Clarus 400 GC Hardware Guide

Clarus 400 GC Hardware Guide
Clarus 400 GC Hardware Guide
Release History
Part Number
Release
09936811
A
Publication Date
September 2007
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 © 2007 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.
Clarus 400 GC is a trademark of PerkinElmer, Inc.
e-ssentials is a trademark of PerkinElmer, Inc.
Table of Contents
Introduction...................................................................................................5
About This Manual .........................................................................................7
Manual Conventions and Screen Abbreviations .............................................9
Glossary of Clarus 400 GC Terms................................................................11
Glossary of Chromatographic Terms............................................................13
Symbols Located on the Clarus 400 GC.......................................................16
System Description......................................................................................17
Introduction...................................................................................................19
Overview of the Clarus 400 GC....................................................................20
About the Keyboard......................................................................................22
About the Screen...........................................................................................23
Function Key Descriptions ...........................................................................24
Control Key Descriptions .............................................................................27
Entry Keys ....................................................................................................29
Parameter Keys .............................................................................................31
Before You Install a Column ....................................................................33
Column Installation Information...................................................................36
Protecting Your Column ...............................................................................38
Turning the Oven Off and On .......................................................................39
Turning Injector Heaters Off and On............................................................40
Turning Detector Heaters Off and On...........................................................42
Using the Built-in Stopwatch........................................................................44
Installing a Packed Column .......................................................................47
Packed Column Injector Overview ...............................................................49
Installing A Capillary Column ..................................................................61
Summary .......................................................................................................64
Materials and Tools Required .......................................................................65
Step A: Turn the Heaters Off: .......................................................................67
Step B: Connect the Column to the Injector: ................................................68
Step C:
Set the Carrier Gas Using Manual Pneumatics...........................82
Step D
Leak Test All New Connections:................................................85
Step E:
Condition the Column and the
Mechanical Joint Between the Pre-column and Column: ..........86
Step G:
Leak Test All New Connections:................................................92
Step H:
Set up the Split Mode for a CAP Injector:..................................93
Calculating a Capillary Column Split Ratio .................................................94
Troubleshooting ..........................................................................................95
Messages Requiring PerkinElmer Service Assistance..................................98
Background Calibration Error Messages ......................................................99
Miscellaneous Error Messages....................................................................100
Illegal Value Error Messages......................................................................103
GC Troubleshooting....................................................................................104
Maintenance ..............................................................................................109
Autosampler Maintenance ..........................................................................112
Syringe Maintenance ..................................................................................117
Injector Maintenance ..................................................................................119
ECD Maintenance.......................................................................................135
FID Maintenance ........................................................................................143
NPD Maintenance.......................................................................................150
TCD Maintenance.......................................................................................168
Practical Hints...........................................................................................169
Reversing TCD Polarity..............................................................................171
Optimizing FID Performance .....................................................................172
Filtering Detector Output............................................................................173
Autozero Display Sensitivity ......................................................................174
Attenuation vs. Detector Output .................................................................175
Appendix U.S. Nuclear Regulations ......................................................177
Nuclear Regulatory Commission Regulations............................................186
Index...........................................................................................................211
Introduction
1
Clarus 400 GC Hardware Guide
About This Manual
The Clarus 400 GC Hardware and Software Manual is your complete detailed guide to
setting up the Clarus 400 GC and integrated autosampler in preparation for running samples.
This manual contains information and procedures for all of the available injectors and
detectors. To benefit the most from this manual, we recommend that you read all of the
chapters in sequence and follow the procedures provided that apply to your specific injectors
and detectors as closely as possible. In most cases, reading one chapter is a prerequisite for
going on to the next.
For detailed safety information please refer to the Clarus 400 GC safety and Preparing Your
Laboratory Guide (0993-6813).
7
Introduction
The manual consists following chapters:
Chapter 1
Introducing the Clarus 400 GC provides an introduction to the manual,
manual conventions, screen abbreviations, a glossary of Clarus 400 GC
terms and a glossary of chromatographic terms.
Chapter 2
System Description describes the Clarus 400 GC and its major features,
including keyboard and display descriptions.
Chapter 3
Before You Install a Column contains general information regarding
column installation and the basic procedures you ought to know in order
to install a column.
Chapter 4
Installing a Packed Column contains procedures for connecting a
packed column to the packed column injector and setting the carrier gas
flow using manual pneumatics.
Chapter 5
Installing a Capillary Column contains procedures for connecting a
capillary column to a Capillary Injector (CAP). It also describes how to
set the gas flows using manual pneumatics.
Chapter 6
Troubleshooting lists the messages that may appear on the screen
display, their causes and cures.
Chapter 7
Maintenance includes a variety of routine and preventive maintenance
procedures for all injectors and detectors.
Chapter 8
Practical Hints contains useful information on attenuation, filtering
detector output, and optimizing FID.
Appendix
A copy of Regulation 10 C.F.R. Section 31.5 of the U.S. Nuclear
Regulatory Commission.
Index
8
Clarus 400 GC Hardware Guide
Manual Conventions and Screen Abbreviations
Manual Conventions
Individual keys are displayed in the text by enclosing the name of the key in square brackets.
For example, [Oven Prog], [Enter], [->Set], [Method], [System], [1], [8], etc.
All temperatures are in degrees Celsius ( C).
Screen displays are presented throughout the text as a double-lined box:
Method 1
READY
75°
Screen Abbreviations
Autosamp – autosampler
AUX – Auxiliary zone
Cap – capillary split/splitless injector
Cmptr – computer
Ctrl – syringe control parameters
ECD – Electron Capture Detector
Equil – equilibration
Extrn – external
FID – Flame Ionization Detector
Gen – generate
GSV – gas sampling valve
Inj – injector
Inj/Vial – injections per vial
9
Introduction
Int – integrator
kPa – kilopascals
NPD – Nitrogen Phosphorus Detector
OnCol – on column
Ovn – oven
Paus – pause
Pkd – packed injector
Pre – # of preinjection syringe washes
Pres – pressure
Prg – autosampler program
Pri – priority sample vial
Psi or psig – pounds per square inch (gauge)
Rec – recorder
Resm – resume
Stpwtch – stopwatch
TCD – Thermal Conductivity Detector
10
Clarus 400 GC Hardware Guide
Glossary of Clarus 400 GC Terms
The glossary of Clarus 400 GC terms are divided into two types:
•Autosampler Terms
•Instrument-Specific Terms
Autosampler Terms
Term
Description
Washes
Washing the syringe.
Pre
The number of prewashes of sample to prime the syringe (no
pumping).
Post
The number of post injection syringe washes with a solvent.
Pumps
The number of times the syringe draws up sample and
evacuates it before acquiring the volume. This is done to
eliminate bubbles.
Mode
The style of injection.
Fast
Fast speed of the syringe during sample injection. This is used
to eliminate discrimination in the needle.
Normal
Normal speed of the syringe during sample injection.
Slow
Slow speed of the syringe during sample injection in order to
inject directly into a wide-bore capillary column, in hot
injection port.
Solv
The number of solvent washes performed before the
preinjection sample washes.
Visc
The number of seconds the plunger pauses when drawing up a
viscous sample into the syringe.
11
Introduction
Instrument-Specific Terms
Term
Description
Background
compensation
A routine that automatically subtracts a stored calibrated
baseline profile from the signal generated during a GC run.
Ballistically
Changing the oven temperature as quickly as possible to reach
a set point.
Detector
background
The detector output signal when no components are being
eluted.
Equilibration
The delay time after the method set points have been reached
before the system becomes READY.
Isothermal method
A method in which the oven temperature remains constant
throughout a GC run.
Method
A collection of parameters that control the GC.
Negative-time
event
A timed event that you set to occur before the instrument
becomes READY.
Parameter
An independent variable used to specify a condition to be met.
Pre-run
The time after equilibration during which negative-time events
are executed.
Range
For a Flame Ionization Detector, range means amplification of
the detector output signal. For a Thermal Conductivity
Detector, range means the bridge current.
Ready
Indicates that all method parameters have reached their set
points and that you can start your analysis.
Run
The time from sample injection to the end of the oven
temperature program.
Sleep mode
The GC can be set to a predefined method for gas savings.
Timed Events
Events that take place before or during a GC run as
specified in a timed events table.
Zone
A heated area in the GC oven, injector, or detector.
12
Clarus 400 GC Hardware Guide
Glossary of Chromatographic Terms*
Adsorption – A process that occurs at the surface of a liquid or solid as a result of the
attractive forces between the adsorbent and the solute. These forces may be physical or
weakly chemical.
Analysis – The complete investigation of a sample by gas chromatographic separation
including identification of the sample components and quantitative measurements.
Anode – The negatively charged electrode in any electrical circuit to which charged particles
and ions are attracted.
Band Broadening – A process that occurs in the GC whereby the peak width for a
component increases the longer the component travels through the column.
Baseline – The detector signal to a recorder or integrator when only the carrier gas is passing
through the detector.
Baseline drift – Any regular change occurring in the baseline signal from the detector,
usually resulting from column temperature and/or gas flow changes.
Blank run – A run without the sample being injected.
Bleed – The evaporation of the stationary phase from a column.
Capillary column (wall coated open tubular column) – A small-internal-diameter column
whose inside wall is coated with a liquid phase.
Carrier gas – The mobile phase of the separation system. An inert gas which transports the
sample from the injector through the column to the detector. This gas is usually helium,
hydrogen, or nitrogen.
Column conditioning – A process for producing a stable column by heating the column with
carrier gas flowing to remove volatile impurities from the stationary phase.
Detectors – Hardware that responds to sample components producing an electrical signal that
can be measured to quantitate the amount of each component present.
*
Reference: Denney, R.C. A Dictionary of Chromatography.
13
Introduction
Flow rate – The mass flow of carrier gas or detector gas in milliliters per minute.
Ghost peaks – Peaks that are not due to sample components, for example, peaks produced by
carrier gas impurities, septum, or components from previous analyses.
Injection port – The hardware through which the sample is introduced to the column by
injection.
Linearity – Quantitatively all detectors will produce a linear response with respect to solute
concentration over a defined range, for example, the Linear Range.
Liquid phase – The material in the column that causes the components to separate because of
partitioning of the components between the mobile phase (carrier gas) and the stationary
phase (liquid phase).
Lowest limit of detection – The smallest amount of sample that can be detected by the
detector being used. Usually defined as any signal that is as great as two times the noise
level. Also referred to as Minimal Detectable Quantity (MDQ).
Mobile phase – The gas which carries the solute (sample) along and over the column
material. This carrier gas is inert and usually helium, nitrogen, or hydrogen.
Noise – Background signal fluctuations arising from a detector response. This response is the
result of the column installed, carrier gas purity, electronic components, etc. The
response of any detector is defined by the signal-to-noise ratio.
Partition Coefficient – The differential solubility of a substance in two different phases. In
the case of gas–liquid chromatography, the sample components reach an equilibrium
between the gas phase (mobile) and the liquid phase (stationary). Each component has a
different partition coefficient thus causing separation in the column.
Pressure programming – Pressure control through an independent four-step, three-ramp
program for each carrier gas channel.
Resolution – The degree of separation between two peaks.
Retention time – The time interval from the point of injection to the appearance of the peak
maximum, of a component’s signal.
14
Clarus 400 GC Hardware Guide
Septum – Silicone rubber material placed in the injection port through which the injection is
made. When the needle is withdrawn, the silicone rubber reseals, thus not allowing any
sample or carrier gas to escape.
Stationary phase – The liquid or solid adsorbent portion of the column that retains
components passing through the GC column.
Syringes – Precision dispensing devices used to deliver sample to the GC. Liquid and gas
syringes are available.
Tailing – When a peak is not symmetrical or Gaussian shaped but the back end is broadened,
it is said to be tailing.
Temperature programming – A technique commonly used to increase the rate of elution of
the components. After the sample is injected into the oven at a specific temperature, the
temperature program increases the oven temperature to the prescribed temperature at a
defined rate (in ºC/min).
Unretained peak – A component that is not retained by the column. The time taken for an
unretained sample to pass through the column is the same time as the time taken for the
carrier gas to pass through.
