2424 Evaporative Light Scattering Detector Operator`s Guide

2424 Evaporative Light Scattering Detector Operator`s Guide
2424 Evaporative Light
Scattering Detector
Operator’s Guide
71500121802/Revision B
Copyright © Waters Corporation 2006−2009
All rights reserved
Copyright notice
© 2006−2009 WATERS CORPORATION. PRINTED IN THE UNITED
STATES OF AMERICA AND IN IRELAND. ALL RIGHTS RESERVED. THIS
DOCUMENT OR PARTS THEREOF MAY NOT BE REPRODUCED IN ANY
FORM WITHOUT THE WRITTEN PERMISSION OF THE PUBLISHER.
The information in this document is subject to change without notice and
should not be construed as a commitment by Waters Corporation. Waters
Corporation assumes no responsibility for any errors that may appear in this
document. This document is believed to be complete and accurate at the time
of publication. In no event shall Waters Corporation be liable for incidental or
consequential damages in connection with, or arising from, its use.
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of Waters Corporation.
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Micromass Ltd.
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Other registered trademarks or trademarks are the sole property of their
owners.
ii
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iii
Contacting Waters
®
Contact Waters with enhancement requests or technical questions regarding
the use, transportation, removal, or disposal of any Waters product. You can
reach us via the Internet, telephone, or conventional mail.
Waters contact information
Contacting medium
Information
Internet
The Waters Web site includes contact
information for Waters locations worldwide.
Visit www.waters.com.
Telephone and fax
From the USA or Canada, phone 800
252-HPLC, or fax 508 872 1990.
For other locations worldwide, phone and fax
numbers appear in the Waters Web site.
Conventional mail
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USA
Safety considerations
Some reagents and samples used with Waters instruments and devices can
pose chemical, biological, and radiological hazards. You must know the
potentially hazardous effects of all substances you work with. Always follow
Good Laboratory Practice, and consult your organization’s safety
representative for guidance.
When you develop methods, follow the “Protocol for the Adoption of Analytical
Methods in the Clinical Chemistry Laboratory,” American Journal of Medical
Technology, 44, 1, pages 30–37 (1978). This protocol addresses good operating
procedures and the techniques necessary to validate system and method
performance.
iv
Safety advisories
Consult Appendix A for a comprehensive list of warning and caution
advisories.
Operating this instrument
When operating this instrument, follow standard quality-control (QC)
procedures and the guidelines presented in this section.
Applicable symbols
Symbol
Definition
Confirms that a manufactured product complies
with all applicable European Community
directives
ABN 49 065 444 751
Australia C-Tick EMC Compliant
Confirms that a manufactured product complies
with all applicable United States and Canadian
safety requirements
This product has been tested to the requirements
of CAN/CSA-C22.2 No. 61010-1, second edition,
including Amendment 1, or a later version of the
same standard incorporating the same level of
testing requirements
Audience and purpose
This guide is intended for personnel who install, operate, and maintain 2424
Evaporative Light Scattering (ELS) detectors.
Intended use of the 2424 ELS detector
Waters designed the 2424 ELS detector to analyze and monitor many
compounds.
v
Calibrating
To calibrate LC systems, follow acceptable calibration methods using at least
five standards to generate a standard curve. The concentration range for
standards should include the entire range of QC samples, typical specimens,
and atypical specimens.
When calibrating mass spectrometers, consult the calibration section of the
operator’s guide for the instrument you are calibrating. In cases where an
overview and maintenance guide, not operator’s guide, accompanies the
instrument, consult the instrument’s online Help system for calibration
instructions.
Quality-control
Routinely run three QC samples that represent subnormal, normal, and
above-normal levels of a compound. Ensure that QC sample results fall within
an acceptable range, and evaluate precision from day to day and run to run.
Data collected when QC samples are out of range might not be valid. Do not
report these data until you are certain that the instrument performs
satisfactorily.
ISM classification
ISM Classification: ISM Group 1 Class B
This classification has been assigned in accordance with CISPR 11 Industrial
Scientific and Medical (ISM) instruments requirements. Group 1 products
apply to intentionally generated and/or used conductively coupled
radio-frequency energy that is necessary for the internal functioning of the
equipment. Class B products are suitable for use in both commercial and
residential locations and can be directly connected to a low voltage,
power-supply network.
vi
EC Authorized Representative
Waters Corporation (Micromass UK Ltd.)
Floats Road
Wythenshawe
Manchester M23 9LZ
United Kingdom
Telephone:
+44-161-946-2400
Fax:
+44-161-946-2480
Contact:
Quality manager
vii
viii
Table of Contents
Copyright notice ................................................................................................... ii
Trademarks ............................................................................................................ ii
Customer comments ............................................................................................ iii
Contacting Waters ............................................................................................... iv
Safety considerations .......................................................................................... iv
Safety advisories .................................................................................................. v
Operating this instrument .................................................................................. v
Applicable symbols .............................................................................................. v
Audience and purpose.......................................................................................... v
Intended use of the 2424 ELS detector............................................................... v
Calibrating .......................................................................................................... vi
Quality-control .................................................................................................... vi
ISM classification ................................................................................................. vi
ISM Classification: ISM Group 1 Class B ......................................................... vi
EC Authorized Representative ........................................................................ vii
1 2424 ELS Detector Optics Principles ................................................ 1-1
Principles of evaporative light scattering detection ...............................
Overview...........................................................................................................
Capabilities ......................................................................................................
ELS detection process......................................................................................
Detection ..........................................................................................................
ELS detection limitations................................................................................
1-2
1-2
1-2
1-2
1-4
1-6
Detector description ........................................................................................
