite/Vespel ferrules used to connect
the column to the injector fitting loosen after the injector
temperature cycles several times. Use graphite ferrules to
eliminate this problem.
Make certain that the tapered end of the ferrule is facing
towards the nut as shown above.
Clarus 500 GC Hardware Guide
5.
Make a clean, square cut on the end of the 0.53-mm column or
on both ends of the 0.53-mm pre-column. Wipe the end with a
tissue soaked in methanol to remove fragments of polyimide or
silica.
CAUTION
Figure 6-40.
A clean, square cut is especially critical to obtain a leak-free
seal in the hourglass needle guide and fused-silica universal
connector.
Example of a clean cut and bad cuts.
6.
Locate the injector fitting in the oven. Then insert the
column/pre-column until it protrudes out the septum end of the
injector.
7.
Thread the nut onto the injector fitting. Then tighten it so that the
column/pre-column can still be moved, but you feel some
resistance.
8.
Push the column/pre-column into the hourglass needle guide and
twist it slightly.
9.
Place the metal septum shield over the hourglass needle guide and
push it into the injector until it is completely seated. Replace the
septum cap.
6-55
Installing a Capillary Column
10.
Tighten the column nut inside the oven until the column cannot be
pulled out of the fitting.
CAUTION
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
You may want to mark the column, just behind the nut, with typewriter "whiteout." The mark will act as a guide when you test to see if the fitting is tight
enough.
CAUTION
6-56
To avoid contaminating the system, make certain that the
nut and ferrule do not contact the mark on the column.
11.
Loosen the septum cap and manually insert the 0.47-mm o.d.
syringe needle into the column/pre-column. With the syringe in
the injector, tighten the septum cap completely. This ensures
smooth movement of the syringe through the septum cap and
into the column/pre-column.
12.
If your column i.d. is smaller than 0.53 mm, connect your
column to the 0.53-mm i.d. pre-column as follows:
a)
Make a clean, even cut on the end of your column and
examine it with a magnifying glass.
b)
Drop some solvent (for example, methanol) into both
sides of the fused-silica universal connector (Part No.
N930-2149, package of 5).
Clarus 500 GC Hardware Guide
c)
Wet a tissue with solvent and wipe the end of the
column.
d)
Insert the column end into the universal connector and
gently twist it. The column should seal in the universal
connector.
13.
Wet a tissue with solvent (for example, methanol) and wipe the
end of the pre-column.
14.
Carefully push the universal connector, with the attached
column, up into the end of the pre-column. Gently twist the
universal connector to seal the connection between the precolumn and universal connector. This connection is called the
mechanical joint.
Figure 6-41.
Connecting the column and universal connector to the precolumn to create the mechanical joint.
6-57
Installing a Capillary Column
CAUTION
Condition the mechanical joint between the pre-column
and column prior to making any analytical runs.
Condition the joint by slowly temperature programming
the oven up to 200 °C and holding it at 200 °C for one
hour. Do not exceed the recommended temperature of
your column. This can be incorporated when you
condition the column, see Step E in this Chapter.
If you replace the column, do not reuse the universal
connector. Cut the column and pre-column from the
universal connector. Replace the universal connector with
a new one. The pre-column ought to be long enough so
that you can reuse it.
If you replace the pre-column, it will also require some
conditioning. If the entire installation is new, the column
conditioning procedure will condition the pre-column, the
column, and the mechanical joint. If you are just
replacing the pre-column, you can condition it and the
mechanical joint by the above procedure. If a high
background persists with a fresh pre-column, condition
the pre-column by only increasing the injector
temperature for one hour
CAUTION
6-58
When using the POC with the autosampler, you must use
a special syringe that has a needle o.d. of 0.47 mm (Part
No. N610-1253 or N610-1380). Refer to Chapter 9 for
more detail. You must only use the "Norm" injection speed
with this syringe in the on-column mode. The "Fast"
injection speed will bend this thin needle and the "Slow"
injection speed may produce peak break up or distorted
peaks. You can achieve better precision in the on-column
mode when injecting sample volumes of 1.0 mL or
greater.
Clarus 500 GC Hardware Guide
Step C: Set the Carrier Gas
This step describes how to set the carrier gas for PPC and manual pneumatics
modules. Refer to the procedure that describes your Clarus 500 GC controls, PPC
or manual pneumatics.
Step C1
Setting the Carrier Gas for PPC Modules.
Step C2
Setting the Carrier Gas Using Manual Pneumatics.
Step C1
Setting the Carrier Gas for PPC Modules
The following procedure describes how to:
•
Set the Carrier Gas Pressure for the Split/Splitless Injector (CAP) and
Programmed Split/Splitless Injector (PSS)
•
Set the Carrier Gas Flow for the Programmed On-Column Injector
(POC)
Setting the Carrier Gas Pressure for the Split/Splitless Injector (CAP)
and Programmed Split/Splitless Injector (PSS)
NOTE: The line pressure should be at least 15 psi greater than the highest carrier gas
pressure setting, up to a maximum of 100 psig.
To set the carrier gas pressure:
1. Turn on the carrier gas at the tank. Then adjust the line pressure to
60 - 90 psig.
6-59
Installing a Capillary Column
2. From the System Status screen select either A or B injector (the example here
shows the A PSS injector ready for setting the carrier gas). In this example,
touch the Channel A PSS injector icon
.
3. In the following window touch the Program screen under the Carrier Gas
field.
6-60
Clarus 500 GC Hardware Guide
4. Touch the program button in the Carrier Gas section and the following screen
will be displayed. Using the plus and minus buttons enter pressure (0.1 to 75
psig for minimum and maximum).
6-61
Installing a Capillary Column
.
5. If a capillary injector is in position A, the drop down menu will allow you to
select Pressure, Flow, or Velocity.
6-62
Clarus 500 GC Hardware Guide
6. Using the plus and minus buttons enter the appropriate values. Once entered
select Close to exit.
NOTE: The pressure readout display is factory configured to display the actual pressure
as psig.
7. Enter a pressure set point. (See Suggested Capillary Column Pressures on
Table 6-5.).
6-63
Installing a Capillary Column
Setting the Carrier Gas Flow for the Programmed On-Column
Injector (POC)
To set the carrier gas flow:
1. Turn on the carrier gas at the tank. Adjust the line pressure to
60 - 90 psig.
2. From the System Status screen select either A or B injector (the example here
shows the B injector ready for setting the carrier gas).
6-64
Clarus 500 GC Hardware Guide
3. In the following window touch the Program button under the Carrier Gas
field.
6-65
Installing a Capillary Column
Using the plus and minus buttons enter pressure (0.1 to 100 psig for minimum
and maximum).
NOTE: If you wish to generate a flow program method, refer to the Clarus 500 Users
Guide (0993-6625).
Step C2 Setting the Carrier Gas Using Manual
Pneumatics
This step includes procedures to set the carrier gas pressure for the split/splitless
(CAP) and programmed split/splitless (PSS) injectors. It also includes procedures
to set the flow for the programmed on-column (POC) injector when using the
optional flow readout or a flowmeter.
6-66
Clarus 500 GC Hardware Guide
Setting the Carrier Gas Pressure for the Split/Splitless Injector (CAP)
and Programmed Split/Splitless Injector (PSS)
Carrier gases for the split/splitless injector (CAP) and programmed split/splitless
injector (PSS) are controlled by adjusting the pressure with the pressure control
knob. The location and appearance of the pneumatic controls for a capillary
injector are shown in the following figure.
Figure 6-42.
CAP and PSS injector pneumatic controls.
To adjust the carrier gas pressure:
1. Turn on the carrier gas at the tank. Adjust the line pressure to 90 psig.
6-67
Installing a Capillary Column
2. From the System Status screen select either A or B injector (the example here
shows the B injector ready for setting the carrier gas).
6-68
Clarus 500 GC Hardware Guide
In the following window touch the Program screen under the Carrier Gas field.
3. Using the plus and minus buttons enter set pressure (0.1 to 75 psig for
minimum and maximum). Adjust the manual control until the set pressure is
obtained (see Figure 6-42).
Suggested Capillary Column Pressures:
The following tables are applicable to both PPC or manual pneumatics versions
of the Clarus 500 GC.
6-69
Installing a Capillary Column
Table 6-2. Calculated Pressure Drops (psig) for 10m Column4
Column I.D. (µm)
_
u5
320
250
100
10
20
30
40
60
80
1.0
2.1
3.1
4.1
6.2
8.3
2.4
4.9
7.3
9.8
14.6
19.5
10.0
21.2
31.8
42.3
63.5
84.7
Table 6-3. Calculated Pressure Drops (psig) for 25m Columns4
4
5
Column I.D. (µm)
_
u5
320
250
100
10
20
30
40
60
80
2.6
5.2
7.8
10.3
15.5
20.7
6.1
12.2
18.3
24.4
36.6
48.8
26.5
52.9
79.4
-
In psig, using helium as a carrier gas at 100 °C.
Average linear velocity (cm/sec).
6-70
Clarus 500 GC Hardware Guide
Table 6-4. Calculated Pressure Drops (psig) for 50m Columns4
Column I.D. (µm)
_
u5
320
250
100
10
20
30
40
60
80
5.2
10.3
15.5
20.7
31.0
41.3
12.2
24.4
36.6
48.8
73.2
-
52.9
-
Setting the Carrier Gas Flow for the Programmed On-Column
Injector (POC) Using the Optional Flow Readout
To set the carrier gas flow with the optional flow readout:
1. Turn on the carrier gas at the tank. Adjust the line pressure to 90 psig.
2. From the System Status screen select either A or B injector (the example here
shows the B injector ready for setting the carrier gas).
6-71
Installing a Capillary Column
3. In the following window touch the Program screen under the Carrier Gas
field.
6-72
Clarus 500 GC Hardware Guide
Using the plus and minus buttons enter pressure (0.1 to 100 psig for minimum
and maximum).
.
4. Type the desired flow set-point value.
5. Adjust the flow by turning the flow control knob counterclockwise to
increase the flow, or clockwise to decrease the flow, until the actual flow
displayed on the top line of the screen equals the displayed set point.
6-73
Installing a Capillary Column
Figure 6-43.
Location of the flow control knob.
Set the Carrier Gas Flow for the Programmed On-Column Injector
(POC) Using the Soap Bubble Flowmeter
To perform this procedure, you must know how to measure carrier gas flow using
a soap bubble flowmeter and the Clarus 500 GC built-in stopwatch. If you are not
familiar with this measurement, please read "Using the Built-in Stopwatch" in
Chapter 4 before you install a column.
To set the carrier gas flow using the soap bubble flowmeter:
1.
6-74
Locate the POC injector fitting inside the column oven. The POC
injector fitting is shown below:
Clarus 500 GC Hardware Guide
Figure 6-44.
POC injector fitting in the column oven.
2. Attach a soap bubble flowmeter to the POC injector fitting.
3. Turn on the carrier gas at the tank. Adjust the line pressure to 90 psig.
4. From the System Status Screen select the Tools button and then select
Utilities.
6-75
Installing a Capillary Column
5. In the Utilities window select the Stopwatch icon.
6-76
Clarus 500 GC Hardware Guide
6. Using the plus and minus buttons enter the appropriate values and press
Start.
7. Start the carrier gas flowing by turning the flow controller knob
counterclockwise and measure the flow.
NOTE: For best accuracy, use a soap bubble flowmeter volume that gives a reading of at
least 30 seconds.
8. Adjust the flow to the desired set point by repeatedly measuring the flow and
turning the flow controller knob counterclockwise to increase the flow,
clockwise to decrease the flow, until the desired flow is obtained.
9. Disconnect the soap bubble flowmeter before proceeding to the next step to
Step D “Leak Test all New Connections.”
Table 6-5. Suggested Capillary Column Flow Rates Using Helium As
Carrier
Column i.d. (µm)
Flow mL/min
250
320
530
0.6 - 0.8
1.0 - 1.5
2.5 - 4.0
6-77
Installing a Capillary Column
Step D
Leak Test All New Connections:
Manual Pneumatics
Test the connection to the capillary injector fitting for leaks using a 50/50
mixture of isopropanol/water or an electronic leak detector. To avoid
contaminating the system, DO NOT use a soap solution for leak testing. Tighten
all leaking connections.
PPC Pneumatics (POC Injector Only)
1. In the following example select the POC from the System Status screen.
2. In the next window select the Program icon.
6-78
Clarus 500 GC Hardware Guide
3. In the program screen enter a minimum value between 0.1 and 100 psig.
Enter a maximum value between 0.1 and 100 psig.
The Clarus 500 GC monitors the inlet column head pressure with a carrier-gas
mass-flow controller in use. You enter the minimum and maximum values after
selecting the carrier-gas Flow mode in configuration. If the inlet column head
pressure drops below or rises above the set limits for more than one minute, a
warning message appears on the display. The following error message will
appear: Carrier (with specific carrier number) unable to maintain pressure.
You should correct the leak; the most common area would be the injector
septum. Then clear the message by touching OK before continuing to use the
GC. This will stop an autosampler program from continuing. If you do not make
any entries, leak checking will not be done. If you are temperature programming,
then the value you enter for the maximum must be above the column head
6-79
Installing a Capillary Column
pressure at the highest oven temperature. You can just enter a value for the
minimum and leave the maximum off (zero).
6-80
Clarus 500 GC Hardware Guide
Step E:
Condition the Column and the
Mechanical Joint Between the Precolumn and Column:
This section contains a suggested temperature program for conditioning a
column. The program starts off by holding the oven temperature at a medium
value for 10 minutes, gradually increasing the oven temperature at a fixed rate
(5 °C/min) to the column operating temperature, then holding that temperature
overnight with the carrier gas flowing.
CAUTION
CAUTION
The temperatures shown in the examples which follow
should be used as guidelines. Please refer to the column
manufacturer's operating instructions for specific
temperature recommendations.
To keep the injector clean, open the split vent to direct
more gas through the injector.
6-81
Installing a Capillary Column
To condition the column:
1. Close the oven door and from the System Status screen press the Oven icon.
2. In the oven screen enter an oven temperature set point of 50 °C and enter a
(Hold) time of 10.
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Clarus 500 GC Hardware Guide
3. To add another program step, enter a RATE of 5(ºC/min).
4. For TEMP 2, enter a set point 25 to 50 ºC above your planned analytical
operating temperature. For example, enter a set point of 200.
CAUTION
To avoid damaging the column, do not enter a
temperature higher than the maximum recommended
temperature specified by the column manufacturer.
6-83
Installing a Capillary Column
5. Configure the injector for the oven mode. From the System Status screen
push the tools button and select the configuration menu
.
6. In the configuration menu select the injector icon. In the following example
injector B has been selected to be configured.
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Clarus 500 GC Hardware Guide
7. Select oven from the temperature control drop down menu.
8. Turn the Detector Temperature off. And. Allow the system to run overnight.
9. In the morning, reset the oven the oven temperature set point to the initial
TEMP at the beginning of the temperature program. See step 4 earlier in this
procedure.
10. Open the oven door. Allow the oven to cool until the oven fan turns off. This
occurs when the oven cools down to 40 °C.
6-85
Installing a Capillary Column
Step F:
Connect the Column to the Detector:
NOTE: Before connecting a wide-bore column (0.53-mm i.d.) to a Photoionization
Detector (PID), remove the 1/8-inch diameter receiver from the PID base.
Figure 6-45. PID receiver viewed inside the column oven
1.
Place the column over the hanger so that no part of the column
touches the bottom or sides of the oven.
2.
Insert a 1/8-inch column nut and graphite ferrule over the free
end of the column as shown below:
Figure 6-46.
6-86
Nut and ferrule on the detector end of a narrow-bore
capillary column.
Clarus 500 GC Hardware Guide
3.
Cut about 1 cm (3/8 inch) from the column end using a wafer scribe
(Part No. N930-1376, pkg. of 10 scribes) or other column cutting tool.
Break off the tubing at the score mark so that the break is clean and
square. Examine the cut with a magnifying glass and compare it to the
following figure:
Figure 6-47.
4.
Example of a good cut and bad cuts.
Mark the column the following distances from the end using typewriter
"white-out" or a felt-tipped pen:
5. From the System Status screen select the Tools menu. From the tools menu
select Utlitities.
6-87
Installing a Capillary Column
6. In the Utilities screen select the Column Length Calc icon.
7. Using the drop down menus you will be able to select the proper detector and
injector for the calculator. The using the plus and minus buttons input the
length from the back of the nut and the Column Length Calculator will
automatically calculate the column length in millimeters or inches.
6-88
Clarus 500 GC Hardware Guide
CAUTION
To avoid contaminating the system, make certain that the
nut and ferrule do not contact the mark on the column.
8. Locate the detector fitting protruding from the right side of the oven roof.
9. Insert the column into the detector fitting, keeping the mark just behind the
column nut.
10. While holding the column in position, hand-tighten the column nut.
11. Hold the detector fitting steady with one of the 7/16-inch wrenches as you
gradually tighten the column nut with the other wrench. Tighten the nut only
until you cannot pull the column out of the nut. DO NOT OVERTIGHTEN
THE NUT!
6-89
Installing a Capillary Column
Figure 6-48.
Capillary column connected to the detector fitting.
CAUTION
CAUTION
6-90
Make certain that no part of the column touches the walls
or bottom of the oven.
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
Clarus 500 GC Hardware Guide
Step G: Leak Test All New Connections:
Test the detector connection for leaks using a 50/50 mixture of isopropanol/water
or an electronic leak detector. To avoid contaminating the system, DO NOT use a
soap solution for leak testing. Tighten all leaking connections.
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Installing a Capillary Column
Step H: Set up the Split Mode for a
CAP or PSS Injector:
The Split Mode is used to analyze concentrated samples. In this mode only part
of the sample enters the column; the remainder is split and vented through a
charcoal filter to atmosphere. This step describes how to set the split mode for
PPC and/or manual pneumatics modules. Refer to the procedure that describes
your Clarus 500 GC controls, PPC or manual pneumatics.
Step H1:
Setting the Split Mode Using PPC.
Step H2:
Setting the Split Mode Using Manual Pneumatics.
NOTE: In the Split Mode, the split vent is always open.
NOTE: The injector is shipped with an unpacked wide-bore injector liner installed.
Remove the liner and pack it with quartz wool before running your analysis.
Refer to Step B, Connect the Column to the Injector, in this chapter
The following procedure assumes that the carrier gas pressure has been set (see
Step C in this chapter).
For information on Setting the Split Mode Using PPC, Setting the Split Mode
Using Manual Pneumatics , Setting up the Splitless Mode for a CAP or PSS
Injector, Setting the Splitless Mode Using PPC Modules, Setting the Splitless
Mode Using Manual Pneumatics see the Clarus 500 GC Users Guide (09936625) Using the Active Method chapter.
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Clarus 500 GC Hardware Guide
PSS and POC Operating Hints:
The Programmed Split/Splitless (PSS) and Programmed On-Column (POC)
injectors can be operated in either the oven-programming mode or the inletprogramming mode. For specific instructions, refer to Chapter 9 of this manual.
CAUTION
If you have the subambient option, the POC and PSS injectors are linked
to the oven subambient option; therefore, you cannot operate the
injectors below the oven subambient temperature.
Oven Programming Mode
This is the default mode for both the POC and the PSS injectors. This mode is the
easiest to operate since only the oven temperature program needs to be entered
into the method. In this mode, the injector will follow the oven temperature
profile plus five degrees Celsius. In this mode, the sample is introduced into the
injector when the temperature of the inlet is at the boiling point of the solvent.
Then start the injector and oven temperature program.
If the initial temperature of the oven is above the boiling point of the solvent you
are using, then it would be better to modify the oven program to start at a lower
temperature or to configure the injector for the Inlet mode and set a temperature
for the injector separate from the oven temperature.
Inlet Programming Mode
This mode permits the use of independent injector temperatures and rates that
you define in the method. The injector will be programmed for injector
temperature 1, injector time 1, injector rate 1, injector temperature 2, injector
time 2, etc. You can program up to three temperatures and two ramps for each
PSS or POC configured in the inlet mode. It is important to set the initial injector
temperature to approximately the boiling point of the solvent you are using.
6-93
Installing a Capillary Column
CAUTION
CAUTION
The PSS can be used in the "hot" split or splitless mode. This,
however, is not recommended for use with the 1 mm i.d. liner; it could
cause solvent flashback in the injector. This mode should be used with
caution depending upon the solvent and temperatures you choose.
Always use the 2-mm i.d. injector liner. See Table 6-1at the beginning
of this chapter.
When using the PSS in the on-column mode, or the POC with the
autosampler, you must use a special syringe that has a needle o.d. of
0.47 mm (Part No. N610-1253 or N610-1380). You must only use the
"Norm" injection speed with this syringe in the on-column mode. The
"Fast" injection speed will bend this thin needle and the "Slow"
injection speed may produce peak break up or distorted peaks. You
can achieve better precision in the on-column mode when sample
volumes of 1.0 uL or greater are injected.
If a column is used extensively at high temperatures (350 °C or greater), the
polyimide may become very brittle. This brittleness will cause the column to
fracture when you try to seal it in the universal adapter. If you wish to continue
using a brittle column, use a low dead-volume union instead of the universal
adapter.
Solvent Purge Mode
The PSS injector can be operated in the solvent purge mode without any
modification. This technique is an enhanced mode of the splitless injection and
may use either the 0.5-µL or 5.0-µL syringe. To obtain better detection limits,
you may also use a 50-µL syringe to make larger volume injections. In the
solvent purge mode, the split vent is open at the time of injection and the PSS
injector temperature is held below the boiling point of the solvent. Once most of
the solvent has vented, the split vent closes and the PSS injector is heated so that
it can transfer the analytes onto the column.
You must select the starting temperature of the PSS injector based on the solvent
you are using. In addition, to eliminate most of the solvent without losing any of
6-94
Clarus 500 GC Hardware Guide
the compounds of interest, you must experimentally determine the minimum split
flow and vent time.
The initial value of the split vent can be ON or OFF, depending upon your
solvent volatility. When you make your injection, the split vent OPENS (turns
ON) and stays open for the time you have selected. After that time, the split vent
CLOSES (turns OFF via a timed event) and the PSS injector heats to the selected
temperature. To help maintain good peak shape and quantitative recovery, we
recommend holding the Clarus 500 GC oven temperature at its starting value
until the PSS injector temperature reaches its final temperature and all of the
sample has been transferred onto the column. To minimize tailing of the residual
solvent and ensure that the system is completely cleaned for the next injection,
start the oven temperature program and re-open the split vent.
The charcoal trap's capacity is too small to handle the large volumes of solvent
and it will saturate quickly. When making large volume injections, we
recommend disconnecting the charcoal trap from the PSS injector. For details,
refer to “Replacing the Charcoal Trap on the Split/Splitless, CAP, and PSS
Injectors” in Chapter 9, Maintenance. To retain the vented solvent, we strongly
recommend a larger capacity charcoal trap after (downstream from) the vent on
the AutoSystem.
NOTE: When using the PSS injector in the split mode, the charcoal trap is required to
maintain the split ratio throughout the injection.
6-95
Installing a Capillary Column
Calculating a Capillary Column Split Ratio
The following procedure and examples show how to calculate the capillary
column split ratio in a PPC version and a manual pneumatics version.
PPC Version
1. Enter the column length, I.D., and vacuum compensation values.
2. Measure the unretained peak time and correct the column length, see
chapter 8.
3. Read the column and split flows from the screen on the Clarus 500
GC.
4. Calculate the Split Ratio:
Flow rate from the split vent in mL/min + Flow rate of the
column
Split Rate =
_________________________________________________________
Flow rate of the column
Manual Pneumatics Version
1. Calculate the volume of a capillary column:
(Length of the capillary column in mm) (column diameter
in mm/2)2 (3.14)
Column Volume =
_________________________________________________________
1000mm3/mL
2. Column flow rate:
Volume of the column in mL
Column Flow Rate =
_________________________________________________________
Retention time of methane in min
6-96
Clarus 500 GC Hardware Guide
3. Calculate the Split Ratio:
Flow rate from the split vent in mL/min + Flow rate of the column
Split Rate =
_________________________________________________________
Flow rate of the column
NOTE: Remember that the split ratio determines how much sample is placed into the
capillary column. A larger split ratio means that less sample is placed in the
column, therefore less sample is analyzed by the detector.
In the manual pneumatics version, always note the CAPILLARY HEAD
PRESSURE. If the pressure changes, so will the SPLIT RATIO.
In order to reproduce the same chromatographic conditions in the future save
the oven temperature program, column head pressure value, and split vent flow
rate value.
In the PPC version, you can directly control the split ratio.
6-97
Installing a Capillary Column
6-98
Prevent
7
Prevent
7-2
Clarus 500 GC Hardware Guide
Overview
PreVent is an enhanced capillary inlet system for the Clarus 500 GC that uses
columns with an inside diameter (i.d.) between 0.25 mm and 0.53 mm. You can
use the pre-column venting technique to:
•
Manage difficult samples
•
Protect the column and gas chromatograph
•
Lower detection limits
•
Increase analytical throughput
PreVent is used in the following five Modes of Operation:
1. Column Isolation
2. Solvent Purge (PSS injector only)
3. Large Volume Injection (PSS injector only)
4. Sample Residue Purge (PSS injector only)
5. Time Saver
This chapter describes how to install the PreVent adapter and restrictor on an
injector or detector. Based on your mode of operation, the PreVent adapter is
installed on either the injector or detector (including TurboMass MS). Turn to
the procedure in this chapter that describes how to install PreVent:
Installing PreVent on an Injector
Installing PreVent on a Detector
Installing PreVent on a TurboMass MS Detector
7-3
Prevent
NOTE: The instructions in this chapter assume that the PreVent option has been
installed in the front injector position (Channel A). The mid-point pressure for
Channel A is controlled by valve 3, and the mid-point pressure for Channel B is
controlled by valve 4.
NOTE: The PreVent option contains a bleed flow of nominally 15 mL/min of carrier gas
that constantly flows and vents to atmosphere when you set the pressure on the
PreVent mid-point module. If your carrier gas is hydrogen, you should connect
tubing to the barbed fitting on the bleed controller (on the underside of the
Clarus 500 GC top cover), and direct it to a venting hood.
7-4
Clarus 500 GC Hardware Guide
Installing PreVent on an Injector
The following procedure describes how to install the PreVent adapter on a
capillary inlet system (CAP and/or PSS) and how to make it ready for an
analysis.
Summary
The following steps summarize how to install an enhanced capillary inlet system
to an injector and get it ready for use:
A. Install the restrictor in the PreVent adapter.
B. Connect the PreVent adapter to the injector.
C. Connect the column to the PreVent adapter.
D. Leak-check the system.
E. Connect the column to the detector.
F. Set the initial pressures.
G. Condition the system.
A.
Install the Restrictor in the PreVent Adapter
The following restrictors are available for the injector:
•
0.06 mm i.d. restrictor (Part No. N610-3080)
•
0.06 mm i.d. to 0.250 mm i.d. restrictor (Part No. N610-0342)
1. Select the appropriate restrictor for your analysis and cut it to the
proper length. Refer to the following table:
7-5
Prevent
Table 7-1 Recommended Restrictors
Injector
Injection
Mode
Restrictor
Part Number
Length
(mm)
Split/Splitless
Split
0.06 mm i.d.
N610-3080
108
Split/Splitless
Splitless
0.06 mm i.d.
N610-3080
108
PSS
Split
0.06 mm i.d. to 0.250 mm
i.d1.
N610-0342
104
PSS
Splitless
0.06 mm i.d. or
N610-3080
104
0.06 mm i.d. to 0.250 mm i.d.
N610-0342
Thread the selected restrictor first through a 0.5 mm graphite ferrule
(Part No. 0990-3700) and then through the PreVent adapter (Part No. N6100328) until 5 mm protrudes through the column connection on the bottom. When
using the 0.06 mm i.d. to 250 mm i.d. restrictor, the narrow end should protrude
through the bottom.
CAUTION
1
7-6
To prevent contamination problems and the need for
extensive conditioning procedures, ensure that all PreVent
components are thoroughly clean. Baking them in an oven
prior to assembly is recommended or wiping with a tissue
dampened with alcohol. Always wear clean gloves when
assembling the PreVent components.
This restrictor is pre-cut to the correct length for PSS.
Clarus 500 GC Hardware Guide
Figure 7-1. Installing the restrictor in the PreVent adapter.
B.
Connect the PreVent Adapter to the Injector
1. Verify that the injector liner is correct for your application. If
necessary, pack the injector liner with quartz wool. For details,
refer to packing a PSS or split/splitless injector liner in Chapter
6.
2. Carefully connect the PreVent adapter by screwing the injector
end of the adapter into the capillary injector fitting until it is
finger tight.
3. Using a 1/4-inch wrench, tighten the PreVent adapter until the
graphite ferrule just starts to tighten on the restrictor.
4. Locate the stainless steel tubing (that supplies the mid-point
pressure) inside the oven.
7-7
Prevent
5. Insert a 1/16-inch nut (Part No. 0990-3392) and a
graphite/Vespel ferrule (Part No. 0992-0107) over the end of
this tubing.
6. Measure and mark the tubing 1/2-inch from the back of the nut.
7. Insert the tubing into side arm on the PreVent adapter, keeping
the mark just behind the nut. Then tighten the nut and ferrule
fingertight.
8. Make a leak-free seal by tightening the PreVent adapter, on the
capillary injector fitting, another 1/4 to 1/2 turn.
Figure 7-2. Capillary injector fitting inside the oven.
C.
Connect the Column to the PreVent Adapter
1. Place the column on the hanger so that no part of the column
touches the bottom or sides of the oven.
2. Insert a 1/16-inch extended nut (Part No. 0990-3392, pkg. of 5),
a graphite/Vespel ferrule (1/16-inch x 0.5 mm Part No. 09920105, pkg. of 10 for 0.25/0.32 i.d. column, or a 1/16-inch x 0.8
mm Part No. 0992-0107, pkg of 10 for a 0.53 mm i.d. column),
and a spacer (Part No. N610-3079), over one end of the column.
7-8
Clarus 500 GC Hardware Guide
CAUTION
Do not use a graphite ferrule since it will extrude up
into the body of the PreVent adapter.
Figure 7-3. Extended nut, graphite/Vespel ferrule, and spacer.
3. Cut about 1 cm (3/8 inch) from the end of the column tubing using a wafer
scribe (Part No. N930-1386, pkg. of 10 scribes) or other column cutting tool.
Break off the tubing at the score mark making sure that the break is clean and
square. Examine the cut with a magnifying glass and compare it to the
following figure:
Figure 7-4. Example of a good column cut and bad cuts.
7-9
Prevent
4. Insert the column end (as shown in Figure 7-5, Step 1) into the hourglass
guide (Part No. N610-3082).
5. Align the end of the restrictor tubing that protrudes from the PreVent adapter
with the open end of the hourglass guide. Then, carefully push the hourglass
guide, with the attached column, up into the PreVent adapter as shown in
Figure 7-5, Step 2. Notice that the restrictor tubing fits inside the column.
NOTE: Slightly twist the column as you push the hourglass guide into the PreVent
adapter.
6. Loosely connect the column nut to the PreVent adapter.
7. Carefully push the column up and into the PreVent adapter until it bottoms in
the adapter. Then pull the column back 3 mm as shown in the following
figure, Step 3.
8. Use two 1/4-inch wrenches to tighten the nut. DO NOT OVERTIGHTEN THE
NUT!
7-10
Clarus 500 GC Hardware Guide
Figure 7-5. Connecting a column to the PreVent injector adapter.
D.
Leak-Check the System
1. Locate the detector end of the column.
2. Seal the column end by firmly inserting the detector end of the column
into the side of a septum to about the mid-point as shown in the
following figure.
7-11
Prevent
Figure 7-6. Column inserted into a septum.
3. Turn on the Clarus 500 GC. When the Clarus 500 GC is turned on, it is set
to the initial default settings.
4. From the System Status screen touch the injector to get to the following
screen. Touch the numeric field until it turns black and use the plus and
minus buttons to get the proper split flow of 1.5 and a ratio of 25.
7-12
Clarus 500 GC Hardware Guide
5. From the Events tab turn off the mid-point carrier gas supply by closing
Valve 3.
6. Allow the system to equilibrate for several minutes, then view the Aux 1
pressure, view the Aux Gas button and view the current psig.
7-13
Prevent
7. Go back to the inject screen to view the pressure read out on the carrier gas
which should be at 0 psig.
8. Set the injector pressure to 75 psig.
9. After approximately 5 minutes, if no leaks exist, the Aux 1 reading should be
stable at approximately 75 psi. If it is low, then leak-check the fitting
connections.
10. If you suspect a leak, test the connections for leaks using a 50/50 mixture of
isopropanol/water or an electronic leak detector. To prevent contaminating the
system, DO NOT use a soap solution for leak testing. Tighten all leaking
connections.
If you detect a leak, check and tighten the fittings on the mid-point pressure tee
and/or the connections on the rear of the Clarus 500 GC.
7-14
Clarus 500 GC Hardware Guide
CAUTION
Do not overtighten the column nut. If this fitting has a
persistent leak, replace the graphite/Vespel ferrule.
11. Turn off the two gas pressures and remove the septum from the end of the
column.
E.
Connect the Column to the Detector
CAUTION
Make certain that no part of the column touches the
walls or bottom of the oven.
NOTE: To connect a column to the TurboMass, refer to the instructions in the
TurboMass User’s Manual (Part No. 0993-8847).
1. Insert a 1/8-inch column nut and graphite ferrule over the free end of the column
as shown in the following figure.
Figure 7-7.
Nut and ferrule on the detector end of a narrow-bore
capillary column.
2. Cut about 1 cm (3/8 inch) from the column end using a wafer scribe
(Part No. N930-1376, pkg. of 10 scribes) or other column cutting tool. Break off
7-15
Prevent
the tubing at the score mark so that the break is clean and square. Examine the
cut with a magnifying glass and compare it to the following figure:
Figure 7-8. Example of a good cut and bad cuts.
3. Mark the column using typewriter "white-out" or a felt-tipped pen. The
distances are calculated using Column Length Calc procedure that follows.
7-16
Clarus 500 GC Hardware Guide
4. From the System Status screen select the Tools menu. From the tools menu
select Utlitities.
5. In the Utilities screen select the Column Length Calc icon.
6. Using the drop down menus you will be able to select the proper detector and
injector for the calculator. The using the plus and minus buttons input the
7-17
Prevent
length from the back of the nut and the Column Length Calculator will
automatically calculate the column length in millimeters or inches.
CAUTION
To prevent contaminating the system, ensure that the nut
and ferrule do not contact the mark on the column.
7. Locate the detector fitting that protrudes through the right side of the oven
roof.
8. Insert the column into the detector fitting, keeping the mark just behind the
column nut.
9. While holding the column in position, hand-tighten the column nut.
10. Holding the detector fitting steady with one of the 7/16-inch wrenches,
gradually tighten the column nut with the other wrench only until you
cannot pull the column out of the nut. DO NOT OVERTIGHTEN THE
NUT!
7-18
Clarus 500 GC Hardware Guide
Figure 7-9. Capillary column connected to the detector fitting.
CAUTION
F.
Do not overtighten column nuts. Overtightening
can cause damage to the ferrule and/or column.
Set the Initial Pressures
To set the mid-point pressure:
1. From the System Status screen select either A or B injector (the example here
shows the B injector ready for setting the carrier gas).
7-19
Prevent
2. In the following window touch the Program Graph screen under the Carrier
Gas field.
7-20
Clarus 500 GC Hardware Guide
3. Using the plus and minus buttons enter the initial value of 30 psig for the
Carrier gas. Press Close to go back to the previous screen (as seen in step 2).
7-21
Prevent
4.
In the Events tab touch the Split event and then press Edit. Set Split 1 to 100
mL/min.
7-22
Clarus 500 GC Hardware Guide
5. From the oven tab set the oven temperature to its highest programmed
temperature.
7-23
Prevent
6. From the Events tab turn off the mid-point carrier gas supply by closing Valve
3.
7-24
Clarus 500 GC Hardware Guide
7. Allow the system to equilibrate for several minutes, then view the Aux 1
pressure, view the Aux Gas button and view the current psig.
Note:
If the Aux 1 pressure is very low, then the graphite ferrule that holds the
restrictor inside the PreVent adapter may be leaking. Remedy this by tightening
the adapter on the injector and observe if there is an improvement.
8. Adjust the pressure until the Aux pressure is maintained at about 1.5 psig
below the required column inlet pressure. Wait a few minutes for the system to
stabilize to ensure that no further changes are required.