15
Introduction
Symbols Located on the Clarus 400 GC
PNEUMATIC SYMBOL
LEGEND
CARRIER
FLOW / PRESSURE
FID
TCD
NO CONNECTION
16
DETECTOR MAKE-UP/
REFERENCE FLOW
HYDROGEN
AIR
NPD
SPLIT FLOW
ECD
System Description
2
Introduction
The Clarus 400 Gas Chromatograph is a dual-channel, temperature-programmable stand-alone
gas chromatograph (GC). It is available in many configurations, such as with or without, an
autosampler and a variety of injector/detector combinations to provide you with total GC
flexibility. The Clarus 400 GC is microprocessor controlled, where you enter the operating
parameters from the color-coded keyboard and view the prompting text and monitor instrument
functions on a large two-line vacuum fluorescence display.
Figure 1. The Clarus 400 GC.
System Description
Overview of the Clarus 400 GC
Your Clarus 400 GC may have none, one, or two of the following detectors installed:
¾ Flame Ionization (FID)
¾
Nitrogen Phosphorus (NPD)
¾ Electron Capture (ECD)
¾
Thermal Conductivity (TCD)
The FID, ECD, TCD, or the NPD, may be installed in either the front or the rear detector
position.
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).
Up to two gas sampling valves may be installed.
The Clarus 400 is a manual pneumatics instrument.
The carrier gas and detector gas controls are built into the pneumatics control panel on the
Clarus 400. The carrier gas controls are used to set the flow for packed injectors and the
pressure for CAP injectors. The detector gas controls are used to set the hydrogen and air for
FID and NPD reference for TCD; and make-up gas for the ECD. Figure 2 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 detector-pneumatic
controls are on the right.
20
Clarus 400 GC Hardware Guide
Channel 1
Channel 2
Figure 2. Example of a dual-channel pneumatics control panel in the Clarus 400
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.
21
System Description
About the Keyboard
The keyboard is your link to the software. The keyboard has 35 keys divided into the
following groups:
•
•
•
•
Note:
Function keys
Parameter keys
Entry keys
Control keys
As you run this instrument you will see software functions on the display that are
not supported by the Clarus 400 GC. Please ignore these functions and continue with your
analysis.
An audible short beep sounds every time a key is pressed. A long beep sounds when an error
has been made. The key groups and their locations are illustrated in Figure 3.
Function Keys
Method
System
Run
Auto
Parameter Keys
Entry Keys
Oven
Temp
Time
Rate
7
8
9
Inject
Temp
Carrier
Gas
Valve
4
5
6
Detect
Temp
Range
Output
on yes
1
2
3
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Control Keys
Figure 3. The Clarus 400 GC keyboard.
22
Clarus 400 GC Hardware Guide
About the Screen
The Clarus 400 GC screen is a 2-line by 20-character vacuum fluorescent display.
Figure 4. Vacuum fluorescent screen.
The screen displays status information, error messages, and interactive menus (method,
system, configuration, autosampler, and background).
23
System Description
Function Key Descriptions
The four function keys, [Method], [System], [Auto], and [Background], give access to the toplevel software menus. The [System] menu, in addition to presenting a number of system
utility options, provides access to the Configuration Mode.
Pressing a function key displays either a one-page menu or the first page of a two-page menu
associated with that key.
System
Auto
Oven
Temp
Time
Rate
7
8
9
Inject
Temp
Carrier
Gas
Valve
4
5
6
Detect
Temp
Range
Output
on yes
1
2
3
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
Figure 5. The Function keys.
24
Run
Method
0 no
Clarus 400 GC Hardware Guide
The Method Function Key
Pressing [Method] displays the first page of the two-page Method Menu.
Method 1
¦ Setup Edit
Active
Copy
>
Method Menu, Page 1
Method 1
¦ Gen Delete
Active
Print
>
Method Menu, Page 2
The commands in the Method Menu provide utilities for managing and editing methods.
Procedures for using these utilities are given in the Clarus 400 Software Guide (0993-6812),
Controlling the Clarus 400 GC chapter. A brief description of these utilities follows.
Command
Description
Setup
Sets up a Stored Method as the Active Method. This option is
not available during a GC run or with active automation.
Edit
Allows you to display and edit a Stored Method.
Copy
Copies an existing method to another method number.
Gen
Allows you to generate a new method from the default method.
Delete
Allows you to delete one of the Stored Methods.
Prnt
Prints a method if a printer is attached.
The System Function Key
Pressing [System] displays the Page 1 of the two-page System Control menu.
System Control
¦ Config
Lock >
System Control Menu, Page 1
System Control
¦ Stpwtch Extrn Prnt
>
System Control Menu, Page 2
The commands in the System Control menu provide a number of system utilities.
Procedures for using these utilities are given in Clarus 400 Software Guide (0993-6812),
“System Utilities.” A brief description of these utilities follows.
25
System Description
Command
Description
Config
Selecting this option puts the system into the Configuration Mode.
The configuration menus allow you to specify configuration details
for a variety of hardware options.
Lock
Locks or unlocks the keyboard. For procedural details see Locking
and Unlocking the Keyboard in Chapter 13, “System Utilities.”
Stpwtch
Accesses the stopwatch function. For procedural details see Chapter
13, “System Utilities.”
Extrn
Used to set up an external computer or printer.
The Auto(sampler) Function Key
Pressing [Auto] displays the first page of the two-page Autosampler (A/S) menu.
A/S Stopped
¦ Prg Ctrl START
>
Autosampler Menu, Page 1
A/S Stopped
¦ Park Clean
Print >
Autosampler Menu, Page 2
The top line displays the autosampler’s status (for example, Stopped). The bottom line
displays menu options.
Autosampler details are too specialized and extensive to be described in this chapter. All
details are provided in Chapter 11, “Controlling the Autosampler.”
The Background Function Key
Pressing [Background] displays the Background menu on the bottom line and the background
status on the top line.
Background 1
Off
¦ Calibrate
Detailed procedures for using this function are given in Clarus 400 Software Guide (09936812), “Background Compensation.”
26
Clarus 400 GC Hardware Guide
Control Key Descriptions
Run
Method
System
Auto
Oven
Temp
Time
Rate
7
8
9
Inject
Temp
Carrier
Gas
Valve
4
5
6
Detect
Temp
Range
Output
on yes
1
2
3
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Figure 6. The Control keys.
The Run Key
Press the [Run] key to start a GC run after manually injecting a sample, continue to run after
an oven hold, or to initiate calibrating a background. Details for using [RUN] for the latter
purpose are given in Clarus 400 Software Guide (0993-6812), “Background Compensation.”
The Reset Oven Key
This key is used to reset the oven temperature during a run.
27
System Description
Reset to oven Temp
¦ 1
2
3
During the execution of a temperature program, you can elect to heat the oven ballistically to
a higher step by selecting the appropriate number from the menu.
Select 1 to stop a run and reset the instrument to the initial method conditions. Additional
details are given in Clarus 400 Software Guide (0993-6812), “Controlling the Clarus 400
GC.”
The Status Escape Key
The [Status Escape] key is used to escape from various environments. The top level to which
you can escape is the System Status screen.
Method 1
READY
75º
A screen similar to that above appears if you escape from the Method, System, Autosampler,
or Background menus.
If you press [Status Escape] a second time, the screen displays the Run End Time, as shown
below.
Method 1
READY
END
13.0m
In the case of a submenu, escape brings you up to a previous menu level.
The Delete Key
Use this key to delete a timed event or oven temperature program step.
28
Clarus 400 GC Hardware Guide
Entry Keys
Run
Method
System
Auto
Oven
Temp
Time
Rate
7
8
9
Inject
Temp
Carrier
Gas
Valve
4
5
6
Detect
Temp
Range
Output
on yes
1
2
3
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Figure 7. The Entry keys.
All Entry keys, except for the [->Set] key, are similar to those on a hand calculator and are
used to enter numeric data, clear an entry, etc.
The [CE] key (Clear Entry) is used to clear a value before it is entered or to clear certain error
messages from the screen.
29
System Description
The [On/Yes 1] and [Off/No 0] keys are multipurpose keys. In addition to using these keys
for entering a numeric 1 or 0, they are used to enter "On" or "Off,” "Yes" or "No" in response
to questions requiring these answers.
The [->Set] key is used to move the screen cursor to a desired screen parameter or menu
option for selection. How to use this key for this purpose is described in the next chapter.
The[->Set] key is also used to activate the Autozero, ignite the FID flame, and actuate
connected valves.
30
Clarus 400 GC Hardware Guide
Parameter Keys
Run
Method
System
Auto
Oven
Temp
Time
Rate
7
8
9
Inject
Temp
Carrier
Gas
Valve
4
5
6
Detect
Temp
Range
Output
on yes
1
2
3
Atten
Auto
Zero
Events
off
Reset
Oven
Status
Escape
Delete
Enter
Set
CE
0 no
Figure 8. The Parameter keys.
The Parameter keys are used to display operation or configuration parameters. Pressing a
Parameter key when you not in the Configuration Mode displays the operating parameter
associated with that key. Operating parameters are described in Clarus 400 Software Guide
(0993-6812), “Controlling the Clarus 400 GC chapter.” In the Configuration Mode, pressing
a Parameter key displays the configuration of the hardware associated with that key.
31
System Description
32
Clarus 400 GC Hardware Guide
Before You Install
a Column
3
33
The moment the Clarus 400 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.
WARNING
This chapter contains general column installation information, and the following
procedures:
•
Protecting your column.
•
Turning the oven off and on.
•
Turning injector heater(s) off and on.
•
Turning detector heater(s) off and on.
•
Using the built-in stopwatch.
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 9 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 9. 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 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.
36
Clarus 400 GC Hardware Guide
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 10. A column hanger installed in the oven rear position.
37
Before You Install
a Column
Protecting Your Column
The Clarus 400 GC provides a means for protecting your column(s) from overheating. It
does this by not allowing the oven to heat up beyond what we call the Oven Maximum
Temperature Limit (OMTL), a value that you set in the Configuration Mode.
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.
The following screen shows an example of an error message:
Illegal Oven Temp
Range: xxx ---> yyy
Where xxx and yyy are the permissible minimum and maximum oven temperatures
respectively. You enter the OMTL in the Oven Maximum screen which is displayed from the
Configuration Mode.
To display the Oven Maximum screen:
1. Press [System].
The first page of the System Control Menu appears:
System Control
¦ Config
Lock
>
2. Press [Enter] [Oven Prog].
Oven Maximum
Temp Limit
Config
¦ 450°
3. Type in the new OMTL (Oven Maximum Temperature Limit), then press [Enter].
4. Press [Status Escape].
38
Clarus 400 GC Hardware Guide
Turning the Oven Off and On
To turn the oven off:
1. Open the oven door.
The following message appears:
OVEN DOOR OPEN
Press CE to Continue
The oven heater turns off.
2. Press [CE].
A status screen similar to the following appears:
Method 1
Ovn
OVN OFF
55°
Notice that as the oven cools down, the actual temperature is continuously updated on the
bottom line. When the oven temperature reaches 40 ºC, the oven fan turns off.
3. Press [Status Escape].
To turn the oven on:
Simply close the oven door.
39
Before You Install
a Column
Turning Injector Heaters Off and On
NOTE: The examples shown below assume that the Clarus 400 GC is in the READY state, position 1
(front) contains a capillary injector, and position 2 (rear) contains a packed injector.
To turn the injector heaters Off:
1. Press [Inject Prog].
A screen similar to the following appears:
Cap 1
Temperature
150°
¦ 150°
2. Press [Off/No 0].
3. Press [Enter].
The screen changes to:
Cap 1 NOT RDY
Temperature
149°
¦ Off
Notice that the injector starts to cool.
4. To turn off the second injector heater, display its screen and press
[Inject Prog] again.
Pkd 2
Temperature
150°
¦ 150°
5. Follow steps 2 and 3 above.
6. Press [Status Escape].
40
Clarus 400 GC Hardware Guide
To turn the injector heaters on:
1. Display the appropriate Injector Temperature Screen by pressing
[Inject Prog] once or twice.
Cap 1
Temperature
30°
¦ Off
2. Enter a temperature set point. For example type: [1] [5] [0], then press [Enter]. The
screen changes to:
Cap 1
NOT RDY
Temperature
40°
¦ 150°
3. Press [Status Escape].
41
Before You Install
a Column
Turning Detector Heaters Off and On
NOTE: The examples shown below assume that the Clarus 400 GC is READY, an FID
has been installed in position 1 (front), and an ECD is in position 2 (rear).
To turn the detector heaters Off:
1. Press [Detect Control].
A screen similar to the following appears:
FID 1
Temperature
150°
¦ 150°
2. Press [Off/No 0].
The screen changes to:
FID 1 NOT RDY
Temperature
150°
¦ 0°
Notice that the cursor is blinking, indicating a new value.
42
Clarus 400 GC Hardware Guide
3. Press [Enter]. The screen changes to:
FID 1 NOT RDY
Temperature
149°
¦ Off
Notice that the detector starts to cool.
4. To turn off the second detector heater, display its screen and press [Detect
Control] again.
ECD 2
Temperature
150°
¦ 150°
5. Follow steps 2 and 3 above.
6. Press [Status Escape].
To turn the detector heaters On:
1. Display the appropriate Detector Temperature screen by pressing [Detect
Control] once or twice.
FID 1 NOT RDY
Temperature
30°
¦ Off
2. Enter a temperature set point.
For example, type: [1] [5] [0], then press [Enter]. The screen changes to:
FID 1 NOT RDY
Temperature
40°
¦ 150°
3. Press [Status Escape].
43
Before You Install
a Column
Using the Built-in Stopwatch
To measure flows, use the stopwatch function with a soap bubble flowmeter. The following
example shows how to measure flows using the built-in stopwatch.
1. Press [System].
The first page of the System Control menu appears:
System Control
¦ Config
Lock >
2. Press [System] again.
The second page of the System Control menu appears:
System Control
¦ Stpwtch Extrn Print >
3. Press [Enter].
The Stopwatch screen appears:
Stopwatch
0.00 m
Flow
Vol ¦ 1
4. Enter the volume of the flowmeter you are using.
For example, change the default to 10 mL by typing [1] [0], then pressing [Enter].
The screen changes to:
Stopwatch
0.00 m
Flow
Vol ¦ 10
Start the Stopwatch
5. When the bubble reaches the first graduation mark, Press [Enter]. This starts the
timer.
44
Clarus 400 GC Hardware Guide
The elapsed time and calculated flow appear on the screen and are continuously
updated.
Stopwatch
0.50 m
Flow 20
Vol ¦ 10
Stop the Stopwatch
6. When the bubble reaches the second graduation mark, press [Enter].
The system freezes, calculates, and displays the flow in mL/min as of that point in
time.
Stopwatch
2.50 m
Flow 4.0
Vol ¦ 10
Reset the Stopwatch
7. Press [CE].
8. Press [Status Escape].
45
Before You Install
a Column
46
Clarus 400 GC Hardware Guide
Installing a Packed
Column
4
47
Clarus 400 GC Hardware Guide
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 1/4-inch glass or metal packed
columns. In addition, by installing the 530 Micron Wide-Bore Adapter Kit (Part No N6120001) you can convert the injector to accept wide-bore capillary columns.
Septum (P/N N662-1028)
Needle Guide
Quartz Liner
(P/N N612-1003)
Gas In
Figure 11. Packed Column Injector.
49
Installing a Packed Column
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 11) and the addition of the adapter fitting (Part No
N610-0083). 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 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 11 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 widebore 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 (P/N N610-1380) and use
the “SLOW" injection mode.
50
Clarus 400 GC Hardware Guide
Standard Packed
Column
Off-Column
Position
On-Column
Position
Hourglass
Standard
Liner
Wide-Bore
Glass
Injector
Liner
Wide-Bore
Glass
Injector
Liner
Silanized
Glass Wool
Silanized
Glass Wool
Hourglass
1 5/8-inches
Mark
Adapter
Fitting
Adapter
Fitting
Adapter
Fitting
530 Micron
Wide-Bore
Column
530 Micron
Wide-Bore
Column
530 Micron
Wide-Bore
Column
Figure 12. Cross sections of three packed injector configurations with a wide-bore
column.
51
Installing a Packed Column
Step 1: Turn off the Heaters
WARNING
The moment the Clarus 400 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 400 GC Software 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
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 (or 620 kPa or 6.2 bar).
3. Press [Carrier Prog] until the appropriate screen appears.
Flow 1
Set
30
¦ 30mL/min
4. Type the desired flow setpoint value and press [Enter].
52
Clarus 400 GC Hardware Guide
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.
HEAD PRESSURE
Flow
Control
Knob
CARRIER FLOW
Figure 13. Flow Control Knob.
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 400 GC Software Guide (0993-6812) before proceeding.
1. Locate the packed injector fitting inside the oven.
53
Installing a Packed Column
Packed Injector Fitting
Figure 14. A packed injector fitting.
6. Attach a soap bubble flowmeter to the packed injector fitting.
7. Turn on the carrier gas at the tank and adjust the line pressure to 90 psig.
8. Press [System] [System] [Enter] to display the stopwatch screen.
9. Start the carrier gas flowing by turning the flow controller knob counterclockwise.
10. Measure the flow.
NOTE: For best accuracy, use a soap bubble flowmeter volume or electronic flowmeter that gives a
reading of at least 30 seconds.
11. 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.
12. Disconnect the soap bubble flowmeter before proceeding to the next step.
54
Clarus 400 GC Hardware Guide
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 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 the following
figure).
Figure 15. 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.
CAUTION
Do not overtighten column nuts. Overtightening causes permanent
damage to the fittings.
55
Installing a Packed Column
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.
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 ºC/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, then press [Oven Prog].
The Oven Temperature screen appears.
Oven
NOT RDY
TEMP 1
¦
30°
75°
2. Enter an oven temperature set point of 50, then press [Enter].
The Oven Time screen appears:
Oven
NOT RDY
0.0m
TIME 1
¦ 999.9m
3. Enter a (Hold) TIME of 10, then press [Enter].
The Oven Rate screen appears:
Oven
NOT RDY
RATE 1
¦
30°
End
4. To add another program step, enter a RATE of 5 (ºC/min).
56
Clarus 400 GC Hardware Guide
A screen similar to the following appears:
Oven
NOT RDY
TEMP 2
¦
40°
50°
5. For TEMP 2, enter a set point 25 ºC to 50 ºC above your planned analytical operating
temperature.
For example, enter a set point of 150.
Oven
NOT RDY
TEMP 2
CAUTION
50°
¦ 150°
To avoid damaging the column, do not enter a temperature higher
than the maximum operating temperature specified by the column
manufacturer.
6. Press [Enter]. The next screen is:
Oven
TIME 2
0.0m
¦ 999.9m
7. Press [Enter]. The next screen is:
Oven
RATE 2
NOT RDY
¦
End
8. Set an Injection Temperature about 50 ºC higher than the TEMP 2 setting.
9. Turn Detector Temperature off. Press [RUN] and allow the system to run overnight.
10. The next morning press [Reset Oven].
A menu similar to the following appears:
Reset to Oven Temp
¦ 1
2
57
Installing a Packed Column
11. Press [Enter]. This resets the oven temperature set point to that specified for TEMP 1 at
the beginning of the temperature program.
12. Open the oven door, then press [CE].
Allow the oven to cool until the oven fan goes off. This occurs when the oven cools
down to 40 ºC.
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 16. Packed column attached to the rear detector fitting.
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.
58
Clarus 400 GC Hardware Guide
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.
Step 7: Leak Test the Column/Detector Connection
The following procedures describe leak testing the column to detector connections.
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 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 400 GC Software Guide,
Active Method chapter for information on setting up detectors).
59
Installing A
Capillary Column
5
Clarus 400 GC Hardware Guide
This chapter describes how to install a capillary column in the Capillary Split/Splitless (CAP)
The information in this chapter is presented as one sequential procedure (Steps A through I)
for all CAP injector with the following procedural steps:
•
Setting carrier gas flow using manual pneumatics
•
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
The CAP injector uses 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.
63
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 Split/Splitless (CAP) injector.
C.
Set the carrier gas to the proper pressure (Set the pressure for the CAP using the
optional flow readout or a flowmeter.)
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.
64
Clarus 400 GC Hardware Guide
Materials and Tools Required
1
•
1/8-inch x 1.0-mm graphite ferrules (P/N 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 (P/N 0990-7273)1
•
Deactivated 0.53-mm i.d. fused silica (P/N N610-1724)
•
Fused-silica universal connector (P/N N930-2149)
•
Capillary column of your choice
•
White-out or felt-tip marker
•
Scribe for cutting columns (P/N N930-1376)
(Pointed scribes are not recommended.)
•
Leak-test solution or electronic leak tester
Shipped in the Clarus 400 GC Shipping Kit.
65
Installing A Capillary Column
1/8-inch Column Nut
(P/N 0990-3453)
1/8-inch Graphite/Vespel Ferrule
(P/N 0990-3981)
1/16-inch Graphite/Vespel Ferrule
(P/N 0990-3700)
1/16-inch Column Nut
(P/N 0990-3392)
Figure 17. Examples of required fittings.
66
Clarus 400 GC Hardware Guide
Step A: Turn the Heaters Off:
CAUTION
The moment the Clarus 400 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 3 of this manual “Before
You Install a Column.” If you have not read this chapter, please do
so before proceeding
67
Installing A Capillary Column
Step B: Connect the Column to the Injector:
This step contains a procedure that describes how to connect a column to Column to the
Split/Splitless (CAP) injector:
Step B:
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 O-ring and flows through the
quartz liner past the column tip.
68
Clarus 400 GC Hardware Guide
Septum (P/N N662-1028)
Septum Purge
Carrier Gas In
O-Ring
(P/N N930-2783)
Split Vent
Quartz Liner
Spit Point
(Column Tip)
Capillary Column
1/4-inch to
1/16-inch
Column Fitting
Figure 18. 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 (P/N N612-1002).
•
Wide-bore (4-mm i.d.) liner (P/N N612-1001).
69
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 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 widebore liner should be used with columns having an i.d. of 0.32 mm or greater.
70
Clarus 400 GC Hardware Guide
Table 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.
Manual ControlPneumatics
The injector pneumatics consist of a manual pneumatics (flow control valves and pressure
regulators) version.
For manual pneumatics, the pneumatics consists 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 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.
71
Installing A Capillary Column
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.
Septum Cap
(P/N N610-0153)
Figure 19. Removing the septum cap.
72
Clarus 400 GC Hardware Guide
3. Remove the injector cover.
Injector
Cover
Figure 20. Removing the injector cover.
4. Loosen the threaded collar by using the spanner (P/N N610-1359) provided, then
remove the threaded collar.
Spanner
(P/N N610-1359)
Figure 21. Loosening the threaded collar.
5. Replace the septum cap on the injector.
6. Pull the septum cap upwards to remove the septum purge assembly.
73
Installing A Capillary Column
Figure 22. Removing the septum purge assembly.
7. 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.
8. Ensure that the CAP injector liner is cool, then twist the CAP injector liner-removal
tool (P/N 0250-6534, see Figure 24) 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 liner-removal 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 23. CAP injector liner-removal tool (P/N 0250-6534).
74
Clarus 400 GC Hardware Guide
Figure 24. Removing a capillary injector liner.
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 (P/N N612-1001)
•
2-mm i.d. and 6-mm o.d. CAP injector narrow-bore liner (P/N N612-1002)
75
Installing A Capillary Column
The narrow-bore liner is generally used for a splitless injection, and the wide-bore liner is
generally used for a split injection. Due to the small internal volume (0.3 mL) of the narrowbore 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 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 (P/N 6102354) 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 (P/N N610-T100), push the quartz wool (P/N 6102354) 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.
2
The recovery of high molecular weight components (e.g., C40) may be improved if the liner is loosely packed.
76
Clarus 400 GC Hardware Guide
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 (P/N N610-T100), push the quartz wool (P/N 6102354) 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 27). 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.