9. Open Valve 3 and set the Aux 1 pressure to the required column inlet pressure;
for example, 1.5 psig higher than the Aux 1 reading established in step 9 above.
This ensures a positive gas flow through the Aux 1 supply to the mid-point tee.
CAUTION
Valve 3 MUST remain open (ON) during PreVent
operation.
7-25
Prevent
Condition the system to ready it for an analysis.
G.
Condition the System
1. Write down the pressures established for Press 1 and Aux 1 in step F.
2. Set Press 1 to 2 psig, Split 1 to 100 mL/min, and Aux 1 to 80 psig.
•
If you are using a PSS, set its temperature to the maximum
programmed temperature.
•
Set the oven to the maximum programmed temperature.
•
Allow the system to bake at this temperature for several hours 
overnight if possible.
•
Shorter conditioning times may be possible, but that depends on
the condition of the PreVent components and condition of the
column.
3. Cool the oven (and if you are using a PSS injector, cool the injector).
4. Reset the initial settings of Press 1 and Aux 1.
The system is now ready to run an analysis.
7-26
Clarus 500 GC Hardware Guide
Installing PreVent on a Detector
This section describes how to install PreVent on a detector (except for
TurboMass MS). The next section describes how to install PreVent on
TurboMass MS.
Summary
The following steps summarize how to install a PreVent adapter to a detector and
make it ready for an analysis:
A. Install the restrictor in the PreVent adapter.
B. Connect the PreVent adapter to the detector.
C. Connect the column to the PreVent adapter to the detector.
D. Leak-check the system.
E. Connect the column to the injector.
F. Set the initial pressures.
G. Condition the system.
A.
Install the Restrictor in the PreVent Adapter
1. Cut the 0.075 mm i.d. restrictor (Part No. N610-3081) to the proper
length for your detector. Refer to the following table:
7-27
Prevent
Table 7-1. Recommended Restrictor Lengths for Detectors
Detector to which you are attaching
the adapter
Restrictor Length
PID
195 mm (7.66 inches)
TCD
163 mm (6.40 inches)
FID
137 mm (5.38 inches)
2
124 mm (4.87 inches)
ElCD
150 mm (5.89 inches)
NPD
137 mm (5.38 inches)
FPD
163 mm (6.40 inches)
ECD
2. Insert a 1/8-inch graphite ferrule over one end of the restrictor tubing.
3. Insert the end of the restrictor tubing into the top of the PreVent detector
adapter (Part No. N610-0329).
4. Feed the restrictor tubing through the PreVent adapter until 5 mm
protrudes through the column connection on the bottom.
2
A glass-lined receiver (P/N N600-0968) is available to reduce high background readings.
7-28
Clarus 500 GC Hardware Guide
Figure 7-10. Installing the restrictor in the PreVent detector adapter.
B.
Connect the PreVent Adapter to the Detector
1. Carefully connect the PreVent adapter by screwing the detector end of
the adapter into the detector fitting until it is finger tight.
2. Using a 7/16-inch wrench, tighten the PreVent adapter until the graphite
ferrule just starts to tighten on the restrictor.
3. Locate the stainless steel tubing (that supplies the mid-point pressure)
inside the oven.
4. Insert a 1/16-inch nut (Part No. 0990-3392) and a graphite/Vespel ferrule
(Part No. 0992-0107) over the end of this tubing.
5. Measure and mark the tubing 1/2-inch from the back of the nut.
6. Insert the tubing into side arm on the PreVent adapter, keeping the mark
just behind the nut. Then tighten the nut and ferrule fingertight.
7-29
Prevent
7. Make a leak-free seal by tightening the PreVent adapter on the detector
fitting another 1/4 to 1/2 turn.
Figure 7-11. Location of the detector fitting.
C.
Connect the Column to the PreVent Adapter
1. Place the column on the hanger so that no part of the column touches the
bottom or sides of the oven.
2. Insert a 1/16-inch extended nut (Part No. 0990-3392, pkg. of 5), a
graphite/Vespel ferrule (1/16-inch x 0.5 mm Part No. 0992-0105, pkg. of
10 for 0.25/0.32 i.d. column or a 1/16-inch x 0.8 mm Part No. 09920107, pkg of 10 for a 0.53 mm i.d. column), and a spacer (Part No.
N610-3079) over one end of the column.
CAUTION
7-30
Do not use a graphite ferrule since it will extrude up into
the body of the PreVent adapter.
Clarus 500 GC Hardware Guide
Figure 7-12. Extended nut, graphite/Vespel ferrule, and spacer.
3. Cut about 1 cm (3/8 inch) from the end of the column tubing using a wafer
scribe (Part No. N930-1386, pkg. of 10 scribes) or other column cutting tool.
Break off the tubing at the score mark making sure that the break is clean and
square. Examine the cut with a magnifying glass and compare it to the
following figure:
Figure 7-13. Example of a good tubing cut and bad cuts.
4. Insert the column end into the hourglass guide (Part No. N610-3082).
5. Align the end of the restrictor tubing that protrudes from the PreVent adapter
with the open end of the hourglass guide. Then carefully push the hourglass
guide, with the attached column, up into the PreVent adapter as shown in the
following figure. Notice that the restrictor tubing fits inside the column.
7-31
Prevent
NOTE: Slightly twist the column as you push the hourglass guide into the PreVent
adapter.
6. Loosely tighten the column nut.
7. Carefully push the column up into the PreVent adapter until it bottoms in the
detector. Then pull the column back 3 mm.
8. Use two 1/4-inch wrenches to tighten the nut. DO NOT OVERTIGHTEN
THE NUT!
Figure 7-14. Connecting a column to the PreVent detector adapter.
7-32
Clarus 500 GC Hardware Guide
D. Leak-Check the System
1. Turn on the Clarus 500 GC. When the Clarus 500 GC is turned on, it is set to
the initial default settings.
2. From the System Status screen touch the injector to get to the following
screen. Turn the detector temperature off.
3. From the Events tab turn off the mid-point carrier gas supply by opening
Valve 3.
7-33
Prevent
4. Allow the system to equilibrate for several minutes, then view the Aux 1
pressure, view the Aux Gas button and view the current psig.
7-34
Clarus 500 GC Hardware Guide
5. Go back to the inject screen to view the pressure read out on the carrier gas
which should be at 0 psig.
7-35
Prevent
6. After approximately 5 minutes, if no leaks exist, the Aux 1 reading should be
stable at approximately 75 psi. If it is low, then leak-check the fitting
connections.
7. If you suspect a leak, test the connections for leaks using a 50/50 mixture of
isopropanol/water or an electronic leak detector. To prevent contaminating the
system, DO NOT use a soap solution for leak testing. Tighten all leaking
connections.
If you detect a leak, check and tighten the fittings on the mid-point pressure tee
and/or the connections on the rear of the Clarus 500 GC.
CAUTION
E.
Do not overtighten the column nut. If this fitting has a
persistent leak, replace the graphite/Vespel ferrule.
Connect the Column to the Injector
CAUTION
Make certain that no part of the column touches the walls
or bottom of the oven.
1. Insert a 1/16-inch extended nut (Part No. 0990-3392, pkg. of 5) and
graphite/Vespel ferrule (1/16-inch x 0.5 mm Part No. 0992-0105,
pkg. of 10 for 0.25/0.32 i.d. column or a 1/16-inch x 0.8 mm Part No.
0992-0107, pkg of 10 for a 0.53 mm i.d. column) over one end of the
column.
7-36
Clarus 500 GC Hardware Guide
Figure 7-15. Extended nut and graphite/Vespel ferrule.
2. Cut about 1 cm (3/8 inch) from the end of the column tubing using a
wafer scribe (Part No. N930-1386, pkg of 10 scribes) or other
column cutting tool. Break off the tubing at the score mark making
sure that the break is clean and square. Examine the cut with a
magnifying glass and compare it to the following figure:
Figure 7-16. Example of a good column cut and bad cuts.
3. Position the column nut on the column so that the back of the nut is
4.4 cm to 5.1 cm (1 3/4 inches to 2 inches) from the end of the
column for the CAP injector.
or
Position the column nut on the column so that the back of the nut is 1
1/2 inches to 1 3/4 inches from the end of the column for the PSS
injector.
7-37
Prevent
4. Using typewriter "white out" or a felt-tipped pen, make a mark on
the column just beyond the back edge of the column nut (see Figure
6-10).
CAUTION
To avoid contaminating the system, make certain that
the nut and ferrule do not contact the mark on the
column.
5. Locate the capillary injector fitting inside the oven.
Refer to the following figures to connect the column to the Cap or PSS
injector.
CAUTION
CAUTION
7-38
The injector terminates in a 1/16-inch fitting. This
fitting is fragile. To preserve the integrity of the fitting,
carefully connect the nut to prevent cross-threading the
fitting and/or overtightening the nut on the fitting. You
can also preserve the integrity of the fitting by allowing
the injector to cool before connecting a nut.
Do not overtighten column nuts. Overtightening can
cause damage to the ferrule and/or column.
Clarus 500 GC Hardware Guide
Figure 7-17. Capillary column attached to a CAP injector fitting.
Figure 7-18. Capillary column attached to PSS injector fitting.
F.
Set the Initial Pressures
To set the mid-point pressure:
7-39
Prevent
1. From the System Status screen select either A or B injector (the example here
shows the B cap injector ready for setting the carrier gas).
2. In the following window touch the Program Graph screen under the Carrier
Gas field.
7-40
Clarus 500 GC Hardware Guide
3. Using the plus and minus buttons enter the initial value of 30 psig for the
Carrier gas. Press Close to go back to the previous screen (as seen in step 2).
4.
In the Events tab touch the Split event and then press Edit. Set Split 1 to 100
mL/min.
7-41
Prevent
5. From the oven tab set the oven temperature to its highest programmed
temperature.
6. From the Events tab turn off the mid-point carrier gas supply by closing
Valve 3.
7-42
Clarus 500 GC Hardware Guide
7. Allow the system to equilibrate for several minutes, then view the Aux 1
pressure, view the Aux Gas button and view the current psig.
Note: If the Aux 1 pressure is very low, then the graphite ferrule that holds the
restrictor inside the PreVent adapter may be leaking. Remedy this by tightening
the adapter on the injector and observe if there is an improvement.
8. Adjust the pressure until the Aux pressure is maintained at about 1.5 psig
below the required column inlet pressure. Wait a few minutes for the system to
stabilize to ensure that no further changes are required.
9. Open Valve 3 and set the Aux 1 pressure to the required column inlet pressure;
for example, 1.5 psig higher than the Aux 1 reading established in step 9 above.
This ensures a positive gas flow through the Aux 1 supply to the mid-point tee.
CAUTION
Valve 3 MUST remain open (ON) during PreVent
operation.
7-43
Prevent
Condition the system to ready it for an analysis.
G.
Condition the System
1. Write down the pressures established in step F
for Press 1 and Aux 1.
2. Set Press 1 to 2 psig, Split 1 to 100 mL/min, and Aux 1 to 80 psig.
3. If you are using a PSS, set its temperature to the maximum programmed
temperature. Set the oven to the maximum programmed temperature.
4. Allow the system to bake for several hours  overnight if possible.
Shorter conditioning times may be possible, but that depends on the condition
of the PreVent components and condition of the column. Cool the oven (and if
you are using a PSS injector, cool the injector.)
5. Reset the initial settings of Press 1 and Aux 1.
The system is now ready to use for an analysis.
7-44
Clarus 500 GC Hardware Guide
Installing PreVent on a TurboMass MS
Detector
This procedure describes how to install PreVent on a TurboMass MS (TMMS)
detector.
Summary
The following steps summarize how to install a PreVent injector adapter to a
TMMS detector and make it ready for an analysis:
A. Prepare the TMMS
C. Install the restrictor in the TMMS Transfer Line.
D. Install the PreVent injector adapter.
E. Connect the column to the PreVent injector adapter.
F. Connect the Transfer Line to the TMMS
G. Leak-check the system.
H. Connect the column to the injector.
I.
Set the initial pressures.
J.
Condition the system
A.
Prepare the TMMS
1. Install the TMMS and Clarus 500 GC according to the instructions
given in the TurboMass Mass Spectrometer and Clarus 500 GC
installation manuals.
2. If a column is installed, cool the Gas Chromatograph oven, the
TMMS ionizer and the TMMS transfer line to ambient temperature.
Vent the detector and remove the column from the transfer line.
7-45
Prevent
Figure 7-19. Preparing the TurboMass Mass Spectrometer.
7-46
Clarus 500 GC Hardware Guide
B. Install the PreVent Injector Adapter in the TMMS
Transfer Line
1. Cut a 40cm length of the 0.075mm i.d. fused silica tubing (Part No. 6103081). Make sure that the two ends are cut clean and square. Wipe the
outside of the tubing with a tissue dampened with methanol.
2. Feed the fused silica tubing through the PreVent injector adapter (Part No.
N610-0328) and a graphitized Vespule ferrule (Part No. 0992-0105) as
shown in the following figure.
Fuse silica tubing
(P/N 610-3081)
Ferrule
(P/N 0992-0105)
PreVent Injector Adapter
(P/N N610-0328)
Figure 7-20. Feeding the fused silica tubing throught the injector adapter.
3. Introduce the fused silica tubing into the TMMS transfer line until it reaches
a stop. Loosely screw the PreVent adapter onto the 1/16” threaded union at
the end of the TMMS transfer line as shown in the following figure.
7-47
Prevent
Figure 7-21. Normal connection of column to TurboMass transfer line.
4. Withdraw the fused silica tubing by about 5mm and using two 1/4 inch
wrenches tighten up the PreVent adapter on the union at the end of the
TMMS transfer line.
5. Cut the fused silica tubing so that about 7mm is exposed beyond the PreVent
adapter as shown in the following figure. The cut should be clean and square.
CAUTION
7-48
Take care when working near the exposed end of the fused
silica tubing. It can be easily broken off.
Clarus 500 GC Hardware Guide
Figure 7-22. Example of a good column cut and bad cuts.
Refer to the following figure as you perform the following procedure.
6. Locate the stainless steel tubing (that supplies the mid-point pressure) inside
the oven.
7. Insert a 1/16-inch nut (Part No. 0990-3392) and a graphite/Vespel ferrule
(Part No. 0992-0107) over the end of this tubing.
8. Measure and mark the tubing 1/2-inch from the back of the nut.
9. Insert the tubing into side arm on the PreVent adapter, keeping the mark just
behind the nut. Then tighten the nut and ferrule fingertight.
10. Make a leak-free seal by using a two 1/4-inch wrenches to tighten the
PreVent adapter on to the union another 1/4 to 1/2 turn.
C.
Connect the Column to the PreVent Injector
Adapter
1.
Place the column on the hanger so that no part of the column touches the
bottom or sides of the oven.
2.
Insert a 1/16-inch extended nut (Part No. 0990-3392, pkg. of 5) a
graphite/ Vespel ferrule (Part No. 0992-0105, pkg. of 10), and a spacer
(Part No. N610-3079) over one end of the column.
7-49
Prevent
CAUTION
Do not use a graphite ferrule since it will extrude up into the body
of the PreVent adapter.
Figure 7-23. Extended nut, graphite/Vespel ferrule, and spacer.
3.
Cut about 1 cm (3/8 inch) from the end of the column tubing using a
wafer scribe (Part No. N930-1386, pkg. of 10 scribes) or other column
cutting tool. Break off the tubing at the score mark making sure that the
break is clean and square. Examine the cut with a magnifying glass and
compare it to the following figure:
Figure 7-24. Example of a good tubing cut and bad cuts.
4.
7-50
Insert the column end into the hourglass guide (Part No. N610-3082).
Clarus 500 GC Hardware Guide
5.
Align the end of the restrictor tubing that protrudes from the PreVent
adapter with the open end of the hourglass guide. Then carefully push the
hourglass guide, with the attached column, into the PreVent adapter as
shown in the following figure, step 2. Notice that the restrictor tubing fits
inside the column.
NOTE: Slightly twist the column as you push the hourglass guide into the PreVent
adapter.
6.
Loosely connect the column nut to the PreVent adapter.
7.
Carefully push the column up and into the PreVent adapter until it
bottoms in the adapter. Then pull the column back 3 mm.
8.
Use two 1/4-inch wrenches to tighten the nut. DO NOT
OVERTIGHTEN THE NUT!
7-51
Prevent
Figure 7-25. Connecting a column to the PreVent adapter in a TMMS
system.
D.
Connect the Transfer Line to the TMMS
Install the PreVent device into the TurboMass .as shown in Figure 7-26.
Take the PreVent ‘injector’ T-piece and screw it onto the 1/16” fitting at the end
of the standard TurboMass transfer line. Be sure the fused silica restrictor is
inserted through it, through the heated transfer line and directly into the
TurboMass ion source.
7-52
Clarus 500 GC Hardware Guide
Ensure that the end of the restrictor is exposed beyond the T-piece to enable the
column to be threaded over it with the aid of an hourglass guide. Figures 7-27
through 7-29 show details of the installation.
Figure 7-31 shows a detail of the column-restrictor interface. Because the
restrictor is inserted directly into the end of the capillary column, there are no
issues with active sites or dead volumes. Therefore an optimum chromatographic
performance is assured.
Figure 7-26. Diagram showing PreVent device installed into the TurboMass
detector (The TuboMass is the figure on the left and the Clarus 500 GC is
the figure on the right).
7-53
Prevent
Figure 7-27. Column is detached and PreVent adapter is attached to
TurboMass transfer line with fused silica restrictor pushed through into
ionizer.
7-54
Clarus 500 GC Hardware Guide
Figure 7-28. Restrictor is sealed within adapter with end protruding.
Midpoint gas supply is connected to port on adapter.
7-55
Prevent
Figure 7-29. Hourglass guides restrictor into capillary column
7-56
Clarus 500 GC Hardware Guide
Figure 7-30. Installation completed.
7-57
Prevent
midpoint gas
fused silica
restrictor
‘hour-glass’
insert
column
TurboMass
transfer line
PreVent
adapter
Figure 7-31. Detail of column-restrictor interface at end of TurboMass
transfer line.
•
Once installed, this PreVent configuration will allow the capillary
column to be back-flushed and so offers the following benefits:
•
Allows injector maintenance without having to cool or vent the vacuum
on the mass spectrometer.
•
Allows a degraded section of column to be removed from its inlet
without the need to cool or pump-down the detector.
•
Facilitates easier column replacement.
•
Reduces risk of air entering the detector in the event of a leak or column
breakage.
7-58
Clarus 500 GC Hardware Guide
•
Prevents column bleed from entering the detector while conditioning or
when the system is idle.
•
Allows the injector liner and quartz wool packing to be deactivated insitu.
•
Reduces analysis times by eliminating the need for extensive temperature
programming to elute unwanted less volatile sample residue from the
column.
•
Increases the life of a column by eliminating temperature programming
completely.
•
Removes the potential of contaminants before they reach the detector.
It will also have the added benefit of maintaining a constant flow of carrier gas
into the MS detector in both forward flow and backflush modes during
temperature programming.
E.
Leak-Check the System
1
Turn on the Clarus 500 GC. When the Clarus 500 GC is turned on, it is set to
the initial default settings.
2
From the System Status screen touch the injector to get to the following
screen. Touch the numeric field until it turns black and use the plus minus
buttons to get the proper split flow of 100 and a ratio of 100.
7-59
Prevent
3.
7-60
Select Valve 3 (or valve 4 if PreVent is installed in channel 2) from the
Event drop down menu.
Clarus 500 GC Hardware Guide
4. Allow the system to equilibrate for several minutes, then view the Aux
1 pressure, view the Aux Gas button and view the current psig.
5.
Go back to the inject screen to view the pressure read out on the carrier
gas which should be at 0 psig.
7-61
Prevent
6. Set the injector pressure to 75 psig.
7. After approximately 5 minutes, if no leaks exist, the Aux 1 reading should be
stable at approximately 75 psi. f it is low, then leak-check the fitting
connections.
8. If you suspect a leak, test the connections for leaks using a 50/50 mixture of
isopropanol/water or an electronic leak detector. To prevent contaminating the
system, DO NOT use a soap solution for leak testing. Tighten all leaking
connections.
If you detect a leak, check and tighten the fittings on the mid-point pressure tee
and/or the connections on the rear of the Clarus 500 GC.
CAUTION
F.
Connect the Column to the Injector
CAUTION
1.
7-62
Do not overtighten the column nut. If this fitting has a
persistent leak, replace the graphite/Vespel ferrule.
Make certain that no part of the column touches the walls
or bottom of the oven.
Insert a 1/16-inch extended nut (Part No. 0990-3392, pkg of 5) and
graphite/ Vespel ferrule (Part No. 0992-0105, pkg of 10) over one end of
the column.
Clarus 500 GC Hardware Guide
Figure 7-32. Extended nut and graphite/Vespel ferrule.
2.
Cut about 1 cm (3/8 inch) from the end of the column tubing using a
wafer scribe (Part No. N930-1386, package of 10 scribes) or other
column cutting tool. Break off the tubing at the score mark making sure
that the break is clean and square. Examine the cut with a magnifying
glass and compare it to the following figure:
Figure 7-33. Example of a good column cut and bad cuts.
3.
Position the column nut on the column so that the back of the nut is
4.4 cm to 5.1 cm (1 3/4 inches to 2 inches) from the end of the column
for the CAP injector.
or
Position the column nut on the column so that the back of the nut is 1 1/2
inches to 1 3/4 inches from the end of the column for the PSS injector.
4.
Using typewriter "white out" or a felt-tipped pen, make a mark on the
column just beyond the back edge of the column nut.
7-63
Prevent
CAUTION
5.
Locate the capillary injector fitting inside the oven. Refer to the
following figures to connect the column to the Cap or PSS injector.
CAUTION
CAUTION
7-64
To avoid contaminating the system, make certain that the nut
and ferrule do not contact the mark on the column.
The injector terminates in a 1/16-inch fitting. This fitting is
fragile. To preserve the integrity of the fitting, carefully
connect the nut to prevent cross-threading the fitting and/or
overtightening the nut on the fitting. You can also preserve the
integrity of the fitting by allowing the injector to cool before
connecting a nut.
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
Clarus 500 GC Hardware Guide
Figure 7-34. Capillary column attached to a CAP injector fitting.
Figure 7-35. Capillary column attached to PSS injector fitting.
G.
Set the Initial Pressures
1. From the System Status screen select the oven icon.
7-65
Prevent
2.
Set the oven to the lowest programmed temperature.
3. Set the TMMS transfer line to its operating temperature.
7-66
Clarus 500 GC Hardware Guide
4. From the Events tab turn off the mid-point carrier gas supply by closing
Valve 3.
5. Start the TMMS vacuum
6. See the gas pressure to 30 psi.
7-67
Prevent
Note:
If the aux 1 pressure is very low, then the graphite ferrule that holds the
restrictor inside the PreVent adapter may be leaking. Remedy this by tightening
the adapter on the injector and observe if there is an improvement.
7. Adjust the pressure until the Aux pressure is maintained at about 1.5
psig below the required column inlet pressure. Wait a few minutes for
the system to stabilize to ensure that no further changes are required.
8. Open Valve 3 and set the Aux 1 pressure to the required column inlet
pressure; for example, 1.5 psig higher than the Aux 1 reading
established in step 9 above. This ensures a positive gas flow through the
Aux 1 supply to the mid-point tee.
CAUTION
7-68
Valve 3 MUST remain open (ON) during PreVent
operation.
Clarus 500 GC Hardware Guide
Condition the system to ready it for an analysis.
H.
Condition the System
1.
Write down the pressures established for Press 1 and Aux 1 in step I.
2.
Set Press 1 to 2 psig, Split 1 to 100 mL/min, and Aux 1 to 80 psig.
3.
Set oven to maximum programmed temperature.
If you are using a PSS, set its temperature to the maximum programmed
temperature.
4.
Allow the system to bake for several hours  overnight if possible.
Shorter conditioning times may be possible, but that depends on the
condition of the PreVent components and condition of the column.
5.
Cool the oven (and if you are using a PSS injector, cool the injector.)
6.
Reset the initial settings of Press 1 and Aux 1.
The system is now ready to use for an analysis.
I.
Replacing the Restrictor
To replace a restrictor in the PreVent injector or detector adapter:
1.
Turn off the Clarus 500 GC oven and detector and wait until they are
cool to the touch.
2.
Turn off all gases.
3.
Using a 1/4-inch wrench, remove the 1/16-inch column nut and the
column from the PreVent adapter.
4.
Using two 1/4-inch wrenches, remove the nut and mid-point pressure
line from the side arm of the PreVent adapter.
7-69
Prevent
5.
Using the appropriate wrenches, remove the PreVent adapter from either
the injector or detector.
•
Use two 1/4-inch wrenches to remove the PreVent adapter from the
injector fitting.
•
Use two 7/16-inch wrenches to remove the PreVent adapter from the
detector fitting.
6. Insert a 1/16-inch rod (Part No. N610-T100) in the column connection end of
the PreVent adapter and push the restrictor tubing and ferrule of the injector
end.
7. Install a new restrictor by referring to the appropriate procedure in this
chapter.
Figure 7-36. Removing a restrictor from a PreVent adapter.
7-70
Clarus 500 GC Hardware Guide
PreVent Operating Techniques
Summary of the PreVent Techniques
Table 7-3 summarizes the various PreVent techniques and the hardware
configurations that support them.
•
Column Isolation
•
Solvent Purge
•
Large Volume Injection
•
Sample Residue Purge
•
Time Saver
Table 7-3. Summary of PreVent Techniques and Supporting Configurations
Technique
Split/Splitless
PSS
Column Isolation
Yes
Yes
Solvent Purge
No
Yes
Large Volume
No
Yes
Injection
Sample Residue Purge
No
Yes
Time Saver
Yes
Yes
* Cannot be used while chromatography is in progress
** Not recommended
Restrictor in
Injector
Yes
Yes
Yes
Restrictor
in Detector
Yes*
Yes
Yes
Yes**
No
Yes
Yes
Table 7-3 demonstrates the advantage of the PSS injector over the conventional
Split/Splitless injector in that all the PreVent techniques are supported by this one
injector. Several of these techniques are possible with a single restrictor
configuration. If a different configuration is required, changing the restrictor type
is a simple operation requiring only a few minutes to perform.
7-71
Prevent
Column Isolation Technique
This technique uses the Injector Restrictor Configuration to fully isolate the
chromatographic column from actions occurring within the injector. Figures 7-37
and 7-38 illustrate the principle.
For sample introduction, the inlet pressure (P1) is set up to be higher than the
mid-point pressure (P2). P1 and P2 are set as described in “Installing PreVent on
the Injector” in this chapter. P2 represents the pressure at the column inlet.
Carrier gas will now flow from the injector, through the restrictor and into the
column, carrying the vaporized sample with it. The sample may be injected
manually using a standard syringe or by autosampler. The injection temperature
and split vent operation are set as for normal split or splitless injection
techniques. The pressures are not adjusted until the injector needs to be isolated.
To isolate the column, Press 1 (P1) is simply reduced to below that of Aux 1 (P2)
causing the carrier gas to flow backwards from the mid-point ‘T’, through the
restrictor, into the injector and out through the split vent. It is important to
ensure that the split vent is open (for example, 50 mL/min) during this step or the
technique will not work.
Split Vent Control (Open or Closed)
F
Injector
Detector
Restrictor
FLOW
Chromatographic Column
P1
Press 1
(20 psig)
P2
Aux 1
(14 psig)
Figure 7-37. Normal operation.
7-72
Clarus 500 GC Hardware Guide
Split Vent Control (50 ml/min)
F
Injector
Detector
Restrictor
FLOW
Chromatographic Column
P1
P2
Press 1
(1 psig)
Aux 1
(14 psig)
Figure 7-38. Column Isolation Mode.
P1 should not be turned off completely, but to a level (for example, 1.0 psig) that
maintains forward flow of carrier gas through the liner to prevent the build-up of
contamination within the liner while the restrictor is being backflushed and also
to maintain a purge flow out of the injector inlet while it is being serviced with
the septum cap removed. The reduction in P1 is not normally included as a timed
event in the Clarus 500 GC method as this will not be routinely adjusted during
each run.
The Column Isolation Mode can be used to support the following actions:
•
Septum exchange and conditioning even during chromatography
•
Liner exchange and conditioning even during chromatography
•
In situ chemical deactivation of the liner even during chromatography
•
Column and detector protection while the instrument is idle
7-73
Prevent
Column Isolation Mode is also possible with the restrictor fitted to the detector as
shown in Figures 7-39 and 7-40. In this instance, however, chromatography is
not possible during column isolation although it now would be possible to
condition a column without the effluent reaching the detector.
Split Vent Control (Open or Closed)
F
Chromatographic Column
Injector
Detector
Restrictor
FLOW
P1
P2
Aux 1
Press 1
(20 psig)
(6 psig)
Figure 7-39. Normal operation.
Split Vent Control (50mL/min)
F
Chromatographic Column
Detector
Injector
Restrictor
FLOW
P1
P2
Press 1
Aux 1
(1 psig)
(6 psig)
Figure 7-40. Alternative Column Isolation Mode.
7-74
Clarus 500 GC Hardware Guide
Solvent Purge Technique
This technique uses the ability of the PSS injector to rapidly change its liner
temperature according to a user-defined program. Figure 7-41 shows how this
ability can be used to remove the solvent from the liner and selectively transfer
the less-volatile sample analytes to the column. This technique is best suited to
splitless injections of low volatility analytes. While the solvent is being purged
from the liner, there is still forward flow into the column and so some of the
solvent will still enter the column (and hence the detector). The PreVent system,
configured as for the Column Isolation Mode may be used to prevent all traces of
the solvent entering the column during the purge process by reversing the flow of
carrier gas at the injector column port.
3
2
1
Step 1 : Sample injected into cool liner
Step 2 : Solvent and other volatile components swept from cool liner and out of split vent
Step 3 : Liner heated and the vaporized residue swept into column
Figure 7-41. Using the PSS to eliminate solvent from the column.
Table 7-4 shows typical entries that would be made in a method to enable a 1minute solvent purge at 100 mL/min and 50 °C. Actual settings will depend
upon the type and volume of solvent involved. The initial settings for P1 and P2
7-75
Prevent
are established as described in this chapter. The column oven is programmed as
for normal splitless injection except that the temperature is not raised until after
the solvent purge step is complete.
Table 7-4. Typical Method for Solvent Purge Technique
Time
INITIAL
INITIAL
INITIAL
INITIAL
Event
SPLIT 1 (F) = 100 mL/min
PSS = 50 °C
AUX 1 (P2) = 14 psig
PRESS 1 (P1) = 2 psig
1.00
SPLIT 1 (F) = OFF
1.01
PRESS 1 (P1) = 20 psig
1.02
2.00
PSS = 350 °C
SPLIT = 50 mL/min
Comment
Purge flow rate.
Purge temperature.
Mid-point pressure at column inlet.
Pressure in injector lower than midpoint to keep solvent out of column.
Close split vent to transfer everything
to column.
Raise injector pressure so carrier gas
flows from liner to column.
Heat liner to vaporize sample residue.
Finally open split vent to clean liner for
next run.
The Solvent Purge Technique may be used to support the following actions:
•
Elimination of peak distortion caused by solvent flooding effects as a
result of excess liquid solvent entering the column and becoming
fractionated by the carrier gas flow
•
Elimination of hostile solvents from sensitive columns and detectors
•
Large volume injections - (See Large Volume Injections below.)
Large Volume Injections (LVI)
The Solvent Purge Technique can also be used to support LVI applications of the
PSS injector. The PSS must be used with a 2-mm i.d. liner which is firmly
packed with glass wool. A large volume of liquid sample (up to 100 µl - a 50-µl
syringe is available for the autosampler) may be injected into the liner which
must be kept at a low temperature to prevent (very) explosive vaporization. The
solvent is purged out of the split vent as for the Solvent Purge Technique. The
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Clarus 500 GC Hardware Guide
purge time and flow rate need to be sufficient to remove all of the solvent (for
example, about 100-200 mL of purge gas is needed to remove 50 µl of n-hexane
at 50 °C). Extended purge times may result in the loss of some of the analytes
and so this technique is only suitable for low volatility compounds (for example,
lower than n-decane). Typical method entries are given in Table 7-5.
Table 7-5. Typical Method for LVI Technique
Time
INITIAL
INITIAL
INITIAL
INITIAL
Event
SPLIT 1 (F) = 100 mL/min
PSS = 50 °C
AUX 1 (P2) = 14 psig
PRESS 1 (P1) = 2 psig
2.00
SPLIT 1 (F) = OFF
2.01
PRESS 1 (P1) = 20 psig
2.02
3.00
PSS = 350 °C
SPLIT = 50 mL/min
Comment
Purge flow rate.
Purge temperature.
Mid-point pressure at column inlet.
Pressure in injector lower than mid-point
to keep solvent out of column.
Close split vent to transfer everything to
column.
Raise injector pressure so carrier gas
flows from liner to column.
Heat liner to vaporize sample residue.
Finally open split vent to clean liner for
next run.
Sample Residue Purge Technique
The separation described under the Solvent Purge Mode can be reversed so that
the volatile sample content enters the column and heavy (unwanted) low
volatility sample residue left in the liner can be purged out through the split vent.
This technique works best with the detector restrictor PreVent configuration so
that the traces of low volatility material that do leave the liner can be backflushed
from the column (see next Section). Use of the injector restrictor configuration
will not prevent some of the low-volatility material from entering the column
during the purge process. The figure below illustrates the separation process
inside the PSS liner.
7-77
Prevent
3
2
1
Step 1 : Sample injected into cool liner
Step 2 : Volatile components swept from cool liner into column
Step 3 : Liner heated and most of the residue swept out of split vent
Figure 7-42. Using the PSS to eliminate low volatility sample material from
the column.
The figures below illustrate how the PreVent system backflushes the heavier
sample from the column. For further details on column backflushing refer to the
“Time Saver Technique” Table 7-6 lists some typical entries in a method for the
Sample Residue Purge technique. The initial settings for P1 and P2 are
established as described in this chapter. Split or splitless injection with either a
split/splitless or PSS injector is possible and the oven temperature program is set
as for normal chromatography.
This technique is useful for the determination of volatile components in heavy
oils, natural extracts, etc.
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Clarus 500 GC Hardware Guide
Split Vent Control (Open or Closed)
F
Chromatographic Column
Detector
Injector
Restrictor
FLOW
P1
P2
Press 1
Aux 1
(20 psig)
(6 psig)
Figure 7-43. Injection and chromatography.
Split Vent Control (100 ml/min)
F
Chromatographic Column
Detector
Injector
Restrictor
FLOW
P1
P2
Press 1
Aux 1
(1 psig)
(80 psig)
Figure 7-44. Column backflush.
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Prevent
Table 7-6. Typical Method for Sample Residue Purge Technique
Time
INITIAL
INITIAL
INITIAL
INITIAL
Event
SPLIT 1 (F) = 100 mL/min
PSS = 200 °C
AUX 1 (P2) = 14 psig
PRESS 1 (P1) = 20 psig
2.00
SPLIT 1 (F) = 100 mL/min
20.00
PRESS 1 (P1) = 5 psig
20.01
AUX 1 (P2) = 80 psig
20.02
PSS = 450 °C
Comment
Injection split flow (can use splitless).
Injection temperature.
Mid-point pressure at column inlet.
Pressure in injector higher than mid-point
to allow sample into column.
Open split vent (if not already) to reduce
the amount of further sample entering
column.
When last peak of interest has eluted,
reduce inlet pressure...
and increase mid-point pressure to
backflush any sample material left in
column.
Heat liner to bake out any sample residue
and purge it out of the split vent.
Time Saver Technique
The PreVent system is able to support the classical, single-column, backflush
technique. The use of PPC pneumatics enables the backflush conditions to be
optimized for rapid backflush of unwanted sample material after the last peak of
interest has eluted. The initial settings for P1 and P2 are established as described
in this chapter. Split or splitless injection with either a split/splitless or PSS
injector is possible and the oven temperature program is set as for normal
chromatography. When the last peak of interest has eluted, the split vent is
opened, P1 is reduced and P2 is increased. Any sample material left in the
column is rapidly backflushed even at low oven temperatures eliminating the
need, in many instances, for temperature programming.
This technique is suitable for the determination of components in any sample
where there is unwanted low-volatility material entering the column. By reducing
the need for temperature programming to remove such material, it reduces the
analysis time and protects the column by not exposing it to high temperatures.
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Table 7-7. Typical Method for Column Backflush Technique
INITIAL
INITIAL
INITIAL
Event
SPLIT 1 (F) = 100 mL/min
AUX 1 (P2) = 14 psig
PRESS 1 (P1) = 20 psig
1.00
SPLIT 1 (F) = 100 mL/min
20.00
PRESS 1 (P1) = 5 psig
20.01
AUX 1 (P2) = 80 psig
Comment
Injection split flow (can use splitless).
Mid-point pressure at column inlet.
Pressure in injector higher than mid-point
to allow sample into column.
Open split vent (if not already) to allow
backflushed components to escape to
vent and help clean liner.
When last peak of interest has eluted,
reduce inlet pressure...
... and increase mid-point pressure to
backflush any sample material left in
column.
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PPC Fundamentals
8
PPC Fundamentals
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Clarus 500 GC Hardware Guide
Introduction
Programmed Pneumatic Control (PPC) is the electronic control of pressures and
flows for inlet, detector, and auxiliary gases. The PPC control modules regulate
pressures and flows using electronically driven variable flow restrictors. The
control modules also contain pressure and flow transducers to provide feedback
for complete monitoring. A PPC controller board drives the variable restrictors
on the control modules by comparing actual pressures and flows with setpoints
determined from user-entered values.
This chapter presents an overview of the concepts and use of Programmable
Pneumatic Control (PPC) of the Clarus 500 GC. In particular, it describes the
following microprocessor-controlled pneumatic functions that comprise PPC:
•
Carrier-gas flow, pressure, and linear-velocity programming
•
Split-flow and split-ratio control
•
Detector-gas flow control
•
Auxiliary-gas pressure and flow control
The following unique pneumatic devices make these control functions possible:
•
Carrier-gas mass-flow controller
•
split-pneumatic controller
•
Detector-gas flow controller
•
Auxiliary pressure controller
Pressure-readout module
You can combine one or more of these modules to create the control functions
required for a specific pneumatic configuration in the GC.
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PPC Fundamentals
A dedicated microprocessor control system reads all operating parameters from
— and sends control signals to — the pneumatic devices. This PPC controller
receives pneumatic setpoints, the ambient temperature, pressure, the oven
temperature, and GC status information from the main Clarus 500 GC processor.
The PPC controller sends back the pneumatic operating parameters and PPC
status information to the main GC processor.
The PPC controller accommodates up to eight flow controllers and/or twelve
pressure controllers, for a maximum of twelve installed PPC devices.
The main Clarus 500 GC processor accepts and stores method setpoints and
timed events for the configured PPC devices. In addition, the main Clarus 500
GC processor contains PPC functions that include calibration and setup utilities,
diagnostics, and fault-condition monitoring.
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Clarus 500 GC Hardware Guide
Carrier Gas Control
The type of primary PPC carrier gas modules and their operation depends on the
inlet (injector) option to which they are connected. For example, the packedcolumn inlet and the programmed-temperature on-column inlet (POC) use a
single carrier gas mass-flow controller plus a pressure-readout module. The
split/splitless (capillary) and programmed-temperature split/splitless (PSS) inlets
use a combination of a carrier gas mass-flow controller and a split-pneumatic
pressure controller. Other carrier-gas controllers may use auxiliary PPC zones
(see Auxiliary Carrier Gas Control).
Packed Column and Programmed-Temperature OnColumn Inlets
The PPC carrier gas mass-flow controller delivers a constant flow rate into a
column. The controller operates by increasing or decreasing the column head
pressure to maintain a constant mass-flow as the column temperature changes, or
if you use different columns. Its internal operation is similar to a conventional
mass-flow controller, but instead of utilizing a spring-and-diaphragm mechanism
for control, the PPC controller reads and sets the flow rate electronically. Unlike
a conventional controller, it constantly monitors the ambient room pressure, the
tank pressure, and the temperature of each flow module, and it compensates as
required to maintain a constant mass-flow output. The schematic in the following
figure illustrates the PPC mass-flow controller configuration for packed column
and POC inlets.
8-5
PPC Fundamentals
Figure 8-1 Schematic of packed column and POC pneumatics
Carrier Gas Mass-Flow Controller Operating Range
The carrier gas mass-flow controller for packed-column inlets has a nominal flow
range of 0 – 30 mL/min for helium carrier gas at 90 psig tank pressure. The
controller for the POC inlet has a range of 0 – 10 mL/min helium for capillary
column applications. The two controllers differ only in the installed flow-range
element (restrictor). By changing the flow-range element, you can use the same
controller in different Clarus 500 GC configurations. The adapter kit for packedcolumn installation of 0.53-mm i.d. capillary columns, for example, contains the
appropriate 0 – 10 mL/min element. After changing the flow-range element, you
must always recalibrate the flow controller.
Mass-Flow Controller Setup
The PPC system stores information about the type, location, and calibration of its
pneumatic devices in battery backed-up random access memory (BRAM). This
information is written into the BRAM during manufacturing. Normally, there is
no need to access or modify the type or location of the PPC controllers. If the
PPC hardware configuration is changed — by installing or removing PPC
devices — the operator must access the PPC connection menus on the Clarus 500
GC touch screen and modify the type and location of the PPC devices.
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Clarus 500 GC Hardware Guide
If the installed hardware does not match the stored configuration, the Clarus 500
GC issues a warning message.
CAUTION
Do not modify the PPC connection information if the PPC
hardware configuration has not changed.
Mass-Flow Controller Calibration
The carrier gas mass-flow controller is factory calibrated to a National Institute
of Standards and Technology (NIST) traceable standard with helium carrier gas;
however, it requires periodic calibration. Recalibration is required after changing
the flow-range element; otherwise the calibration frequency is up to the
individual operator. The controller accommodates changing the carrier gas (to
other than helium) by approximating a new set of calibration parameters based on
the new gas. The approximation is good but controller recalibration is
recommended for the best accuracy. It is good laboratory practice to recalibrate
all measuring and control devices periodically.
The mass-flow controller calibration procedure consists of specifying the
reference temperature and pressure; zeroing the internal sensors in the flow
controller with the tank pressure off; specifying the correct carrier gas type and
installing the correct flow-range element; measuring the background flow rate at
zero-flow with the tank pressure on; and measuring the flow rate at 60% of fullscale flow. This procedure is built into the Clarus 500 GC firmware.
Once the PPC is set up and calibrated you must configure it
Carrier Gas Mass-Flow Controller Configuration
Once the carrier gas mass-flow controller has been set up and calibrated for the
PPC system, you must configure its operating mode on the Clarus 500 GC
keypad. For packed-column and POC inlets the selections are Zero, Flow, or
Pressure.
8-7
PPC Fundamentals
1. From the System Status Screen touch the Tools button.
2. From the tools drop down menu select Configuration
3. In the Configuration touch screen touch the PPC icon
8-8
.
.
Clarus 500 GC Hardware Guide
4. In the PPC touch screen touch PPC Configure bar.
5. A popup warning appears, select OK.
8-9
PPC Fundamentals
6. On the Configure PPC Devices screen touch the Zero bar then touch OK to
set the gas flow to zero.
Headspace Analysis
Headspace analysis is the analysis of the vapor lying in equilibrium over a
solid/liquid sample in a sealed vial.
For practical headspace analysis the sample is sealed in a vapor tight vial, placed
in an thermostatted oven and heated to a pre-determined temperature.
The sample vial contains the volatile material in equilibrium between the
solid/liquid sample and the vapor lying over it.
After equilibrium is reached between solid/liquid phase and the vapor phase, a
defined amount of the vapor is taken and carried to the column in the gas
chromatograph for analysis. With this technique only highly volatile substances
reach the column, the non-volatile substances remain in the sample vial.
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Clarus 500 GC Hardware Guide
Using this technique, samples containing constituents which are unsuitable for
injection with a syringe can be analyzed (e.g. polymers, highly viscous liquids).
Suitable fields of application are in the analysis of polymers, certifying of the
volatile components in drinks and foodstuffs, blood alcohol levels, water and
environmental analysis.
For information on vacuum see the section on Vacuum Compensation later in
this chapter.
Capillary and Programmed Split/Splitless Inlets
A packed-column or POC inlet requires only a source of flow-controlled carrier
gas; however, split-type inlet systems are more complex. The capillary and
programmed-temperature split/splitless (PSS) inlets have identical split
pneumatics. The split pneumatics occupy two PPC control zones, one for column
inlet pressure control and one for split flow rate control.
Split Pneumatic Setup
The PPC system stores information about the type, location, and calibration of its
pneumatic devices in battery-backed-up random access memory (BRAM). This
information is written into the BRAM during manufacturing. Normally, there is
no need to access or modify the type or location of the PPC controllers. If the
PPC hardware configuration is changed — by installing or removing PPC
devices — you must access the PPC connection menus on the Clarus 500 GC
keypad and modify the type and location of the PPC devices. If the installed
hardware does not match the stored configuration, the Clarus 500 GC issues a
warning message.
CAUTION
Do not modify the PPC setup information if the PPC hardware
configuration has not changed.
8-11
PPC Fundamentals
Split Pneumatic Control
A split system such as the capillary or PSS inlet pneumatics controls three
parameters: the split flow, the inlet pressure, and the septum purge flow. See the
following figure that shows two diagrams showing the forward pressure mode
(splitless control) and the backpressure mode (split control) of the PPC split
pneumatics in the Clarus 500 GC.
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Clarus 500 GC Hardware Guide
Septum Purge
∆p
Controller
Temperature
Pressure
Regulator
∆p
Restrictor
Charcoal Trap
Flow
Monitor
∆p
Solenoid
Valve
(Closed)
Pressure Control
∆p
Ambient Pressure
Forward Pressure Mode (Splitless Control)
Septum Purge
∆p
Controller
Temperature
Pressure
Regulator
∆p
Restrictor
Charcoal Trap
Total Split Flow Control
∆p
Pressure Control
Solenoid
Valve
(Open)
∆p
Ambient Pressure
Backpressure Mode (Split Control)
Figure 8-2 Schematic of the split PPC pneumatics
8-13
PPC Fundamentals
Split Flow ─ A mass-flow controller supplies carrier gas to the split or PSS inlet
system. This is the same mass-flow controller used for packed or POC inlets, but
here it is used with a 0 – 300 mL/min flow-range element (fixed restrictor).
Carrier gas passes through the flow controller and into the inlet (injector) at the
connection labeled Carrier In. Some of the gas flows across the septum and out
the septum purge, while the rest flows down through the inlet liner. At the
bottom of the liner, a fraction of the carrier gas enters the column, and the
balance flows back up the outside of the liner and out the split vent. An electrical
solenoid valve provides positive split flow shutoff when required.
Inlet Pressure ─ A pressure transducer connected at the split vent (before the
charcoal trap) measures the inlet pressure at the head of the column. The inlet
pressure may range from 0 – 100 psig.
Septum Purge ─ A constant-flow device (fixed pressure regulator) regulates the
septum purge flow at approximately 3 mL/min, independently of the inlet
pressure. The regulator is preset in the factory; it is not adjustable.
Split Pneumatic Calibration
The split flow controller requires periodic calibration. The controller is factory
calibrated to a National Institute of Standards and Technology (NIST) traceable
standard with helium carrier gas. Recalibration is required upon changing the
flow-range element; otherwise, the calibration frequency is up to the individual
operator. The PPC controller accommodates changing the carrier gas to other
than helium by approximating a new set of calibration parameters based on the
new gas. The approximation is good but controller recalibration is recommended
for the best accuracy. It is good laboratory practice to recalibrate all measuring
and control devices periodically.
The calibration procedure consists of specifying the reference temperature and
pressure; zeroing the internal sensors in the flow controller with the tank pressure
off; specifying the flow-range element and carrier gas type; measuring the
background flow rate at zero-flow with the tank pressure on; and measuring the
flow rate at 60% of full-scale flow. This procedure is built into the Clarus 500
GC firmware.
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Clarus 500 GC Hardware Guide
Split Pneumatic Carrier Gas Configuration
Once the split pneumatic system has been set up and calibrated on the PPC
system you must configure its operating mode by using the Clarus 500 GC touch
screen. There are configuration choices for column carrier-gas control and split
flow or ratio control.
The PPC controller includes a mathematical model of a capillary column. This
model is enabled by setting Capillary Control Mode ON (see Capillary Control
Mode, below). The PPC controller uses this model to calculate the column exit
flow at ambient pressure and temperature, the column average linear gas
velocity, and the inlet split ratio in real time. You may choose to control the
column flow or velocity, in which case the PPC controller calculates the pressure
required to maintain the flow or velocity setpoint. You may also choose to
control the split ratio; in this case the PPC controller calculates the split flow rate
required to obtain the setpoint split ratio.
The PPC controller microprocessor carries out the method setpoint program for
both carrier-gas channels by taking the setpoint pressure, flow, or velocity value;
the column dimensions; the carrier-gas type; the reference temperature and
pressure; the oven actual temperature; and the ambient pressure. It calculates the
other two parameters in real time. For pressure control, it calculates the flow and
velocity; for flow control, it calculates the pressure and velocity; for velocity
control, it calculates the pressure and flow. These calculations track ambient
pressure changes, changing oven temperatures, and the execution of the multiramp carrier-gas program. In each case, the actual pressure in the inlet is
controlled by the calculated or method pressure setpoint.
For more information on these internal calculations, see the section on “Theory
of Capillary Column Control,” in this chapter.
Capillary Control Mode
The first choice for split carrier-gas control is the Capillary Control Mode. This
parameter may be set On or Off. Each carrier gas channel may be setup with or
without capillary control.
Off ─ uses direct pressure control of the column through a multi-step pressure
program and carrier gas timed events. You can directly control the split flow
8-15
PPC Fundamentals
control through the initial setpoint and timed-event control of the split flow
controller. Split ratio control, capillary column flow, and capillary column
velocity control and information are not available. This mode of operation does
not require knowledge of the capillary column dimensions.
On ─ enables indirect control of capillary column flow or velocity in addition to
direct pressure control, each through a multi-step program and timed events. This
mode also enables direct split flow or indirect split ratio control of the split flow
controller. The display reports actual pressure, flow, velocity, split flow, and split
ratio. In this mode you must enter accurate column length and diameter
information (except for pressure-controlled operation with oven tracking).
Carrier Gas Configuration without Capillary Column Control
When capillary control is turned off for a split PPC controller, the choices for
carrier-gas control are None and Pressure.
None ─ removes the split pneumatics from the GC method and turns off the split
flow and pressure.
Pressure ─ enables direct pressure control of the split inlet. The PPC controller
uses a 5 psig initial setpoint with an infinite hold time when Pressure is first
selected. The user may add up to three additional setpoints, ramps, and hold
times. This mode also enables direct split flow control (see below).
Carrier Gas Configuration with Capillary Column Control ON
In this mode the choices for carrier-gas control are None, Pressure, Flow, and
Velocity. With pressure control you may select either Pressure: Program or
Pressure: Oventrack.
None ─ removes the split pneumatics from the GC method and turns off the split
flow and pressure.
Pressure: Program ─ enables direct pressure control of the column pressure. The
split carrier-gas pressure program mode gives a multi-ramp program with realtime calculation and display of flow and velocity, plus flow control or ratio
8-16
Clarus 500 GC Hardware Guide
control of the split flow. The PPC controller uses a 5 psig initial setpoint with an
infinite hold time when Pressure: Program is first selected. The pressure range
is 0 – 100 psig. You may add up to three additional setpoints, ramps, and hold
times.
Pressure: Oventrack ─ also enables direct carrier-gas pressure control. The PPC
controller automatically varies the initial inlet pressure so that the capillary
column flow rate remains constant as the oven temperature changes away from
its initial setpoint value. The PPC controller uses a 5 psig initial setpoint when
Pressure: Oventrack is first selected. Multi-ramp programming is not available.
This mode allows only direct flow control of split flow; however, this mode can
be used for constant column flow control when you do not know your column
dimensions.
Flow ─ enables indirect capillary column mass-flow control. The PPC controller
calculates the inlet pressure required to maintain the method flow program
setpoints from the column dimensions, carrier-gas type, oven temperature, and
ambient pressure. The display shows the flow, pressure, and calculated average
linear gas velocity. The PPC controller uses a 2 mL/min initial setpoint with an
infinite hold time when Flow is first selected. The column flow has a total flow
range of 0 – 500 mL/min (including the split flow). You may add up to three
additional setpoints, ramps, and hold times. This mode enables flow control or
split ratio control of the split flow.
Velocity ─ enables indirect capillary column average linear gas velocity control.
The PPC controller calculates the inlet pressure required to maintain the method
velocity program setpoints from the column dimensions, carrier-gas type, oven
temperature, and ambient pressure. The display shows the velocity, pressure, and
calculated flow rate. The PPC controller uses a 30 cm/s initial setpoint with an
infinite hold time when Velocity is first selected. You may add up to three
additional setpoints, ramps, and hold times. The carrier-gas velocity has a range
of 0–200 cm/s. This mode enables flow control or split ratio control of the split
flow.
Column Dimensions
After selecting any of the capillary control modes (except Pressure: Oventrack)
the Clarus 500 GC prompts you for the column dimensions. These parameters
8-17
PPC Fundamentals
control the relationships between the pressure, flow, and velocity as calculated by
the PPC controller. If the column dimensions are inaccurate, the PPC controller
will produce incorrect readings and will incorrectly control the column flow,
velocity, and split ratio.
Column Length
The column length defaults to 25.0 meters. It has a range from 1.0 – 200.0
meters. Small errors in the column length affect the average linear velocity and
the flow rate only slightly. See the section “PPC Tips and Techniques” at the
end of this chapter for procedures to correct errors in column length.
Column Inner Diameter
The column inner diameter defaults to 250 µm. It has a range from 50 –1000 µm.
Small errors in the column inner diameter strongly affect the average linear
velocity and the flow rate.
Vacuum Compensation
The next Clarus 500 GC split pneumatic configuration parameter in the capillary
control mode is vacuum compensation. The PPC controller uses a mathematical
model of a capillary column to determine pressure – flow – velocity
relationships. The column outlet pressure plays an important role in these
calculations. The PPC controller continually monitors the barometric pressure
because normal daily atmospheric pressure fluctuations affect the column
average linear gas velocity—and thus retention times—if the controlling system
does not compensate. Vacuum compensation controls the role of the outlet
pressure in the PPC controller. Vacuum compensation may be set On or Off.
Off ─ causes the PPC controller to assume that the column outlet is at
atmospheric pressure.
On ─ causes the PPC controller to assume that the column outlet is at vacuum.
This setting is appropriate for GC-MS systems with a direct interface where the
column enters the mass-spectrometer source. Vacuum compensation should be
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Clarus 500 GC Hardware Guide
turned off when an open-split interface is used since it keeps the GC column
outlet close to atmospheric pressure.
Split Control Mode Configuration
The last Clarus 500 GC carrier-gas configuration parameter is the split control
mode. The ratio of the total flow through the inlet liner to the column flow rate
— the fraction of sample vapor entering the column, or the split ratio — controls
the quantitative transfer of sample into the column. For split ratio control the PPC
system must know both the column flow rate and the total gas flow through the
inlet liner.
When capillary control is off, the PPC system does not compute the capillary
column flow rate or the split ratio; only split flow control is possible. With
capillary control on (except for Pressure: Oventrack mode) the PPC controller
calculates the column flow rate and the split ratio.
The choices for split-flow control are Flow or Ratio. There is no choice for
None, since the split pneumatics will not operate without incoming carrier-gas
flow. Setting the carrier-gas configuration to None automatically sets the splitflow controller configuration to none.
Flow ─ enables direct split flow control of the carrier gas mass-flow controller.
You enter a split vent flow rate in the method. The PPC controller adds an
optional offset to obtain the total split flow (see “Split Flow Offset” below) and
sets that amount at the flow controller. The Clarus 500 GC also displays the
calculated split ratio if capillary control is on.
Ratio ─ enables indirect split ratio control of the carrier gas mass-flow controller.
The user enters a split ratio in the method. The PPC controller calculates the
required split vent flow from the column flow rate and adds an optional offset to
obtain the total split flow (see “Split Flow Offset” below) and sets that amount
at the flow controller. The Clarus 500 GC also displays the calculated split flow
rate defined by the following equation:
total split flow = split flow + septum purge flow + column flow
NOTE: Any carrier system leaks will add to the observed total split flow.
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PPC Fundamentals
Split Flow Offset
The PPC controller sets and monitors the total split flow through the inlet system.
The split ratio is based on the flow out the split vent. Since the septum purge
flow is taken from the total split flow rate before passing through the inlet liner,
across the column entrance, and out the split vent, split ratio calculations must
account for the flow reduction. The Clarus 500 GC includes a split flow offset
parameter that is accessed from the CONFIG CARRIER menus when a split
controller is setup. This parameter may be set to Fixed or Auto.
Fixed ─ prompts the user to enter the septum purge offset value. This offset is the
septum purge flow plus the column flow. The initial column flow is displayed on
the [Carrier Prog] key when the GC is READY at its initial setpoints with
capillary control ON. The PPC controller adds this offset to the method setpoint
split flow rate to obtain the actual flow delivered to the split inlet. The septum
purge flow is factory set at 3 mL/min. To measure the actual septum purge offset,
set the carrier pressure to 5 psig or greater and turn off the split flow (set to 0).
The remaining split vent flow displayed is the septum purge flow, plus the
column flow. The actual septum purge flow can be measured from the split vent
bulkhead fitting.
Auto ─ measures the offset flow rate before each run by momentarily setting the
split vent flow to 0, waiting for the remaining flow to stabilize, and then
recording its magnitude. During this time the GC status is PRE-RUN. This
operation occurs after equilibration, and before executing any Pre-Run timed
events (events with negative times). The Auto measurement includes both
column and septum purge flows.
NOTE: The split flow screen (shown below) displays the flow from the injector vent as
the setpoint and the total split system flow as the actual values.
The value in the upper right carrier is the total split flow. The value in the lower
right corner is the split vent setpoint.
The flow measured at the split vent fitting on top of the GC is the vent flow plus
the septum purge flow.
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Clarus 500 GC Hardware Guide
Split Pneumatic Operation
Once the split system has been configured, you may modify the default setpoints
in the active GC method, edit the setpoints in stored methods, or generate a new
method and enter split pneumatic setpoints. The following parameters control
split pneumatic operation.
Initial Carrier Setpoint
The PPC controller takes setpoints of flow, velocity or pressure depending on the
configured split pneumatic carrier gas mode. It receives its initial setpoint from
the active GC method. The initial setpoint is established upon setting up a
method, ending a run, or otherwise resetting the instrument. The PPC controller
holds the setpoint constant at the initial value if no additional carrier-gas entries
are made in the GC method.
Carrier Gas Program
The GC method accommodates up to three additional carrier-gas program steps
consisting of a hold time, ramp rate, and plateau setpoint. Sequential setpoints
may be greater than or less than the preceding setpoint; the PPC controller will
program the split pneumatics with a positive or negative ramp as required. The
carrier gas resets to the initial setpoint value in the method at the end of the GC
oven program, even if a carrier-gas program is in progress. The carrier gas also
resets if the end of the carrier-gas program occurs before the end of the oven
program.
Carrier Gas Timed Events
You may also program carrier-gas timed events to produce step changes in the
setpoint. Carrier-gas timed events can occur before or after a run starts. A
carrier-gas timed event supersedes the method setpoint value at the time the event
occurs. However, if the carrier-gas program in the method advances to a new
step after a carrier-gas event, the new program step or ramp takes control.
Split Flow or Ratio Setpoint
The GC method includes an initial split flow or ratio setpoint. This setpoint is
established upon setting up a method, ending a run, or otherwise resetting the
8-21
PPC Fundamentals
instrument. The PPC controller holds the setpoint constant at the initial value if
no additional carrier-gas entries are made in the GC method.
Split Flow or Ratio Timed Events
The split flow or ratio is changed to a new setpoint by a split timed event. Split
flow or ratio events can occur before or after a run starts. A split flow or ratio
event supersedes the method setpoint value at the time the event occurs.
Theory of Capillary Column Control
This section gives an overview of the theory behind PPC. For more detailed
information please refer to Reference [1].
The Clarus 500 GC Programmable Pneumatic Control system can program
capillary column pressure, flow, or velocity. It accomplishes this by calculating
and maintaining the column pressure drop required by the carrier-gas program
and column temperature. The PPC controller then reads the actual pressure and
uses that value to calculate the actual column flow rate and average linear gas
velocity. The column dimensions, ambient pressure, and carrier-gas type also
enter into the equations.
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Clarus 500 GC Hardware Guide
Column Temperature Effects
Figure 8-3 Carrier-gas viscosity–temperature relationships1
The viscosity of the carrier gas changes with the column temperature. As the
column temperature increases, so does the carrier-gas viscosity. The increasing
viscosity raises the resistance of the carrier gas to being pushed through the
column. Thus, higher column pressure drops are required to maintain column
flow or average linear velocity at higher temperatures. Conversely, keeping the
pressure drop across the column constant while increasing the column
temperature causes the flow rate and linear velocity to drop off.
Figure 8-3 illustrates the effect of column temperature on carrier-gas viscosity.
Notice that the viscosity is different for each carrier gas, and that the “slopes” of
the curves are also different in each case. For each carrier gas, the Clarus 500 GC
1
J. V. Hinshaw and L.S. Ettre, “Introduction to Open-Tubular Column Gas
Chromatography,” (Advanstar Communications, 1994), p. 25. (Part number
N930-6007).
8-23
PPC Fundamentals
includes an accurate model of this viscosity-temperature relationship as
represented by the lines in Figure 8-3.
8-24
Clarus 500 GC Hardware Guide
3.5
(a)
Flow (mL/min)
3.0
2.5
2.0
1.5
1.0
0.5
0.0
-100 -50
0
50
100
150
200
250
300
350
400
450
Column Temperature (°C)
50
45
(b)
Velocity (cm/s)
40
35
30
25
20
15
10
5
0
-100 -50
0
50
100
150
200
250
300
350
400
450
Column Temperature (°C)
Figure 8-4 Effect of column temperature on (a) flow and (b) velocity
Column: 25-m x 250-µm i.d. Helium carrier at 12 psig constant
pressure drop.
The viscosity changes caused by increasing temperature affect the flow and
velocity through a column with a constant pressure drop. As shown in Figure 8-4,
both flow and velocity decrease across the column temperature range. This
8-25
PPC Fundamentals
decreasing flow and velocity can cause loss of column efficiency as well as
changes in flow-sensitive detector operation during programmed-temperature
analyses. In this case, the column pressure drop was selected so that the average
linear velocity was close to 30 cm/s at 50 °C; at 350 °C the velocity drops to
around 20 cm/s. The effect on flow is more severe, dropping from 1.19 mL/min
at 50 °C to 0.4 mL/min at 350 °C.
Without PPC, compensation for this effect is difficult and limited. Although it is
possible to program the PPC controller pressure to crudely compensate, it is
much easier and more accurate to use either the flow-programmed or velocityprogrammed modes instead.
Flow Programmed Operation
The PPC controller operates in a pressure-, flow-, or velocity-programmed mode.
The flow-programmed mode is useful in applications where the column flow rate
must be held constant, or where the operator wishes to express the column carrier
program in flow terms. Figure 8-5 shows the pressure program and velocity that
result when a 50-m x 530 µm i.d. column operates with nitrogen carrier at a
constant 4 mL/min flow across a range of temperatures.
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Clarus 500 GC Hardware Guide
14
Pressure drop (psig)
12
(a)
10
8
6
4
2
0
-100 -50
0
50
100
150
200
250
300
350
400
450
350
400
450
Column Temperature (°C)
50
45
Velocity (cm/s)
40
(b)
35
30
25
20
15
10
5
0
-100 -50
0
50
100
150
200
250
300
Column Temperature (°C)
Figure 8-5 Effect of column temperature on (a) pressure and (b) velocity.
Column: 50-m x 530-µm i.d. Nitrogen carrier at 4 mL/min constant mass
flow
8-27
PPC Fundamentals
Velocity Programmed Operation
Programming the PPC controller in average linear gas velocity mode adjusts the
column pressure drop to maintain the setpoint velocity as the oven temperature
and ambient pressure change. This helps ensure better repeatability of
chromatograms from one instrument to another — assuming the ovens are
calibrated to a common temperature reference standard—by eliminating effects
due to differences in altitude or weather. Differences in the columns, however,
are not accounted for.
40
Pressure drop (psig)
35
30
25
(b)
(a)
20
15
10
5
0
-100
-50
0
50
100
150
200
250
300
350
400
450
Column Temperature (°C)
Figure 8-6 Effect of altitude on pressure programs. Column: 15-m x 100-µm
i.d. Hydrogen carrier at 30 cm/s constant average linear gas velocity. (a):
Sea level; (b): 3000 m altitude
Figure 8-6 shows two pressure-temperature curves, one for a constant velocity of
30 cm/s on a 15-m x 100 µm i.d column with hydrogen carrier with an
atmospheric pressure equivalent to sea level, and the other for the same column
at the equivalent of 3 000 m altitude. When operating the oven at a constant
temperature with identical columns, all solute retention times will be the same in
both cases because the velocities are unchanged.
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Clarus 500 GC Hardware Guide
With oven temperature programming, the retention times will be very similar but
not quite the same due to slight differences in the velocity profiles across the two
columns at different altitudes.
Pressure / Oventrack Mode
Pressure drop (psig)
60
50
40
30
20
10
0
-100 -50
0
50
100
150
200
250
300
350
400
450
Column Temperature (°C)
Figure 8-7 Pressure program in oventrack mode. Helium carrier at 25 psig,
50 °C initial conditions
The Pressure: Oventrack operating mode maintains a constant column mass
flow as the column temperature changes by adjusting the inlet pressure as
required. No knowledge of column dimensions is required in this mode: only the
initial pressure and temperature are specified. Figure 8-7 shows the pressuretemperature profile for Pressure: Oventrack mode with an initial pressure of 25
psig at 50 °C with helium carrier gas. This operating mode is convenient for
mass-spectrometric or thermal-conductivity detectors where column dimensions
are not important.
8-29
PPC Fundamentals
Vacuum Compensation
45
Pressure drop (psig)
40
35
30
25
20
(b)
(a)
15
10
5
0
-100 -50
0
50
100
150
200
250
300
350
400
450
Column Temperature (°C)
Figure 8-8 Pressure program (a) without and (b) with vacuum
compensation. Column: 60-m x 320 µm i.d. Helium carrier at 2 mL/min
constant flow
When using a mass-spectrometric detector with the column exit under vacuum, it
is necessary to reduce the column pressure drop to account for the reduced exit
pressure. The effect of putting the column exit under vacuum is shown in Figure
8-8 for a 60-m x 320 µm i.d. column with helium carrier at a 2 mL/min constant
flow rate.
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Clarus 500 GC Hardware Guide
Detector Gas Flow Control
The Clarus 500 GC can control up to two detectors, each with up to two primary
detector gas flow controllers. The GC determines the type of controllers required
for each detector by sensing the presence of the detector amplifier board. Certain
detectors, such as the ElCD/PID combination, use additional auxiliary detector
gas control zones (see “Auxiliary Detector Gas Control,” below).
The Clarus 500 GC PPC detector gas flow controller delivers a set flow rate of
gas into a device (detector) at atmospheric pressure. Unlike the carrier gas
controller, the detector gas controller does not compensate for significant
changes in its outlet pressure. It is not suitable for providing column flow. The
detector gas controller is not affected by normal changes in the incoming gas
supply pressure. The PPC controller compensates for changes in each detector
gas controller’s internal temperature. Figure 8-9 illustrates the detector flow
control module.
Figure 8-9 Schematic of a detector gas flow control module
8-31
PPC Fundamentals
Detector Gas Flow Controller Operating Range
The detector gas flow controller operating range depends on the detector in use.
Each flow controller uses a flow-range element (fixed restrictor) that determines
the available flow range for a particular gas. The nominal detector gas flow lies
within 20–50% of the full-scale controller range for the factory-installed flowrange elements. The flow-range elements should not be changed unless the
controller is to be used with a different detector. Please refer to Chapter 9,
“Maintenance,” the Practical Hints section for information on individual flowrange elements for specific detectors.
NOTE: Only the fixed restrictor changes for various requirements.
Detector Gas Flow Controller Setup
The PPC system stores information about the type, location, and calibration of its
pneumatic devices in battery-backed-up random access memory (BRAM). This
information is written into the BRAM during manufacturing; normally there is no
need to access or modify the type or location of the PPC controllers. If the PPC
hardware configuration is changed — by installing or removing PPC devices —
you must access the PPC connection menus on the Clarus 500 GC keypad and
modify the type and location of the PPC devices. See “Connecting the PPC
Modules” in Chapter 13, “System Utilities,” for detailed instructions.
CAUTION
Do not modify the PPC connection information if the PPC
hardware configuration has not changed.
Detector Gas Flow Controller Calibration
The detector gas mass-flow controller requires periodic calibration and the
calibration is gas specific. The controller is factory calibrated to a National
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Clarus 500 GC Hardware Guide
Institutes of Standards Technology (NIST) traceable standard with air, hydrogen,
or helium gas, depending on the detector type. Recalibration is required upon
changing the gas or the flow-range element; otherwise, the calibration frequency
is up to the individual operator. It is good laboratory practice to recalibrate all
measuring and control devices periodically.
The detector gas flow controller calibration procedure consists of specifying the
reference temperature and pressure; zeroing the internal sensors in the flow
controller with the tank pressure off; specifying the flow-range element; selecting
the gas type (for reference or makeup only); then measuring the flow rate at 20%
and 40% of full-scale flow. This procedure is built into the Clarus 500 GC
firmware. See Chapter 13, “System Utilities,” for detailed instructions.
Detector Gas Mass-Flow Controller Operation
For flame-type detectors, setting up the detector gas flow controllers sets a
default flow rate equal to the nominal flow specified for the detectors. For
detectors with makeup or reference gases the flow rate defaults to 30 mL/min.
Once the detector gas flow controllers have been set up and calibrated on the
PPC system, the operator must enter their flow rates on the Clarus 500 GC touch
screen.
Unlike carrier gas flows, detector gas flow rates do not appear in the GC method.
Instead, they are set in the GC configuration. There are no timed events that
modify detector flows. Detector gas flow controllers may be set up as Auxiliary
gas flow zones if it is necessary to incorporate them into the GC method or to
modify them with timed events. See “Auxiliary Detector Gas Control” below
for further information.
Flame Gases
The Clarus 500 GC automatically determines gas types for flame detectors,
including the flame-ionization (FID), flame-photometric (FPD), nitrogenphosphorous (NPD), and Electrolytic Conductivity Detector (ElCD or Hall).
NOTE: The combination ElCD/PID detector system uses an auxiliary detector gas flow
controller for the ElCD hydrogen supply. Please see the Detectors chapter for
further information.
8-33
PPC Fundamentals
Once the flame gas controllers are set up, you may modify the default flow rates
as required by entering new values under the in the GC configuration.
Flame Ignition
The PPC version of the FID has flameout detection and an auto-ignite feature.
Flameout detection occurs 0.5 minutes into the PRE-RUN time and it measures
the user-entered baseline threshold level in mV. If the threshold level is
exceeded, the flame is considered lit; otherwise, the Clarus 500 GC detects that
the flame is out, and auto-ignite automatically lights the flame before the start of
a run. You can also manually light the flame at any time by pressing the ignite
button on the touch screen.
Makeup and Reference Gases
The Clarus 500 GC automatically determines the presence of reference and
makeup gases for detectors. The thermal-conductivity detector (TCD) uses
reference gas. The electron-capture detector (ECD), photoionization detector
(PID), and, optionally, the thermal-conductivity detector (TCD) use makeup gas.
Makeup and reference gases operate in a fashion similar to flame gases, except
that you may change the gas type in the PPC controller setup.
Once the makeup or reference gas controllers are set up, you may modify the
default flow rates as required by entering new values in the active.
Detector makeup gas flow controllers may be set up as Auxiliary gas flow zones
if it is necessary to incorporate them into the GC method or to modify them with
timed events. See “Auxiliary Detector Gas Control” below for further
information.
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Clarus 500 GC Hardware Guide
Auxiliary Pressure and Flow Control
In addition to carrier and detector gas control, the Clarus 500 GC accommodates
up to four auxiliary PPC controllers. The auxiliary zones can control carrier gas
mass-flow controllers, pressure controllers, pressure readouts, and detector gas
flow controllers. These zones all have an initial setpoint, and incorporate timedevent changes.