SPLITLESS PACKING
SPLIT PACKING
O-Rings
O-Ring
Glass Wool
Loosely
Packed
Glass Wool
Loosely
Packed
Glass Wool
Tightly Packed
Dimple
Dimple
Wide Bore Liner
(Part No. N610-1538)
Narrow Bore Liner
(Part No. N610-1744)
Wide Bore Liner
(Part No. N610-1538)
Figure 25. CAP injector liners packed with quartz wool.
Step 4. Reinstall the Liner in the CAP Injector.
To reinstall the liner:
1.
Install a new O-ring near the ground portion of the liner.
77
Installing A Capillary Column
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 (P/N N6101359).
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 (P/N 0990-3392) and 1/16-inch graphite ferrule (0.8
mm i.d., P/N 0992-0141 or 0.5 mm i.d., P/N 0990-3700) over one end of the column
as shown below:
1/16-inch Column Nut
(P/N 0990-3392)
White-Out
1/16-inch Graphite/Vespel Ferrule
(P/N 0990-3700)
Figure 26.
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.
78
Clarus 400 GC Hardware Guide
2.
Cut off about 1 cm (3/8 inch) from the column end using a wafer scribe (P/N N9301376, 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:
Good Cut
Bad Cuts
Figure 27. Example of a good cut and bad cuts.
3. Position the column not on the column so that the back of the nut is 4.4 cm to 5.1 (1 ¾
inches to 2 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 26).
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.
79
Installing A Capillary Column
Capilary
Injector
Fitting
Figure 28. Capillary injector fitting inside the oven.
6. 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.
7. Using two 1/4-inch wrenches, tighten the column nut only until the column cannot be
pulled out of the fitting.
CAUTION
80
Do not overtighten column nuts. Overtightening can cause
damage to the ferrule and/or column.
Clarus 400 GC Hardware Guide
Figure 29. Capillary column attached to capillary injector fitting.
81
Installing A Capillary Column
Step C: Set the Carrier Gas Using Manual
Pneumatics
This step describes how to set the carrier gas for manual pneumatics modules. Refer to the
procedure Setting the Carrier Gas Using Manual Pneumatics.
This step includes procedures to set the carrier gas pressure for the split/splitless (CAP).
Setting the Carrier Gas Pressure for the Split/Splitless Injector (CAP)
Carrier gases for the split/splitless injector (CAP) 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.
I
0
SPLIT FLOW
Pressure
Control
Knob
CARRIER PRESSURE
Figure 30.
CAP pneumatic controls.
To adjust the carrier gas pressure:
1. Turn on the carrier gas at the tank. Adjust the line pressure to 90 psig (or 620 kPa or 6.2
bar).
2. Press [Carrier Prog].If a capillary injector is in position 1, the Pressure Readout appear.
Pres 1
Set
82
¦
25.0
25.0 Psi
Clarus 400 GC Hardware Guide
If the capillary injector is in position 2, press [Carrier Prog] again.
Note:
The Pressure Readout display is factory configured to display the actual pressure as psig. To
display the actual pressure as kilopascals (kPa), refer to Clarus 400 GC Software Guide
(09936812), “Initial Setup Procedures” chapter.
3. Enter a pressure set point. (See Suggested Capillary Column Pressures below.)
4. Turn the pressure control knob until the readout on the top line equals the set point.
Suggested Capillary Column Pressures:
The following tables are manual pneumatics of the Clarus 400 GC.
Table 2. Calculated Pressure Drops (psig) for 10m Column3
Column I.D. (μm)
_
u4
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 3. Calculated Pressure Drops (psig) for 25m Columns4
3
4
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).
83
Installing A Capillary Column
Table 4. Calculated Pressure Drops (psig) for 50m Columns4
84
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
-
Clarus 400 GC Hardware Guide
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.
85
Installing A Capillary Column
Step E:
Condition the Column and the Mechanical
Joint Between the Pre-column 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.
To condition the column:
1. Close the oven door and press [Oven Prog].
The Oven Temperature screen appears.
Oven
NOT RDY
TEMP 1
¦
30°
75°
2. Enter an oven temperature set point of 50 ºC and press [Enter].
The Oven Time screen appears.
Oven
TIME 1
0.0m
¦ 999.9m
3. Enter a (Hold) TIME of 10 and press [Enter].
86
Clarus 400 GC Hardware Guide
The Oven Rate screen appears.
Oven
RATE 1
NOT RDY
¦
30°
End
4. To add another program step, enter a RATE of 5(ºC/min).
A screen similar to the following appears.
40°
¦ 50°
Oven
NOT RDY
TEMP 2
5. 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:
50°
¦ 200°
Oven
NOT RDY
TEMP 2
CAUTION
To avoid damaging the column, do not enter a
temperature higher than the maximum recommended
temperature specified by the column manufacturer.
6. Press [Enter].
The following screen appears:
Oven
TIME 2
0.0m
¦ 999.9m
7. Press [Enter].
The following screen appears:
Oven
RATE 2
NOT RDY
¦
End
8. Configure the injector for the oven mode. Refer to the Clarus 400 GC Software Guide
(09936812), Initial Setup Procedures chapter.
87
Installing A Capillary Column
9. Turn the Detector Temperature off.
10. Press [RUN]. Allow the system to run overnight.
11. In the morning, press [Reset Oven].
12. A menu similar to the following appears:
Reset to Oven Temp
¦ 1
2
13. Press [Enter].
14. This resets the oven temperature set point to that specified for TEMP 1 at the beginning of
the temperature program.
15. Open the oven door, then press [CE].
16. Allow the oven to cool until the oven fan turns off. This occurs when the oven cools down
to 40ºC.
88
Clarus 400 GC Hardware Guide
Step F:
Connect the Column to the Detector:
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:
1/8-inch Column Nut
(P/N 0990-3453)
White-Out
1/8-inch Graphite/Vespel Ferrule
(P/N 0990-3981)
Figure 31. Nut and ferrule on the detector end of a narrow-bore capillary column.
3.
Cut about 1 cm (3/8 inch) from the column end using a wafer scribe
(P/N 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:
Good Cut
Bad Cuts
Figure 32. Example of a good cut and bad cuts.
4.
Mark the column the following distances from the end using typewriter "white-out"
or a felt-tipped pen:
89
Installing A Capillary Column
Column
Diameter
≤0.53 mm i.d.
Detector to which you are
attaching the column
FID
Distance from back of
nut
2.75 inches (70 mm)
5
≤0.53 mm i.d.
ECD
≤0.53 mm i.d.
TCD
4 inches (103 mm)
≤0.53 mm i.d.
NPD
3 inches (77 mm)
CAUTION
2.5 inches (64 mm)
To avoid contaminating the system, make certain that the
nut and ferrule do not contact the mark on the column.
5. Locate the detector fitting protruding from the right side of the oven roof.
6. Insert the column into the detector fitting, keeping the mark just behind the column nut.
7. While holding the column in position, hand-tighten the column nut.
8. 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!
5
A glass-lined receiver (P/N N600-0968) is available to reduce high background readings.
For more details, see the Important on page 8-22.
90
Clarus 400 GC Hardware Guide
Detector
Fitting
Column
Nut
Figure 33.
Capillary column connected to the detector fitting.
CAUTION
CAUTION
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.
91
Installing A Capillary Column
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.
92
Clarus 400 GC Hardware Guide
Step H: Set up the Split Mode for a CAP 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 manual pneumatics modules. Refer to the
procedure that describes your Clarus 400 GC manual pneumatics control..
Step H: 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 Manual Pneumatics , Setting up the
Splitless Mode for a CAP, Setting the Splitless Mode Using Manual Pneumatics see the
Clarus 400 GC Software Guide (0993-6625) “Using the Active Method” chapter.
93
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 manual pneumatics version.
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
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.
94
Troubleshooting
6
This chapter contains the following sections:
•
Messages Requiring PerkinElmer Service Assistance
•
Background Calibration Error Messages
•
Miscellaneous Error Messages
•
Illegal Value Error Messages
•
GC Troubleshooting
Troubleshooting
Messages Requiring PerkinElmer Service Assistance
If any of the following messages appear, call your PerkinElmer Service Representative.
A/S control error
Elevator not init.
A/S control error
Tower not init.
A/S control error
Invalid vial
A/S control error
Slot not found
A/S control error
Invalid syringe size
A/S control error
Encoder read error
A/S control error
Encoder position err
A/S control error
Phase error
A/S control error
Bad injection
A/S control error
Bad sensor state
A/S control error
Bad motor mode
A/S control error
Bad motor speed
A/S control error
Carousel not init.
A/S control error
Bad slot
A/S control error
Vial sensor not init.
INSTRUMENT SHUTDOWN
xxxxxPRT ERROR
xxxxxERROR
PRT NOT FOUND
INSTRUMENT SHUTDOWN
xxxxxNO HEAT
INSTRUMENT SHUTDOWN
xxxxxTHERM. RUNAWAY
98
Clarus 400 GC Hardware Guide
Background Calibration Error Messages
NOTE: The following error messages appear before a calibration run starts.
Message
B/G CAL ERROR
Isothermal Method
B/G CAL ERROR
Negative ramp
B/G CAL ERROR
Run Time < 2.0 m
B/G CAL ERROR
Run Time > 999 m
B/G CAL ERROR
HOLD event in Run
B/G CAL ERROR
Oven reset
Cause
Action
You are attempting to perform
background calibration using
an isothermal method.
Background calibration cannot
be performed on an isothermal
method.
Your temperature program has
a negative ramp. You cannot
calibrate the background when
the oven temperature is
decreasing.
Use a temperature
program.
The run time is less than 2.0
minutes.
Increase the run time to
between 2.0 and 999
minutes.
The run time is greater than
999 minutes.
Decrease the run time to
between 2.0 and 999
minutes.
Your timed events table
contains a HOLD.
Review your timed events
table and delete any
HOLD events.
You probably pressed [Reset]
during a run.
Don't press [Reset].
Check your oven
temperature program
and remove any negative
ramps.
99
Troubleshooting
Miscellaneous Error Messages
Message
Cause
Action
Events table full
32 events maximum
You cannot enter more
than 32 events into a timed
events table.
Press [CE], then reduce
the number of events.
Duplicate event time
Enter another time
You entered an event time
that already exists. Two
events cannot occur
simultaneously.
Press [CE], either enter an
exclusive new time for this
event, or change the time
for the duplicate event.
OVEN CONTROL ERROR
No Coolant
The oven is trying to cool
but cannot. You probably
did not turn on the flow of
coolant.
Turn on the flow of
coolant.
A/S control error
Syringe error.
There is no syringe in the
autosampler or it is
incorrectly installed.
Reinstall syringe.
A/S control error
Vial sensor not init
Vial sensor is stuck in the
on position when tower is
not over a vial.
Check that the vial sensor
is moving freely. If the
error persists, call your
PE rep.
In single program mode, no
vials in tray. In
multiprogram mode vial
not found in the range
specified in the
autosampler program.
Put vials in tray.
A/S error
No vial
100
Clarus 400 GC Hardware Guide
In multiprogram mode, all
methods specified are Off.
Turn at least one method
on.
There are no injectors
configured.
Configure at least one
injector.
There are no detectors
configured.
Configure at least one
detector.
You are trying to redirect
the detector output with
only one detector
configured.
Make certain that both
detectors are configured.
TCD filaments exceeded
maximum temperature
Make certain that carrier
gas is flowing and that the
TCD and filament current
are within acceptable
limits.
A waste or wash vial has
been removed.
Replace vial.
Flow too high for
'lo' calibration
When calibrating the flow
readout, the measured rate
is too high for accurate
calibration.
Decrease the flow.
Flow too low
for 'hi' calibration
In calibrating the flow
readout, the measured rate
is too low for accurate
calibration.
Increase the flow.
A/S error
No programs active
NO INLET CONFIG
Press CE to continue
NO DETECTOR CONFIG
Press CE to continue
Can't select output
w/only one detector
Filament FIL OVR 100
Temperature
150
A/S
No
Error
w/w vial
101
Troubleshooting
Enter the correct code.