Auxiliary Carrier Gas Control
The Clarus 500 GC controls up to two primary carrier-gas zones and up to four
primary detector gas zones. In addition, up to four carrier gas mass flow
controllers, pressure controllers, or pressure readouts may be set up as auxiliary
PPC carrier zones, subject to a maximum of eight flow controllers (carrier plus
detector flow) and twelve zones total in the PPC system. The auxiliary flow
control zones do not accommodate split pneumatics, which must be configured as
the primary carrier control zones on the GC.
Auxiliary Carrier Gas Setup
The PPC system stores information about the type, location, and calibration of its
pneumatic devices in battery-backed-up random access memory (BRAM). This
information is written into the BRAM during manufacturing; normally there is no
need to access or modify the type or location of the PPC controllers. Some
factory installed options use auxiliary carrier-gas zones. In order to use other
auxiliary zones the operator must access the PPC connection menus on the Clarus
500 GC touch screen and modify the type and location of the PPC devices. For
auxiliary carrier-gas control you may choose either a carrier gas mass-flow
controller, a pressure controller, or a pressure readout.
CAUTION
Do not modify the PPC connection information if the PPC
hardware configuration has not changed.
8-35
PPC Fundamentals
Auxiliary Carrier Gas Mass-Flow Controller Calibration
The calibration procedure for mass-flow controllers designated as auxiliary
carrier gas zones is the same as for controllers designated as primary carrier
zones. Please refer to the section “Mass-Flow Controller Calibration” in this
chapter.
Auxiliary Carrier Gas Zone Operation
Once the auxiliary carrier gas zone has been set up, you may modify the default
setpoints in the active GC method, edit the carrier-gas setpoints in stored
methods, or generate a new method and enter carrier-gas setpoints. The following
parameters control the auxiliary carrier gas.
Initial Auxiliary Carrier Gas Setpoint
The auxiliary carrier gas zone takes setpoints of flow or pressure depending on
the configured controller. It receives its initial setpoint from the active GC
method. The initial setpoint is established upon setting up a method, ending a
run, or resetting the instrument. The setpoint is held constant at the initial value
if no additional auxiliary carrier entries are made in the GC method. The initial
auxiliary carrier gas setpoint appears after touching Carrier Program button in
the GC method.
Auxiliary Carrier Gas Timed Events
You may program auxiliary carrier-gas timed events to produce step changes in
the setpoint. Auxiliary carrier-gas events can occur before or after a run starts.
An auxiliary carrier-gas event supersedes the method setpoint value at the time
the event occurs.
Auxiliary Detector Gas Control
The Clarus 500 GC controls up to four primary detector gas zones and up to two
primary carrier-gas zones. In addition, up to four detector gas flow controllers
may be set up as auxiliary PPC detector zones, subject to a maximum of eight
8-36
Clarus 500 GC Hardware Guide
flow controllers (carrier plus detector flow) and twelve zones total in the PPC
system.
Auxiliary Detector Gas Setup
The PPC system stores information about the type, location, and calibration of its
pneumatic devices in battery-backed-up random access memory (BRAM). This
information is written into the BRAM during manufacturing: normally there is no
need to access or modify the type or location of the PPC controllers. Some
factory installed detectors use auxiliary detector gas zones. In order to use other
auxiliary zones the operator must access the PPC CONNECTION menus on the
Clarus 500 GC touch screen and modify the type and location of the PPC
devices.
CAUTION
Do not modify the PPC connection information if the PPC
hardware configuration has not changed.
Auxiliary Detector Gas Flow Controller Calibration
The calibration procedure for detector gas flow controllers designated as
auxiliary detector gas zones is the same as for controllers designated as primary
detector zones. Please refer to the section “Detector Gas Flow Controller
Calibration” in this chapter.
Auxiliary Detector Gas Zone Operation
Once the auxiliary detector gas zone has been set up, you may modify the default
setpoints in the active GC method, edit the detector gas setpoints in stored
methods, or generate a new method and enter detector gas setpoints. The
following parameters control the auxiliary detector gas.
Initial Auxiliary Detector Gas Setpoint
The auxiliary detector gas zone takes flow setpoints. It receives its initial
setpoint from the active GC method. The initial setpoint is established upon
8-37
PPC Fundamentals
setting up a method, ending a run, or resetting the instrument. The setpoint is
held constant at the initial value if no additional auxiliary detector gas entries are
made in the GC method.
Auxiliary Detector Gas Timed Events
You may program auxiliary detector gas timed events to produce step changes in
the setpoint. Auxiliary detector gas events can occur before or after a run starts.
An auxiliary detector gas event supersedes the method setpoint value at the time
the event occurs.
8-38
Clarus 500 GC Hardware Guide
PPC Tips and Techniques
This section contains tips and techniques that you will find useful when using
PPC.
Effect of Flow on Pressurization Rate
When first turned on, when a higher setpoint pressure is programmed, the PPC
carrier-gas zones require some time to come up to pressure. The pressurization
rate is a function of the type of inlet, the incoming carrier-gas flow rate and the
outgoing column and septum purge flow rate (if applicable).
For typical packed columns the inlet will pressurize within one minute. For a
POC inlet where the column flow rate is low it may take longer to reach a steadystate inlet pressure. The PPC gas-leak monitor will not trigger until five minutes
have elapsed, which should be enough time in all cases.
For capillary or PSS inlets, setting a high inlet pressure and a low split flow rate
(but not a zero flow) can result in the inlet never coming to pressure because the
incoming split flow is less than the column plus septum purge rates. A zero splitflow rate is treated as a special condition for splitless injection and will not cause
this problem. In general, use a minimum split flow rate that is the greater of 20
mL/min or four times the sum of the column and septum-purge flows.
NOTE: If the column pressurization rate (psig/min) is too low, increase the split flow
rate during this time.
If you want to quickly pressurize the column in the split mode, temporarily
increase the split vent flow while pressurizing the column. You can set the split
vent flow up to a maximum of 500 mL/min.
Correcting the Column Dimensions
The PPC controller relies on operator input of column dimensions to calculate
pressure – flow and pressure – velocity relationships. If the column dimensions
are incorrect, then the calculations will be inaccurate. In general, actual column
diameters are within ±2 µm of the nominal specified value. Column lengths may
vary for used columns because the ends may have been cut off.
8-39
PPC Fundamentals
Alternatively, the column dimensions may be unknown. In such cases set the
Carrier mode to pressure and oventrack, if you need to maintain a constant
column flow rate.
Correcting the Column Length
The average linear gas velocity is the most accurate measure of capillary column
conditions, because the low flow rates are difficult to measure. By measuring the
average velocity you can compare it to the displayed velocity on the GC, and
then make a correction to the column length. This procedure assumes that the
column inner diameter entered into the Clarus 500 GC is correct.
Set Up the Clarus 500 GC
Install a column and turn on the GC. In Configuration set the CAPILLARY
CONTROL MODE ON, and choose the VELOCITY mode. Enter the nominal
column length and exact diameter. Select the split FLOW mode. In the Method,
accept the default velocity of 30 cm/s, or choose another value. Set the oven
temperature to at least 100 °C, isothermal.
Determine the Unretained Peak Time
Inject 1–5 µL of methane (natural gas) and time how long it takes for the
methane peak to elute from the column. This is best done by recording the
methane chromatogram with a data handling system and reading the methane
peak time off the chromatogram or report. You may use methylene chloride
(CH2Cl2) vapor for an ECD.
Calculate the Actual Average Linear Gas Velocity
Calculate the average linear gas velocity ( u ) from this formula:
L
u = PPC X 10
tM
8-40
Clarus 500 GC Hardware Guide
where LPPC is the column length (in meters) entered in the Clarus 500 GC and
tM is the measured methane peak time in seconds.
Compute the Correction Factor
Compare the measured velocity ( u ) to the displayed velocity ( u PPC ) and
compute the column length correction factor (f):
u
f = PPC
u
If the correction factor is less than 0.8 or greater than 1.2, then you should double
check the column diameter and nominal length for errors.
Enter the Corrected Column Length
Now, go back to the GC configuration and enter the corrected column length
(Lnew):
Lnew = f ⋅ LPPC
Check the New Length
Upon entering the new length the PPC controller will change the inlet pressure
up or down to reflect the new conditions. If the measured velocity was less than
the displayed value, then the PPC controller will reduce the pressure so that the
measured velocity is now equal to the displayed value. If the measured velocity
was higher, then the PPC controller will increase the inlet pressure. Check the
new value by measuring the methane peak time again. Your calculated linear
velocity should now be very close to the displayed value.
Splitless Injection
Splitless injection refers to a technique that has a zero split flow rate during
injection with an increased split flow rate after injection is complete. There are
two ways to accomplish splitless injection on the Clarus 500 GC.
8-41
PPC Fundamentals
Zero Initial Split Flow
For this method, you set the initial split flow to zero and enter a timed event after
injection (typically at 1–2 minutes) that sets the split vent flow to 50–100
mL/min. The Clarus 500 GC will automatically turn off the split vent flow at the
end of the run.
Zero Split Flow by Pre-Run Event
In some cases — with a PSS inlet in particular — it may not be desirable to have
zero split vent flow while the instrument is cooling and recycling for another run.
Set the initial split vent flow to 50–100 mL/min. Then enter a timed event at -2
minutes to set the split vent flow to 0, and enter another event after injection
(typically at 1–2 minutes) that sets the split vent flow to 50–100 mL/min.
Pressure-Pulse Injection
Pressure-pulse injection refers to a technique that facilitates sample transfer from
inlet to column by raising the inlet pressure (column flow and velocity) above the
normal level for injection, and then lowering it back to a normal setting for peak
elution.
To perform pressure-pulse injection, enter a Pre-Run timed event at −1 minute
that raises the pressure, flow, or velocity — depending on the operating mode —
to a level 2–20 times the method’s initial setpoint value. Then enter another
timed event 1–2 minutes into the run that reestablishes the initial method
setpoint. If you are using a carrier-gas program, then set a 1–2 minute step 1 hold
time in the program. The carrier-gas program will “take over” the PPC system at
the end of the hold period. To discharge the pressure-pulse, the split flow must
have a non-zero volume at the time of discharge. To rapidly change the pressure
pulse, the split flow should be zero or as large as possible during pressurization.
Reducing Carrier-Gas Consumption
You can significantly reduce carrier-gas consumption with a split or PSS inlet by
setting the initial split flow to 20 mL/min, using a Pre-Run timed event at −2
minutes to increase the flow for split injection or to set the flow to 0 for splitless
8-42
Clarus 500 GC Hardware Guide
injection, and then reducing the split flow back to 20 mL/min after completion of
the injection. You should delay the flow reduction until at least 5 minutes or
longer after injection, or after a PSS inlet has reached its final temperature.
Don’t forget to include a timed event at 1–2 minutes that sets the flow to 50–100
mL/min for splitless injection.
8-43
Maintenance
9
Maintenance
9-2
Clarus 500 GC Hardware Guide
This chapter contains procedures for:
•
Autosampler Maintenance — changing a syringe and replacing a viallocator mechanism.
•
Syringe Maintenance — cleaning the 5-µL and 50-µL syringe plungers.
•
Injector Maintenance — changing septa, changing and repacking
packed-injector liners, changing and repacking injector liners on the
capillary (CAP), programmed split/splitless (PSS), and programmed oncolumn (POC) injectors, and changing the charcoal trap on the
split/splitless injector.
•
ECD Maintenance — baking out ECD cells, cleaning the ECD anode,
and wipe testing an ECD cell.
•
FID Maintenance — replacing the FID jet, cleaning the FID jet,
replacing an O-ring in the FID collector, and cleaning the FID collector
and cap.
•
PID Maintenance — changing PID lamps, cleaning PID lamp windows,
changing PID lamp window seals, and positioning disks.
•
ElCD Maintenance — replacing the ElCD reaction tube and cleaning
ElCD cells.
•
NPD Maintenance — changing and conditioning the NPD bead and
replacing an NPD jet.
•
FPD Maintenance — cleaning or replacing an FPD optical filter
assembly, cleaning the detector liner, cleaning/replacing the detector
window, replacing the photomultiplier tube, and cleaning and replacing
the FPD jet.
•
PPC Maintenance — replacing PPC module restrictors.
9-3
Maintenance
Autosampler Maintenance
Autosampler maintenance consists of changing a syringe and replacing a vial
locator mechanism.
9-4
Clarus 500 GC Hardware Guide
Changing a Syringe
1. From the System Status screen select the Run icon.
2. On the Run Type page select the Autosampler radio button and the Task tab.
The following page will appear.
9-5
Maintenance
3. Select the Park button and the autosampler tower moves to the park position
(facing the front of the Clarus 500 GC).
4. Open the tower door on the autosampler tower cover.
9-6
Clarus 500 GC Hardware Guide
Figure 9-1 Autosampler tower in the park position
9-7
Maintenance
Removing a Syringe
1. Locate the plunger assembly shown in the previous illustration.
Then, refer to the following figure, as you lift up the plunger cap handle and
rotate it until it rests on the collar. Then release the plunger cap handle.
Figure 9-2 Plunger assembly
2. Hold the syringe by the barrel or syringe nut (see the following figure) and
turn the carriage thumbscrew clockwise until the syringe is free.
3. Gently pull the top of the syringe forward until it just clears the carriage
assembly.
4. Gently lift the syringe out of the carriage assembly.
9-8
Clarus 500 GC Hardware Guide
Figure 9-3 Removing a syringe
9-9
Maintenance
Installing a Syringe
Please refer to Figures 9-2 through 9-4 as you follow these steps.
1. Guide the needle through the hole in the carriage thumbscrew, then thread
the needle through the needle guide. Use your fingers as a guide.
2. Rest the top of the plunger on the plunger cap slide, which is a shelf located
on the underside of the plunger assembly.
3. While holding the syringe nut, engage the carriage thumbscrew on the
threaded part of the syringe by turning the carriage thumbscrew
counterclockwise.
4. Continue turning the thumbscrew counterclockwise. This slowly lowers the
needle. Carefully guide the needle through the needle guide into the vial
locator.
5. Tighten the carriage thumbscrew.
Figure 9-4 Installing a syringe
9-10
Clarus 500 GC Hardware Guide
Replacing the Vial-Locator Mechanism
The vial-locator mechanism will wear out with extended use and require
replacement. If the autosampler begins missing vials, or if the hole for the
syringe needle begins to plug, it is an indication that you should replace the viallocator mechanism
To replace a vial-locator mechanism:
1. Remove the two shoulder screws that secure the locator to the autosampler
tower frame. Remove the two springs, then remove the vial locator. Discard
the vial locator.
2. Mount the new vial locator (Part Number N610-1182) on the autosampler
tower frame.
3. Install the two shoulder screws through the two springs and into the vial
locator. This secures the vial locator to the autosampler tower frame.
WARNING
When securing the vial-locator molding, be sure that the flag is
centered (not touching either side) in the sensor. If it touches a
side, adjust the flag by loosening and then tightening the screws.
DO NOT ADJUST THE SENSOR.
9-11
Maintenance
Figure 9-5 Exploded view of the vial locator
9-12
Clarus 500 GC Hardware Guide
Syringe Maintenance
Syringe maintenance consists of cleaning the 5-µL and 50-µL syringe plungers
and servicing idle syringes.
Cleaning the 5-µL and 50-µL Syringe Plungers
The 5-µL and 50-µL syringe plungers should be cleaned regularly, after
approximately 500 injections, since insolubles can build up and cause friction.
To clean the syringe plunger:
1. Remove the syringe using the procedure described in the preceding section.
2. Remove the plunger from the syringe barrel.
3. Wipe the plunger with a tissue soaked in an appropriate solvent.
4. Replace the plunger.
5. Pull and expel the same solvent through the barrel several times.
6. Replace the syringe using the procedure descried in the preceding section.
NOTE: Only syringes distributed by PerkinElmer should be used with the Clarus 500
GC. Plungers are not interchangeable from syringe to syringe.
Servicing Idle Syringes
Syringes that are not used for several hours could "freeze," i.e., the syringe
plunger will not move. To avoid this condition, PARK the tower, then remove
and clean the syringe plunger as described above.
NOTE: If you notice the Clarus 500 GC precision degrading, replace the syringe. The
Clarus 500 GC syringe is a consumable part. After extended use, you will need to
replace it.
9-13
Maintenance
Injector Maintenance
CAUTION
If you are analyzing reactive compounds, you should use deactivated
liners and wool which are appropriate for your sample type.
Injector maintenance consists of changing septa, changing and repacking injector
liners, changing the hourglass needle guide on the POC injector, changing and
repacking CAP and PSS injector liners, removing a broken liner from the PSS
injector body, changing the charcoal trap or replacing charcoal on the
split/splitless CAP and PSS injectors.
Changing Septa
Septa should be replaced on a regular basis. How often depends on the type of
septa used, the temperature of the injection port, and the number of injections
made.
The septum shipped with your instrument is a Thermogreen LB-2 Septa (Part
Number N662-1028, package of 50). This septum can handle over 200 injections
at moderate temperatures.
To change a septum:
1. Turn off the injector heater and allow the injector to cool.
2. Remove the septum cap.
3. Pry the old septum from the septum cap with a screwdriver.
4. Insert a new septum in the septum cap.
5. Replace the septum cap.
9-14
Clarus 500 GC Hardware Guide
NOTE: To minimize the possibility of contamination, avoid unnecessary handling of
septa.
Figure 9-6 Changing a septum
Changing and Repacking Packed Column Injector
Liners
To improve the performance of the injector used with packed columns, insert a
small amount of quartz wool (Part Number N610-2354) into the top portion of
the injector liner (Part Number N610-1048). The quartz wool accomplishes two
things: (1) it wipes the end of the syringe needle to insure that reproducible
sample volumes are injected, and (2) it retains any nonvolatile components
present in your sample, making cleaning the liner easier.
9-15
Maintenance
The injector liner should be removed and the wool packing replaced on a regular
basis, particularly if your samples contain nonvolatile components that could
build up on the wool. This could cause adsorption of peaks of interest, tailing,
and loss of sensitivity.
You can remove the wool with a small hook on the end of a thin wire, or blow it
out using compressed air.
To remove a packed injector liner and install new wool:
1.
Turn off the injector heater.
Allow the injector to cool until it is slightly warm to the touch. Cooling
the injector to a temperature that is too low (<100 °C) will make it
difficult to remove the injector liner.
2.
Remove the septum cap (see Figure 9-6).
3.
Remove the septum shield (Part Number N610-1050) with the large end
of the liner-removal tool (Part Number N610-0102).
Figure 9-7 Liner-Removal Tool (Part Number N610-0102)
4.
9-16
Press the small end of the liner-removal tool into the injector liner, then
pull the injector liner out.
Clarus 500 GC Hardware Guide
Figure 9-8 Removing the packed column injector liner
NOTE: To avoid contaminating the quartz wool when packing the injector liner, wear
vinyl, powder-free, disposable gloves (for example, the same type of gloves used
to perform maintenance on a mass spectrometer).
5.
Take a small piece of quartz wool and twist it into an elongated shape so
that you can insert it into the injector liner. Then, using the supplied
1/16-inch rod (Part Number N610-T100), push the quartz wool into the
injector liner. Loosely pack a 1-inch (2.5 cm) piece of quartz wool into
the top portion of the liner (see the following figure).
6.
Replace the injector liner, septum shield, and septum cap.
9-17
Maintenance
Figure 9-9 Packed column injector liner (Part Number N610-1048) packed
with wool
Changing the Hourglass Needle Guide on the
Programmed On-Column (POC) Injector
To change the hourglass needle guide:
1. Turn off the injector heater. Allow the injector to cool until it is
slightly warm to the touch.
2.
Remove the septum cap.
Figure 9-10 Removing a septum cap
9-18
Clarus 500 GC Hardware Guide
3.
Remove the septum shield (Part Number N610-1702) with the large end
of the liner-removal tool (Part Number N610-0102).
4.
Remove the hourglass needle guide (see the following figure) with a pair
of tweezers or small pliers.
Figure 9-11 Cutaway view of the POC injector showing the location of the
hourglass needle guide
9-19
Maintenance
5.
Install the new hourglass needle guide (Part Number N610-1703).
6.
Replace the septum shield.
7.
Replace the septum cap.
8.
Reinstall your column.
Refer to Chapter 6, Installing a Capillary Column, for the proper procedures.
Changing and Repacking Capillary Split/Splitless
(CAP) and Programmed Split/Splitless (PSS) Injector
Liners
The procedure below is applicable to the following injector liners:
Injector Liner
Size
Part Number
CAP wide-bore liner
4.0-mm i.d. and a 6.0-mm o.d.
N612-1001
CAP narrow-bore liner
2.0-mm i.d. and a 6.0-mm o.d.
N612-1002
PSS wide-bore liner
2.0-mm i.d. and a 4.0-mm o.d.
N612-1004
PSS narrow-bore liner
1.0-mm i.d. and a 4.0-mm o.d.
N612-1006
PSS on-column liner
--
N610-1539
Removing a CAP or PSS Injector Liner
The liner-removal procedure is similar for CAP and PSS wide-bore and narrowbore liners. To remove the liners, you need a CAP liner-removal tool (Part
Number 0250-6534) or a PSS liner-removal tool (Part Number 0250-6247) as
shown below.
9-20
Clarus 500 GC Hardware Guide
Figure 9-12 CAP and PSS liner-removal tools
To remove a capillary injector liner:
1. Turn off the injector heater.
Allow the injector to cool until it is slightly warm to the touch. Cooling the
injector to a temperature that is too low (<80 °C) will make it difficult to
remove the injector liner.
2. Remove the septum cap.
Figure 9-13 Removing the septum cap
3. Remove the injector cover.
9-21
Maintenance
Injector Cover
(P/N N610-1762)
Figure 9-14 Removing the injector cover
4. Loosen the threaded collar using the spanner (Part Number N610-1359)
provided, then remove the threaded collar.
Figure 9-15 Loosening the threaded collar
5. Replace the septum cap on the injector.
6. Pull the septum cap upwards to remove the septum purge assembly.
9-22
Clarus 500 GC Hardware Guide
Figure 9-16 Removing the septum purge assembly
The carrier gas inlet line is coiled. This allows you to pull the septum purge
assembly over to the side and gain access to the injector liner.
NOTE: The inlet line used in PPC capillary injectors (CAP and PSS) is coiled but the
septum purge assembly does not terminate in a snubber as shown. Instead it is
connected to a PPC module. The coil of the inlet line is long enough so that you
can pull the septum purge assembly out of the opening in the top cover and gain
access to the injector liner.
7. Insert the CAP liner-removal tool (Part Number 0250-6534) over the end of
the CAP liner and lift the liner out of the injector.
OR
Insert the PSS liner-removal tool (Part Number 0250-6247) over the end of the
PSS liner and lift liner out of the injector.
CAUTION
The liner must be cool (no hotter than 100 °C) or the liner-removal
tool will melt! The end of the liner-removal tool may flare out with
use. If this happens,
9-23
Maintenance
Figure 9-17 Removing an injector liner
NOTE: If the quartz liner breaks inside the CAP injector, it can be removed by first
removing the column, then removing with a 9/16-inch wrench the 1/4-inch
injector fitting that is inside the oven. The liner should fall out of the injector
with the fitting. If the liner is stuck, you can push it out from the top or bottom of
the injector.
CAUTION
The PSS injector liner does not have a 1/4-inch fitting like the CAP
injector. Be very careful when removing this liner to prevent breaking
it. Do not cool the injector below 80 °C. This will make it easier to
remove the liner and O-ring. As the injector cools, the O-ring adheres
to the metal base.
NOTE: Each capillary liner has an O-ring installed on the frosted portion of the CAP
liner and on the part furthest away from the dimple on the PSS injector. If the Oring has adhered to the injector, you may not be able to easily remove the liner
(step 7 above). If this is the case, use a small screwdriver to dislodge the O-ring
before removing the liner and O-ring.
9-24
Clarus 500 GC Hardware Guide
About O-Rings
CAUTION
Each time a capillary injector liner is removed, you should
replace the O-ring, especially if the O-ring adheres to the
injector body and you had to pry it loose with a screwdriver.
This action may damage the O-ring thereby causing a bad seal if
the damaged O-ring is reinstalled.
If your results produce background contamination when a new O-ring is first
installed, condition the injector at the maximum temperature of the O-ring (listed
below). Depending on the type of column used, you may first want to remove the
column before baking it out at a high temperature.
NOTE: High-temperature seals should be used at temperatures of 300 °C or higher.
These seals are available in Kalrez or graphite from PerkinElmer’s catalog
service (in the U.S. dial: 1-866-762-4000) or on-line at www. perkinelmer.com.
Viton maximum temperature of 250 °C is recommended for the mass
spectrometer.
9-25
Maintenance
Injector O-Rings
Recommended Maximum Temperature
CAP Injector
N610-1374
Silicone (pkg .of 10)
250 °C
N610-1378
Graphite (pkg. of 5)
450 °C
N930-2782
Kalrez (pkg. of 1)
450 °C
N930-2783
Viton (pkg. of 1)
250 °C (not recommended for use with ECD)
PSS Injector
N610-1751
Graphite (pkg. of 5)
450 °C
0992-1004
Kalrez (pkg. of 1)
450 °C
N610-1747
Viton (pkg. of 10)
250 °C (not recommended for use with ECD)
Selecting an Appropriate CAP Injector Liner
Select the correct CAP liner for your application and pack it with quartz wool.
The CAP injector uses the following two liners:
•
CAP wide-bore liner (Part Number N612-1001); 4.0-mm i.d. and 6.0mm o.d.
•
CAP narrow-bore liner (Part Number N612-1002); 2.0-mm i.d. and 6.0mm o.d.
9-26
Clarus 500 GC Hardware Guide
The narrow-bore liner is generally used for a splitless injection, and the widebore liner is generally used for a split injection. Due to the small internal volume
(0.3 mL) of the narrow-bore liner, prevent overfilling the liner with vapor
(caused by solvent expansion upon injection) by limiting the amount of sample
injected to 0.5 µL. The wide-bore liner is used for splitless injection volumes
over 0.5 µL, since its internal volume is 1.25 mL. The sample size should be
limited to a maximum of 2 µL for hydrocarbon solvents, and less than that for
high-expansion solvents such as water or CH2Cl2.
If the wide-bore liner is used for splitless injection, the splitless sampling time
(the vent-on time) should be more than one minute. Also, lower initial oven
temperatures may be required to give good resolution in the first few minutes
after the solvent peak elutes. The wide-bore liner should be used with columns
having an i.d. of 0.32 mm or greater.
Packing the CAP Injector Liner with Quartz Wool
We recommend packing a small amount of quartz wool in the top portion of the
liner to wipe the syringe needle regardless of the liner type or injector mode (for
example, split or splitless). This packing assures that reproducible volumes are
injected by wiping the syringe needle every time it is inserted.
Remove the liner and replace the quartz wool packing on a regular basis,
particularly if your samples contain nonvolatile components that could build up
on the wool. This buildup could cause adsorption of peaks of interest, tailing, and
loss of sensitivity.
Remove the wool by making a small hook on the end of a thin wire and using
that to pull it out, or blow it out using compressed air.
NOTE: To avoid contaminating the quartz wool when packing the injection liner, wear
vinyl, powder-free, disposable gloves (for example, the same type of gloves used
to perform maintenance on a mass spectrometer).
9-27
Maintenance
Packing a CAP Injector Liner for Split Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then using the supplied 1/16-inch rod (Part Number
N610-T100), push the quartz wool into the liner. Pack the wool snuggly∗ from
the dimple upwards [about 1 in. (2.5 cm)]. Loosely pack quartz wool in the top
portion of the liner to wipe the syringe needle upon injection.
Packing a CAP Injector Liner for Splitless Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then using the supplied 1/16-inch rod (Part Number
N610-T100), push the quartz wool into the liner. Pack a 1-inch (2.5 cm) piece of
quartz wool loosely below the top ground portion of the liner (see the following
figure). The sample is then injected into the wool, thereby preventing the delivery
of sample beyond the column. The wool also wipes the syringe needle upon
injection.
∗
9-28
The recovery of high-molecular-weight components (e.g., C40
and higher) may be improved if the liner is packed loosely.
Clarus 500 GC Hardware Guide
Figure 9-18 CAP injector liners packed with quartz wool
9-29
Maintenance
NOTE: As you can see in Figure 9-18, each CAP injector liner has an O-ring installed
on the ground portion. If the O-ring has adhered to the liner, it may not be easy
to remove the liner. (If this is the case, use a small screwdriver to dislodge the
O-ring before removing the liner and O-ring).
Reinstalling the Liner in the CAP Injector
1. Install a new O-ring near the ground portion of the liner.
2. Insert the liner in the injector body.
3. Place the septum purge assembly over the liner.
4. Press the septum purge assembly down to correctly position the liner in the
injector.
Selecting an Appropriate PSS Injector Liner
Select the correct PSS liner for your application and pack it with quartz wool.
The PSS injector uses the following three liners:
•
PSS injector wide-bore liner (Part Number N612-1004); 2.0-mm i.d.
•
PSS injector narrow-bore liner (Part Number N612-1006); 1.0-mm i.d.
•
PSS injector on-column (hourglass) liner (Part Number N610-1539)
In general, operate the PSS in the inlet-programmed mode with the 2-mm or 1mm-i.d. liner for PSS split or splitless injection. For PSS on-column operation,
use the hourglass liner and the oven-program mode.
The 2-mm-i.d. PSS liner that is used for either split or splitless operation should
be packed with quartz wool as described in this chapter. The 1-mm-i.d. PSS liner
may give better early-eluting peak resolution in the split or splitless mode. It
should be used for samples with early-eluting peaks for which additional solute
trapping/focusing cannot be obtained by lowering the initial oven temperature or
by using a column with thicker stationary-phase film.
9-30
Clarus 500 GC Hardware Guide
Packing the PSS Injector Liner with Quartz Wool
CAUTION
Never pack the hourglass liner with quartz wool.
Pack a small amount of quartz wool in the top portion of the liner to wipe the
syringe needle regardless of the liner type or injector mode (for example, split or
splitless). Packing assures that reproducible volumes are injected by wiping the
syringe needle every time it is inserted.
Remove the liner and replace the quartz wool packing on a regular basis,
particularly if your samples contain nonvolatile components that could build up
on the wool. This could cause adsorption of peaks of interest, tailing, and loss of
sensitivity. You can remove the wool by making a small hook on the end of a
thin wire and using that to pull it out, or blow it out using compressed air.
NOTE: To avoid contaminating the quartz wool when packing the injection liner, wear
vinyl, powder-free, disposable gloves (for example, the same type of gloves worn
when performing maintenance on a mass spectrometer).
Packing a CAP Injector Liner for Split Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then, using the supplied 1/16-inch rod (Part Number
N610-T100), push the quartz wool into the liner. Pack the wool tightly∗ from the
dimple upwards [about 1 in. (2.5 cm)]. Loosely pack quartz wool in the top
portion of the liner to wipe the syringe needle upon injection.
* The recovery of high-molecular-weight components (e.g., C40
and higher) may be improved if the liner is packed loosely.
9-31
Maintenance
Packing a CAP Injector Liner for Splitless Operation
Take a small piece of quartz wool and twist it into an elongated shape so that you
can insert it into the liner. Then, using the supplied 1/16-inch rod (Part Number
N610-T100), push the quartz wool into the liner. Pack a 1-inch (2.5 cm) piece of
quartz wool loosely below the top ground portion of the liner (see the following
figure). The sample is then injected into the wool, thereby preventing the delivery
of sample beyond the column. The wool also wipes the syringe needle upon
injection.
NOTE: The narrow-bore liner is more difficult to pack because of its small inner
diameter. However, there is a dimple in the middle of the liner to hold the wool in
place. Do not pack the wool too tightly!
Figure 9-19 PSS injector liners packed with quartz wool
NOTE: As you can see in the preceding figure, each PSS injector liner has an O-ring
installed near the end furthest away from the dimple. If the O-ring has adhered to
9-32
Clarus 500 GC Hardware Guide
the liner, it may not be easy to remove the liner. If this is the case, use a small
screwdriver to dislodge the O-ring before removing the liner and O-ring.
Reinstalling the Liner in the PSS Injector
1. Install a new O-ring on the top portion of the liner.
2. Insert the liner in the injector body.
3. Place the septum purge assembly over the liner.
4. Press the septum purge assembly down to correctly position the liner in the
injector.
Make sure that you secure the septum purge assembly tightly to the injector base
with the 1/4-inch spanner.
Removing a Broken Liner from the PSS Injector Body
If a liner breaks in the PSS injector body, the best way to remove all pieces of
quartz is to remove the injector from the Clarus 500 GC.
To remove a broken PSS liner from the injector:
1.
Turn off the Clarus 500 GC. Allow the injector to cool until it is slightly
warm to the touch.
2.
Disconnect and remove the column from the injector.
3.
Loosen the two screws the secure the Clarus 500 GC top cover and raise
the top cover until it locks in the raised position.
4.
Remove the top cover from the PSS injector. Mark the position of the
injector on the metal deck with a pencil.
5.
Remove the screw that secures the fan assembly to the PSS injector, then
remove the fan assembly (see the following figure).
6.
Remove the two screws that secure the PSS injector to the metal deck.
7.
Remove the cable clamps that hold the heater and sensor wires and the
gas tubing (see the following figure).
9-33
Maintenance
8.
Carefully lift the PSS injector out of the Clarus 500 GC. Invert the PSS
injector and remove all of the broken quartz liner from it.
9.
Reinstall the PSS injector to the Clarus 500 GC and reinstall the fan
assembly.
10.
Lower the Clarus 500 GC top cover and properly align the PSS injector
with the top cover before you completely tighten the PSS injector
mounting screws.
Figure 9-20 Removing the fan assembly from the PSS injector
CAUTION
To prevent autosampler needle damage after the Clarus 500 GC top
cover has been opened and closed, verify that the autosampler tower
is aligned with both injectors.
Do this by manually rotating the autosampler tower and stopping over
injector 1 and injector 2 to check that the vial locator is in the center of
the septum cap. If the vial locator does not align with the center of the
septum cap, loosen the two hold-down screws that secure the top cover
(see Figure 9-22). Then move the top cover so that the vial locator is
aligned with the center of the septum cap. Secure the Clarus 500 GC top
cover in this position by tightening the two screws.
9-34
Clarus 500 GC Hardware Guide
Figure 9-21 Location of the cable clamps that secure the wires and tubing
9-35
Maintenance
Changing the Charcoal Trap or Replacing
Charcoal on the Split/Splitless CAP and PSS
Injectors
The charcoal trap will eventually become saturated. When this occurs, ghost
peaks and changes in split ratio will be observed.
Removing a Charcoal Trap
1.
Turn off the Clarus 500 GC. Allow the injectors/detectors to become
cool to the touch.
2.
Loosen the two hold-down screws on the top cover of the Clarus 500 GC
(see following figure) and raise the top cover until the cover locks in the
raised position.
Figure 9-22 Location of the top cover hold-down screws
3.
9-36
Remove the septum cap, then remove the top cover from the injector.
Clarus 500 GC Hardware Guide
4.
Loosen the threaded collar using the 1/4-inch spanner (Part Number
N610-1359) provided, then remove the threaded collar.
5.
Replace the septum cap on the injector.
6.
Pull the septum cap upwards to remove the septum purge assembly.
7.
Using an 1/8-inch wrench, loosen the fittings that are connected to the
charcoal trap and remove the charcoal trap (see the following figure). If
you have a PPC charcoal trap, use a 1/4-inch wrench to loosen the fitting
that connects the trap to the transducer.
9-37
Maintenance
Installing a New Charcoal Trap
1.
Install a new PPC version charcoal trap (Part Number N610-0331) or the
manual pneumatics version charcoal trap (Part Number N610-0275), or
just replace the charcoal in your current trap.
For Manual Pneumatics (Part Number N610-0275)
Replace the charcoal by removing the glass wool plug from the 1/4-inch tubing
end of the charcoal filter. Empty the old charcoal from the charcoal filter.
Repack the charcoal filter with activated charcoal (30-60 mesh, Part Number
0330-0904). Plug the end of the charcoal filter with a small piece of silanized
glass wool. Reinstall the charcoal trap.
For PPC Pneumatics (Part Number N610-0331)
Replace the charcoal by removing the glass wool plug from the 1/4-inch tubing
end. Empty the old charcoal and the glass wool plug at the 1/8-inch end. Push a
small glass wool plug from the 1/4-inch end to the end of the 1/4-inch tube (near
the 1/8-inch end) then fill with charcoal (Part Number 0330-0904) and plug the
end with a small piece of silanized glass wool.
Figure 9-23 Charcoal Trap on an injector controlled by PPC (left) or
manual pneumatics (right)
2.
9-38
Replace the septum purge assembly and remove the septum cap.
Clarus 500 GC Hardware Guide
3.
Replace the threaded collar and tighten it using the spanner.
4.
Replace the injector cover then replace the septum cap.
5.
Lower the Clarus 500 GC top cover and tighten the two hold-down
screws.
CAUTION
To prevent autosampler needle damage after the Clarus 500 GC top
cover has been opened and closed, verify that the autosampler tower
is aligned with both injectors.
Do this by manually rotating the autosampler tower and stopping over
injector 1 and injector 2 to check that the vial locator is in the center of
the septum cap. If the vial locator does not align with the center of the
septum cap, loosen the two hold-down screws that secure the top cover
(see Figure 9-22). Then move the top cover so that the vial locator is
aligned with the center of the septum cap. Secure the Clarus 500 GC top
cover in this position by tightening the two screws.
9-39
Maintenance
ECD Maintenance
If you observe that the ECD background is higher than normal for your operating
conditions, the cell could be contaminated.
You can view the ECD background reading from the Clarus 500 GC touch screen
by selecting the signal tab in the ECD tab. Also select the signal tab to display
the detector background and the AutoZero button. Press the AutoZero button to
have the system on autozero.
Under normal operating conditions, the ECD background will be up to 7 mV.
If you suspect cell contamination, first eliminate column bleed by lowering the
oven temperature to ambient. If bleed is not the problem and the high background
coincided with changing the carrier gas tank, the carrier gas may be
contaminated. To check for this condition:
1. Cool the ECD to <100 ºC.
2. Remove the column from the ECD, then cap the ECD with a 1/8 inch steel
plug (Part Number 0990-3098).
3. Increase the make-up flow. If the background remains the same as the makeup flow increases, the carrier gas could be contaminated. (The ECD is a
concentration-sensitive detector. Increasing the make-up gas flow would
normally dilute the contamination and cause a decrease in the background.)
If bleed or carrier gas contamination is not the problem, bake the ECD using
the following procedure.
Baking the ECD
1. Remove the column, then cap the ECD with a plug (Part Number 09903098).
2. Increase the flow of make-up gas to 60 mL/min and raise the detector
temperature to 450 °C.
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Clarus 500 GC Hardware Guide
3. Bake the system until the background returns to normal levels. This could
take from hours to several days.
NOTE: It may also help to remove the column and increase the oven temperature to 450
°C to bake out the lower portion of the ECD body.
Changing the Charcoal Traps
The ECD is shipped with charcoal traps (Part Number N660-0037) installed in
the make-up and injector pneumatics lines to remove contamination from the
needle valve, flow controller, or pressure regulator. The traps should be replaced
periodically.
To change charcoal traps:
1. Turn off the Clarus 500 GC and allow the injectors/detectors to cool.
2. Loosen the two hold-down screws on the Clarus 500 GC top cover (see
Figure 9-22) and raise the top cover until it locks in the raised position.
3. Disconnect the charcoal traps from the make-up gas and injector lines.
4. Install new charcoal traps.
Cleaning the ECD Anode
WARNING
THE FOLLOWING PROCEDURE MUST BE PERFORMED ONLY AT
LABS THAT HOLD A SPECIFIC NRC LICENSE, NOT A GENERAL
LICENSE. ALL OF THE MATERIALS USED TO CLEAN THE ANODE
MUST BE DISPOSED OF IN ACCORDANCE WITH THE NRC
REGULATIONS REGARDING RADIOACTIVE MATERIAL.
NOTE: If a dirty or contaminated ECD is suspected, try baking out the detector before
using this procedure.
NOTE: Wear plastic or rubber gloves when cleaning the ECD anode.
To clean the ECD anode:
9-41
Maintenance
1. Turn off the ECD heater and allow the system to cool to room temperature.
2. Unscrew the knurled ring and lift out the anode assembly (see the following
figure).
3. Place the collector assembly on top of a beaker of hexane with the anode
tube submerged and soak for several minutes. DO NOT submerge the side
arm in the hexane; submerge only the anode.
4. Remove the anode assembly and wipe it dry with a tissue.
5. Replace the anode assembly, then tighten the knurled ring.
6. Turn on the detector temperature and observe that the background signal has
returned down to a normal level.
Figure 9-24 Isometric view and cross section view of the ECD
9-42
Clarus 500 GC Hardware Guide
Wipe Testing an ECD Cell
CAUTION
Until the results of the wipe test are known, use caution and suitable
protection when handling the cell and equipment in contact with it. Wear
disposable plastic or rubber gloves when performing this test.
It is strongly recommended that you become familiar with the NRC regulation
covering the use of Nickel-63, as well as any other national, state, or local
requirements.
To perform the wipe test:
1. Turn the instrument off and allow the detector to become cool to the touch.
2. Gain access to the detector by lifting the detector cover (see the following
figure).
9-43
Maintenance
Figure 9-25 The detector cover
3. Remove the two screws holding down the ECD insulating cover, then
remove the insulating cover (see the following figure). (Removing the
insulating cover exposes the knurled ring and detector outlet.)
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Clarus 500 GC Hardware Guide
DO NOT DISMANTLE THE ECD CELL!
WARNING
Figure 9-26 ECD insulating cover
9-45
Maintenance
Figure 9-27 ECD surfaces to wipe
4. Using the instructions included with the wipe-test kit (Part Number 00091667) supplied with the detector, wipe the external surfaces of the items
shown in the previous figure with the “low Activity Source” filter papers or
stick swab:
CAUTION
9-46
•
Detector outlet
•
Knurled ring
•
Detector fitting
Do not remoisten the wipe-test paper once it has been moistened or
any part of the ECD has been wiped. Do not allow any of the wipetest solution to enter the cell.
Clarus 500 GC Hardware Guide
5. Place the wipe-test paper in the container provided in the wipe-test kit.
Include a data sheet stating that the wipe test was performed on a
PerkinElmer electron capture detector cell (Part Number N610-0063) and the
date of the test.
6. Request a new wipe-test kit to be sent with the test results.
7. Return the envelope to:
National Leak Test Center
P.O. Box 486
North Tonawanda, New York 14120
Tel: 716-693-0550
NOTE: The sensitivity of the wipe test is 0.0001 µCi.
9-47
Maintenance
Disposal and Refurbish/Refoil of an ECD Cell
If it is necessary to dispose of an ECD cell, contact:
Nuclear Radiation Development Corp.
2937 Alt. Blvd. North
Grand Island, NY 14072
Tel: (716) 773-7634
Fax: (716) 773-7744
for disposal instructions and current fees.
In addition, report the ECD cell disposal to:
PerkinElmer Instruments LLC
Radiation Safety Officer
710 Bridgeport Ave.
Shelton CT 06484
and
Nuclear Material Safety and Safeguard
U.S. Nuclear Regulatory Commission
Washington, DC 20251
and/or
your state and local agency, if applicable.
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Clarus 500 GC Hardware Guide
FID Maintenance
FID maintenance consists of replacing the FID jet, cleaning the FID jet, replacing
an o-ring in the collector, and cleaning the FID collector and cap.
Replacing a FID Jet
NOTE: The FID jet rarely becomes plugged. However, if plugging occurs, it is usually
sample dependent. It is recommended that you replace a plugged jet rather than
clean it.
To replace the FID jet:
Before you begin, extinguish the flame via the keyboard by setting the
hydrogen flow to “0” or if you have manual pneumatics, turn the
outer knob on the hydrogen needle valve completely clockwise to off.
WARNING
1.
Turn off the Clarus 500 GC power.
The FID is hot and can cause serious burns! To prevent injury, allow
the detector to become cool to the touch.
WARNING
2.
Open the detector cover (see Figure 9-25).
3.
Remove the polarizing cable from the pin on the polarizing filter
assembly.
9-49
Maintenance
Figure 9-28 FID polarizing voltage wire
4.
Loosen the knurled ring, then lift the FID collector off of the FID base
and put it out of the way.
5.
Insert the nozzle removal tool (Part Number N610-3188) into the FID
base and lift the nozzle out of the FID base. Do not unscrew it.
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Clarus 500 GC Hardware Guide
Nozzle Removal
Tool (P/N N610-3188)
Nozzle
FID Base
Figure 9-29 Removing the nozzle assembly from the FID base
6.
Insert a 1/4-inch nutdriver into the FID base to engage the 1/4-inch nut
on the FID jet assembly.
7.
Loosen the FID jet assembly (turn the 1/4-inch nut counterclockwise)
and pull it out of the FID. You should be able to pull out the FID jet
assembly with the nutdriver. If not, then pull out the FID jet assembly
with a pair of forceps or needle nose pliers.
9-51
Maintenance
Figure 9-30 Cross section view of the FID
8.
Insert a new FID jet assembly (Part Number N610-0361) and secure it in
place with the 1/4-inch nut driver.
9.
Insert the nozzle assembly into the FID base until you feel it bottom.
10.
Insert the FID collector back on the FID base and tighten the knurled
ring.
11.
Reconnect the polarizing wire to the polarizing pin on the FID collector.
12.
Turn on the FID heater and allow it to return to the temperature setting.
13.
Re-ignite the flame.
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Clarus 500 GC Hardware Guide
Cleaning a FID Jet
Although it is not recommended, you may try to clean the FID jet as a last resort.
Use one or both of the following techniques:
•
Based on your analytical application, wash the jet with an appropriate
solvent.
•
Dislodge the plug with a fine wire such as a syringe needle, then blow
out loosened debris using compressed air.
Replacing the O-Ring in the FID Collector
Since the O-ring in the FID collector is in contact with the heated surface of the
FID base, you will notice over time that it has become brittle or broken and must
be replaced.
WARNING
The FID is hot and can cause serious burns! To prevent injury,
extinguish the FID flame, turn off the FID heater, and allow the
detector to become cool to the touch.
To replace the O-ring in the FID collector:
1.
Remove the polarizing voltage wire from the polarizing pin (Figure 28).
2.
Loosen the knurled ring, then lift the FID collector off of the FID base.
3.
Remove the old O-ring (see the following figure) from the FID collector
and insert a new O-ring (Part Number 0990-2143).
4.
Insert the FID collector back on the FID base and tighten the knurled
ring.
5.
Connect the polarizing wire to the polarizing pin on the FID collector.
9-53
Maintenance
6.
Turn on the FID heater and allow it to return to the temperature setting.
7.
Re-ignite the flame.
Cleaning the FID Collector and Cap
Occasionally clean the collector and cap if you are running samples that may
generate soot, for example, carbon disulfide.
WARNING
The FID is hot and can cause serious burns! To prevent injury,
extinguish the FID flame, turn off the FID heater, and allow the
detector to become cool to the touch.
To clean the FID collector:
1. If necessary, disconnect the amplifier coaxial cable, and other wires from the
FID collector.
2. Loosen the knurled ring on the collector and remove the collector from the
FID base.
3. Using a pipe cleaner, wipe the inside of the collector and then the outside of
the collector near the top.
4. Wash the collector with a laboratory soap such as Alconox. Try to keep the
side-arm dry.
5. Air dry the collector replace it on the FID base, and tighten the knurled ring
to secure the collector in place.
6. If you disconnected the amplifier coaxial cable and any wires from the FID
collector, reconnect them to the FID collector.
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Clarus 500 GC Hardware Guide
Figure 9-31 View of the FID collector and O-ring
9-55
Maintenance
PID Maintenance
Routine PID maintenance consists of the following:
•
Changing PID lamps
•
Cleaning PID lamp windows
•
Changing PID lamp window seals and positioning disks
Procedures for performing these tasks follow.
WARNING
CAUTION
The PID operates at a high temperature and voltage. To avoid
injury, before attempting maintenance procedures, disconnect the
PID from line power and allow it to cool to room temperature.
To avoid contamination, wear rubber gloves or use tweezers when
disassembling the PID.
Changing a PID Lamp
To change a PID lamp:
1.
Disconnect the instrument from line power.
2.
Allow the system to cool to room temperature.
3.
Place a piece of paper towel to the right of the detector area (see shaded
area in the following figure) to cover the space between the oven skin
9-56
Clarus 500 GC Hardware Guide
and the electronics compartment of the Clarus 500 GC. This will prevent
the lamp housing fasteners (see next step) from falling into the
instrument when they are loosened.
Figure 9-32 Placing a towel in the space between detector and electronics
compartment
4.
Please examine the previous figure. While pressing down on the top of
the PID (lamp housing), remove the four fasteners securing the lamp
housing to the detector and place them in a safe place.
5.
Slowly ease up on the lamp housing. As you do, the spring inside the
housing (see the following figure) will push the housing up. Pull off the
lamp housing and reveal the spring. The spring is quite powerful and it
may shoot off if the lamp housing is removed too quickly.
6.
Remove the spring.
9-57
Maintenance
7.
Replace the worn out or damaged lamp, window seal, and positioning
disk.
8.
Replace the spring and housing.
9.
While holding the lamp housing down tightly, replace the four fasteners
previously removed.
10.
Remove the paper inserted in step 3.
Cleaning PID Lamp Windows
CAUTION
Wear rubber gloves to avoid contaminating the lamp window.
To clean PID lamp windows:
1. Remove the lamp using steps 1 through 7 in the previous procedure.
9-58
Clarus 500 GC Hardware Guide
Figure 9-33 Exploded view of the PID
2. First clean the window with a moist, clean Kimwipe or other lint-free tissue.
Use a gentle, circular motion.
3. Complete the cleaning by using a tissue moistened with cleaning compound
supplied (Part Number 0330-2775).
4. Rinse the window using a warm (30 °C) solution of a mild dishwashing
detergent in water.
9-59
Maintenance
5. Rinse with warm (30 °C) distilled water.
6. Dry with air or a lint-free tissue.
7. Ensure that a new lamp window seal and a new positioning disk are in place
(see Figure 9-33). Then position the lamp over the window seal, place the
spring over the lamp, and place the housing over the lamp and spring.
8. While holding the lamp housing down tightly, replace the four fasteners
previously removed.
Changing PID Lamp Window Seals and Positioning
Disks
CAUTION
New seals and positioning disks must be baked (preferably in a vacuum
oven) before use for one to two hours at 240 °C.
To change PID lamp window seals and positioning disks, refer to the previous
figure and follow this procedure:
1. Wearing rubber gloves to avoid contaminating the lamp window, remove the
lamp using the appropriate steps in the previous procedure.
2. The lamp window seal will either be in the center of the positioning disk or
stuck to the lamp window. Using a pair of tweezers, remove the lamp
window seal.
3. Lift out the positioning disk.
4. Replace the positioning disk with a new one, making certain that you do not
crease or bend it.
5. Place a new lamp window seal in the center of the positioning disk. Viewing
the detector from the end, make certain that the opening in the seal is lined
9-60
Clarus 500 GC Hardware Guide
up with the ion chamber opening. The whole window seal must rest on the
gold-plated ceramic portion of the ionization chamber.
6. Position the lamp over the seal, place the spring over the lamp, and place the
housing over the lamp and spring.
7. Secure the lamp housing with the four fasteners.
Leak-Test
You can check for leaks by turning on the make-up gas and checking the flow
rates at the detector inlet and outlet to make certain they are equal.
9-61
Maintenance
ElCD Maintenance
ElCD maintenance consists of replacing the ElCD reaction tube and cleaning
ElCD cells. It is good practice to periodically replace solvent to avoid possible
contamination due to increasing concentrations of ionic and other materials.
Discard the first 50 – 100 mL of solvent (when replacing the solvent or resin
tube) before cycling solvent through the cell.
Replacing the ElCD Reactor Tube
Figure 9-34 Reactor tube location on the ElCD
1. Turn off the controller and reactor. Allow the reactor to cool to room
temperature.
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Clarus 500 GC Hardware Guide
2. Referring to the previous figure, locate the upper hex nut on top of the
reactor. This nut is attached to a Teflon tube by means of a union. While
holding the upper hex nut with one wrench, loosen the union hex nut with
another wrench. You will then be able to remove the union and Teflon tube
as one piece, exposing the reactor tube.
3. Loosen and remove the screw on the side of the reactor housing. Gently turn
the reactor housing counterclockwise as far as possible. Then gently pull the
reactor tube out, twisting it back and forth if necessary.
4. Locate the end of the new reactor tube that has a cross-drilled hole. Gently
insert this end through the seal until it bottoms, then turn the reactor housing
clockwise as far as possible. Secure the reactor housing by replacing the
screw on the side.
5. Reattach the Teflon tube union and tighten the hex nut loosened in step 2.
6. Set the carrier gas and check for leaks using the procedures in “Setting up the
ELCD,” in the Setting up the Detectors chapter in the Clarus 500 GC Users
Guide (0993-6225).
Replacing the Sealing Ring
The sealing ring should be replaced if you have difficulty either removing or
replacing a reactor tube (see previous page).
To replace sealing rings:
1. Turn off the controller and reactor. Allow the reactor to cool to room
temperature.
2. Refer to previous figure and locate the upper hex nut on top of the reactor.
This nut is attached to a Teflon tube by means of a union. While holding the
upper hex nut with one wrench, loosen the union hex nut with another
wrench. You will then be able to remove the union and Teflon tube in one
piece, exposing the reactor tube.
3. Loosen and remove the screw on the side of the reactor housing. Gently turn
the reactor housing counterclockwise. Then lift the reactor housing from the
assembly and place it to one side.
9-63
Maintenance
4. Using a hollow spin-tight wrench, remove the swaging screw and lift out the
reactor tube with the graphite/Vespel ferrule and metal ring.
5. Insert the new graphite/Vespel ferrule (Part Number N660-1084) and metal
ring (Part Number N660-1085).
6. Locate the end of the new reactor tube that has a cross-drilled hole. Gently
insert this end through the seal until it bottoms, then replace the swaging
screw and tighten it. Replace the reactor housing, turning it clockwise as far
as possible. Secure the reactor housing by replacing the screw on the side.
7. Reattach the Teflon tube union and tighten the hex nut loosened in step 3.
8. Set the carrier gas and check for leaks using the procedures in “Setting up the
ELCD,” in the Setting up the Detectors chapter in the Clarus 500 GC Users
Guide.
Figure 9-35 Location of the ElCD conductivity cell
9-64
Clarus 500 GC Hardware Guide
Cleaning the Conductivity Cell
To clean the conductivity cell, refer to the following figure and follow this
procedure:
1.
Turn off the controller and the hydrogen.
2.
Disconnect the solvent inlet line from the top of the cell and insert it into
the solvent reservoir.
3.
Disconnect the gas inlet line from the side of the cell.
4.
Pull the cell body away from the cell mounting bracket and slip off the
solvent return line from the bottom of the cell.
5.
Remove the screws from the bottom of the cell.
6.
Pull out the electrode assembly.
Figure 9-36 Cross section view of the ElCD conductivity cell
7.
Pull out the inner electrode and place it in a 100-mL beaker.
9-65
Maintenance
8.
Cover the inner electrode with distilled water and sonicate for 10
minutes. Discard the water.
9.
Repeat steps 7 and 8 using n-propanol.
10.
Reassemble and install the cell, following steps 7 back to 1.
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Clarus 500 GC Hardware Guide
NPD Maintenance
NPD maintenance consists of changing and conditioning the NPD bead and
replacing a NPD jet.
Changing the NPD Bead
The Nitrogen Phosphorus Detector utilizes a glass bead containing alkali metal
(single bead Part Number N612-0092 or package of five Part Number N6120093) to detect organically bound nitrogen and phosphorus compounds. In time,
the bead will not respond, or the wire on which the bead is placed may break.
The bead is considered a consumable part.
If you cannot achieve a response at your normal operating background (0.25 mV
or greater with the detector range set to x1), increase the potentiometer setting
(try higher settings). If you cannot achieve a response at higher settings, the bead
must be replaced.
NOTE: An indication of a broken bead wire is that the bead does not glow when you
increase the bead potentiometer setting (by turning it clockwise).
To change the NPD bead:
1.
Lift open the detector cover.
2.
Locate the bead potentiometer.
If the NPD is installed in the front detector position, the bead
potentiometer is located on the left side of the detector panel. If the NPD
is installed in the rear detector position, the bead potentiometer is located
on the right side of the detector panel.
3.
Turn the NPD bead off by turning the potentiometer counterclockwise.
NOTE: If two NPDs are installed, turn both beads off, even if you are only replacing one
bead.
4.
Turn off the Clarus 500 GC.
9-67
Maintenance
The gases can remain on during this procedure, but the detector
should be cool to the touch to protect you from getting burned.
WARNING
5.
Remove the NPD collector assembly (see the following figure) by
loosening its knurled ring and lifting the collector assembly upward.
CAUTION
Lift the collector assembly straight up so that it does not chip the
ceramic header of the bead assembly. You may find it easier to
remove the coaxial cable from the collector assembly before you
remove the collector assembly from the detector body (see the
following figure).
6.
Remove the screw that secures the bead transformer assembly to the top of
the Clarus 500 GC oven.
7.
Carefully remove the bead portion from the detector body by lifting the
bead transformer assembly straight up and out of the detector body.
8.
Remove the bead assembly from the transformer assembly by unplugging it
from the connector (see the following figure).
9.
Plug a new bead assembly (Part Number N612-0092) into the connector on
the bead transformer. The connector is keyed so that the bead assembly can
only be inserted one way.
10. Carefully insert the bead portion of the bead assembly in the detector body
as shown in (see the following figure).
11. Secure the bead transformer to the top of the oven with the screw removed
in step 6 of this procedure.
12. Replace the collector assembly on the detector body, and secure it by
tightening the knurled ring. If the coaxial cable was removed, connect it to
the collector assembly.
9-68
Clarus 500 GC Hardware Guide
NOTE: Check that the polarizing wire has not fallen off the detector. If it has, replace it
(Figure 9-37).
13.
Turn on the Clarus 500 GC.
Figure 9-37 Exploded view of the NPD bead assembly
9-69
Maintenance
Conditioning a New NPD Bead for Use with a Packed
Column
CAUTION
Never condition a NPD bead when a column is connected to the detector
fitting. To properly condition the NPD bead, the column must be
removed from the detector fitting and the detector fitting must be
capped.
1.
Open the oven door and allow the oven to cool.
2.
Loosen and remove the column nut from the detector fitting using a 7/16inch wrench. Remove the column from the detector fitting.
3.
Install a 1/8-inch Swagelok plug (Part Number N930-0061) on the
detector fitting. Provide a leak-free seal by tightening the plug with a
7/16-inch wrench.
4.
Close the oven door and continue to flow carrier gas through the column.
5.
Set the hydrogen flow, air flow, and all temperatures to operating
conditions.
6.
Set the detector range to x1.
7.
Select the signal tab
to display the detector background and the
AutoZero button. Press the AutoZero button to have the system on
autozero.
9-70
Clarus 500 GC Hardware Guide
When the bead is turned off, the background value should be 0 ±0.25
mV. Write down the background value with the bead off.
8.
Open the detector cover and locate the bead potentiometer dial (see
Figure 9-33).
If the NPD is detector 1 (front position), the potentiometer is located on
the left side of the panel. If the NPD is detector 2 (rear position), the
potentiometer is located on the right side of the panel.
9.
Turn the bead potentiometer dial clockwise to apply current to the bead.
Slowly increase the setting to 700 on the dial.
The millivolt reading on the autozero display will begin to increase. A
maximum reading of 997.61 mV at a range setting of x1 is required to
condition the bead.
9-71
Maintenance
10.
Monitor the display for about one minute at this setting. If the millivolt
reading is less than 997.61, increase the bead potentiometer setting by an
increment of 10 (to 710) and wait about one minute.
Repeat this process until the bead potentiometer setting produces a
maximum signal of 997.61 mV.
11.
Allow the bead to "condition" at this setting for one hour. The
background readout will drift downward during the process.
12.
After conditioning the bead, lower the bead potentiometer dial setting to
600. Remove the Swagelok plug from the detector fitting and reinstall
the packed column.
13.
Make sure the column flow is properly set and select the signal tab
to display the detector background produced by carrier gas flow and the
AutoZero button. Press the AutoZero button to have the system on
autozero.
The bead background will be less due to cooling effects.
9-72
Clarus 500 GC Hardware Guide
14.
Turn the bead potentiometer dial clockwise until you achieve a reading
of 0.25 mV above the "off" reading, with the detector range set to x1 as
noted in step 7 of this procedure.
15.
Once the system has stabilized, it is ready for operation.
If you are unable to achieve adequate sensitivity for your standard, increase the
background of the NPD. Increasing intervals of 0.25 mV are recommended.
NOTE: 1. The bead will be stable for several hours of operation but will drift in time. At
the start of each day, adjust the background reading to the setting you are using
and allow a few minutes for it to stabilize.
2. Due to the loss of alkali metal with use, the nature of the bead is to drift over
time. We strongly recommend using an internal standard for quantitative
analysis.
3. The bead can operate at higher background settings. The higher the setting the
greater the signal and noise. Therefore, the signal to noise ratio will not increase
dramatically. Operate at the lowest possible setting to achieve the required
sensitivity. This will also prolong the life of the bead.
9-73
Maintenance
CAUTION
The bead should be turned off by turning the bead potentiometer dial
fully counterclockwise before you turn off the Clarus 500 GC.
Remember that the bead has a finite life. You can extend the bead
life by turning the bead off when it is not in use for an extended
period of time (for example, over the weekend).
Conditioning a New NPD Bead for Use with a
Capillary Column (0.53 mm i.d. and smaller)
1.
Make sure the capillary column is installed in the detector (refer to
Chapter 6) and the carrier gas is flowing through the column. If the
column is a wide-bore column, lower the column flow to 1.0 mL/min or
less.
2.
Set the hydrogen flow, air flow, and all temperatures to operating
conditions.
3.
Set the detector range to x1.
4.
Select the signal tab
to display the detector background and the
AutoZero button. Press the AutoZero button to have the system on
autozero.
9-74
Clarus 500 GC Hardware Guide
When the bead is off, the background value should be 0 ±0.25 mV. Write down
the background value with the bead off.
5.
Open the detector cover and locate the bead potentiometer dial.
If the NPD is detector 1 (front position), the potentiometer is located on
the left side of the panel. If the NPD is detector 2 (rear position), the
potentiometer is located on the right side of the panel.
6.
Turn the bead potentiometer dial clockwise to apply current to the bead.
Slowly increase the setting to 700 on the dial.
The millivolt reading on the autozero display will begin to increase. A
maximum reading of 997.61 mV at a range setting of x1 is required to
condition the bead.
7.
Monitor the display for about one minute at this setting. If the millivolt
reading is less than 997.61, increase the bead potentiometer setting by an
increment of 10 (to 710), and wait about one minute.
9-75
Maintenance
Repeat this process until the bead potentiometer setting produces a
maximum signal of 997.61 mV.
8.
Allow the bead to "condition" at this setting for one hour. The
background readout will drift downward during this process.
9.
After conditioning the bead, readjust the column flow if necessary.
10.
Select the signal tab
to display the detector background and the
AutoZero button. Press the AutoZero button to have the system on
autozero.
11.
Turn the bead potentiometer dial clockwise or counterclockwise until
you achieve a reading of 0.25 mV above the "off" reading with the
detector range set to x1 (see step 4 of this procedure).
12.
Once the system has stabilized, it is ready for operation.
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Clarus 500 GC Hardware Guide
If you are unable to achieve adequate sensitivity for your standard, increase the
background of the NPD. Increasing the background in intervals of 0.25 mV is
recommended.
NOTE: 1. The bead will be stable for several hours of operation but will drift in time. At
the start of each day, adjust the background reading to the setting you are using
and allow a few minutes for it to stabilize.
2. Due to the loss of alkali metal with use, the nature of the bead is to drift over
time. We strongly recommend using an internal standard for quantitative
analysis.
3. The bead can operate at higher background settings. The higher the setting the
greater the signal and noise. Therefore, the signal to noise ratio will not increase
dramatically. Operate at the lowest possible setting to achieve the required
sensitivity. This will also prolong the life of the bead.
CAUTION
Before you turn off the Clarus 500 GC, turn off the bead by turning the
bead potentiometer dial fully counterclockwise. Remember that the
bead has a finite life. You can extend the bead life by turning the bead
off when it is not in use for long periods of time (for example, over the
weekend).
Replacing an NPD Jet
NOTE: The NPD jet rarely becomes plugged. However, if the jet does become plugged, it
is usually because of the type of sample used. We recommend replacing a
plugged NPD jet.
To replace an NPD jet:
1.
Turn off the bead by turning the potentiometer dial fully
counterclockwise.
2.
Turn off the Clarus 500 GC.
3.
Turn off the hydrogen and air flows.
4.
Open the detector cover.
9-77
Maintenance
Wait until the detector is cool to the touch to protect you from getting
burned.
WARNING
5.
Loosen the knurled ring on the collector assembly, then remove the
collector assembly (see the following figure).
Figure 9-38 Location of the NPD jet assembly
9-78
Clarus 500 GC Hardware Guide
CAUTION
Lift the collector straight up so that it does not chip the ceramic
header of the bead assembly. You may find it easier to remove the
coaxial cable from the collector before you remove the collector (see
the previous figure).
6.
Remove the screw that secures the bead transformer assembly to the top
of the Clarus 500 GC oven.
7.
Remove the bead assembly from the detector body by lifting the entire
bead transformer assembly straight up and out of the detector body (see
Figure 9-38).
NOTE: Carefully place the bead transformer assembly out of the way so that the bead is
not damaged. You may want to remove (unplug) the bead assembly from the
transformer in order to protect the bead.
8.
Remove the polarizing wire. This exposes a spring-loaded polarizing pin,
which is a piece of wire about 3/8-inch long (see the following figure).
9-79
Maintenance
Liner Removal Tool
(P/N N610-0102)
Nozzle Assembly
Polarizing Cable
Polarizing Pin
NPD Chimney
Figure 9-39 Removing the NPD nozzle assembly and polarizing wire
9.
Grasp and pull the spring-loaded polarizing pin using a pair of needle
nose pliers with your left hand. Maintain a steady pull on the springloaded pin.
10.
With your right hand, insert the large end of the liner removal tool (Part
Number N610-0102) into the NPD chimney so that it engages the nozzle
assembly. Then remove the nozzle assembly by lifting it out.
9-80
Clarus 500 GC Hardware Guide
11.
Still maintaining a steady pull on the spring-loaded polarizing pin, use
your right hand to hold a pair of curved pliers or forceps and remove the
ceramic insulator (not shown) from the detector body.
12.
Still maintaining a steady pull on the spring-loaded polarizing pin, use
your right hand to insert a 1/4-inch nutdriver (Part Number N610-1297
provided in shipping kit) into the NPD chimney (see Figure 9-39) and
engage the nut on top of the NPD jet assembly.
13.
Loosen the NPD jet assembly by turning the nut counterclockwise. Then
pull the jet assembly out of the NPD with the nutdriver.
If you cannot pull the jet assembly out with the nutdriver, use a pair of
forceps or pliers.
14.
Install a new jet assembly (Part Number N610-0038) by reversing steps 5
through 13.
9-81
Maintenance
FPD Maintenance
The most common causes of FPD performance deterioration which results in a
decrease of the signal-to-noise ratio are as follows:
•
Dirty optical filter
•
Dirty detector liner
•
Dirty window
•
Defective photomultiplier tube
•
Dirty jet
Cleaning/Replacing an Optical Filter Assembly
Obtain one of the following filters before you begin:
•
Sulfur Filter Assembly, Part Number N600-0637 (standard shipping
filter) (Purple)
•
Phosphorus Filter Assembly, Part Number N600-0981 (Yellow)
•
Tin Filter Assembly, Part Number L413-5472 (Orange)
To clean or replace an optical filter assembly:
1. Turn off the photomultiplier voltage by selecting the following screen.
Locate PMT Voltage on the screen and select OFF.
9-82
Clarus 500 GC Hardware Guide
2. Extinguish the flame by turning off the hydrogen needle valve. (Turn the
outer knob fully clockwise.)
CAUTION
The photomultiplier tube can be damaged if exposed to light while
voltage is ON. Never remove the detector cap or Photomultiplier tube
WITH the voltage on.
3. Turn off the Clarus 500 GC and allow the detector to cool.
4. Loosen the knurled nut that secures the photomultiplier tube assembly to the
detector body.
5. Slide the photomultiplier tube assembly away from the detector. If the FPD is
detector 1 (front position), slide the photomultiplier tube assembly to the left.
If the FPD is detector 2 (rear position), slide the photomultiplier tube
assembly back.
9-83
Maintenance
6. Remove the filter assembly by pulling it out of the photomultiplier tube
assembly. Clean the filter assembly with lens paper.
7. Insert the cleaned filter or a replacement filter with the colored side facing
the photomultiplier tube assembly. The sulfur filter is purple, the phosphorus
filter is yellow, the tin filter is orange.
8. Insert the filter end of the photomultiplier tube assembly into the detector
body and secure it with the knurled nut.
Cleaning/Replacing the Detector Liner
To clean or replace the detector liner:
1. Turn off the photomultiplier voltage by selecting the following screen.
Locate PMT Voltage on the screen and select OFF.
2. Extinguish the flame by turning off the hydrogen needle valve. (Turn the
outer knob fully clockwise.)
9-84
Clarus 500 GC Hardware Guide
CAUTION
The photomultiplier tube can be damaged if exposed to light while
voltage is ON. Never remove the detector cap or Photomultiplier tube
WITH the voltage on.
3. Turn off the Clarus 500 GC and allow the detector to cool.
4. Remove the cap (see the following figure).
5. Lift out the glass liner and O-ring. Clean the liner by washing it in a soap
solution and/or solvent.
Figure 9-40 Removing a glass liner from the FPD
9-85
Maintenance
6. Insert the glass liner and O-ring into the detector body, then replace the cap.
NOTE: Replace the glass liner (Part Number N600-3057) if it is chipped or if it cannot be
cleaned. Replace a worn O-ring (Part Number 0990-2247).
Cleaning/Replacing the Detector Window
To clean or replace the detector window:
1.
Turn off the photomultiplier voltage by selecting the following screen.
Locate PMT Voltage on the screen and select OFF.
2.
Extinguish the flame by turning off the hydrogen needle valve. (Turn the
outer knob fully clockwise.)
9-86
Clarus 500 GC Hardware Guide
CAUTION
3.
The photomultiplier tube can be damaged if exposed to light while
voltage is ON. Never remove the detector cap or Photomultiplier
tube WITH the voltage on.
Turn off the Clarus 500 GC and allow the detector to cool.
Removing the Window
1.
Loosen the knurled nut that secures the photomultiplier tube assembly to
the detector body.
2.
Slide the photomultiplier tube assembly away from the detector body. If
the FPD is detector 1 (front position), slide it to the left. If the FPD is
detector 2 (rear position), slide it back.
3.
Remove the cap (see the following figure).
4.
Lift out the glass liner and O-ring from the detector body.
5.
Remove the two hex head screws from the base of the FPD by using a
3/32-inch hex wrench. Then lift the detector body off the base.
6.
Remove the spacer from the light pipe on the detector body.
7.
Push the detector window out of the light pipe on the detector body (see
the following figure). You can do this by inserting the end of a small pair
of curved pliers into the top opening on the detector body. Then push the
window out of the light pipe.
8.
Remove the seal from the window.
9-87
Maintenance
Figure 9-41 Removing a FPD detector window
Cleaning and Replacing the Window
1.
Clean the window with soap and water. If necessary, replace the window
and seal (Part Number N930-0096).
2.
Install the seal on the clean window.
3.
Place the detector window on the window holder so that the spring
portion of the seal faces the beveled edge in the window holder (see the
following figure).
4.
Use the spacer to insert the window into the light pipe on the detector
body. Push the window and holder completely into the light pipe.
9-88
Clarus 500 GC Hardware Guide
Figure 9-42. Inserting a seal and window assembly into the FPD body
5.
Insert the detector body on the detector base. Secure the detector body
with the hex screws.
6.
Replace the detector liner, O-ring, and detector cap on the detector body.
7.
Connect the photomultiplier tube assembly to the light pipe on the
detector body.
8.
Turn on the detector heater. Then turn on the photomultiplier tube and
light the flame.
Replacing the Photomultiplier Tube
To replace the photomultiplier tube:
1.