Incorrect keyboard
unlock code
Invalid Method #
x x x x x
Int. Error
Turn Power
102
XXXXXX
OFF/ON
You have entered an
invalid Method #.
Internal Software error.
Enter a valid Method #.
Clarus 400 GC Hardware Guide
Illegal Value Error Messages
The following error messages appear if you enter a value outside of the permissible range.
Each screen displays the permissible range for the specific parameter you are entering. To
correct the problem, press [CE], then enter a number within the displayed range.
Illegal Value
Range 1 - 82
Illegal Value
Range 1 - 15
Illegal Value
Range 0.0 - 0.5
Illegal Value
Range 0.0 - 5.0
Illegal Value
Range 1 - 3
Illegal Value
Range x - x
103
Troubleshooting
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.
CAUTION
If the display shows Sleep Mode do not activate this mode
since this function is only available in the PPC option. The
PPC option is not available on the Clarus 400 GC. If you
inadvertently select this option, reboot the Clarus 400 G.
Once the instrument is rebooted select the Config screen
and switch off the Sleep Mode so the Clarus 400 GC will
function properly
There are several sources of problems in gas chromatography:
104
•
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.
Clarus 400 GC Hardware Guide
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. (See page 116 for part numbers.)
•
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 (P/N N662-1028).
•
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.
1. Note the symptoms - define the problem. Compare your runs with good analyses, that is,
with the results normally obtained.
2. 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.
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.
105
Troubleshooting
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.
106
Clarus 400 GC Hardware Guide
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.
Table 3. READY and START Connections at TB1
Connection
Function
READY OUT
TB1-10 (C), 11 (NO), 12 (NC)
Instrument READY OUT Relay: These contacts are
used to tell an external device that the Clarus 400 GC
is ready. The normally open contact (NO) is closed
in the Ready state.
START OUT
TB1-7 (C), 8 (NO), 9 (NC)
Instrument START OUT Relay: These contacts are
used to start an external device when the Clarus 400
GC starts a chromatographic run. The normally open
contact is closed for 1 sec when a run is started.
EXT. READY
(TB1-5, 6)
TB1-6 is signal
External Ready In: The Clarus 400 GC requires that
these contacts be shorted together to become ready
and is shipped with a link across them. When using
an external device, such as an integrator, remove the
link and wire the device to provide a contact closure
indicating the Ready state. This will prevent the
instrument from becoming ready before the external
device is ready.
TB1-5 is ground
EXT. START
(TB1-3, 4)
TB1-4 is signal
External Start In: Shorting these contacts will cause
the Clarus 400 GC to start a chromatographic run. It
is equivalent to pressing the RUN key.
TB1-3 is ground
107
Troubleshooting
108
Clarus 400 GC Hardware Guide
Maintenance
7
109
This chapter contains procedures for:
•
Autosampler Maintenance — changing a syringe and replacing a vial-locator
mechanism.
•
Syringe Maintenance — cleaning the 5-μL and 50-μL syringe plungers and part
numbers for syringes.
•
Injector Maintenance — changing septa, changing and repacking packed-injector
liners, changing and repacking injector liners on the capillary (CAP) 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.
•
NPD Maintenance — changing and conditioning the NPD bead and replacing an
NPD jet.
•
TCD Maintenance
Maintenance
Autosampler Maintenance
Autosampler maintenance consists of changing a syringe and replacing a vial locator
mechanism.
Changing a Syringe
1. Press [Auto] [Auto].
A/S
¦ Park
STOPPED
Clean Print >
2. Select Park, then press [Enter].
The autosampler tower moves to the park position (facing the front of the Clarus
400 GC).
3. Open the tower door on the autosampler tower cover.
Tower Door
Autosampler
Tower Cover
Plunger
Assembly
Figure 34. Autosampler tower in the park position.
112
Clarus 400 GC Hardware Guide
Removing a Syringe
1. Locate the plunger assembly shown in Figure 34. Then, refer to Figure 35 as you lift up
the plunger cap handle and rotate it until it rests on the collar. Then release the plunger
cap handle.
Plunger Cap
Handle
Lift
Turn
Pin
Pin
Collar
Figure 35. 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.
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Maintenance
Tower Door
AutoSampler
Tower Cover
Plunger
Cap Slide
Plunger
Assembly
Syringe
Carriage
Assembly
Syringe
Nut
Carriage
Thumbscrew
Figure 36. Removing a syringe.
Installing a Syringe
Please refer to Figures 35 through 37 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 needle locator.
5. Tighten the carriage thumbscrew.
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Clarus 400 GC Hardware Guide
Tower Door
AutoSampler
Tower Cover
Plunger
Cap Slide
Plunger
Assembly
Carriage
Assembly
Syringe
Syringe
Nut
Carriage
Thumbscrew
Figure 37. Installing a syringe.
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 begins to plug, it is an
indication that you should replace the vial-locator 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 (P/N 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.
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Maintenance
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.
Figure 38. Exploded view of the vial locator.
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Clarus 400 GC Hardware Guide
Syringe Maintenance
Syringe maintenance consists of cleaning the 5-μL and 50-μL syringe plungers and servicing
idle syringes.
Syringe
Part Number
5-μL (0.63 mm O.D.) Teflon-tipped plunger (Std)
N610-1390
0.5- μ L (0.63 mm O.D.)
N610-1252
0.5- μ L (0.47 mm O.D.)
N610-1253
5- μ L (0.63 mm O.D.)
N610-1251
5- μ L (0.47 mm O.D.)
N610-1380
50- μ L (0.63 mm O.D.)
N610-1760
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 400 GC. Plungers
are not interchangeable from syringe to syringe.
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Maintenance
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 400’s precision degrading, replace the syringe. The autosampler
syringe is a consumable part. After extended use, you will need to replace it.
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Clarus 400 GC Hardware Guide
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 and repacking CAP liners, changing the charcoal trap or replacing charcoal on the
split/splitless CAP 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 (P/N 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.
NOTE: To minimize the possibility of contamination, avoid unnecessary handling of septa.
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Maintenance
Septum Cap
(P/N N610-0153)
Septum
(P/N N662-1028
Pack of 50 Each)
Shiny Surface
Down
Septum Cap
(P/N N610-0153)
Figure 39. 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 (P/N N610-2354) into the top portion of the injector liner (P/N 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.
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.
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Clarus 400 GC Hardware Guide
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 ºC) will make it difficult to remove the injector liner.
2. Remove the septum cap (see Figure 39).
3. Remove the septum shield (P/N N610-1050) with the large end of the liner-removal tool
(P/N N610-0102).
Figure 40. Liner-Removal Tool (P/N N610-0102).
4. Press the small end of the liner-removal tool into the injector liner, then pull the injector
liner out.
Packed Injector Liner
Figure 41. Removing the packed column injector liner.
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Maintenance
NOTE: To avoid contaminating the quartz wool when packing the injector liner, wear vinyl, powderfree, disposable gloves (for example, the same type of gloves used to perform maintenance on
the 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 (P/N 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.
Figure 42. Packed column injector liner (P/N N610-1048) packed with wool.
Changing and Repacking Capillary Split/Splitless (CAP)
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
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Clarus 400 GC Hardware Guide
Removing a CAP Liner
The liner-removal procedure is similar for CAP and PSS wide-bore and narrow-bore liners.
To remove the liners, you need a CAP liner-removal tool (P/N 0250-6534) as shown below.
Figure 43. CAP 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 (<100 ºC) will make it difficult to remove the injector
liner.
2. Remove the septum cap.
Septum Cap
(P/N N610-0153)
Figure 44. Removing the septum cap.
3. Remove the injector cover.
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Maintenance
Injector Cover
(P/N N610-1762)
Figure 45. Removing the injector cover.
4. Loosen the threaded collar using the spanner (P/N N610-1359) provided, then remove the
threaded collar.
Spanner
(P/N N610-1359)
Figure 46. Loosening the threaded collar.
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Clarus 400 GC Hardware Guide
5. Replace the septum cap on the injector.
6. Pull the septum cap upwards to remove the septum purge assembly.
7. 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. Insert the CAP liner-removal tool
(P/N 0250-6534) over the end of the CAP liner and lift the liner out of the injector
Septum Purge Snubber
Figure 47. Removing the septum purge assembly.
CAUTION
The liner must be cool (no hotter than 100 °C) or the linerremoval tool will melt! The end of the liner-removal tool
may flare out with use. If this happens, cut off the flared
end with a razor blade or scissors.
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Maintenance
PSS Liner-Removal Tool (P/N 0250-6247)
Figure 48. 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.
NOTE: Each capillary liner has an O-ring installed on the frosted portion of the CAP liner. 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. See the following page for O-ring part numbers.
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Clarus 400 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 in the following
table). 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 our web site www.perkinelmer.com or by calling in the
U.S. 1-800-762-4000, outside the US contact your local PerkinElmer Sales office. Viton
(maximum temperature of 250 ºC) is recommended for the mass spectrometer.
Injector O-Rings
Recommended Maximum Temperature
CAP Injector
N610-1374
Silicone (pkg .of 10)
250 ºC
N610-1378
Graphite (pkg. of 5)
450 ºC
N930-2782
Kalrez (pkg. of 1)
450 ºC
N930-2783
Viton (pkg. of 1)
250 ºC (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 (P/N N612-1001); 4.0-mm i.d. and 6.0-mm o.d.
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Maintenance
•
CAP narrow-bore liner (P/N N612-1002); 2.0-mm i.d. and 6.0-mm o.d.
The narrow-bore liner is generally used for a splitless injection, and the wide-bore liner is
generally used for a split injection. Due to the small internal volume (0.3 mL) of the narrowbore 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 (P/N N610-2345) 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 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 (P/N N610-T100), push the quartz wool
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Clarus 400 GC Hardware Guide
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.
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 (P/N 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.
SPLITLESS PACKING
SPLIT PACKING
O-Rings
O-Ring
Glass Wool
Loosely
Packed
Glass Wool
Loosely
Packed
Glass Wool
Tightly Packed
Dimple
Dimple
Wide Bore Liner
(Part No. N610-1538)
∗
Narrow Bore Liner
(Part No. N610-1744)
Wide Bore Liner
(Part No. N610-1538)
The recovery of high-molecular-weight components (e.g., C40 and higher) may be improved
if the liner is packed loosely.
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Maintenance
Figure 49. CAP injector liners packed with quartz wool.
NOTE: As you can see in the previous figure, 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.
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Clarus 400 GC Hardware Guide
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.
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 (P/N 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.
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 (P/N 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!
Changing the Charcoal Trap or Replacing Charcoal on the
Split/Splitless CAP Injectors
The charcoal trap will eventually become saturated. When this occurs, ghost peaks and
changes in split ratio will be observed.
* The recovery of high-molecular-weight components (e.g., C40 and higher)
may be improved if the liner is packed loosely.
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Maintenance
Removing a Charcoal Trap
1. Turn off the Clarus 400 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 400 GC (see the
following figure) and raise the top cover until the cover locks in the raised position.
Hold-Down Screws
Under Cover
Detector
Cover
Electronics
Cover
Autosampler
Tower
Hold-Down
Screw
Figure 50. Location of the top cover hold-down screws.
3. Remove the septum cap, then remove the top cover from the injector.
4. Loosen the threaded collar using the 1/4-inch spanner (P/N 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).
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Clarus 400 GC Hardware Guide
Installing a New Charcoal Trap
1. Install the manual pneumatics version charcoal trap (P/N N610-0275), or just replace the
charcoal in your current trap.
Manual Pneumatics (P/N 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, P/N 0330-0904). Plug the end of the charcoal filter
with a small piece of silanized glass wool. Reinstall the charcoal trap.
Figure 51. Charcoal Trap on an injector controlled by manual pneumatics
(right).
2. Replace the septum purge assembly and remove the septum cap.
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 400 GC top cover and tighten the two hold-down screws.
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Maintenance
CAUTION
To prevent autosampler needle damage after the Clarus 400
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 15-22).
Then move the top cover so that the vial locator is aligned with
the center of the septum cap. Secure the Clarus 400 GC top
cover in this position by tightening the two screws.
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Clarus 400 GC Hardware Guide
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
400 GC display by pressing [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. Remove the column from the ECD, then cap the ECD with a plug (P/N 0990-3098).
2. Increase the make-up flow.
If the background remains the same as the make-up flow increases, the carrier gas could
be contaminated. (The ECD is a concentration-sensitive detector. Increasing the makeup 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 (P/N 0990-3098).
2. Increase the flow of make-up gas to 60 – 100 mL/min and raise the detector temperature
to 450 ºC.
3. Bake the system until the background returns to normal levels. This could take 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.
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Maintenance
Changing the Charcoal Traps
The ECD is shipped with charcoal traps (P/N 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 400 GC and allow the injectors/detectors to cool.
2. Loosen the two hold-down screws on the Clarus 400 GC top cover (see Figure 50) 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:
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).
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Clarus 400 GC Hardware Guide
3. Place the anode in a beaker of hexane 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 to a
normal level..
Figure 52. Isometric view and cross section view of the ECD.
137
Maintenance
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 cool to the touch.
2. Gain access to the detector by lifting the detector cover (see the following figure).
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Clarus 400 GC Hardware Guide
Detector Cover
Figure 53. 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.)
DO NOT DISMANTLE THE ECD CELL!
WARNING
139
Maintenance
Detector Cap
Insulating Cover
Screw
Screw
Figure 54. ECD insulating cover.
Detector Outlet
Knurled Ring
Detector Fitting
(inside the oven)
140
Clarus 400 GC Hardware Guide
Figure 55. ECD surfaces to wipe.
4. Using the instructions included with the wipe-test kit (P/N 0009-1667) supplied with the
detector, wipe the external surfaces of the items shown in Figure 55 with the “low
Activity Source” filter papers:
•
•
•
Detector outlet
Knurled ring
Detector fitting
CAUTION
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 wipe-test solution to enter the cell.
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 (P/N
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.
141
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 400 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 by turning the outer knob on
the hydrogen needle valve completely clockwise.
WARNING
1. Turn off the Clarus 400 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 53).
3. Remove the polarizing cable from the pin on the polarizing filter assembly.
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Maintenance
Polarizing
Voltage Wire
Figure 56. 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 (P/N N610-3188) into the FID base and lift the nozzle out
of the FID base.
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Clarus 400 GC Hardware Guide
Nozzle Removal
Tool (P/N N610-3188)
Nozzle
FID Base
Figure 57. 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.
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Maintenance
FID Base
1/4-inch Nut
Jet Assembly
(P/N N610-0361)
(Shown removed)
Detector
Fitting
Figure 58. Cross section view of the FID.
8. Insert a new FID jet assembly (P/N 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 400 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.
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
WARNING
To replace the O-ring in the FID collector:
1. Remove the polarizing voltage wire from the polarizing pin (Figure 56).
2. Loosen the knurled ring, then lift the FID collector off of the FID base.
3. Remove the old O-ring (shown in Figure 59) from the FID collector and insert a new Oring (P/N 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.
6. Turn on the FID heater and allow it to return to the temperature setting.
7. Re-ignite the flame.
147
Maintenance
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.
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.
WARNING
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.
148
Clarus 400 GC Hardware Guide
O-Ring
(Part No. 0990-2143)
Knurled
Ring
Collector
Figure 59. View of the FID collector and O-ring.
149
Maintenance
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 that contains alkali metal ions (single
bead P/N N612-0092 or package of five P/N N612-0093) to detect organically bound
nitrogen and phosphorus compounds. Examine the NPD and make sure it does not
have any broken weld or wires. Operation of the bead in an NPD detector leads to
gradual loss of the alkali metal ions, and in time, the bead will not respond and need to be
replaced. 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 (in 0.25 mV increments).
If you cannot achieve a response at higher settings up to 2mV, then you should recondition
the BEAD and be certain that all your gas flows are accurate. Make certain that hydrogen
flow is within +/- 10% of 2 ml/minute flow rate and that you precisely followed the
conditioning procedure instructions.
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 compartment cover (see Figure 53).
2. Locate the bead potentiometer.
3. 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.
4. 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.
5. Press the Oven key and check that the GC oven temperature is set to 50 ºC or below
150
Clarus 400 GC Hardware Guide
6. Open the oven door and check to see if a column is attached to the NPD detector on
which the bead is to be changed.
7. If a column is attached the NPD detector in question, remove it from the detector with an
open-end wrench (7/16 inch wrench for 1/8 inch stainless steel tube nut). Use a second
7/16 inch open-end wrench on the NPD detector base (to avoid applying torque on the
detector body brazed fitting). Allow the detector end of the capillary column and column
nut to rest on the base of the floor of the oven.
8. Attach a 1/8 inch stainless steel Cap Nut (N930-0061) to the NPD detector in place of
the 1/8 inch stainless steel tube nut. This step is in preparation for conditioning the new
bead, to make sure the specified flows of detector gases pass upwards across a bead to
be conditioned.
151
Maintenance
1/8 inch
Stainless Steel
Cap Nut
N930-0091
9. Check the Detector temperatures by pressing the Detector Temp Key
10. If the detector temperature of any detector installed is over 100 ºC, set the detector
temperature to OFF or the minimum allowed value.
11. When detector temperatures show residual temperature values below 100 ºC, turn off the
Clarus 400 GC and unplug the line cord from the line voltage for general safety.
The gases can remain on during this procedure, but the detector
should be cool to the touch to protect you from getting burned.
WARNING
12. Remove the NPD collector assembly (see Figure 60) by loosening its knurled ring and
lifting the collector assembly upward.
152
Clarus 400 GC Hardware Guide
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).
13. Remove the screw that secures the bead transformer assembly to the top of the Clarus
400 GC oven.
14. Carefully remove the bead portion from the detector body by lifting the bead transformer
assembly straight up and out of the detector body.
15. Remove the bead assembly from the transformer assembly by unplugging it from the
connector (see Figure 60).
16. Plug a new bead assembly (P/N N612-0092) into the connector on the bead transformer.
The connector is keyed so that the bead assembly can only be inserted one way.
17. Carefully insert the bead portion of the bead assembly in the detector body as shown in
Figure 60.
18. Secure the bead transformer to the top of the oven with the screw removed in step 6 of
this procedure.
19. 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.
NOTE: Check that the polarizing wire has not fallen off the detector. If it has, replace it (Figure 62).
20. Reinsert the line cord in the wall socket and switch on the Clarus 400 GC.
153
Maintenance
Bead Transformer
Mounting Screw
Collector Assembly
Knurled
Ring
NPD Bead Assembly
(Single bead P/N N612-0092)
(Package of 5 beads P/N N612-0093)
Bead
Transformer
Assembly
Connector
Bead Portion
Bead Assembly
Polarizing Wire
Polarizing Clip
Detector Body
Figure 60. Exploded view of the NPD bead assembly.
154
Clarus 400 GC Hardware Guide
Conditioning a New NPD Bead
NPD bead sensitivity and service lifetime are greatly influenced by factors external to the
bead. Critical factors that contribute to obtaining optimal sensitivity, stable performance, and
long lifetime are the following:
¾
¾
¾
¾
¾
Strict adherence to recommended conditioning procedure
Accurate control of hydrogen gas flow
Protection from exposure to chlorinated solvents
Minimized exposure to methanol, ethanol, water
Proper setting of baseline current
For more tips on extending the life of your NPD bead please see the following section,
Maximizing the NPD Bead Life.
We have found that 99% of bead sensitivity problems are the result of the failure to maintain
proper external conditions. A properly conditioned NPD bead should have normal acceptable
sensitivity with a baseline setting in the range of 0.5 to 1.0 millivolts. Optimally, the bead
should be conditioned with the detector capped and all carrier flows removed during the
conditioning process for best results
NOTE: Do NOT try to operate the bead at any current level prior to initial conditioning by the steps
of the procedure given below. Similarly, do NOT set the bead current to give 0.5 to 1.0 mV
baseline using the bead current potentiometer for any length of time prior to formal
conditioning, and do NOT try to stabilize the bead or bake it out overnight as if it were
another type of detector (e.g. ECD prior to conditioning it.)
PerkinElmer recommends conditioning the beads exactly as instructed in the following steps
in order to obtain optimum performance and longest serviceable life of the beads.
155
Maintenance
Conditioning the Bead:
1. Check that the column has been removed from the detector, and that a CAP fitting (P/N
N930-0061) has been threaded securely onto the oven end of the NPD detector.
NOTE: Bead conditioning is preferably done without exposing the bead to helium or other carrier
gas.
2. Check that the bead current potentiometer (see Figure 61) is turned all the way down by
rotating the knob in a counterclockwise direction (zero current).
3. Now install the bead.
Figure 61. Detector Compartment and location of Bead Current Potentiometer.
156
Clarus 400 GC Hardware Guide
4. Adjust flow of detector air to 100 ml / min
5. Adjust flow of detector Hydrogen to 2 ml / min.
6.
Let the flows stabilize.
NOTE: The Hydrogen line specifically must be allowed to flow sufficiently to purge any air that
intruded by diffusion during any period of stopped flow. Required purge time will depend on
length and volume of H2 gas line between the tank and the GC.
7. Verify flows to be accurate and consistent with the specified values. Adjust as needed
to produce the correct flows.
NOTE: Verification of H2 flow is especially important since the value is relatively low and a small
error can lead to a large change in detector response. To measure the NPD detector air and
hydrogen flows accurately, use a flow meter connected directly to the gas
supply lines. This will require disconnecting the detector gas input fittings from the
bulkhead and placing the flow meter directly on the stainless steel tubing of the Hydrogen
and Air lines. See the following figure.
157
Maintenance
Figure 62. Identification of NPD Detector Gas Bulkhead Fittings.
8. Reconnect the detector gas fittings to the bulkhead connector after verifying the NPD
detector gas flows. Take care that the hydrogen line (red tape) is connected to the
hydrogen bulkhead fitting and the air line is connected to the air bulkhead fitting. Do
not all these gas connections to be reversed. Check that the air supply line goes to the
detector air inlet and the hydrogen line goes to the detector hydrogen inlet.
9. Set the detector temperature to 250 ºC and allow the temperature to rise to the set point
ant then stabilize for about 10 minutes.
10. Turn the bead current potentiometer up slowly (especially above a 600 setting on the
bead current potentiometer dial) and observe the millivolts value on the display.
Above 600, turn the potentiometer dial up 10 units and wait 30 seconds. This is to
allow for the initial activation of bead activity which has some induction time. Observe
158
Clarus 400 GC Hardware Guide
the detector millivolt response on the display. You will observe that at the critical
point the detector response will rise rapidly as bead activity is initiated. An excessive
potentiometer setting is not helpful. When the bead response begins to be observed on
the display, slowly adjust the potentiometer until the response rises to just reach the
“stable rail”, the maximum level of 996.61 mV.
NOTE: The term “a stable rail” means attaining conditions such that the limiting maximum signal
value does not decrease to a lower value for 30 seconds. The objective of the next step is to
find the minimum potentiometer setting that produces a detector output at the 997.61 mV rail
value that remains constant for at least 30 seconds.
11. After it appears a stable rail of 997.61 mV has been achieved, stop increasing the
potentiometer setting and check to see that the 997.61 mV reading does not
immediately begin drop. If it does drop, gradually increase the potentiometer until it is
observed that the 997.61 mV value is stable and does not immediately begin to drop
with a static potentiometer setting. The 997.61 mV response level should be
maintained for the first 15 to 20 minutes after which the level may be allowed to drift
downward
12. Leave the bead at this high potentiometer setting for one hour only.
13. After 1 hour adjust the current potentiometer down to achieve a baseline of 0.5 to 0.75
mV.
14. Allow the detector to stabilize for 30 minutes at the 0.5 to 0.75 mV setting. Some
drifting up may occur.
15. After 30 minutes stabilization time, adjust the current potentiometer to produce a
baseline of around 0.75 mV and the bead will be ready for operation.