Turn off the photomultiplier voltage by selecting the following screen.
Locate PMT Voltage on the screen and select OFF.
9-89
Maintenance
2.
Extinguish the flame by turning off the hydrogen needle valve. (Turn the
outer knob fully clockwise.)
CAUTION
The photomultiplier tube can be damaged if exposed to light while
voltage is ON. Never remove the detector cap or Photomultiplier
tube WITH the voltage on.
3.
Turn off the Clarus 500 GC and allow the detector to cool.
4.
Remove the two screws from the base of the photomultiplier assembly
using a 7/64-inch hex wrench (see the following figure).
9-90
Clarus 500 GC Hardware Guide
Figure 9-43 Exploded view of a FPD photomultiplier tube
5.
Pull the photomultiplier tube and base out of the housing.
6.
Carefully unplug the photomultiplier tube from the base. Be careful not
to dislodge the O-ring and plastic seal.
7.
Align the key in the new photomultiplier tube with the key hole in the
socket.
8.
Plug the new photomultiplier tube (Part Number 0997-2321) into the
socket in the base.
9-91
Maintenance
CAUTION
9.
Do not force the key into an incorrect position. Do not touch the
glass. Do not expose the photomultiplier tube to any bright, direct
light
Position the photomultiplier tube in the housing so that the cathode (the
horizontal filament grating; not visible in Figure 9-43) faces the detector
body. Align the holes in the plastic seal with the holes in the base.
CAUTION
Make certain that the photomultiplier tube cathode is facing the
detector body
10.
Secure the base to the photomultiplier housing with the two screws
removed in step 4 of this procedure.
11.
Turn on the Clarus 500 GC. Then turn on the hydrogen flow and the
photomultiplier tube, and light the flame.
NOTE: A new photomultiplier tube may require several hours to stabilize.
CAUTION
a.
9-92
When a replacement tube is installed, the noise should be about 2%
at attenuation 8 with the linearizer off. If it is not, modify the
voltage setting until this level of noise is achieved. Adjust the
voltage as follows:
In the System Status screen select Tools for the configuration menu.
Clarus 500 GC Hardware Guide
b.
In the Configuration screen select the FPD photomultiplier screen to
view the voltage
c.
Using the touch pad increase the percent (%) value or to increase the
voltage in 0.1% increments or decrease the voltage in 0.1% increments,
by using the up or down arrows.
NOTE: The millivolt setting is displayed in the upper-right corner. This number will be
close to zero and will only change slightly as the photomultiplier tube voltage is
modified.
Cleaning/Replacing the FPD Jet
To clean or replace the FPD jet:
1. Turn off the photomultiplier voltage by selecting the following screen.
Locate PMT Voltage on the screen and select OFF.
9-93
Maintenance
2. Extinguish the flame by turning off the hydrogen needle valve. (Turn the
outer knob fully clockwise.)
CAUTION
The photomultiplier tube can be damaged if exposed to light while
voltage is ON. Never remove the detector cap or Photomultiplier
tube WITH the voltage on.
3. Turn off the Clarus 500 GC and allow the detector to cool.
4. Remove the two screws from the base of the FPD by using a 3/32-inch hex
wrench. Lift the detector body and the attached photomultiplier tube
assembly off the detector base. This exposes the FPD jet (see the following
figure).
5. Insert a 1/4-inch nutdriver (Part Number N610-1297) over the FPD jet.
9-94
Clarus 500 GC Hardware Guide
6. Turn the nutdriver counterclockwise until the jet assembly is completely
loosened. Then remove the jet assembly from the detector base.
7. Clean the jet in a suitable solvent (such as methanol or acetone) and scrape
off any deposits with a cotton swab on a piece of soft wood. DO NOT
INSERT WIRE OR HARD TOOLS INTO THE JET. Replacement jets are
available from PerkinElmer by ordering Part Number N610-0245.
8. Insert the jet in the detector base and secure it with the 1/4-inch nutdriver.
9. Replace the detector body and the attached photomultiplier tube assembly.
10. Turn on the Clarus 500 GC. Then turn on the hydrogen flow and the
photomultiplier voltage, and light the flame.
9-95
Maintenance
Figure 9-44 Cutaway view of a FPD showing the jet assembly
9-96
Clarus 500 GC Hardware Guide
PPC Maintenance
PPC maintenance consists of replacing a plugged or restricted PPC module
restrictor.
Replacing a Restrictor
To replace a restrictor:
1.
Locate the PPC module on the rear of the Clarus 500 GC.
Figure 9-45 Location of a PPC module restrictor
2.
Turn off all gases to the module on which you are replacing the
restrictor.
3.
Using a 1/2-inch socket or open-end wrench, loosen and remove the
restrictor and install a new restrictor.
4.
Turn on the gas and check for leaks.
5.
Calibrate the PPC module.
9-97
Maintenance
Zeroing the Pressure
The Clarus 500 GC PPC modules are zeroed at the factory, prior to shipping, but
it should be periodically checked to identify any change. This is particularly
important if there have been large changes in the ambient temperature from
22 ºC. For information about zeroing the pressure, refer to the “Clarus 500 Users
Guide.”
PPC Restrictor Information
Available Restrictors
Restrictor Number
Color
Helium Flow at 30 PSIG, vent
to atmosphere
1
Silver
1 mL/min
2
Red
3 mL/min
3
Yellow
10 mL/min
4
Black
30 mL/min
5
Green
100 mL/min
6
Blue
300 mL/min
9-98
Clarus 500 GC Hardware Guide
Restrictors for Carrier Gas Control
Injector
Restrictor
Number
Helium Flow (mL/min)
(with a 90 psig inlet pressure and a
10 psig drop across the restrictor)
Packed
4 (std)
30
Split/Splitless or
PSS
6 (std)
300
Split/Splitless or
PSS
4 (acc)
30
POC
3 (std)
10
POC
2 (acc)
3
9-99
Maintenance
Restrictors for Detector Gas Control
NOTE: Maintain an inlet pressure between 60 and 90 psig.
Detector
Gas
Restrictor
Number
Nominal Flow
Required
(mL/min)
FID
Air
6
450
FID
Hydrogen
4
45
NPD
Air
5
100
NPD
Hydrogen
1
2
FPD
Air
5
90
FPD
Hydrogen
4
75
ECD
Argon/Methane 4
30
ECD
Nitrogen
4
30
TCD
Helium
4
30
TCD
Hydrogen
3
30
ElCD
Hydrogen
3
25
9-100
Clarus 500 GC Hardware Guide
Practical Hints
Reversing TCD Polarity
The following examples indicate when you may want to change the TCD
polarity.
•
When one of the components being analyzed has a higher thermal
conductivity than the carrier gas.
•
For example, if hydrogen is a sample component and helium the carrier
gas, set up a timed event to reverse the polarity of the TCD prior to
elution of the hydrogen (to generate a positive peak for the hydrogen).
Then change the polarity back for the remaining components.
•
If negative peaks are produced when two packed injectors are installed,
each has a different column attached, and you are running two different
analyses. Change the polarity to produce positive peaks.
•
When two packed injectors are installed with two identical columns and
the TCD is being operated at maximum sensitivity. In this case, alternate
the column into which the sample is being injected in order to expose
both sets of filaments (reference and sample) to sample, thus keeping the
filaments more electrically balanced.
•
To change the TCD polarity, enter a negative detector range. For
example, TCD ranges of +2 and –2 have opposite polarities.
Optimizing FID Performance
FID sensitivity is affected primarily by the hydrogen flow. The optimum
hydrogen flow varies slightly if the column flow changes dramatically. For
example, if you go from a packed column with a flow rate of 30 mL/min or
higher to a capillary column with flows of 2 mL/min or less, the optimum
hydrogen flow will be a different value.
9-101
Maintenance
The hydrogen flows recommended in this manual assume packed column flow
rates. If you switch from a packed to a capillary column, re-optimizing the
hydrogen flow will help to improve the FID sensitivity.
The following is the suggested FID optimization procedure after you have
switched from a packed to a capillary column.
1. Prepare a one component standard.
2. Set up the carrier gas flow.
3. Set up the hydrogen and air flows, then ignite the flame.
4. Make 2 to 3 injections at varying hydrogen flows.
The optimum hydrogen flow is that which produces the maximum area counts.
Optimizing ElCD Performance
You may improve the response on the ElCD by setting a slightly lower hydrogen
flow. When using a standard injector at several different hydrogen flows (from
25 mL/min to 10 mL/min), select the hydrogen flow setting that provides the best
signal.
Filtering Detector Output
You can select one of three software filters from the Filter Menu.
If your column delivers a peak width at half height of ≥1 s, select 200. If your
column delivers a peak width at half height of <1 s, select 50.
A value of 800 should be used only with caution to minimize the signal-to-noise
ratio. Try 800 with your application. If the peak height and area are not affected
but the noise is decreased, then 800 will improve the signal-to-noise ratio.
NOTE: The ECD has values of 200 and 800 only.
9-102
Clarus 500 GC Hardware Guide
Autozero Display Sensitivity
The maximum detector signals for various detectors that produce a 1-V reading
on the Autozero Display are as follows:
FID, NPD, or PID (nA, Range 1) – 21.3
FID, NPD, or PID (nA, Range 20) – 426
TCD (mV) – 510
ECD (KHz) – 150
ElCD (V) (10-V input selected) – 10
∗
∗
ElCD (V) (1-V input selected) – 1
Install the ElCD by connecting the 10-V output from the ElCD control box to the
10-V input on the ElCD Clarus 500 GC amplifier.
9-103
Maintenance
Attenuation vs. Detector Output
The following table lists attenuation vs. the maximum detector signal producing
100% deflection on a 1-mV recorder.
1
NPD, PID
and FID (fA)
Range 1
3.3x102
2
6.7x102
4
Atten
NPD, PID
and FID (fA)
Range 20
6.7x103
TCD (µV)
ECD (Hz)
ElCD (µV)
10-V input
ElCD (µV)
1-V input
1.7x101
8.0
2.3
1.7x10
2
1.3x104
1.6x10
4.7
3.4x10
2
3.4x101
1.3x103
2.7x104
3.2x10
9.4
6.3x10
2
6.3x101
8
2.7x103
5.3x104
6.4x10
19.0
1.3x10
3
1.3x102
16
5.3x103
1.1x105
1.3x102
38.0
2.5x10
3
2.5x102
32
1.1x104
2.1x105
2.6x102
75.0
5.0x10
3
5.0x102
64
2.1x104
4.3x105
5.1x102
150.0
1.0x10
4
1.0x103
128
4.3x104
8.5x105
1x103
3.0x10
2
2.0x10
4
2.0x103
256
8.5x104
1.7x106
2x103
6.0x10
2
4.0x10
4
4.0x103
512
1.7x105
3.4x106
4.1x103
1.2x10
3
8.0x10
4
8.0x103
1024
3.4x105
6.8x106
8.2x103
2.4x10
3
1.6x10
5
1.6x104
2048
6.8x105
1.4x107
1.6x104
4.8x10
3
3.2x10
5
3.2x104
4096
1.4x106
2.7x107
3.3x104
9.6x10
3
6.4x10
5
6.4x104
8192
2.7x106
5.5x107
6.6x104
1.9x10
4
1.3x10
6
1.3x105
16384
5.4x106
1.1x108
1.3x105
3.8x10
4
2.6x10
6
2.6x105
9-104
Clarus 500 GC Hardware Guide
32768
NPD, PID
and FID (fA)
Range 1
1.1x107
65536
2.2x107
Atten
NPD, PID
and FID (fA)
Range 20
2.2x108
4.4x108
TCD (µV)
ECD (Hz)
2.6x105
7.7x10
4
5.2x105
1.5x10
5
ElCD (µV)
10-V input
5.1x10
6
ElCD (µV)
1-V input
5.1x105
1.0x106
1.0x10
7
The following table lists attenuation vs. the maximum detector signal producing a
1-V output to an integrator.
Atten
NPD, PID
and FID (pA)
Range 1
NPD, PID
and FID (pA)
Range 20
1
2
4
8
16
32
64
3.3x102
6.7x102
1.3x103
2.7x103
5.3x103
1.1x104
2.1x104
6.7x103
1.3x104
2.7x104
5.3x104
1.1x105
2.1x105
4.3x105
TCD (mV)
ECD (kHz)
8.0
1.6x10
3.2x10
6.4x10
1.3x102
2.6x102
5.1x102
2.3
4.7
9.4
19.0
38.0
75.0
150.0
ElCD
(mV)
10-V input
ElCD
(mV)
1-V input
1.7x102
3.4x102
6.3x102
1.3x103
2.5x103
5.0x103
1.0x104
1.7x101
3.4x101
6.3x101
1.3x102
2.5x102
5.0x102
1.0x103
Prolonging the Life of a PID UV Lamp
Lamp life decreases at elevated temperatures. (For example, when conditioning
the detector above 250 °C.) To increase lamp life, substitute a disc (Part Number
N0330-2989) for the UV lamp during such procedures.
Optimizing ECD Performance
ECDs are extremely sensitive. Therefore, care should be taken to avoid
contamination from any part of the system (for example, pneumatics, injector,
column, gases, etc.). To help assure a clean system: condition the column, bake
out the injector and detector, use clean tubing, and use pure filtered gases.
9-105
Maintenance
CAUTION
To minimize detector contamination, run the ECD hot, at a
temperature of at least 375 °C.
Optimizing FPD Performance
About Ionization Gas Flows
FPD sensitivity is affected by both the hydrogen flow and the air flow. Hydrogen
has a true optimum flow; that is, above or below a certain flow there is less
response. Air, on the other hand, is more critical. That is, below a certain flow
there is no response at all. The flows provided in the Clarus 500 Users Guide are
in the optimum range, but there may be slight variation from detector to detector.
Optimizing FPD Gas Flows
To optimize gas flows:
1.
Set the hydrogen flow to 65 mL/min.
2.
Set the air flow to 90 mL/min.
3.
Set the detector temperature to 250 °C, and wait for the detector to reach
that temperature.
4.
Light the flame.
5.
Prepare a one-component standard (sulfur, phosphorus, or tin, depending
on the filter installed).
6.
Make two or three injections.
7.
Increase the hydrogen flow by 5 mL/min and repeat the injections.
8.
Continue increasing the hydrogen, and running the sample, until a
maximum signal is obtained. Set the hydrogen at that flow.
9-106
Clarus 500 GC Hardware Guide
9.
Repeat the above procedure, varying the air flow by 5 mL/min (both
below and above 90 mL/min).
10.
Set the air flow to at least 10 mL/min above the flow that previously
produced no response.
Quenching
When hydrocarbons co-elute with the sulfur compound (or phosphorus or tin
compound depending on which filter is being used), they will “quench” the
flame, thereby causing a diminished response, or no response at all, to the peak
of interest. To avoid this problem, complete separation and elution of all peaks is
necessary. Because the FPD is a selective detector, hydrocarbons may not show
as significant peaks. We recommend that you first profile your sample by using
the same column with either an FID or TCD. All peaks will then be seen and you
can determine the necessary conditions to completely separate and elute all
compounds.
PSS and POC Operating Hints
Both of the Programmed Split/Splitless (PSS) and Programmed On-Column
(POC) injectors can be operated in either the oven programming mode or the
inlet programming mode. For specific operation, refer to the Clarus 500 Users
Guide.
Oven Programming Mode
This is the default mode for both the POC and the PSS injectors. This mode is the
easiest to use, since only the oven temperature program needs to be entered into
the method. In this mode, the injector will follow the oven temperature profile
plus 5 °C. In this mode, the sample should be introduced into the injector when
the temperature of the inlet is at the boiling point of the solvent. Then
temperature program the injector and oven.
If the initial temperature of the oven is above the boiling point of the solvent you
are using, then it would be better to modify the oven program to start at a lower
temperature or to configure the injector for the Inlet mode and set a temperature
for the injector separate from the oven temperature.
9-107
Maintenance
Inlet Programming Mode
This mode permits the use of independent injector temperatures and rates that
you define in the method. The injector will be programmed for injector
temperature 1, injector time 1, injector rate 1, injector temperature 2, injector
time 2, etc. You can program up to three temperatures and two ramps for each
PSS or POC configured in the inlet mode.
It is important to set the initial injector temperature to about the boiling point of
the solvent you are using.
CAUTION
CAUTION
9-108
The PSS injector can be used in the "hot" split or splitless mode.
However, this is not recommended due to liner size and could cause
solvent flashback in the injector. This mode should be used with
caution, depending upon the solvent and temperatures you choose.
When using the PSS injector in the on-column mode or the POC
injector with the autosampler, you must use a special syringe that has
a needle o.d. of 0.47 mm (Part Number N610-1253 or N610-1380).
Refer to the Clarus 500 Users Guide for more detail. You must use
only the "Norm" injection speed with this syringe in the on-column
mode. The "Fast" injection speed will bend this thin needle and the
"Slow" injection speed may produce peak breakup or distorted peaks.
You can achieve better precision in the on-column mode when sample
volumes of 1.0 L or greater are injected.
Clarus 500 GC Hardware Guide
CAUTION
If you have the subambient option, the POC and PSS injectors are
linked to the oven subambient option; therefore, you cannot operate
the injectors below the oven subambient temperature.
If a column is used extensively at high temperatures (350 °C or greater), the
polyimide may become very brittle. This brittleness will cause the column to
fracture when you try to seal it in the universal adapter. If you wish to continue to
use the brittle column, a low dead volume union may be a helpful alternative.
9-109
Maintenance
PPC Restrictor Information
Available Restrictors
Restrictor Number
Color
Helium Flow at 30 PSIG, vent to
atmosphere
1
Silver
1 mL/min
2
Red
3 mL/min
3
Yellow
10 mL/min
4
Black
30 mL/min
5
Green
100 mL/min
6
Blue
300 mL/min
Restrictors for Carrier Gas Control
Injector
Restrictor
Number/Color
Helium Flow (mL/min)
(with a 90 psig inlet pressure and a 10
psig drop across the restrictor)
Packed
4 (std)/Black
30
Split/Splitless or
PSS
6 (std)/Blue
300
Split/Splitless or
PSS
4 (acc)/Black
30
POC
3 (std)/Yellow
10
POC
2 (acc)/Red
3
9-110
Clarus 500 GC Hardware Guide
Restrictors for Detector Gas Control
NOTE: Maintain an inlet pressure between 60 and 90 psig.
Detector
Gas
Restrictor
Number/Color
Nominal Flow
Required (mL/min)
FID
Air
6/Blue
450
FID
Hydrogen
4/Black
45
NPD
Air
5/Green
100
NPD
Hydrogen
1/Silver
2
FPD
Air
5/Green
90
FPD
Hydrogen
4/Black
75
ECD
Argon/Methane
4/Black
30
ECD
Nitrogen
4/Black
30
TCD
Helium
4/Black
30
TCD
Hydrogen
3/Yellow
30
ElCD
Hydrogen
3/Yellow
25
9-111
Maintenance
9-112
Troubleshooting
10
Troubleshooting
10-2
Clarus 500 GC Hardware Guide
This chapter contains the following sections:
•
Instrument Error Messages
•
Autosampler Error Messages
•
GC Troubleshooting
•
ElCD Troubleshooting
10-3
Troubleshooting
Error Messages
The error messages are shown on the touch screen display.
Table 10-1 Instrument Error Messages
Error Messages
Timed Events Error
Events table is full.
32 events maximum.
Timed Events Error
Duplicate event time.
Enter a value at least 0.1 minute different.
RS 232 Timeout Error.
Device failed to respond within specified time frame.
Oven Control Error
No Coolant available. Check coolant supply.
PPC Hardware Fault
Power instrument OFF, wait 10 seconds and then power ON. If problem persists
Call your PerkinElmer Service representative.
AutoSampler Error
No vial found at location xx.
AutoSampler Error
No autosampler programs active.
Background Calibration Error
Isothermal Method selected. Background calibration required temperature program
method.
Background Calibration Error
Negative temperature ramp specified. Background calibration requires positive
temperature ramps.
Background Calibration Error
Run Time is less than 1.0 minute.
Background Calibration Error
Run Time is greater than 999 minutes.
Background Calibration Error
HOLD Event is present in temperature program ramp. This is not permitted.
10-4
Clarus 500 GC Hardware Guide
Error Messages Continued
No Inlet Configured
Select Configuration on the Tools menu to access configuration settings.
No Detector Configured
Select Configuration on the Tools menu to access configuration settings.
Flow Calibration Error
Flow too high for ‘low’ calibration.
Check flow and repeat calibration.
Flow Calibration Error
Flow too low for ‘hi’ calibration.
Please check flow and repeat calibration.
AutoSampler Error
Access door open.
Close door.
AutoSampler Error
No post wash specified. Set post-inject field in configuration to a minimum of 1.
Relay Fault
Turn power OFF for 10 seconds and then ON. If problem persists Call your
PerkinElmer Service representative.
Temperature Error
Unable to reach specified temperature.
Check coolant.
PPC Error
PPC Carrier xx not connected.
Check PPC Carrier module connections.
PPC Error
PPC Detector xx not connected.
Check PPC Detector module connections.
PPC Error
The AUX flow PPC module being calibrated is not connected.
Connect the AUX PPC flow module and calibrate.
PPC Error
Selected connection is currently assigned.
Select another connection.
PPC Error
Warning: the PPC Alarm is OFF! If this is correct, press OK.
To enable the PPC Alarm, select PPC Alarm ON in configuration setup.
10-5
Troubleshooting
Error Messages Continued
Ignite Error
The detector xx failed to ignite.
Check the hydrogen and air flows.
Ignite Error
The detector xx failed to ignite.
The hydrogen and air supplies are OFF. Turn the gases ON.
Table 2 Oven Error Messages.
Oven Error Messages
Temperature sensor fault OPEN. Cycle the power OFF for 10 seconds then
ON. If the error persists call the PerkinElmer Service Center.
Temperature sensor fault SHORT. Cycle the power OFF for 10 seconds then
ON. If the error persists call the PerkinElmer Service Center.
No Heat. Cycle the power OFF for 10 seconds then ON. If the error persists
call the PerkinElmer Service Center.
Temperature exceeds setpoint! Instrument has shut down. Cycle the power
OFF for 10 seconds then ON. If the error persists call the your PerkinElmer
Service representative.
A/S control error
<autosampler error>
10-6
Clarus 500 GC Hardware Guide
Table 3 Autosampler error messages.
Autosampler Error Messages
Bad Sensor state
Bad motor mode
Bad motor speed
Elevator not initialising
Syringe error. Input value exceeds maximum volume of installed
syringe.
Carousel not initialising
Tower not initialising
No W/W vial present
Invalid vial number
Invalid injection port
Slot not found firmware to clarify Tower location sensor not finding slot.
No vial at position xx.
Invalid syringe size
Encoder read error (reserved)
Encoder position err
Bar Code error (reserved)
Encoder position err
Bar Code error (reserved)
Vial Sensor not initialising
Phase error
Reserved for barcode reader
Bad slot firmware to clarify Tower slot is wrong width.
Bad volume firmware to clarify Incorrect volume for syringe.
Bad injection firmware to clarify Injection failed.
Bad motor id firmware to clarify Tried to move invalid motor.
Illegal command firmware to clarify Illegal command to Autosampler
10-7
Troubleshooting
Table 3 –Formatted errors.
Error Messages
Cannot delete oven
program step <step number>
Cannot delete inlet
program step <step number>
Invalid Method<method number>
in sequence
Carrier <carrier number> unable to
maintain pressure
Split leaking
flow above max
FID flame out
Touch OK to continue
Warning: Car<inlet number> Inlet
< 50 Psi, Touch OK to continue
10-8
Clarus 500 GC Hardware Guide
GC Troubleshooting
The cardinal rule in troubleshooting your gas chromatograph is "If it ain't broke,
don't fix it." When things are working fine, leave well enough alone, but when
problems occur, this section will help you identify what could be wrong and how
to solve your problem.
There are several sources of problems in gas chromatography:
The operator: When the operator is new to chromatography and/or a new
instrument, problems can be introduced during the learning curve. Once the
operator becomes familiar with both the technique and the instrument, this
problem source diminishes greatly.
The sample: Unlike clean standards, real world samples such as environmental
samples, can introduce problems because they are difficult to handle, have
complicated matrices, contain unknown constituents, etc..
The column: The column is most often the major factor contributing to poor
analyses. The more a column is used, the greater the possibility of
contamination, loss of substrate, etc. Columns do not last forever and should be
changed when results become suspect.
The gas flow system: Leaks are a major concern in gas chromatography and can
lead to many problems.
The electronics: The problem must be identified as either chromatographic or
hardware. Electronics used in the system can malfunction.
Data handling: Today, most chromatographers rely on sophisticated data
handling systems to integrate their results. Some problems can be related to the
incorrect setting of data handling parameters.
10-9
Troubleshooting
Spare Components.
Following is a list of items you should have on hand to help solve problems.
New syringes – a syringe can break, become plugged or begin leaking. Always
have spares available.
Duplicate columns – a column does not last forever; therefore, a duplicate
column should be on hand in the event that your separation begins to degrade.
Also, capillary columns can be damaged if oxygen is introduced at high
temperatures. A duplicate column will allow you to identify if the column is the
cause of the problem.
Septa – this is the one area of the gas chromatograph which requires routine
maintenance. Always have spare septa available.
Leak detector – the gas flow system can be a problem as fittings wear with age
and can begin to leak. A leak detector should be available to help find and fix
leaks.
Injector liners – are made of glass and can be easily broken when removed. A
supply of spare liners should therefore be kept on hand. Please remember that
you cannot run satisfactory analyses without an injector liner.
Logical Troubleshooting Steps.
There are some simple steps that should be taken when trying to locate the
problem. Use the following guide to troubleshoot your GC.
Note the symptoms - define the problem. Compare your runs with good analysis,
that is, with the results normally obtained.
Systematically eliminate possible causes.
The first rule here is, "What did you change last?" Many times a problem arises
when a change is made to the system, such as changing a gas tank, septum, or
glass liner. If the problem occurred after such a change, then the change is the
most likely cause of the problem.
10-10
Clarus 500 GC Hardware Guide
Change the simplest thing first. For example, if you suspect a gas leak, the easiest
change to make is the GC septum instead of replumbing the internal pneumatics.
Change only one GC parameter at a time and check for its effect. If you change
three items at once and your problem goes away, you may not know which of the
three moves or combination of moves corrected the problem. This way, if the
problem happens again, you will know exactly what corrective action to take.
Dual Identical Channels Only
If your GC is a dual-channel system (dual identical detectors and dual identical
injectors):
1. Try switching the column to the second channel. If the problem is corrected,
then the problem was caused by the detector, injector, amplifier, or the
pneumatics.
2. Replace each of the above components one at a time to identify which one is
defective. If the problem is the same as before you switched the column, you
should suspect the column, syringe, standard or sample, electronics, or data
handling device.
10-11
Troubleshooting
ElCD Troubleshooting
ElCD problems are generally similar to those encountered with other detectors,
that is, loss of response, excessive noise, peak tailing, etc.
Problem causes are also similar to those for other detectors principally, column
bleed, leaks, contamination, improperly installed components, etc.
Sometimes noise in the ElCD can be reduced by cooling the reactor or venting.
It should be noted, however, that opening the vent can temporarily increase the
background signal and noise by exposing previously unwashed areas to solvent
which may dissolve material that can modify the conductivity.
An increase in background or noise when the reactor is off indicates possible
contamination of the solvent system or conductivity cell components.
10-12
Appendix I U.S.
Nuclear Regulations
NOTE: All USNRC regulations can be obtained through the internet at
www.nrc.gov/reading-rm/
I
Appendix I
Appendix 1-2
Clarus 500 GC Hardware Guide
Appendix I - SUPPLEMENT 2
Agreement States
Alabama
Kirksey E. Whatley, Director
Office of Radiation Control
The Alabama Department of Public Health
The RSA Tower, Suite 700
P.O. Box 303017
Montgomery, AL 36130-3017
PH (334)206-5391 FX (334)206-5387
INET: [email protected]
Arizona
Aubrey V. Godwin, Director
Arizona Radiation Regulatory Agency
4814 South 40th Street
Phoenix, AZ 85040
PH (602)255-4845 ext. 222 FX (602)4370705
INET: [email protected]
Arkansas
Jared W. Thompson, Program Leader
Division of Radiation Control &
Emergency Mgmt
Radioactive Materials Program,
Department of Health
Freeway Medical, Suite 100
5800 West 10th Street
Little Rock, AR 72204-1755
PH (501)661-2108 FX (501)661-2468
INET: [email protected]
California
Edgar D. Bailey, C.H.P., Chief
Radiologic Health Branch
Division of Food, Drugs, and Radiation
Safety
California Department of Health Services
P.O. Box 942732
Sacramento, CA 94234-7320
PH (916)322-3482 FX (916)324-3610
INET: [email protected]
Colorado
Warren E. (Jake) Jacobi, Program Manager
Laboratory & Radiation Services Division
Colorado Department of Public Health &
Environment
8100 Lowry Boulevard
Denver, CO 80230-6928
PH (303)692-3036 FX (303)692-3692
INET: INET: [email protected]
Florida
William A. Passetti, Chief
Bureau of Radiation Control
Florida Department of Health
4052 Bald Cypress Way, SE, Bin C21
Tallahassee, FL 32399-1741
PH (850)245-4266 FX (850)487-0435
INET: [email protected]
Georgia
Thomas E. Hill, Manager
Radioactive Materials Program
Department of Natural Resources
4244 International Parkway, Suite 114
Atlanta, GA 30354
PH (404)362-2675 FX (404)362-2653
INET: [email protected]
Illinois
Thomas W. Ortciger, Director
Illinois Department of Nuclear Safety
1035 Outer Park Drive
Springfield, IL 62704
PH (217)785-9868 FX (217)524-4724
INET: [email protected]
Iowa
Donald A. Flater, Chief
Bureau of Radiological Health
Iowa Department of Public Health
Appendix I-3
Appendix I
401 SW 7th Street, Suite D
Des Moines, IA 50309
PH (515)281-3478 FX (515)725-0318
INET: [email protected]
Kansas
Victor L. Cooper, Section Chief
Air Operating Permit & Compliance Section
Bureau of Air & Radiation
Division of Environment
Kansas Department of Health &
Environment
1000 SW Jackson, Suite 310
Topeka, KS 66612-1366
PH (785)296-1561 FX (785)291-3953
INET: [email protected]
Kentucky
John A. Volpe, Ph.D., Manager
Radiation Health & Toxic Agents Branch
Cabinet for Health Services
275 East Main Street
Frankfort, KY 40621-0001
PH (502)564-7818 ext 3692 FX (502)5641492
INET: [email protected]
Louisiana
Michael Henry, Senior Environmental
Scientist, Permitting Division
Department of Environmental Quality
Office of Environmental Services
Permits Division
7290 Bluebonnet Road
Baton Rouge, LA 70884-2135
PH (225)765-0892 FX (225)765-0222
INET: [email protected]
Maine
Jay Hyland, Program Manager
Radiation Control Program
Division of Health Engineering
10 State House Station
Augusta, ME 04333
Appendix 1-4
PH (207)287-5677 FX (207)287-3059
INET: [email protected]
Maryland
Roland G. Fletcher, Manager
Radiological Health Program
Air and Radiation Management
Administration
Maryland Department of the Environment
2500 Broening Highway
Baltimore, MD 21224
PH (410)631-3300 FX (410)631-3198
INET: [email protected]
Massachusetts
Robert M. Hallisey, Director
Radiation Control Program
Department of Public Health
174 Portland Street, 5th Floor
Boston, MA 02114
PH (617)727-6214 FX (617)727-2098
INET: [email protected]
Minnesota
Linda Bruemmer, Manager
Section of Asbestos, Indoor Air, Lead and
Radiation
Division of Environmental Health
Department of Health
121 E. Seventh Place, Suite 220
P.O. Box 64975
St. Paul, MN 55164-0975
PH (651)215-0945 FX (651)215-0975
INET: [email protected]
Mississippi
Robert W. Goff, Director
Division of Radiological Health
State Department of Health
3150 Lawson Street, P.O. Box 1700
Jackson, MS 39215-1700
PH (601)987-6893 FX (601)987-6887
INET: [email protected]
Clarus 500 GC Hardware Guide
Nebraska
New York
Dick Nelson, Director
Department of Regulation and Licensure
Nebraska Health and Human Services
System
P.O. Box 95007
Lincoln, NE 68590-5007
PH (402)471-8566 FX (402)471-9449
INET: [email protected]
Clayton Bradt, Principal Radiophysicist
New York State Dept. of Labor
Radiological Health Unit
Building 12, Room 169
State Office Building Campus
Albany, NY 12240
PH (518)457-1202 FX (518)485-7406
INET: [email protected]
New Hampshire
Diane E. Tefft, Administrator
Radiological Health Bureau
Division of Public Health Services
Health and Welfare Building
6 Hazen Drive
Concord, NH 03301-6527
PH (603)271-4588 FX (603)225-2325
INET: [email protected]
Nevada
Stanley R. Marshall, Supervisor
Radiological Health Section
Health Division
Department of Human Resources
1179 Fairview Drive, Suite 102
Carson City, NV 89701-5405
PH (775)687-5394 ext. 276, FX (775)6875751
INET: [email protected]
New Mexico
William Floyd, Manager
Radiation Control Bureau
Field Operations Division
Environment Department
1190 St. Francis Drive
P.O. Box 26110
Santa Fe, NM 87502
PH (505)476-3236 FX (505)476-3232
INET: [email protected]
John P. Spath, Director
Radioactive Waste Policy and Nuclear
Coordination
New York State Energy Research &
Development Authority
Corporate Plaza West
286 Washington Avenue Extension
Albany, NY 12203-6399
PH (518)862-1090 ext.3302 FX (518)8621091
INET: [email protected]
Paul J. Merges, Ph.D., Director,
Bureau of Radiation and Hazardous Site
Management
New York State Department of
Environmental Conservation
625 Broadway
Albany, NY 12233-7255
PH (518)402-8605 FX (518)402-9025
INET: [email protected]
Karim Rimawi, Ph.D., Director
Bureau of Environmental Radiation
Protection
New York State Department of Health
547 River Street
Troy, NY 12203
PH (518)402-7590 FX (518)402-7554
INET: [email protected]
Gene Miskin, Director
Bureau of Radiological Health
New York City Department of Health
Two Lafayette Street, 11th Floor
New York, NY 10007
PH (212)676-1556 FX (212)676-1548
INET: [email protected]
Appendix I-5
Appendix I
North Carolina
Beverly O. Hall, Acting Director
Division of Radiation Protection
Department of Environment & Natural
Resources
3825 Barrett Drive
Raleigh, NC 27609-7221
PH (919)571-4141 FX (919)571-4148
INET: [email protected]
North Dakota
Terry L. O'Clair, Director
Division of Air Quality
North Dakota Department of Health
1200 Missouri Avenue
P.O. Box 5520
Bismarck, ND 58506-5520
PH (701)328-5188 FX (701)328-5200
INET: [email protected]
Ohio
Roger L. Suppes, Chief
Bureau of Radiation Protection
Ohio Department of Health
35 East Chestnut Street
Columbus, OH 43266
PH (614)644-7860 FX (614)466-0381
INET: [email protected]
Oklahoma
Mike Broderick, Environmental Program
Administrator
Radiation Management Section
Oklahoma Department of Environmental
Quality
P.O. Box 1677
Oklahoma City, OK 73101-1677
PH (405)702-5155 FX (405)702-5101
INET: [email protected]
Oregon
Terry D. Lindsey, Acting Manager
Oregon Radiation Protection Services
Appendix 1-6
Section
800 N.E. Oregon Street, Suite 260
Portland, OR 97232
PH (503)731-4014 ext. 660 FX (503)7314081
INET: [email protected]
Pennsylvania
David Allard, CHP, Director
Bureau of Radiation Protection
Department of Environmental Protection
Rachel Carson State Office Building
P.O. Box 8469
Harrisburg, PA 17105-8469
PH (717)787-2480 FX (717)783-8965
INET: [email protected]
Rhode Island
Marie Stoeckel, Chief
Division of Occupational & Radiological
Health
Department of Health
3 Capitol Hill, Room 206
Providence, RI 02908-5097
PH (401)222-2438 FX (401)222-2456
INET: [email protected]
South Carolina
T. Pearce O'Kelley, Chief
Bureau of Radiological Health
Department of Health & Environmental
Control
2600 Bull Street
Columbia, SC 29201
PH (803)545-4400 FX (803)545-4412
INET: [email protected]
Henry Porter, Assistant Director
Division of Waste Management
Bureau of Land and Waste Management
Department of Health & Environmental
Control
2600 Bull Street
Columbia, SC 29201
Clarus 500 GC Hardware Guide
PH (803)896-4245 FX (803)896-4242
INET: [email protected]
Tennessee
L. Edward Nanney, Director
Division of Radiological Health
Tennessee Department of Environment and
Conservation
L&C Annex, Third Floor
401 Church Street
Nashville, TN 37243-1532
PH (615)532-0360 FX (615)532-7938
INET: [email protected]
Texas
Richard A. Ratliff, P.E., L.M.P. Chief
Bureau of Radiation Control
Texas Department of Health
1100 West 49th Street
Austin, TX 78756-3189
PH (512)834-6679 FX (512)834-6708
INET: [email protected]
Washington
John L. Erickson, Director
Division of Radiation Protection
Department of Health
Building #5
P.O. Box 47827
7171 Cleanwater Lane
Olympia, WA 98504-7827
PH (360)236-3210 FX (360)236-2255
INET: [email protected]
Wisconsin
Paul Schmidt, Manager
Radiation Protection Unit
Bureau of Public Health
Department of Health and Family Services
P.O. Box 309
Madison, WI 53701-0309
PH (608)267-4792 FX (608)267-4799
INET: [email protected]
Susan Jablonski
Health Physicist and Technical Advisor
Office of Permitting, Remediation &
Registration
Texas Natural Resource Conservation
Commission
P.O. Box 13087, MS 122
Austin, TX 78711-3087
PH (512)239-6731 FX (512)239-5151
INET: [email protected]
Utah
William J. Sinclair, Director
Division of Radiation Control
Department of Environmental Quality
168 North 1950 West
P.O. Box 144850
Salt Lake City, UT 84114-4850
PH (801)536-4250 FX (801)533-4097
INET: [email protected]
Appendix I-7
Appendix I
U.S. Nuclear Regulatory Commission Regional Offices
REGION
ADDRESS
TELEPHONE
I
WPI's Region
U.S. Nuclear Regulatory
Commission, Region I
475 Allendale Road
King of Prussia, PA 19406-1415
(800) 432-1156
II
U.S. Nuclear Regulatory
Commission, Region II
101 Marietta St., N.W., Suite 2900
Atlanta, GA 30323-0199
(800) 577-8510
III
U.S. Nuclear Regulatory
Commission, Region III
801 Warrenville Road
Lisle, IL 60137-5927
(800) 522-3025
IV
U.S. Nuclear Regulatory
Commission, Region IV
611 Ryan Plaza Drive, Suite 400
Arlington, TX 76011-8064
(800) 952-9677
Walnut Creek Field
Office
U.S. Nuclear Regulatory Commission
1450 Maria Lane
Walnut Creek, CA 94596-5368
(800) 882-4672
Appendix 1-8
Clarus 500 GC Hardware Guide
Nuclear Regulatory Commission Regulations
The following NRC regulations are from Title 10 Energy in the Code of Federal
Regulations revised as of June 30, 1996.