16. Take note of this setting on the potentiometer dial for future use.
17. Turn down the potentiometer setting counterclockwise to zero and set the detector
temperature to OFF. This is a preparatory move for the next step
159
Maintenance
WARNING
There is no benefit in leaving the bead at the high setting
(997.61) any longer than one hour. Leaving it at the high pot
setting overnight or for extended periods will tend to degrade
life and sensitivity of the bead.
NOTE: The typical known failure mode for NPD beads are broken wires or defects in welds. If
intermittent contact of the wires to the bead is suspected, then examine any questionable NPD
very carefully for physical defects with a magnifying glass for a crack in a weld of the bead to
a contact post.
NOTE: Halogenated solvents MUST NOT be used with an NPD detector. The life and
performance of the alkali bead will be severely impaired by contact with chlorinated
compounds. Avoid using stationary phases containing these compounds whenever possible.
Although sample solutions based on hydroxylic solvents can be analyzed, solvents such as
water, methanol and ethanol will reduce bead performance and life, and they should be
avoided whenever possible.
1. REMOVE the 1/8 inch stainless Steel CAP fitting (from step 2) mounted on the GC oven
side of the NPD detector. Caution: this part may be hot to the touch.
160
Clarus 400 GC Hardware Guide
Now Remove
Detector Cap Nut
2. Reconnect the GC column to the NPD detector as shown below.
3. Insert the capillary column into the NPD detector (77 mm from the back of the 1/8 inch
stainless steel nut).
4. Set up the exit end of the column for an insertion depth in the NPD of 77 mm, measured
from the back of the 1/8 inch stainless-steel nut.
NOTE: A spare injector septum inserted on column first (behind the 1/8 inch stainless steel nut)
helps stabilize installation at desired depth.
161
Maintenance
5. Set the detector temperature to 250 oC (as in step 11) and allow the temperature to stabilize
for about 10 minutes.
6. Check that the injector temperature is suitable for operation with the type of sample to be
analyzed/
7. Set up the desired method on the GC or in TotalChrom if using software control of the GC.
CAUTION
162
Detector gases must be on before proceeding. Recheck
hydrogen, air and carrier flows for correct values.
Clarus 400 GC Hardware Guide
8. Make a final adjustment of the potentiometer dial for the Bead voltage to the same dial
setting as noted in step 7on page 17 as an estimated adjustment. Now do a fine adjustment
to achieve a stable baseline of 0.75mV.
9. Allow the NPD detector to stabilize with the final baseline conditions 2 to 5 minutes.
Maximizing the NPD Bead Life
NPD bead life, optimal performance and sensitivity are greatly influenced by the following
external factors: proper conditioning, accurate hydrogen gas flow, purity of gases used,
solvents used, and baseline current settings.
In addition exposure to water or the use of methanol, ethanol and/or halogenated compounds
can degrade the life and performance of the bead.
The following bullets highlight how you can extend the NPD bead life.
¾ Use the lowest practical baseline current setting to achieve your desired sensitivity (.5
to .75 is typical).
¾ Make certain that your H2 flow is accurate with a calibrated H2 meter at the
bulkhead H2 line of the NPD detector. The actual flow must not vary more then +/0.2 mL/min then the 2.0 mL/min setpoint when measured at the detector bulkhead.
¾ Make certain the precise conditioning procedure outlined by PerkinElmer is adhered
to.
¾ Turn off the bead when not in use by lowering the potentiometer current.
¾ Run clean samples and keep the inlet/liner clean to minimize contamination.
¾ Keep the detector temperature high >150 º C to reduce moisture and other
contaminants.
¾ If the NPD is off for an extended period of time in a high humidity environment,
water may accumulate in the detector. To evaporate this water, set the detector
temperature to 150°C and maintain it for at least 30 minutes prior to operation.
¾ NPD beads will need reconditioning depending on the length of time not in use and
the ambient environment they are stored in.
¾ Column bleed from lower grade columns or columns being run near the
top of their temperature range can reduce bead life.
163
Maintenance
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 400 GC.
3. Turn off the hydrogen and air flows.
4. Open the detector cover (see Figure 53).
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
(Figure 63).
164
Clarus 400 GC Hardware Guide
Collector
Assembly
Knurled Ring
NPD Bead
Assembly
(Single bead P/N N612-0093)
(package of five beads P/N N61200093)
Chimney
NPD Jet
Assembly
(P/N N610-0038)
Figure 63. Location of the NPD jet assembly.
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 Figure 60).
6. Remove the screw that secures the bead transformer assembly to the top of the Clarus
400 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 60).
165
Maintenance
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).
Figure 64. Removing the NPD nozzle assembly and polarizing wire.
166
Clarus 400 GC Hardware Guide
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 spring-loaded pin.
10. With your right hand, insert the large end of the liner removal tool (P/N N610-0102) into
the NPD chimney so that it engages the nozzle assembly. Then remove the nozzle
assembly by lifting it out.
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 (P/N N610-1297 provided in shipping kit) into the NPD
chimney (see Figure 60) 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 (P/N N610-0038) by reversing steps 5 through 13.
167
Maintenance
TCD Maintenance
The TCD requires no specific maintenance.
CAUTION
168
The filament of the TCD will by damaged if current is applied
without the gas flow on.
Clarus 400 GC Hardware Guide
Practical Hints
8
169
Clarus 400 GC Hardware Guide
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.
171
Practical Hints
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.
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.
172
Clarus 400 GC Hardware Guide
Filtering Detector Output
You can select one of three software filters from the Filter Menu. To display a Filter Menu,
press [System] [Enter] [Atten]. A menu similar to the following appears:
FID 1 Filter
50 ¦ 200 800
Config
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.
173
Practical Hints
Autozero Display Sensitivity
The maximum detector signals for various detectors that produce a 1-V reading on the
Autozero Display are as follows:
FID or NPD (nA, Range 1) – 21.3
FID or NPD (nA, Range 20) – 426
TCD (mV) – 510
ECD (KHz) – 150
174
Clarus 400 GC Hardware Guide
Attenuation vs. Detector Output
The following table lists attenuation vs. the maximum detector signal producing 100%
deflection on a 1-mV recorder.
NPD and FID
(fA) Range 1
Atten
NPD and FID
(fA) Range 20
3.3x102
6.7x102
6.7x103
1.3x104
1.3x103
2.7x103
2.7x104
5.3x104
5.3x103
1.1x104
1.1x105
2.1x105
2.1x104
4.3x104
4.3x105
8.5x105
8.5x104
1.7x105
1.7x106
3.4x106
3.4x105
6.8x105
6.8x106
1.4x107
1.4x106
2.7x106
2.7x107
5.5x107
32768
5.4x106
1.1x107
1.1x108
2.2x108
65536
2.2x107
4.4x108
1
2
4
8
16
32
64
128
256
512
1024
2048
4096
8192
16384
TCD (μV)
ECD (Hz)
8.0
2.3
1.6x10
4.7
3.2x10
9.4
6.4x10
1.3x102
19.0
2.6x102
5.1x102
38.0
75.0
1x103
2x103
150.0
3.0x102
6.0x102
4.1x103
8.2x103
1.2x103
2.4x103
1.6x104
3.3x104
4.8x103
9.6x103
6.6x104
1.3x105
1.9x104
3.8x104
2.6x105
5.2x105
7.7x104
1.5x105
The following table lists attenuation vs. the maximum detector signal producing a 1-V output
to an integrator.
Atten
NPD and FID
(pA)
Range 1
NPD and FID
(pA)
Range 20
3.3x102
6.7x102
6.7x103
1.3x104
1.3x103
2.7x103
2.7x104
5.3x104
32
5.3x103
1.1x104
1.1x105
2.1x105
64
2.1x104
4.3x105
1
2
4
8
16
TCD (mV)
ECD (kHz)
8.0
2.3
1.6x10
4.7
3.2x10
9.4
6.4x10
1.3x102
19.0
2.6x102
5.1x102
38.0
75.0
150.0
175
Practical Hints
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.
CAUTION
176
To minimize detector contamination, run the ECD hot, at a
temperature of at least 375 °C.
Appendix
U.S.
Nuclear Regulations
NOTE: All USNRC regulations can be obtained through the internet at www.nrc.gov/reading-rm/
Clarus 400 GC Hardware Guide
Appendix - 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
179
Appendix
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
180
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 400 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]
181
Appendix
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
182
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 400 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]
183
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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
185
Appendix
U.S.
Nuclear Regulations
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)-816-5100.
(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 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.
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(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)(vii),
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 20186, Apr. 25,
1995; 66 FR 64738, Dec. 14, 2001; 67 FR 3585, Jan. 25, 2002]
§ 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) A lens 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) A lens dose equivalent exceeding 15 rems (0.15 Sv); or
(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 paragraphs (a) and (b) of this section by
telephone to the NRC Operations Center (301) 816-5100.
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U.S.
Nuclear Regulations
(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; 63 FR 39483, July 23, 1998]
§ 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
(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
overexposed1 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 and must be
clearly labeled "Privacy Act Information: Not for Public Disclosure."
(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 either by mail addressed to
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Clarus 400 GC Hardware Guide
the U.S. Nuclear Regulatory Commission, ATTN: Document Control Desk, Washington, DC 205550001; by hand delivery to the NRC's offices at 11555 Rockville Pike, Rockville, Maryland; or, where
practicable, by electronic submission, for example, Electronic Information Exchange, or CD-ROM.
Electronic submissions must be made in a manner that enables the NRC to receive, read, authenticate,
distribute, and archive the submission, and process and retrieve it a single page at a time. Detailed
guidance on making electronic submissions can be obtained by visiting the NRC's Web site at
http://www.nrc.gov/site-help/e-submittals.html, by calling (301) 415-0439, by e-mail to [email protected],
or by writing the Office of Information Services, U.S. Nuclear Regulatory Commission, Washington,
DC 20555-0001. A copy should be sent to the appropriate NRC Regional Office listed in appendix D
to this part.
[56 FR 23406, May 21, 1991, as amended at 60 FR 20186, Apr. 25, 1995; 61 FR 65127, Dec. 10,
1996; 68 FR 14309, Mar. 25, 2003; 68 FR 58802, Oct. 10, 2003; 70 FR 69421, Nov. 16, 2005; 72 FR
33386, Jun. 18, 2007]
1
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.
[56 FR 23406, May 21, 1991, as amended at 60 FR 20186, 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
189
Appendix
U.S.
Nuclear Regulations
(4) Possess high-level radioactive waste at a geologic repository operations area pursuant to part 60 or
63 of this chapter; or
(5) Possess spent fuel in an independent spent fuel storage installation (ISFSI) pursuant to part 72 of
this chapter; or
(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
Quantity of radionuclide1 in curies
Cesium-137
1
Cobalt-60
1
Gold-198
100
Iodine-131
1
Iridium-192
10
Krypton-85
1,000
Promethium-147
Techetium-99m
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 by an
appropriate method listed in § 20.1007 or via the REIRS Web site at http://www.reirs.com.
[56 FR 23406, May 21, 1991, as amended at 56 FR 32072, July 15, 1991; 66 FR 5578, Nov. 2, 2001;
68 FR 58802, Oct. 10, 2003]
§ 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 securing full information, find that the transfer is in
accordance with the provisions of the Act and shall give its consent in writing.
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Clarus 400 GC Hardware Guide
(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 molybdenum-99/technetium99m 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 § 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
(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.
(i) Security requirements for portable gauges.
Each portable gauge licensee shall use a minimum of two independent physical controls that form
tangible barriers to secure portable gauges from unauthorized removal, whenever portable gauges are
not under the control and constant surveillance of the licensee.
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Nuclear Regulations
[30 FR 8185, June 26, 1965, as amended at 38 FR 33969, Dec. 10, 1973; 43 FR 6922, Feb. 17, 1978;
48 FR 32328, July 15, 1983; 52 FR 1295, Jan. 12, 1987; 52 FR 8241, Mar. 17, 1987; 53 FR 19245,
May 27, 1988; 53 FR 23383, June 22, 1988; 54 FR 14061, Apr. 7, 1989; 58 FR 7736, Feb. 9, 1993; 59
FR 61780, Dec. 2, 1994; 65 FR 79187, Dec. 18, 2000; 70 FR 2009, Jan. 12, 2005]
§ 30.35 Financial assurance and record keeping for decommissioning.
(a)(1) 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.
(2) Each holder of, or applicant for, any specific license authorizing the possession and use of sealed
sources or plated foils of half-life greater than 120 days and in quantities exceeding 1012 times the
applicable quantities set forth in appendix B to part 30 (or when a combination of isotopes is involved
if R, as defined in § 30.35(a)(1), divided by 1012 is greater than 1), shall submit a decommissioning
funding plan as described in paragraph (e) of this section. The decommissioning funding plan must be
submitted to NRC by December 2, 2005.
(b) Each applicant for a specific license authorizing possession and use of byproduct material of halflife 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 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
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$1,125,000 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.
(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.
(5) Waste collectors and waste processors, as defined in 10 CFR part 20, Appendix G, must provide
financial assurance in an amount based on a decommissioning funding plan as described in paragraph
(e) of this section. The decommissioning funding plan must include the cost of disposal of the
maximum amount (curies) of radioactive material permitted by license, and the cost of disposal of the
maximum quantity, by volume, of radioactive material which could be present at the licensee's facility
at any time, in addition to the cost to remediate the licensee's site to meet the license termination
criteria of 10 CFR part 20. The decommissioning funding plan must be submitted by December 2,
2005.
(d) Table of required amounts of financial assurance for decommissioning by quantity of material.
Licensees required to submit the $1,125,000 amount must do so by December 2, 2004. Licensees
required to submit the $113,000 or $225,000 amount must do so by June 2, 2005. Licensees having
possession limits exceeding the upper bounds of this table must base financial assurance on a
decommissioning funding plan.
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)(1), divided by 104 is greater than 1 but R divided by 105 is less than or equal to
$1,125,000
1.)
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)(1), divided by 103 is greater than 1 but R divided by 104 is less than or equal to
1.)
10
225,000
12
Greater than 10 but less than or equal to 10 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)(1), divided by 1010 is greater than, 1, but R divided by 1012 is less
than or equal to 1)
113,000
(e) Each decommissioning funding plan must contain a cost estsimate 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
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the facility. Cost estimates must be adjusted at intervals not to exceed 3 years. 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 requriements 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 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.
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(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.
(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:
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(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; 63 FR 29541, June 1, 1998;
68 FR 57335, Oct. 3, 2003]
§ 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.
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(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
(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.
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(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
(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:
(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 NRC using an appropriate method listed in § 30.6(a); and a copy must be sent to the appropriate
NRC Regional office listed in appendix D to part 20 of this chapter. 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; 68 FR 58804, Oct. 10,
2003]
1
The commercial telephone number for the NRC Operations Center is (301) 816-5100.
§
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30.51 Records.
(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 halflife 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).
(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:
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(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]
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.
§ 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]
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§ 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 of the NRC's Office of
Nuclear Material Safety and Safeguards, using an appropriate method listed in § 30.6(a). 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; 68 FR 58804, Oct. 10, 2003]
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 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]
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§ 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 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]
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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
Er 169
Er 171
Eu 152
(T/2=9.2 Hrs)
Eu 155
F 18
Gd 153
Gd 159
Ga 72
Ge 71
Au 196
Au 198
Au 199
Hf 181
H 3.
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)
Erbium (68)
Europium (63)
Fluorine (9)
Gadolinium (64)
Gallium (31)
Germanium (32)
Gold (79)
Hafnium (72)
Hydrogen (1)
Col. I
Gas concentration
μCi/ml {1}
1x10-3
4x10-7
4x10_-7
1x10_-6
9x10_-7
2x10_-6
5x10_-6
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
9x10_-4
1x10_-3
6x10_-4
2x10_-3
8x10_-3
2x10_-3
8x10_-4
4x10_-4
2x10_-2
2x10_-3
5x10_-4
2x10_-3
7x10_-4
3x10_-2
203
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Nuclear Regulations
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)
Potassium (19)
Praseodymium (59)
Promethium (61)
Rhenium (75)
Rhodium (45)
Rubidium (37)
Ruthenium (44)
204
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
Pt 193m
Pt 197m
Pt 197
K 42
Pr 142
Pr 143
Pm 147
Pm 149
Re 183
Re 186
Re 188
Rh 103m
Rh 105
Rb 86
Ru 97
Ru 103
3x10_-9
3x10_-9
8x10_-8
1x10_-8
2x10_-7
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
1x10_-2
1x10_-2
1x10_-3
3x10_-3
3x10_-4
5x10_-4
2x10_-3
4x10_-4
6x10_-3
9x10_-4
6x10_-4
1x10_-1
1x10_-3
7x10_-4
4x10_-4
8x10_-4
Clarus 400 GC Hardware Guide
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)
Vanadium (23)
Xenon (54)
Ytterbium (70)
Yttrium (39)
Zinc (30)
Zirconium (40)
Beta and/or gamma emitting
byproduct material not listed
above with half-life less than 3
years.
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
V 48
Xe 131m
Xe 133
Xe 135
Yb 175
Y 90
Y 91m
Y 91
Y 92
Y 93
Zn 65
Zn 69m
Zn 69
Zr 95
Zr 97
9x10_-8
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
3x10_-4
4x10_-6
3x10_-6
1x10_-6
1x10_-10
1x10_-3
2x10_-4
3x10_-2
3x10_-4
6x10_-4
3x10_-4
1x10_-3
7x10_-4
2x10_-2
6x10_-4
2x10_-4
1x10_-6
205
Appendix
U.S.
Nuclear Regulations
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
[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 § 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.
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Clarus 400 GC Hardware Guide
(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 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 on-off 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
207
Appendix
U.S.
Nuclear Regulations
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, within 30 days after the transfer of a device to a specific licensee or export, furnish a report
to the Director of Nuclear Material Safety and Safeguards, ATTN: Document Control Desk/ GLTS,
using an appropriate method listed in § 30.6(a) of this chapter. 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 §§ 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: Document Control
Desk/GLTS, using an appropriate method listed in § 30.6(a) of this chapter-(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 providing the Director of the Office of Nuclear Material Safety and Safeguards, by an
appropriate method listed in § 30.6(a) of this chapter, a written justification for the request.
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Clarus 400 GC Hardware Guide
(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.
(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 § 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 storage only. However, when devices are put
209
Appendix
U.S.
Nuclear Regulations
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.
[39 FR 43532, Dec. 16, 1974, as amended at 40 FR 8785, Mar. 3, 1975; 40 FR 14085, Mar. 28, 1975;
42 FR 25721, May 19, 1977; 42 FR 28896, June 6, 1977; 43 FR 6922, Feb. 17, 1978; 53 FR 19246,
May 27, 1988; 56 FR 23471, May 21, 1991; 56 FR 61352, Dec. 3, 1991; 58 FR 67659, Dec. 22, 1993;
64 FR 42275, Aug. 4, 1999; 65 FR 79188, Dec. 18, 2000; 68 FR 58804, Oct. 10, 2003]
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.
210
Index
A
Abbreviations, screen, 9
About
O-rings, 127
the keyboard, 22
Attenuation vs. detector output, 175
Autosampler
Function key, 26
plunger assembly, 113
replacing
syringe, 112
vial locator,, 115
syringe, installing, 114
AutoSystem
glossary, 12
B
Bead, NPD, changing, 150
C
CAP, abbreviation, 9
Capillary column
attaching to detector, 89
calculating a capillary column split ratio, 94
condition the column, 86
connect the column to the detector, 89
connect the column to the injector, 68
installing
materials required, 65
overview, 68
summary, 64
tools required, 65
leak test, 85, 92
set up for split mode, 93
turn the heaters off, 67
Capillary column pressures, 83
Capillary column pressures, suggested values, 83
Capillary injector
fitting, 79
Index
liner packing, 76
Carrier gas flow
setting
using flow readout, 52
using soap bubble flowmeter, 53
Carrier gas pressure
setting, 82
Changing
charcoal trap, 132
septa, 119
Charcoal trap, changing, 132
Chromatographic terms, glossary, 13
Clean vs. bad cuts, 79
Cleaning the syringe, 117
Cmptr, abbreviation, 9
Column
before installing, 35
protecting, 38
Column hangers, installing, 36
Control key
Delete, 28
Run, 27
Control Key
Reset Oven, 57
Conventions, 9
Ctrl, abbreviation, 9
D
Delete control key, 28
Detector
output vs. attenuation, 175
Detector heater
turning off, 42
Detector Heater Screen, 42
E
ECD
abbreviation, 9
maintenance, 135
wipe testing, 138
ECD insulating cover, 140
Entry keys, 29
Off/No, 29
On/Yes, 29
Equil, abbreviation, 9
Error messages
background calibration, 99
illegal value, 103
212
requiring service assistance, 98
Extrn, abbreviation, 9
F
FID
abbreviation, 9
cross section view, 147
jet cleaning, 147
jet replacing, 143
performance, optimizing, 172
Fitting
capillary injector, 79
packed column injector, 53
Flow readout
using, 52
Function key
auto(sampler), 26
Method, 25
System, 25
Function keys
description of, 24
G
Gen, abbreviation, 9
Ghost Peaks, 14
Glossary
autosampler terms, 11
AutoSystem specific, 12
chromatographic terms, 13
GSV, abbreviation, 9
H
Hangers, column, 36
I
Inj, abbreviation, 9
Inj/vial, abbreviation, 9
Injector fittings, 36
Injector heater
turning on, 40
Installing
capillary column
materials required, 65
overview, 68
summary, 64
tools required, 65
2
Clarus 400 GC Hardware Guide
Int, abbreviation, 10
J
Jet assembly
FID, replacing, 143, 147
NPD, replacing, 164
K
Key
Autosampler function, 26
Method function, 25
parameter, 31
System function, 25
Keyboard
about the, 22
kPa, abbreviation, 10
L
Leak test
manual pneumatics
packed column detector fittinng, 59
packed column
injector fitting, 56
Liner removal tool, 121
M
Maintenance, 111
Menu
auto(sampler), 26
System Control, 25
Method function key, 25
N
NPD
changing a bead, 150
cross section view, 164
NPD, abbreviation, 10
O
Off/No entry key, 29
On/Yes entry key, 29
OnCol, abbreviation, 10
Optimizing FID performance, 172
O-rings
about, 127
Oven
Max Temp Limit Screen, 38
turning heater off, 39
turning heater on, 39
Overview
AutoSystem XL GC, 19
installing a capillary column, 68
Ovn, abbreviation, 10
P
Packed column
attaching
to detector, 58
to packed injector, 55
Packed column injector
fitting, 53
Packed column injector liner
changing, 120
repacking, 120
Packed injector
liner removal tool, 121
removing the liner, 121
Packed injector liner
removing, 121
Parameter keys, 31
Paus, abbreviation, 10
Pkd, abbreviation, 10
Practical hints, 171
Pre, abbreviation, 10
Pres, abbreviation, 10
Pressure Programming, 14
Prg, abbreviation, 10
Pri, abbreviation, 10
Protecting columns, 38
Psi, abbreviation, 10
psig, abbreviation, 10
R
Repacking
packed column injector liners, 120
Reset Oven control key, 57
Resm, abbreviation, 10
Reversing TCD polarity, 171
213
Index
Run control key, 27
S
Screen
abbreviations, 9
detector heater, 42
Oven Max Temp, 38
Septa, changing, 119
Set entry key, 29
Setting up
split mode, 93
Soap bubble flowmeter
using, 53
Spare components, 105
Split liner, 77, 129
Split mode
setting up, 93
Splitless liner, 77, 129
Stopwatch
resetting, 45
starting, 44
stopping, 45
using, 44
Stpwtch, abbreviation, 10
214
Syringe
cleaning, 117
servicing an idle, 118
System Control Menu, 25
System function key, 25
T
TCD
abbreviation, 10
TCD polarity, reversing, 171
Temperature Programming, 15
Top cover hold down screws, 132
Troubleshooting, 97
dual identical channels, 107
spare components, 105
W
Wipe test
See Wipe testing ECD, 138
Wipe testing
ECD, 138
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