Subpart M-Reports
Source: 56 FR 23406, May 21, 1991, unless otherwise noted.
§ 20.2201 Reports of theft or loss of licensed material.
(a) Telephone reports. (1) Each licensee shall report by telephone as follows:
(i) Immediately after its occurrence becomes known to the licensee, any lost, stolen, or
missing licensed material in an aggregate quantity equal to or greater than 1,000 times the
quantity specified in Appendix C to Part 20 under such circumstances that it appears to
the licensee that an exposure could result to persons in unrestricted areas; or
(ii) Within 30 days after the occurrence of any lost, stolen, or missing licensed material
becomes known to the licensee, all licensed material in a quantity greater than 10 times
the quantity specified in Appendix C to Part 20 that is still missing at this time.
(2) Reports must be made as follows:
(i) Licensees having an installed Emergency Notification System shall make the reports
to the NRC Operations Center in accordance with § 50.72 of this chapter, and
(ii) All other licensees shall make reports by telephone to the NRC Operations Center
(301-951-0550).
(b) Written reports. (1) Each licensee required to make a report under paragraph (a) of
this section shall, within 30 days after making the telephone report, make a written report
setting forth the following information:
(i) A description of the licensed material involved, including kind, quantity, and
chemical and physical form; and
(ii) A description of the circumstances under which the loss or theft occurred; and
(iii) A statement of disposition, or probable disposition, of the licensed material
involved; and
(iv) Exposures of individuals to radiation, circumstances under which the exposures
occurred, and the possible total effective dose equivalent to persons in unrestricted areas;
and
(v) Actions that have been taken, or will be taken, to recover the material; and
(vi) Procedures or measures that have been, or will be, adopted to ensure against a
recurrence of the loss or theft of licensed material.
(2) Reports must be made as follows:
(i) For holders of an operating license for a nuclear power plant, the events included in
paragraph (b) of this section must be reported in accordance with the procedures
Appendix I-9
Appendix I
described in § 50.73(b), (c), (d), (e), and (g) of this chapter and must include the
information required in paragraph (b)(1) of this section, and
(ii) All other licensees shall make reports to the Administrator of the appropriate NRC
Regional Office listed in appendix D to Part 20.
(c) A duplicate report is not required under paragraph (b) of this section if the licensee is
also required to submit a report pursuant to §§ 30.55(c), 40.64(c), 50.72, 50.73, 70.52,
73.27(b), 73.67(e)(3)(vi), 73.67(g)(3)(iii), 73.71, or 150.19(c)
of this chapter.
(d) Subsequent to filing the written report, the licensee shall also report any additional
substantive information on the loss or theft within 30 days after the licensee learns of
such information.
(e) The licensee shall prepare any report filed with the Commission pursuant to this
section so that names of individuals who may have received exposure to radiation are
stated in a separate and detachable part of the report.
[56 FR 23406, May 21, 1991, as amended at 58 FR 69220, Dec. 30, 1993; 60 FR 20183,
Apr. 25, 1995]
§ 20.2202 Notification of incidents.
(a) Immediate notification. Notwithstanding any other requirements for notification,
each licensee shall immediately report any event involving byproduct, source, or special
nuclear material
possessed by the licensee that may have caused or threatens to cause any of the following
conditions(1) An individual to receive(i) A total effective dose equivalent of 25 rems
(0.25 Sv) or more; or
(ii) An eye dose equivalent of 75 rems (0.75 Sv) or more; or
(iii) A shallow-dose equivalent to the skin or extremities of 250 rads (2.5 Gy) or more;
or
(2) The release of radioactive material, inside or outside of a restricted area, so that, had
an individual been present for 24 hours, the individual could have received an intake five
times the annual limit on intake (the provisions of this paragraph do not apply to
locations where personnel are not normally stationed during routine operations, such as
hot-cells or process enclosures).
(b) Twenty-four hour notification. Each licensee shall, within 24 hours of discovery of
the event, report any event involving loss of control of licensed material possessed by the
licensee that may have caused, or threatens to cause, any of the following conditions:
(1) An individual to receive, in a period of 24 hours(i) A total effective dose equivalent exceeding 5 rems (0.05 Sv); or
(ii) An eye dose equivalent exceeding 15 rems (0.15 Sv); or
Appendix 1-10
Clarus 500 GC Hardware Guide
(iii) A shallow-dose equivalent to the skin or extremities exceeding 50 rems (0.5 Sv); or
(2) The release of radioactive material, inside or outside of a restricted area, so that, had
an individual been present for 24 hours, the individual could have received an intake in
excess of one occupational annual limit on intake (the provisions of this paragraph do not
apply to locations where personnel
are not normally stationed during routine operations, such as hot-cells or process
enclosures).
(c) The licensee shall prepare any report filed with the Commission pursuant to this
section so that names of individuals who have received exposure to radiation or
radioactive material are stated
in a separate and detachable part of the report.
(d) Reports made by licensees in response to the requirements of this section must be
made as follows:
(1) Licensees having an installed Emergency Notification System shall make the reports
required by paragraphs (a) and (b) of this section to the NRC Operations Center in
accordance with 10 CFR 50.72; and
(2) All other licensees shall make the reports required by paragraph (a) and (b) of this
section by telephone to the NRC Operations Center (301) 816-5100 and by telegram,
mailgram, or facsimile to the Administrator of the appropriate NRC Regional
Office listed in appendix D to 10 CFR part 20.
(e) The provisions of this section do not include doses that result from planned special
exposures, that are within the limits for planned special exposures, and that are reported
under § 20.2204.
[56 FR 23406, May 21, 1991, as amended at 56 FR 40766, Aug. 16, 1991; 57 FR 57879,
Dec. 8, 1992; 59 FR 14086, Mar. 25, 1994]
§ 20.2203 Reports of exposures, radiation levels, and concentrations of radioactive
material exceeding the limits.
a) Reportable events. In addition to the notification required by §20.2202, each
licensee shall submit a written report within 30 days after learning of any of the
following occurrences:
(1) Any incident for which notification is required by §20.2202; or
(2) Doses in excess of any of the following:
(i) The occupational dose limits for adults in §20.1201; or
(ii) The occupational dose limits for a minor in §20.1207; or
(iii) The limits for an embryo/fetus of a declared pregnant woman in
§20.1208; or
(iv) The limits for an individual member of the public in §20.1301; or
(v) Any applicable limit in the license; or
Appendix I-11
Appendix I
(vi) The ALARA constraints for air emissions established under
§20.1101(d); or
(3) Levels of radiation or concentrations of radioactive material in -(i) A restricted area in excess of any applicable limit in the license; or
(ii) An unrestricted area in excess of 10 times any applicable limit set
forth in this part or in the license (whether or not involving exposure of
any individual in excess of the limits in §20.1301); or
(4) For licensees subject to the provisions of EPA's generally applicable
environmental radiation standards in 40 CFR part 190, levels of radiation or
releases of radioactive material in excess of those standards, or of license
conditions related to those standards.
(b) Contents of reports. (1) Each report required by paragraph (a) of this section
must describe the extent of exposure of individuals to radiation and radioactive
material, including, as appropriate:
(i) Estimates of each individual's dose; and
(ii) The levels of radiation and concentrations of radioactive material
involved; and
(iii) The cause of the elevated exposures, dose rates, or concentrations;
and
(iv) Corrective steps taken or planned to ensure against a recurrence,
including the schedule for achieving conformance with applicable limits,
ALARA constraints, generally applicable environmental standards, and
associated license conditions.
(2) Each report filed pursuant to paragraph (a) of this section must include for
each occupationally overexposed(7) individual: the name, Social Security account
number, and date of birth. The report must be prepared so that this information is
stated in a separate and detachable part of the report.
(c) For holders of an operating license for a nuclear power plant, the occurrences
included in paragraph (a) of this section must be reported in accordance with the
procedures described in §50.73(b), (c), (d), (e), and (g) of this chapter and must
also include the information required by paragraph (b) of this section.
Occurrences reported in accordance with §50.73 of this chapter need not be
reported by a duplicate report under paragraph (a) of this section.
(d) All licensees, other than those holding an operating license for a nuclear
power plant, who make reports under paragraph (a) of this section shall submit
the report in writing to the U.S. Nuclear Regulatory Commission, Document
Control Desk, Washington, DC 20555, with a copy to the appropriate NRC
Regional Office listed in appendix D to part 20.
Appendix 1-12
Clarus 500 GC Hardware Guide
[56 FR 23406, May 21, 1991, as amended at 60 FR 20186, Apr. 25, 1995; 61 FR
65127, Dec. 10, 1996]
7
With respect to the limit for the embryo-fetus (§20.1208), the identifiers should
be those of the declared pregnant woman.
§20.2204 Reports of planned special exposures.
The licensee shall submit a written report to the Administrator of the appropriate NRC
Regional Office listed in appendix D to Part 20 within 30 days following any planned
special
exposure conducted in accordance with § 20.1206, informing the Commission that a
planned special exposure was conducted and indicating the date the planned special
exposure occurred and the information required by § 20.2105.
[Amended 60 FR 20183, Apr. 25, 1995]
§ 20.2205 Reports to individuals of exceeding dose limits.
When a licensee is required, pursuant to the provisions of §§20.2203, 20.2204, or
20.2206, to report to the Commission any exposure of an identified occupationally
exposed individual, or an identified member of the public, to radiation or radioactive
material, the licensee shall also provide a copy of the report submitted to the Commission
to the individual. This report must be transmitted at a time no later than the transmittal to
the Commission.
[60 FR 36043, July 13, 1995]
§20.2206 Reports of individual monitoring.
(a) This section applies to each person licensed by the Commission to(1) Operate a nuclear reactor designed to produce electrical or heat energy pursuant to
§50.21(b) or §50.22 of this chapter or a testing facility as defined in §50.2 of this chapter;
or
(2) Possess or use byproduct material for purposes of radiography pursuant to Parts 30
and 34 of this chapter; or
(3) Possess or use at any one time, for purposes of fuel processing, fabricating, or
reprocessing, special nuclear material in a quantity exceeding 5,000 grams of contained
uranium-235, uranium-233, or plutonium, or any combination thereof pursuant to part 70
of this chapter; or
(4) Possess high-level radioactive waste at a geologic repository operations area
pursuant to part 60 of this chapter; or
(5) Possess spent fuel in an independent spent fuel storage installation (ISFSI) pursuant
to part 72 of this chapter; or
Appendix I-13
Appendix I
(6) Receive radioactive waste from other persons for disposal under part 61 of this
chapter; or
(7) Possess or use at any time, for processing or manufacturing for distribution pursuant
to parts 30, 32, 33 or 35 of this chapter, byproduct material in quantities exceeding any
one of the following quantities:
Radionuclide
Cesium-137
Cobalt-60
Gold-198
Iodine-131
Iridium-192
Krypton-85
Promethium-147
Techetium-99m
Quantity of radionuclide1 in curies
1
1
100
1
10
1,000
10
1,000
1
The Commission may require as a license condition, or by rule, regulation, or order pursuant to § 20.2302,
reports from licensees who are licensed to use radionuclides not on this list, in quantities sufficient to cause
comparable radiation levels.
(b) Each licensee in a category listed in paragraph (a) of this section shall submit an
annual report of the results of individual monitoring carried out by the licensee for each
individual for whom monitoring was required by § 20.1502 during that year. The
licensee may include additional data for individuals for whom monitoring was provided
but not required. The licensee shall use Form NRC 5 or electronic media containing all
the information required by Form NRC 5.
(c) The licensee shall file the report required by
§ 20.2206(b), covering the preceding year, on or before April 30 of each year. The
licensee shall submit the report to the REIRS Project Manager, Office of Nuclear
Regulatory Research, U.S. Nuclear Regulatory Commission, Washington, DC 20555.
[56 FR 23406, May 21, 1991, as amended at 56 FR 32072, July 15, 1991]
§ 30.34 Terms and conditions of licenses.
(a) Each license issued pursuant to the regulations in this part and the regulations in parts
31 through 36 and 39 of this chapter shall be subject to all the provisions of the Act, now
or hereafter in effect, and to all valid rules, regulations and orders of the Commission.
(b) No license issued or granted pursuant to the regulations in this part and parts 31
through 36, and 39 nor any right under a license shall be transferred, assigned or in any
manner disposed of, either voluntarily or involuntarily, directly or indirectly, through
transfer of control of any license to any person, unless the Commission shall, after
Appendix 1-14
Clarus 500 GC Hardware Guide
securing full information, find that the transfer is in accordance with the provisions of the
Act and shall give its consent in writing.
(c) Each person licensed by the Commission pursuant to the regulations in this part and
parts 31 through 36 and 39 shall confine his possession and use of the byproduct material
to the locations and purposes authorized in the license. Except as otherwise provided in
the license, a license issued pursuant to the regulations in this part and parts 31 through
36 and 39 of this chapter shall carry with it the right to receive, acquire, own, and possess
byproduct material. Preparation for shipment and transport of byproduct material shall be
in accordance with the provisions of part 71 of this chapter.
(d) Each license issued pursuant to the regulations in this part and parts 31 through 36
and 39 shall be deemed to contain the provisions set forth in section 183b. - d., inclusive,
of the Act, whether or not these provisions are expressly set forth in the license.
(e) The Commission may incorporate, in any license issued pursuant to the regulations in
this part and parts 31 through 36 and 39, at the time of issuance, or thereafter by
appropriate rule, regulation or order, such additional requirements and conditions with
respect to the licensee's receipt, possession, use and transfer of byproduct material as it
deems appropriate or necessary in order to:
(1) Promote the common defense and security;
(2) Protect health or to minimize danger to life or property;
(3) Protect restricted data;
(4) Require such reports and the keeping of such records, and to provide for such
inspections of activities under the license as may be necessary or appropriate to effectuate
the purposes of the Act and regulations thereunder.
(f) Licensees required to submit emergency plans by §30.32(i) shall follow the
emergency plan approved by the Commission. The licensee may change the approved
without Commission approval only if the changes do not decrease the effectiveness of the
plan. The licensee shall furnish the change to the appropriate NRC Regional Office
specified in §30.6 and to affected offsite response organizations within six months after
the change is made. Proposed changes that decrease, or potentially decrease, the
effectiveness of the approved emergency plan may not be implemented without prior
application to and prior approval by the Commission.
(g) Each licensee preparing technetium-99m radiopharmaceuticals from molybdenum99/technetium-99m generators shall test the generator eluates for molybdenum-99
breakthrough in accordance with §35.204 of this chapter. The licensee shall record the
results of each test and retain each record for three years after the record is made.
(h)(1) Each general licensee that is required to register by Sec. 31.5(c)(13) of this chapter
and each specific licensee shall notify the appropriate NRC Regional Administrator, in
writing, immediately following the filing of a voluntary or involuntary petition for
bankruptcy under any chapter of title 11 (Bankruptcy) of the United States Code by or
against:
(i) The licensee;
(ii) An entity (as that term is defined in 11 U.S.C. 101(14)) controlling the licensee or
listing the license or licensee as property of the estate; or
Appendix I-15
Appendix I
(iii) An affiliate (as that term is defined in 11 U.S.C. 101(2)) of the licensee.
(2) This notification must indicate:
(i) The bankruptcy court in which the petition for bankruptcy was filed; and
(ii) The date of the filing of the petition.
§ 30.35 Financial assurance and record keeping for decommissioning.
a) Each applicant for a specific license authorizing the possession and use of unsealed
byproduct material of half-life greater than 120 days and in quantities exceeding 105
times the applicable quantities set forth in appendix B to part 30 shall submit a
decommissioning funding plan as described in paragraph (e) of this section. The
decommissioning funding plan must also be submitted when a combination of isotopes is
involved if R divided by 105 is greater than 1 (unity rule), where R is defined here as the
sum of the ratios of the quantity of each isotope to the applicable value in appendix B to
part 30.
(b) Each applicant for a specific license authorizing possession and use of byproduct
material of half-life greater than 120 days and in quantities specified in paragraph (d) of
this section shall either -(1) Submit a decommissioning funding plan as described in paragraph (e) of this section;
or
(2) Submit a certification that financial assurance for decommissioning has been provided
in the amount prescribed by paragraph (d) of this section using one of the methods
described in paragraph (f) of this section. For an applicant, this certification may state
that the appropriate assurance will be obtained after the application has been approved
and the license issued but before the receipt of licensed material. If the applicant defers
execution of the financial instrument until after the license has been issued, a signed
original of the financial instrument obtained to satisfy the requirements of paragraph (f)
of this section must be submitted to NRC before receipt of licensed material. If the
applicant does not defer execution of the financial instrument, the applicant shall submit
to NRC, as part of the certification, a signed original of the financial instrument obtained
to satisfy the requirements of paragraph (f) of this section.
(c)(1) Each holder of a specific license issued on or after July 27, 1990, which is of a type
described in paragraph (a) or (b) of this section, shall provide financial assurance for
decommissioning in accordance with the criteria set forth in this section.
(2) Each holder of a specific license issued before July 27, 1990, and of a type described
in paragraph (a) of this section shall submit, on or before July 27, 1990, a
decommissioning funding plan as described in paragraph (e) of this section or a
certification of financial assurance for decommissioning in an amount at least equal to
$750,000 in accordance with the criteria set forth in this section. If the licensee submits
the certification of financial assurance rather than a decommissioning funding plan, the
licensee shall include a decommissioning funding plan in any application for license
renewal.
Appendix 1-16
Clarus 500 GC Hardware Guide
(3) Each holder of a specific license issued before July 27, 1990, and of a type described
in paragraph (b) of this section shall submit, on or before July 27, 1990, a
decommissioning funding plan as described, in paragraph (e) of this section, or a
certification of financial assurance for decommissioning in accordance with the criteria
set forth in this section.
(4) Any licensee who has submitted an application before July 27, 1990, for renewal of
license in accordance with §30.37 shall provide financial assurance for decommissioning
in accordance with paragraphs (a) and (b) of this section. This assurance must be
submitted when this rule becomes effective November 24, 1995.
(d) Table of required amounts of financial assurance for decommissioning by quantity of
material.
greater than 104 but less than or equal to 105 times the applicable quantities of appendix B
to part 30 in unsealed form. (For a combination of isotopes, if R, as defined in §30.35(a),
divided by 104 is greater than 1 but R divided by 105 is less than or equal to 1.) ....
$750,000
greater than 103 but less than or equal to 104 times the applicable quantities of appendix B
to part 30 in unsealed form. (For a combination of isotopes, if R, as defined in §30.35(a),
divided by 103 is greater than 1 but R divided by 104 is less than or equal to 1.) ....
$150,000
greater than 1010 times the applicable quantities of appendix B to part 30 in sealed
sources or plated foils. (For a combination of isotopes, if R, as defined in §30.35(a),
divided by 1010 is greater than 1). .... $75,000
(e) Each decommissioning funding plan must contain a cost estimate for
decommissioning and a description of the method of assuring funds for decommissioning
from paragraph (f) of this section, including means for adjusting cost estimates and
associated funding levels periodically over the life of the facility. The decommissioning
funding plan must also contain a certification by the licensee that financial assurance for
decommissioning has been provided in the amount of the cost estimate for
decommissioning and a signed original of the financial instrument obtained to satisfy the
requirements of paragraph (f) of this section.
(f) Financial assurance for decommissioning must be provided by one or more of the
following methods:
(1) Prepayment. Prepayment is the deposit prior to the start of operation into an account
segregated from licensee assets and outside the licensee's administrative control of cash
or liquid assets such that the amount of funds would be sufficient to pay
decommissioning costs. Prepayment may be in the form of a trust, escrow account,
government fund, certificate of deposit, or deposit of government securities.
(2) A surety method, insurance, or other guarantee method. These methods guarantee that
decommissioning costs will be paid. A surety method may be in the form of a surety
bond, letter of credit, or line of credit. A parent company guarantee of funds for
decommissioning costs based on a financial test may be used if the guarantee and test are
as contained in appendix A to this part. A parent company guarantee may not be used in
combination with other financial methods to satisfy the requirements of this section. For
Appendix I-17
Appendix I
commercial corporations that issue bonds, a guarantee of funds by the applicant or
licensee for decommissioning costs based on a financial test may be used if the guarantee
and test are as contained in appendix C to this part. For commercial companies that do
not issue bonds, a guarantee of funds by the applicant or licensee for decommissioning
costs may be used if the guarantee and test are as contained in appendix D to this part.
For nonprofit entities, such as colleges, universities, and nonprofit hospitals, a guarantee
of funds by the applicant or licensee may be used if the guarantee and test are as
contained in appendix E to this part. A guarantee by the applicant or licensee may not be
used in combination with any other financial methods used to satisfy the requirements of
this section or in any situation where the applicant or licensee has a parent company
holding majority control of the voting stock of the company. Any surety method or
insurance used to provide financial assurance for decommissioning must contain the
following conditions:
(i) The surety method or insurance must be open-ended or, if written for a specified term,
such as five years, must be renewed automatically unless 90 days or more prior to the
renewal date, the issuer notifies the Commission, the beneficiary, and the licensee of its
intention not to renew. The surety method or insurance must also provide that the full
face amount be paid to the beneficiary automatically prior to the expiration without proof
of forfeiture if the licensee fails to provide a replacement acceptable to the Commission
within 30 days after receipt of notification of cancellation.
(ii) The surety method or insurance must be payable to a trust established for
decommissioning costs. The trustee and trust must be acceptable to the Commission. An
acceptable trustee includes an appropriate State or Federal government agency or an
entity which has the authority to act as a trustee and whose trust operations are regulated
and examined by a Federal or State agency.
(iii) The surety method or insurance must remain in effect until the Commission has
terminated the license.
(3) An external sinking fund in which deposits are made at least annually, coupled with a
surety method or insurance, the value of which may decrease by the amount being
accumulated in the sinking fund. An external sinking fund is a fund established and
maintained by setting aside funds periodically in an account segregated from licensee
assets and outside the licensee's administrative control in which the total amount of funds
would be sufficient to pay decommissioning costs at the time termination of operation is
expected. An external sinking fund may be in the form of a trust, escrow account,
government fund, certificate of deposit, or deposit of government securities. The surety
or insurance provisions must be as stated in paragraph (f)(2) of this section.
(4) In the case of Federal, State, or local government licensees, a statement of intent
containing a cost estimate for decommissioning or an amount based on the Table in
paragraph (d) of this section, and indicating that funds for decommissioning will be
obtained when necessary.
(5) When a governmental entity is assuming custody and ownership of a site, an
arrangement that is deemed acceptable by such governmental entity.
Appendix 1-18
Clarus 500 GC Hardware Guide
(g) Each person licensed under this part or parts 32 through 36 and 39 of this chapter
shall keep records of information important to the decommissioning of a facility in an
identified location until the site is released for unrestricted use. Before licensed activities
are transferred or assigned in accordance with §30.34(b), licensees shall transfer all
records described in this paragraph to the new licensee. In this case, the new licensee will
be responsible for maintaining these records until the license is terminated. If records
important to the decommissioning of a facility are kept for other purposes, reference to
these records and their locations may be used. Information the Commission considers
important to decommissioning consists of -(1) Records of spills or other unusual occurrences involving the spread of contamination
in and around the facility, equipment, or site. These records may be limited to instances
when contamination remains after any cleanup procedures or when there is reasonable
likelihood that contaminants may have spread to inaccessible areas as in the case of
possible seepage into porous materials such as concrete. These records must include any
known information on identification of involved nuclides, quantities, forms, and
concentrations.
(2) As-built drawings and modifications of structures and equipment in restricted areas
where radioactive materials are used and/or stored, and of locations of possible
inaccessible contamination such as buried pipes which may be subject to contamination.
If required drawings are referenced, each relevant document need not be indexed
individually. If drawings are not available, the licensee shall substitute appropriate
records of available information concerning these areas and locations.
(3) Except for areas containing only sealed sources (provided the sources have not leaked
or no contamination remains after any leak) or byproduct materials having only half-lives
of less than 65 days, a list contained in a single document and updated every 2 years, of
the following:
(i) All areas designated and formerly designated restricted areas as defined in 10 CFR
20.1003 (For requirements prior to January 1, 1994, see 10 CFR 20.3 as contained in the
CFR edition revised as of January 1, 1993.);
(ii) All areas outside of restricted areas that require documentation under §30.35(g)(1).
(iii) All areas outside of restricted areas where current and previous wastes have been
buried as documented under 10 CFR 20.2108; and
(iv) All areas outside of restricted areas that contain material such that, if the license
expired, the licensee would be required to either decontaminate the area to meet the
criteria for decommissioning in 10 CFR part 20, subpart E, or apply for approval for
disposal under 10 CFR 20.2002.
(4) Records of the cost estimate performed for the decommissioning funding plan or of
the amount certified for decommissioning, and records of the funding method used for
assuring funds if either a funding plan or certification is used.
[53 FR 24044, June 27, 1988, as amended at 56 FR 23471, May 21, 1991; 58 FR 39633,
July 26, 1993; 58 FR 67659, Dec. 22, 1993; 58 FR 68730, Dec. 29, 1993; 59 FR 1618,
Jan. 12, 1994; 60 FR 38238, July 26, 1995; 61 FR 24673, May 16, 1996; 62 FR 39090,
July 21, 1997]
Appendix I-19
Appendix I
§ 30.41 Transfer of byproduct material.
(a) No licensee shall transfer byproduct material except as authorized pursuant to this
section.
(b) Except as otherwise provided in his license and subject to the provisions of
paragraphs (c) and (d) of this section, any licensee may transfer byproduct material:
(1) To the Department;
(2) To the agency in any Agreement State which regulates radioactive material pursuant
to an agreement under section 274 of the Act;
(3) To any person exempt from the licensing requirements of the Act and regulations in
this part, to the extent permitted under such exemption;
(4) To any person in an Agreement State, subject to the jurisdiction of that State, who
has been exempted from the licensing requirements and regulations of that State, to the
extent permitted under such exemption;
(5) To any person authorized to receive such byproduct material under terms of a
specific license or a general license or their equivalents issued by the Atomic Energy
Commission, the Commission, or an Agreement State;
(6) To a person abroad pursuant to an export license issued under part 110 of this
chapter; or
(7) As otherwise authorized by the Commission in writing. (c) Before transferring
byproduct material to a specific licensee of the Commission or an Agreement State or to
a general licensee who is required to register with the Commission or with an Agreement
State prior to receipt of the byproduct material, the licensee transferring the material shall
verify that the transferee's license authorizes the receipt of the type, form, and quantity of
byproduct material to be transferred.
(d) The following methods for the verification required by paragraph (c) of this section
are acceptable:
(1) The transferor may have in his possession, and read, a current copy of the
transferee's specific license or registration certificate;
(2) The transferor may have in his possession a written certification by the transferee
that he is authorized by license or registration certificate to receive the type, form, and
quantity of byproduct material to be transferred, specifying the license or registration
certificate number, issuing agency and expiration date;
(3) For emergency shipments the transferor may accept oral certification by the
transferee that he is authorized by license or registration certificate to receive the type,
form, and quantity of byproduct material to be transferred, specifying the license or
registration certificate number, issuing agency and expiration date: Provided, That the
oral certification is confirmed in writing within 10 days;
(4) The transferor may obtain other sources of information compiled by a reporting
service from official records of the Commission or the licensing agency of an Agreement
State as to the identity of licensees and the scope and expiration dates of licenses and
registration; or
Appendix 1-20
Clarus 500 GC Hardware Guide
(5) When none of the methods of verification described in paragraphs (d)(1) to (4) of
this section are readily available or when a transferor desires to verify that information
received by one of such methods is correct or up-to-date, the transferor may obtain and
record confirmation from the Commission or the licensing agency of an Agreement State
that the transferee is licensed to receive the byproduct material.
[38 FR 33969, Dec. 10, 1973, as amended at 40 FR 8785, Mar. 3, 1975; 43 FR 6922, Feb.
17, 1978]
RECORDS, INSPECTIONS, TESTS, AND REPORTS
§ 30.50 Reporting requirements.
(a) Immediate report. Each licensee shall notify the NRC as soon as possible but not
later than 4 hours after the discovery of an event that prevents immediate protective
actions necessary to avoid exposures to radiation or radioactive materials that could
exceed regulatory limits or releases of licensed material that could exceed regulatory
limits (events may include fires, explosions, toxic gas releases, etc.).
(b) Twenty-four hour report. Each licensee shall notify the NRC within 24 hours after
the discovery of any of the following events involving licensed material:
(1) An unplanned contamination event that:
(i) Requires access to the contaminated area, by workers or the public, to be restricted
for more than 24 hours by imposing additional radiological controls or by prohibiting
entry into the area;
(ii) Involves a quantity of material greater than five times the lowest annual limit on
intake specified in appendix B of §§ 20.1001-20.2401 of 10 CFR part 20 for the material;
and
(iii) Has access to the area restricted for a reason other than to allow isotopes with a
half-life of less than 24 hours to decay prior to decontamination.
(2) An event in which equipment is disabled or fails to function as designed when:
(i) The equipment is required by regulation or license condition to prevent releases
exceeding regulatory limits, to prevent exposures to radiation and radioactive materials
exceeding regulatory limits, or to mitigate the consequences of an accident;
(ii) The equipment is required to be available and operable when it is disabled or fails to
function; and
(iii) No redundant equipment is available and operable to perform the required safety
function.
(3) An event that requires unplanned medical treatment at a medical facility of an
individual with spreadable radioactive contamination on the individual's clothing or body.
(4) An unplanned fire or explosion damaging any licensed material or any device,
container, or equipment containing licensed material when:
(i) The quantity of material involved is greater than five times the lowest annual limit on
intake specified in appendix B of §§ 20.1001-20.2401 of 10 CFR part 20 for the material;
and
Appendix I-21
Appendix I
(ii) The damage affects the integrity of the licensed material or its container.
(c) Preparation and submission of reports. Reports made by licensees in response to the
requirements of this section must be made as follows:
(1) Licensees shall make reports required by paragraphs (a) and (b) of this section by
telephone to the NRC Operations Center.{1} To the extent that the information is
available at the time of notification, the information provided in these reports must
include:
|{1} The commercial telephone number for the NRC Operations |Center is (301) 8165100.
(i) The caller's name and call back telephone number;
(ii) A description of the event, including date and time;
(iii) The exact location of the event;
(iv) The isotopes, quantities, and chemical and physical form of the licensed material
involved; and
(v) Any personnel radiation exposure data available.
(2) Written report. Each licensee who makes a report required by paragraph (a) or (b) of
this section shall submit a written follow-up report within 30 days of the initial report.
Written reports prepared pursuant to other regulations may be submitted to fulfill this
requirement if the reports contain all of the necessary information and the appropriate
distribution is made. These written reports must be sent to the U.S. Nuclear Regulatory
Commission, Document Control Desk, Washington, DC 20555, with a copy to the
appropriate NRC Regional office listed in appendix D of 10 CFR part 20. The reports
must include the following:
(i) A description of the event, including the probable cause and the manufacturer and
model number (if applicable) of any equipment that failed or malfunctioned;
(ii) The exact location of the event;
(iii) The isotopes, quantities, and chemical and physical form of the licensed material
involved;
(iv) Date and time of the event;
(v) Corrective actions taken or planned and the results of any evaluations or
assessments; and
(vi) The extent of exposure of individuals to radiation or to radioactive materials
without identification of individuals by name.
(3) The provisions of § 30.50 do not apply to licensees subject to the notification
requirements in
§ 50.72. They do apply to those part 50 licensees possessing material licensed under part
30, who are not subject to the notification requirements in § 50.72.
[56 FR 40767, Aug. 16, 1991, as amended at 59 FR 14086, Mar. 25, 1994]
§ 30.51 Records.
Appendix 1-22
Clarus 500 GC Hardware Guide
(a) Each person who receives byproduct material pursuant to a license issued pursuant
to the regulations in this part and parts 31 through 36 of this chapter shall keep records
showing the receipt, transfer, and disposal of the byproduct material as follows:
(1) The licensee shall retain each record of receipt of byproduct material as long as the
material is possessed and for three years following transfer or disposal of the material.
(2) The licensee who transferred the material shall retain each record of transfer for
three years after each transfer unless a specific requirement in another part of the
regulations in this chapter dictates otherwise.
(3) The licensee who disposed of the material shall retain each record of disposal of
byproduct material until the Commission terminates each license that authorizes disposal
of the material.
(b) The licensee shall retain each record that is required by the regulations in this part
and parts 31 through 36 of this chapter or by license condition for the period specified by
the appropriate regulation or license condition. If a retention period is not otherwise
specified by regulation or license condition, the record must be retained until the
Commission terminates each license that authorizes the activity that is subject to the
recordkeeping requirement.
(c)(1) Records which must be maintained pursuant to this part and parts 31 through 36
of this chapter may be the original or a reproduced copy or microform if such reproduced
copy or microform is duly authenticated by authorized personnel and the microform is
capable of producing a clear and legible copy after storage for the period specified by
Commission regulations. The record may also be stored in electronic media with the
capability for producing legible, accurate, and complete records during the required
retention period. Records such as letters, drawings, specifications, must include all
pertinent information such as stamps, initials, and signatures. The licensee shall maintain
adequate safeguards against tampering with and loss of records.
(2) If there is a conflict between the Commission's regulations in this part and parts 31
through 36 and 39 of this chapter, license condition, or other written Commission
approval or authorization pertaining to the retention period for the same type of record,
the retention period specified in the regulations in this part and parts 31 through 36 and
39 of this chapter for such records shall apply unless the Commission, pursuant to §
30.11, has granted a specific exemption from the record retention requirements specified
in the regulations in this part or parts 31 through 36 and 39 of this chapter.
(d) Prior to license termination, each licensee authorized to possess radioactive material
with a half-life greater than 120 days, in an unsealed form, shall forward the following
records to the appropriate NRC Regional Office:
(1) Records of disposal of licensed material made under §§ 20.2002 (including burials
authorized before January 28, 1981 {1}), 20.2003, 20.2004, 20.2005; and | {1} A
previous § 20.304 permitted burial of small |quantities of licensed materials in soil before
January |28, 1981, without specific Commission authorization. |See § 20.304 contained in
the 10 CFR, parts 0 to 199, |edition revised as of January 1, 1981. (2) Records required
by
§ 20.2103(b)(4).
Appendix I-23
Appendix I
(e) If licensed activities are transferred or assigned in accordance with § 30.34(b), each
licensee authorized to possess radioactive material, with a half-life greater than 120 days,
in an unsealed form, shall transfer the following records to the new licensee and the new
licensee will be responsible for maintaining these records until the license is terminated:
(1) Records of disposal of licensed material made under §§ 20.2002 (including burials
authorized before January 28, 1981 {1}), 20.2003, 20.2004, 20.2005; and | {1} A
previous § 20.304 permitted burial of small |quantities of licensed materials in soil before
January |28, 1981, without specific Commission authorization. |See § 20.304 contained in
the 10 CFR, parts 0 to 199, |edition revised as of January 1, 1981.
(2) Records required by § 20.2103(b)(4).
(f) Prior to license termination, each licensee shall forward the records required by §
30.35(g) to the appropriate NRC Regional Office.
[41 FR 18301, May 5, 1976, as amended at 43 FR 6922, Feb. 17, 1978; 52 FR 8241, Mar.
17, 1987; 53 FR 19245, May 27, 1988; 58 FR 7736, Feb. 9, 1993; 61 FR 24669, May 16,
1996]
§ 30.52 Inspections.
(a) Each licensee shall afford to the Commission at all reasonable times opportunity to
inspect byproduct material and the premises and facilities wherein byproduct material is
used or stored.
(b) Each licensee shall make available to the Commission for inspection, upon
reasonable notice, records kept by him pursuant to the regulations in this chapter.
[30 FR 8185, June 26, 1965]
§ 30.53 Tests.
Each licensee shall perform, or permit the Commission to perform, such tests as the
Commission deems appropriate or necessary for the administration of the regulations in
this part and parts 31 through 36 and 39 of this chapter, including tests of:
(a) Byproduct material;
(b) Facilities wherein byproduct material is utilized or stored; (c) Radiation detection
and monitoring instruments; and
(d) Other equipment and devices used in connection with the utilization or storage of
byproduct material.
[30 FR 8185, June 26, 1965, as amended by 43 FR 6922, Feb. 17, 1978; 52 FR 8241,
Mar. 17, 1987; 58 FR 7736, Feb. 9, 1993]
Appendix 1-24
Clarus 500 GC Hardware Guide
§ 30.55 Tritium reports.
(a)-(b) [Reserved]
(c) Except as specified in paragraph (d) of this section, each licensee who is authorized
to possess tritium shall report promptly to the appropriate NRC Regional Office listed in
appendix D of part 20 of this chapter by telephone and telegraph, mailgram, or facsimile
any incident in which an attempt has been made or is believed to have been made to
commit a theft or unlawful diversion of more than 10 curies of such material at any one
time or more than 100 curies of such material in any one calendar year. The initial report
shall be followed within a period of fifteen (15) days by a written report submitted to the
appropriate NRC Regional Office which sets forth the details of the incident and its
consequences. Copies of such written report shall be sent to the Director, Office of
Nuclear Material Safety and Safeguards, U.S. Nuclear Regulatory Commission,
Washington, DC 20555. Subsequent to the submission of the written report required by
this paragraph, the licensee shall promptly inform the Office of Nuclear Material Safety
and Safeguards by means of a written report of any substantive additional information,
which becomes available to the licensee, concerning an attempted or apparent theft or
unlawful diversion of tritium.
(d) The reports described in this section are not required for tritium possessed pursuant
to a general license provided in part 31 of this chapter or for tritium contained in spent
fuel.
[37 FR 9208, May 6, 1972, as amended at 38 FR 1271, Jan. 11, 1973; 38 FR 2330, Jan.
24, 1973; 41 FR 16446, Apr. 19, 1976; 43 FR 6922, Feb. 17, 1978; 46 FR 55085, Nov. 6,
1981; 49 FR 24707, June 15, 1984; 52 FR 31611, Aug. 21, 1987]
ENFORCEMENT
§ 30.61 Modification and revocation of licenses.
(a) The terms and conditions of each license issued pursuant to the regulations in this
part and parts 31 through 35 of this chapter shall be subject to amendment, revision or
modification by reason of amendments to the Act, or by reason of rules, regulations and
orders issued in accordance with the terms of the Act.
(b) Any license may be revoked, suspended or modified, in whole or in part, for any
material false statement in the application or any statement of fact required under section
182 of the Act, or because of conditions revealed by such application or statement of fact
or any report, record or inspection or other means which would warrant the Commission
to refuse to grant a license on an original application, or for violation of, or failure to
observe any of the terms and provisions of the Act or of any rule, regulation or order of
the Commission.
(c) Except in cases of willfulness or those in which the public health, interest or safety
requires otherwise, no license shall be modified, suspended or revoked unless, prior to the
Appendix I-25
Appendix I
institution of proceedings therefor, facts or conduct which may warrant such action shall
have been called to the attention of the licensee in writing and the licensee shall have
been accorded an opportunity to demonstrate or achieve compliance with all lawful
requirements.
[30 FR 8185, June 26, 1965, as amended at 35 FR 11460, July 17, 1970; 43 FR 6922,
Feb. 17, 1978]
§ 30.62 Right to cause the withholding or recall of byproduct material. The
Commission may cause the withholding or recall of byproduct material from any licensee
who is not equipped to observe or fails to observe such safety standards to protect health
as may be established by the Commission, or who uses such materials in violation of law
or regulation of the Commission, or in a manner other than as disclosed in the application
therefor or approved by the Commission.
[30 FR 8185, June 26, 1965, as amended at 40 FR 8785, Mar. 3, 1975]
§ 30.63 Violations.
(a) The Commission may obtain an injunction or other court order to prevent a violation
of the provisions of(1) The Atomic Energy Act of 1954, as amended; (2) Title II of the Energy
Reorganization Act of 1974, as amended; or
(3) A regulation or order issued pursuant to those Acts.
(b) The Commission may obtain a court order for the payment of a civil penalty
imposed under section 234 of the Atomic Energy Act:
(1) For violations of(i) Sections 53, 57, 62, 63, 81, 82, 101, 103, 104, 107, or 109 of the Atomic Energy Act
of 1954, as amended;
(ii) Section 206 of the Energy Reorganization Act;
(iii) Any rule, regulation, or order issued pursuant to the sections specified in paragraph
(b)(1)(i) of this section;
(iv) Any term, condition, or limitation of any license issued under the sections specified
in paragraph (b)(1)(i) of this section.
(2) For any violation for which a license may be revoked under section 186 of the
Atomic Energy Act of 1954, as amended.
[57 FR 55072, Nov. 24, 1992]
§ 30.64 Criminal penalties.
(a) Section 223 of the Atomic Energy Act of 1954, as amended, provides for criminal
sanctions for willful violation of, attempted violation of, or conspiracy to violate, any
regulation issued under sections 161b, 161i, or 161o of the Act. For purposes of section
Appendix 1-26
Clarus 500 GC Hardware Guide
223, all the regulations in part 30 are issued under one or more of sections 161b, 161i, or
161o, except for the sections listed in paragraph (b) of this section.
(b) The regulations in part 30 that are not issued under sections 161b, 161i, or 161o for
the purposes of section 223 are as follows:
§§ 30.1, 30.2, 30.4, 30.5, 30.6, 30.8, 30.11, 30.12, 30.13, 30.15, 30.16, 30.31, 30.32,
30.33, 30.37, 30.38, 30.39, 30.61, 30.62, 30.63, 30.64, 30.70, 30.71, and 30.72.
[57 FR 55072, Nov. 24, 1992]
Schedules
§ 30.70 Schedule A-exempt concentrations.
[See footnotes at end of this table]
Element (atomic number)
Isotope
Antimony (51)
Sb 122
Sb 124
Sb 125
A 37
A 41
As 73
As 74
As 76
As 77
Ba 131
Ba 140
Be 7
Bi 206
Br 82
Cd 109
Cd 115m
Cd 115
Ca 45
Ca 47
C 14
Ce 141
Ce 143
Ce 144
Cs 131
Cs 134m
Cs 134
Cl 38
Cr 51
Co 57
Co 58
Co 60
Cu 64
Dy 165
Dy 166
Argon (18)
Arsenic (33)
Barium (56)
Beryllium (4)
Bismuth (83)
Bromine (35)
Cadmium (48)
Calcium (20)
Carbon (6)
Cerium (58)
Cesium (55)
Chlorine (17)
Chromium (24)
Cobalt (27)
Copper (29)
Dysprosium (66)
Col. I
Gas concentration
µCi/ml {1}
1x10-3
4x10-7
4x10_-7
1x10_-6
9x10_-7
Col. II
Liquid and solid
concentration µCi/ml{2}
3x10-4
2x10-4
1x10-3
5x10_-3
5x10_-4
2x10_-4
8x10_-4
2x10_-3
3x10_-4
2x10_-2
4x10_-4
3x10_-3
2x10_-3
3x10_-4
3x10_-4
9x10_-5
5x10_-4
8x10_-3
9x10_-4
4x10_-4
1x10_-4
2x10_-2
6x10_-2
9x10_-5
4x10_-3
2x10_-2
5x10_-3
1x10_-3
5x10_-4
3x10_-3
4x10_-3
4x10_-4
Appendix I-27
Appendix I
Erbium (68)
Europium (63)
Fluorine (9)
Gadolinium (64)
Element (atomic number)
Gallium (31)
Germanium (32)
Gold (79)
Hafnium (72)
Hydrogen (1)
Indium (49)
Iodine (53)
Iridium (77)
Iron (26)
Krypton (36)
Lanthanum (57)
Lead (82)
Lutetium (71)
Manganese (25)
Mercury (80)
Molybdenum (42)
Neodymium (60)
Nickel (28)
Niobium (Columbium)
(41).
Osmium (76)
Palladium (46)
Phosphorus (15)
Platinum (78)
Appendix 1-28
Er 169
Er 171
Eu 152
(T/2=9.2 Hrs)
Eu 155
F 18
Gd 153
Gd 159
Isotope
Ga 72
Ge 71
Au 196
Au 198
Au 199
Hf 181
H 3.
In 113m
In 114m
I 126
I 131
I 132
I 133
I 134
Ir 190
Ir 192
Ir 194
Fe 55
Fe 59
Kr 85m
Kr 85
La 140
Pb 203
Lu 177
Mn 52
Mn 54
Mn 56
Hg 197m
Hg 197
Hg 203
Mo 99
Nd 147
Nd 149
Ni 65
Nb 95
Nb 97
Os 185
Os 191m
Os 191
Os 193
Pd 103
Pd 109
P 32
Pt 191
9x10_-4
1x10_-3
6x10_-4
2x10_-6
Col. I
5x10_-6
3x10_-9
3x10_-9
8x10_-8
1x10_-8
2x10_-7
2x10_-3
8x10_-3
2x10_-3
8x10_-4
Col. II
4x10_-4
2x10_-2
2x10_-3
5x10_-4
2x10_-3
7x10_-4
3x10_-2
1x10_-2
2x10_-4
2x10_-5
2x10_-5
6x10_-4
7x10_-5
1x10_-3
2x10_-3
4x10_-4
3x10_-4
8x10_-3
6x10_-4
1x10_-6
3x10_-6
2x10_-4
4x10_-3
1x10_-3
3x10_-4
1x10_-3
1x10_-3
2x10_-3
3x10_-3
2x10_-4
2x10_-3
6x10_-4
3x10_-3
1x10_-3
1x10_-3
9x10_-3
7x10_-4
3x10_-2
2x10_-3
6x10_-4
3x10_-3
9x10_-4
2x10_-4
1x10_-3
Clarus 500 GC Hardware Guide
Potassium (19)
Praseodymium (59)
Element (atomic number)
Promethium (61)
Rhenium (75)
Rhodium (45)
Rubidium (37)
Ruthenium (44)
Samarium (62)
Scandium (21)
Selenium (34)
Silicon (14)
Silver (47)
Sodium (11)
Strontium (38)
Sulfur (16)
Tantalum (73)
Technetium (43)
Tellurium (52)
Terbium (65)
Thallium (81)
Thulium (69)
Tin (50)
Tungsten (Wolfram) (74)
Pt 193m
Pt 197m
Pt 197
K 42
Pr 142
Pr 143
Isotope
Pm 147
Pm 149
Re 183
Re 186
Re 188
Rh 103m
Rh 105
Rb 86
Ru 97
Ru 103
Ru 105
Ru 106
Sm 153
Sc 46
Sc 47
Sc 48
Se 75
Si 31
Ag 105
Ag 110m
Ag 111
Na 24
Sr 85
Sr 89
Sr 91
Sr 92
S 35
Ta 182
Tc 96m
Tc 96
Te 125m
Te 127m
Te 127
Te 129m
Te 131m
Te 132
Tb 160
Tl 200
Tl 201
Tl 202
Tl 204
Tm 170
Tm 171
Sn 113
Sn 125
W 181
W 187
Col. I
9x10_-8
1x10_-2
1x10_-2
1x10_-3
3x10_-3
3x10_-4
5x10_-4
Col. II
2x10_-3
4x10_-4
6x10_-3
9x10_-4
6x10_-4
1x10_-1
1x10_-3
7x10_-4
4x10_-4
8x10_-4
1x10_-3
1x10_-4
8x10_-4
4x10_-4
9x10_-4
3x10_-4
3x10_-3
9x10_-3
1x10_-3
3x10_-4
4x10_-4
2x10_-3
1x10_-4
1x10_-4
7x10_-4
7x10_-4
6x10_-4
4x10_-4
1x10_-1
1x10_-3
2x10_-3
6x10_-4
3x10_-3
3x10_-4
6x10_-4
3x10_-4
4x10_-4
4x10_-3
3x10_-3
1x10_-3
1x10_-3
5x10_-4
5x10_-3
9x10_-4
2x10_-4
4x10_-3
7x10_-4
Appendix I-29
Appendix I
Vanadium (23)
Xenon (54)
Element (atomic number)
Ytterbium (70)
Yttrium (39)
Zinc (30)
Zirconium (40)
V 48
Xe 131m
Xe 133
Xe 135
Isotope
Yb 175
Y 90
Y 91m
Y 91
Y 92
Y 93
Zn 65
Zn 69m
Zn 69
Zr 95
Zr 97
Beta and/or gamma emitting
byproduct material not listed
above with half-life less than 3
years.
3x10_-4
4x10_-6
3x10_-6
1x10_-6
Col. I
1x10_-10
--------------------------------------------------------------------------Footnotes to Schedule A:
{1}Values are given only for those materials normally used as gases.
{2}æCi/gm for solids.
Note 1: Many radioisotopes disintegrate into isotopes which are also
radioactive. In expressing the concentrations in Schedule A, the activity
stated is that of the parent isotope and takes into account the daughters.
Note 2: For purposes of § 30.14 where there is involved a
combination of isotopes, the limit for the combination should be
derived as follows:
Determine for each isotope in the product the ratio between the
concentration present in the product and the exempt concentration
established in Schedule A for the specific isotope when not in
combination. The sum of such ratios may not exceed ``1'' (i.e., unity).
Example:
Concentration of Isotope A in Product
-------------------------------------Exempt concentration of Isotope A
Concentration of Isotope B in Product
--------------------------------------<= 1
Exempt concentration of Isotope B
Appendix 1-30
Col. II
1x10_-3
2x10_-4
3x10_-2
3x10_-4
6x10_-4
3x10_-4
1x10_-3
7x10_-4
2x10_-2
6x10_-4
2x10_-4
1x10_-6
Clarus 500 GC Hardware Guide
[30 FR 8185, June 26, 1965, as amended at 35 FR 3982, Mar. 3, 1970; 38 FR 29314, Oct.
24, 1973; 59 FR 5520, Feb. 7, 1994]
§ 31.5 Certain detecting, measuring, gauging, or controlling devices and certain
devices for producing light or an ionized atmosphere.(2)
(a) A general license is hereby issued to commercial and industrial firms and research,
educational and medical institutions, individuals in the conduct of their business, and
Federal, State or local government agencies to acquire, receive, possess, use or transfer,
in accordance with the provisions of paragraphs (b), (c) and (d) of this section, byproduct
material contained in devices designed and manufactured for the purpose of detecting,
measuring, gauging or controlling thickness, density, level, interface location, radiation,
leakage, or qualitative or quantitative chemical composition, or for producing light or an
ionized atmosphere.
(b)(1) The general license in paragraph (a) of this section applies only to byproduct
material contained in devices which have been manufactured or initially transferred and
labeled in accordance with the specifications contained in-(i) A specific license issued under Sec. 32.51 of this chapter; or
(ii) An equivalent specific license issued by an Agreement State.
(2) The devices must have been received from one of the specific licensees described in
paragraph (b)(1) of this section or through a transfer made under paragraph (c)(9) of this
section.
(c) Any person who acquires, receives, possesses, uses or transfers byproduct material in
a device pursuant to the general license in paragraph (a) of this section:
(1) Shall assure that all labels affixed to the device at the time of receipt and bearing a
statement that removal of the label is prohibited are maintained thereon and shall comply
with all instructions and precautions provided by such labels;
(2) Shall assure that the device is tested for leakage of radioactive material and proper
operation of the on-off mechanism and indicator, if any, at no longer than six-month
intervals or at such other intervals as are specified in the label; however:
(i) Devices containing only krypton need not be tested for leakage of radioactive material,
and
(ii) Devices containing only tritium or not more than 100 microcuries of other beta and/or
gamma emitting material or 10 microcuries of alpha emitting material and devices held in
storage in the original shipping container prior to initial installation need not be tested for
any purpose;
(3) Shall assure that the tests required by paragraph (c)(2) of this section and other
testing, installation, servicing, and removal from installation involving the radioactive
materials, its shielding or containment, are performed:
(i) In accordance with the instructions provided by the labels; or
(ii) By a person holding a specific license pursuant to parts 30 and 32 of this chapter or
from an Agreement State to perform such activities;
(4) Shall maintain records showing compliance with the requirements of paragraphs
(c)(2) and (c)(3) of this section. The records must show the results of tests. The records
Appendix I-31
Appendix I
also must show the dates of performance of, and the names of persons performing,
testing, installing, servicing, and removing from the installation radioactive material and
its shielding or containment. The licensee shall retain these records as follows:
(i) Each record of a test for leakage or radioactive material required by paragraph (c)(2)
of this section must be retained for three years after the next required leak test is
performed or until the sealed source is transferred or disposed of.
(ii) Each record of a test of the on-off mechanism and indicator required by paragraph
(c)(2) of this section must be retained for three years after the next required test of the onoff mechanism and indicator is performed or until the sealed source is transferred or
disposed of.
(iii) Each record that is required by paragraph (c)(3) of this section must be retained for
three years from the date of the recorded event or until the device is transferred or
disposed of.
(5) Shall immediately suspend operation of the device if there is a failure of, or damage
to, or any indication of a possible failure of or damage to, the shielding of the radioactive
material or the on-off mechanism or indicator, or upon the detection of 185 bequerel
(0.005 microcurie) or more removable radioactive material. The device may not be
operated until it has been repaired by the manufacturer or other person holding a specific
license to repair such devices that was issued under parts 30 and 32 of this chapter or by
an Agreement State. The device and any radioactive material from the device may only
be disposed of by transfer to a person authorized by a specific license to receive the
byproduct material in the device or as otherwise approved by the Commission. A report
containing a brief description of the event and the remedial action taken; and, in the case
of detection of 0.005 microcurie or more removable radioactive material or failure of or
damage to a source likely to result in contamination of the premises or the environs, a
plan for ensuring that the premises and environs are acceptable for unrestricted use, must
be furnished to the Director of Nuclear Material Safety and Safeguards, ATTN: GLTS,
U.S. Nuclear Regulatory Commission, Washington, DC 20555-0001 within 30 days.
Under these circumstances, the criteria set out in Sec. 20.1402, ``Radiological criteria for
unrestricted use,'' may be applicable, as determined by the Commission on a case-by-case
basis;
(6) Shall not abandon the device containing byproduct material;
(7) Shall not export the device containing byproduct material except in accordance with
part 110 of this chapter;
(8)(i) Shall transfer or dispose of the device containing byproduct material only by export
as provided by paragraph (c)(7) of this section, by transfer to another general licensee as
authorized in paragraph (c)(9) of this section, or to a person authorized to receive the
device by a specific license issued under parts 30 and 32 of this chapter, or part 30 of this
chapter that authorizes waste collection, or equivalent regulations of an Agreement State,
or as otherwise approved under paragraph (c)(8)(iii) of this section.
(ii) Shall furnish a report to the Director of Nuclear Material Safety and Safeguards,
ATTN: GLTS, U.S. Nuclear Regulatory Commission, Washington, DC 20555-0001
Appendix 1-32
Clarus 500 GC Hardware Guide
within 30 days after the transfer of a device to a specific licensee or export. The report
must contain-(A) The identification of the device by manufacturer's (or initial transferor's) name,
model number, and serial number;
(B) The name, address, and license number of the person receiving the device (license
number not applicable if exported); and
(C) The date of the transfer.
(iii) Shall obtain written NRC approval before transferring the device to any other
specific licensee not specifically identified in paragraph (c)(8)(i) of this section.
(9) Shall transfer the device to another general licensee only if-(i) The device remains in use at a particular location. In this case, the transferor shall give
the transferee a copy of this section, a copy of Secs. 31.2, 30.51, 20.2201, and 20.2202 of
this chapter, and any safety documents identified in the label of the device. Within 30
days of the transfer, the transferor shall report to the Director of Nuclear Material Safety
and Safeguards, ATTN: GLTS, U.S. Nuclear Regulatory Commission, Washington, DC
20555-0001-(A) The manufacturer's (or initial transferor's) name;
(B) The model number and the serial number of the device transferred;
(C) The transferee's name and mailing address for the location of use; and
(D) The name, title, and phone number of the responsible individual identified by the
transferee in accordance with paragraph (c)(12) of this section to have knowledge of and
authority to take actions to ensure compliance with the appropriate regulations and
requirements; or
(ii) The device is held in storage by an intermediate person in the original shipping
container at its intended location of use prior to initial use by a general licensee.
(10) Shall comply with the provisions of §§20.2201, and 20.2202 of this chapter for
reporting radiation incidents, theft or loss of licensed material, but shall be exempt from
the other requirements of parts 19, 20, and 21, of this chapter.
(11) Shall respond to written requests from the Nuclear Regulatory Commission to
provide information relating to the general license within 30 calendar days of the date of
the request, or other time specified in the request. If the general licensee cannot provide
the requested information within the allotted time, it shall, within that same time period,
request a longer period to supply the information by submitting a letter to the Director,
Office of Nuclear Material Safety and Safeguards, U.S. Nuclear Regulatory Commission,
Washington, DC 20555-0001 and provide written justification as to why it cannot
comply.
(12) Shall appoint an individual responsible for having knowledge of the appropriate
regulations and requirements and the authority for taking required actions to comply with
appropriate regulations and requirements. The general licensee, through this individual,
shall ensure the day-to-day compliance with appropriate regulations and requirements.
This appointment does not relieve the general licensee of any of its responsibility in this
regard.
Appendix I-33
Appendix I
(13)(i) Shall register, in accordance with paragraphs (c)(13)(ii) and (iii) of this section,
devices containing at least 370 MBq (10 mCi) of cesium-137, 3.7 MBq (0.1 mCi) of
strontium-90, 37 MBq (1 mCi) of cobalt-60, or 37 MBq (1 mCi) of americium-241 or any
other transuranic (i.e., element with atomic number greater than uranium (92)), based on
the activity indicated on the label. Each address for a location of use, as described under
paragraph (c)(13)(iii)(D) of this section, represents a separate general licensee and
requires a separate registration and fee.
(ii) If in possession of a device meeting the criteria of paragraph (c)(13)(i) of this section,
shall register these devices annually with the Commission and shall pay the fee required
by Sec. 170.31 of this chapter. Registration must be done by verifying, correcting, and/or
adding to the information provided in a request for registration received from the
Commission. The registration information must be submitted to the NRC within 30 days
of the date of the request for registration or as otherwise indicated in the request. In
addition, a general licensee holding devices meeting the criteria of paragraph (c)(13)(i) of
this section is subject to the bankruptcy notification requirement in Sec. 30.34(h) of this
chapter.
(iii) In registering devices, the general licensee shall furnish the following information
and any other information specifically requested by the Commission-(A) Name and mailing address of the general licensee.
(B) Information about each device: the manufacturer (or initial transferor), model
number, serial number, the radioisotope and activity (as indicated on the label).
(C) Name, title, and telephone number of the responsible person designated as a
representative of the general licensee under paragraph (c)(12) of this section.
(D) Address or location at which the device(s) are used and/or stored. For portable
devices, the address of the primary place of storage.
(E) Certification by the responsible representative of the general licensee that the
information concerning the device(s) has been verified through a physical inventory and
checking of label information.
(F) Certification by the responsible representative of the general licensee that they are
aware of the requirements of the general license.
(iv) Persons generally licensed by an Agreement State with respect to devices meeting
the criteria in paragraph (c)(13)(i) of this section are not subject to registration
requirements if the devices are used in areas subject to NRC jurisdiction for a period less
than 180 days in any calendar year. The Commission will not request registration
information from such licensees.
(14) Shall report changes to the mailing address for the location of use (including change
in name of general licensee) to the Director of Nuclear Material Safety and Safeguards,
ATTN: GLTS, U.S. Nuclear Regulatory Commission, Washington, DC 20555-0001
within 30 days of the effective date of the change. For a portable device, a report of
address change is only required for a change in the device's primary place of storage.
(15) May not hold devices that are not in use for longer than 2 years. If devices with
shutters are not being used, the shutter must be locked in the closed position. The testing
required by paragraph (c)(2) of this section need not be performed during the period of
Appendix 1-34
Clarus 500 GC Hardware Guide
storage only. However, when devices are put back into service or transferred to another
person, and have not been tested within the required test interval, they must be tested for
leakage before use or transfer and the shutter tested before use. Devices kept in standby
for future use are excluded from the two-year time limit if the general licensee performs
quarterly physical inventories of these devices while they are in standby.
(d) The general license in paragraph (a) of this section does not authorize the manufacture
or import of devices containing byproduct material.
2
Persons possessing byproduct material in devices under a general license in Sec. 31.5
before January 15, 1975, may continue to possess, use, or transfer that material in
accordance with the labeling requirements of Sec. 31.5 in effect on January 14, 1975.
Appendix I-35
Appendix I
`
Appendix 1-36
Appendix II
Ionization Potential
II
Appendix II-2
Clarus 500 GC Hardware Guide
For your convenience, we have reproduced ionization potentials for
representative compounds in the following categories:
•
Some atoms and simple molecules
•
Paraffins and cycloparaffins
•
Alkyl halides
•
Aliphatic alcohols, ethers, thiols, and sulfides
Appendix II-3
Appendix II-4
Clarus 500 GC Hardware Guide
Appendix II-5
Appendix II-6
Index
A
About This Manual, 1-3
Attenuation vs. detector output, 9-104
Autosampler
changing a syringe, 5
installing a syringe, 10
maintenance, 4
replacing the vial-locator mechanism, 11
Autosampler Error Messages, 10-7
B
Bead, NPD, changing, 9-67
Bead, NPD, conditioning, 9-70
C
CAP Injector Liner, 9-26
Capillary column
attaching to detector, 6-86
attaching to injector, 6-36
calculating a capillary column split ratio, 6-96
condition the column, 6-81
connect the column to the detector, 6-86
connect the column to the injector, 6-8
connect the column to the POC, 6-50
connect the column to the PSS, 6-24
installing
materials required, 6-5
overview, 6-8
summary, 6-4
tools required, 6-5
leak test, 6-78, 6-91
PSS and POC operating hints, 6-93
set up for split mode, 6-92
turn the heaters off, 6-7
Capillary column pressures, 6-69
Capillary column pressures, suggested values, 6-70
Capillary injector
fitting, 6-22
liner packing, 6-17, 9-31
Carrier Gas
PPC
Mass Flow Controller, 8-6
Carrier gas flow
setting
using soap bubble flowmeter, 5-15
Carrier gas pressure
setting, 6-67
Changing
charcoal trap, 9-36
septa, 14
Charcoal trap, changing, 9-36
Chemicals
Definitions of Warnings, 2-21
Hazardous, 2-20
Clean vs. bad cuts, 6-19, 6-37
Cleaning the syringe, 13
Column
before installing, 4-3
protecting, 4-6
Column hangers, installing, 4-4
Compressed gases, safety practices, 2-16
Conventions
Notes, cautions and warnings, 1-5
text, 1-5
D
Detector
output vs. attenuation, 9-104
Detector window, FPD, 9-86
E
ECD
cell failure, 2-14
damage, 2-14
labels, 2-13
performance, optimizing, 9-105
purchasers, 2-12
reporting radioactive exposure, 2-14
reporting theft or losses, 2-14
testing for radioactive leaks, 2-14
U.K. regulations, 2-15
wipe testing, 9-43
ECD Disposal, 9-48
ECD insulating cover, 9-45
ECD Maintenance
cleaning the anode, 9-41
ECD Maintenance, 9-40
ECID Maintenance
replacing the sealing ring, 9-63
EICD
performance, optimizing, 9-102
EICD Maintenance, 9-62
ElCD
attaching a packed column, 5-25
conductivity cell
cleaning, 9-65
cross section view, 9-65
replacing
reactor tube, 9-62
troubleshooting, 10-12
Electrical Safety, 2-8
Electrical, safety practices, 2-9
Electromagnetic Compatibility, 1-6
EMC see Electromagnetic Compatibility, 1-6
Environmental Conditions, 2-6
Error Messages, 10-4
I-2
F
FID
cross section view, 9-53
jet cleaning, 9-53
jet replacing, 9-49
performance, optimizing, 9-101
FID Maintenance, 9-49
Fitting
capillary injector, 6-22
packed column injector, 5-15
FPD
cleaning
detector liner, 9-84
detector window, 9-86
optical filter assembly, 9-82
performance, optimizing, 9-106
replacing
detector liner, 9-84
detector window, 9-86
optical filter assembly, 9-82
photomultiplier tube, 9-89
FPD Maintenance, 9-82
G
Gas Cylinders, 2-16
GC Troubleshooting, 10-9
H
Hangers, column, 4-5
heated zones, safety practices, 2-4
hourglass needle guide, replacing, 18
I
Injector fittings, 4-4
Installing
capillary column
materials required, 6-5
overview, 6-8
summary, 6-4
tools required, 6-5
packed column
materials required, 5-5
overview, 5-3
summary, 5-4
tools required, 5-5
J
Jet assembly
FID, replacing, 9-49, 9-53
FPD, cleaning, 9-93
FPD, replacing, 9-93
NPD, replacing, 9-77
L
Labels
Warning Signs, 1-8
Leak test
manual pneumatics
packed column detector fittinng, 5-27
packed column
injector fitting, 5-20
M
Maintenance, 3
autosampler, 4
autosampler, changing a Syringe, 5
autosampler, installing a Syringe, 10
autosampler, replacing the vial-locator
mechanism, 11
CAP injector Liner, 9-26
ECD, 9-40
ECD disposal, 9-48
ECD, cleaning the anode, 9-41
ECID, replacing the sealing ring, 9-63
EICD,, 9-62
FID, 9-49
FPD, 9-82
NPD, 9-67
PID, 9-56
PID, changing lamp window seals, 9-60
PID, cleaning the lamp, 9-58
PPC, 9-97
Midpoint pressure
PreVent Injector, setting, 7-19, 7-39
N
NPD
bead conditioning
for a capillary column, 9-74
for a packed column, 9-70
changing a bead, 9-67
cross section view, 9-77
NPD Maintenance, 9-67
O
Optical filter assembly, FPD, 9-82
Optimizing FID performance, 9-102
Oven Error Messages, 10-6
Overview
Clarus 500 GC, 3-3, 3-4
installing a capillary column, 6-8
PPC fundamantals, 8-3
touch screen, 3-7
P
Packed column
attaching
to an ElCD, 5-25
to detector, 5-24
to packed injector, 5-20
installing
materials required, 5-5
overview, 5-3
summary, 5-4
tools required, 5-5
Packed column injector
fitting, 5-15
Packed column injector liner
changing, 15
repacking, 15
Packed injector
removing the liner, 16
Packed injector liner
removing, 16
Photomultiplier tube, FPD, 9-89
PID
changing a lamp, 9-56
prolonging the life of a UV lamp, 9-105
PID Maintenance
changing lamp window seals, 9-60
cleaning the lamp, 9-58
PID Maintenance, 9-56
POC
operating hints, 9-107
POC operating hints, 6-93
PPC
auxiliary pressure and flow control, 8-34
capillary and PSS inlets, 8-11
carrier gas configuration, 8-16
carrier gas control, 8-5
detector gas flow control, 8-30
headspace analysis, 8-10
introduction, 8-3
mass-flow controller, 8-6
restrictor, replacing, 9-97
schematic of detector gas, 8-30
I-3
schematic of split PPC, 8-11
split control mode configuration, 8-19
theory
column temperature effects, 8-22
flow programmed operation, 8-26
pressure/oventrack operation, 8-28
velocity programmed operation, 8-27
theory of capillary column control, 8-22
tips and techniques, 8-38
correcting column dimensions, 8-39
effect of flow on pressurization rate, 8-38
pressure-pulse injection, 8-41
reducing carrier gas consumption, 8-42
vacuum compensation, 8-18, 8-29
PPC Maintenance, 9-97
PPC Restrictor Information, 9-98, 9-110
Practical hints, 9-101
Precautions, 2-5
PreVent
Column Isolation Technique, 7-72
initial pressures, 7-19, 7-39
Large Volume Injections, 7-77
Operating Techniques, 7-71
Overview, 7-3
Solvent Purge Technique, 7-75
Time Saver Technique, 7-80
TurboMass
connecting TurboMass transfer line, 7-52
PreVent adapter
detector
installation summary, 7-27
installing a column, 7-30
installing a restrictor, 7-27
injector
installation summary, 7-5
installing a column, 7-8
installing a restrictor, 7-5
leak checking, 7-11
restrictor replacement, 7-69
TurboMass
installation summary, 7-45
installing a column, 7-49
installing a restrictor, 7-47
Programmed Pneumatic Control
definition, 8-3
Protecting columns, 4-6
PSS
operating hints, 9-107
PSS operating hints, 6-93
R
Radioactive exposure, reporting, 2-14
Repacking
I-4
packed column injector liners, 15
Restrictor, replacing a PPC, 9-97
Reversing TCD polarity, 9-101
S
Safety
chemical use, 2-20
compressed gases, 2-16
ECD Radioactive Hazards, 2-12
electrical, 2-9
generic warnings, 2-3
heated zones, 2-4
high voltage, 2-8
moving the Clarus GC, 2-11
thermal runaway protection, 2-4
ventilation, 2-16
Safety Information, 2-5
electrical safety, 2-8
environmental conditions, 2-6
gas cylinders, 2-16
Septa, changing, 14
Setting up
split mode, 6-92
Soap bubble flowmeter
using, 5-15
Spare components, 10-10
Spare Components, 10-10
Split liner, 6-18, 9-28
Split mode
setting up, 6-92
Splitless liner, 6-18, 9-28
Syringe
cleaning, 13
servicing an idle, 13
T
TCD polarity, reversing, 9-101
Top cover hold down screws, 9-36
Touch Screen, 3-7
Troubleshooting, 10-3
autosampler error messages, 10-7
dual identical channels, 10-11
ElCD, 10-12
error messages, 10-4
formatted errors, 10-8
oven error messages, 10-6
spare components, 10-10
steps, 10-10
V
Ventilation, safety practices, 2-16
Wipe test
See Wipe testing ECD, 9-43
Wipe testing
ECD, 9-43
W
Warnings
Hazardous Chemical, 2-21
I-5
I-6
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