Signal processing and noise calculations........................................................
Calibrating the photomultiplier tube (PMT)..................................................
Filtering noise ..................................................................................................
Electronics and data acquisition .....................................................................
1-7
1-8
1-8
1-8
1-9
Table of Contents
ix
Nebulizer .......................................................................................................... 1-9
Optics bench ..................................................................................................... 1-9
Temperature control ...................................................................................... 1-10
Startup diagnostics ........................................................................................ 1-11
Lamp energy and performance ..................................................................... 1-12
Rear panel ...................................................................................................... 1-13
References ........................................................................................................ 1-13
2 Setting up the Detector ........................................................................ 2-1
Introduction ....................................................................................................... 2-2
Before you begin ............................................................................................... 2-2
Unpacking and inspecting .............................................................................. 2-3
Selecting a site within a laboratory .............................................................
Site selection requirements .............................................................................
Detector dimensions ........................................................................................
Power requirements.........................................................................................
Gas requirements.............................................................................................
2-3
2-4
2-5
2-6
2-7
Making the gas supply connection ............................................................... 2-7
Venting the exhaust hose ................................................................................ 2-8
Connecting to the electricity source .......................................................... 2-11
Installing the nebulizer assembly ............................................................... 2-12
Connecting the siphon drain tubing .......................................................... 2-14
Routing the siphon drain tubing down the front of the detector................. 2-14
Routing the siphon drain tubing to the rear of the detector ....................... 2-15
Connecting the drip tray ............................................................................... 2-18
Required materials ........................................................................................ 2-18
Connecting the nebulization gas to the nebulizer .................................. 2-19
Connecting a column or second detector .................................................. 2-19
Required materials ........................................................................................ 2-19
x
Table of Contents
Making signal connections ...........................................................................
Connecting the Ethernet cable......................................................................
Network installation guidelines....................................................................
Connecting to other instruments ..................................................................
Connecting the Waters column heater module ............................................
2-20
2-22
2-23
2-25
2-33
3 Operating the Detector ......................................................................... 3-1
Starting up the detector ..................................................................................
Initializing the detector ...................................................................................
Using the display .............................................................................................
Detector Home and Message screen icons......................................................
3-2
3-2
3-4
3-5
Using the keypad ............................................................................................... 3-7
Navigating the user interface ...................................................................... 3-13
Navigating to and from the Home screen..................................................... 3-13
Preparing to start a run ................................................................................ 3-15
Primary and secondary functions ................................................................. 3-15
Setting up a run ...............................................................................................
Setting the nebulizer and drift tube temperature .......................................
Setting the gain and gas pressure ................................................................
Setting the column heater module temperature ..........................................
Resetting the stop flow output switch ..........................................................
Operating the trace and scale functions.......................................................
Setting the data rate......................................................................................
Setting the filter time constant.....................................................................
Setting the switch output ..............................................................................
Setting the analog signal output...................................................................
Setting auto zero options ...............................................................................
3-17
3-18
3-19
3-21
3-21
3-22
3-24
3-24
3-25
3-25
3-25
Configuring the detector ...............................................................................
Configuring event inputs...............................................................................
Configuring stop flow output.........................................................................
Setting pulse periods .....................................................................................
Selecting the type of nebulizer ......................................................................
Setting the display contrast ..........................................................................
3-26
3-27
3-28
3-28
3-29
3-29
Table of Contents
xi
Displaying system information ..................................................................... 3-30
Using help ...................................................................................................... 3-30
Operating the detector .................................................................................. 3-30
Standalone operation..................................................................................... 3-31
Auto-optimizing gain and LSU-FS ............................................................... 3-31
Programming methods and events .............................................................
Overview of methods .....................................................................................
Programming timed events ...........................................................................
Programming threshold events.....................................................................
Storing a method............................................................................................
Retrieving a method ......................................................................................
Viewing events within a method...................................................................
Resetting a method ........................................................................................
Clearing events ..............................................................................................
3-34
3-34
3-35
3-37
3-38
3-39
3-39
3-39
3-40
Conserving lamp life ...................................................................................... 3-41
Changing chromatographic conditions ..................................................... 3-43
Shutting down the detector .......................................................................... 3-44
Periodic maintenance .................................................................................... 3-45
4 Maintaining the Detector ..................................................................... 4-1
Contacting Waters technical service ............................................................ 4-2
Maintenance considerations .......................................................................... 4-2
Safety and handling......................................................................................... 4-2
Spare parts ....................................................................................................... 4-3
Replacing the lamp cartridge ........................................................................ 4-3
Replacing the nebulizer .................................................................................. 4-6
Cleaning the nebulizer ultrasonically ......................................................... 4-9
Cleaning the drift tube .................................................................................. 4-12
Servicing the vapor trap ............................................................................... 4-13
xii
Table of Contents
Replacing fuses ................................................................................................ 4-14
Cleaning the instrument’s exterior ............................................................ 4-15
5 Diagnostic Functions and Troubleshooting .................................... 5-1
Error messages .................................................................................................. 5-2
Startup error messages ................................................................................... 5-2
Operational error messages ............................................................................ 5-2
User-selectable diagnostic functions ........................................................... 5-2
Overview........................................................................................................... 5-2
“Sticky diagnostics” tests................................................................................. 5-4
Running diagnostic tests ................................................................................. 5-5
Running the Auto Gain diagnostic function................................................... 5-5
Input and output diagnostic functions ........................................................... 5-6
Lamp, display, and keypad diagnostic functions ........................................... 5-8
Gas and temperature control diagnostic functions ...................................... 5-10
Sample and reference energy diagnostic function ....................................... 5-12
Generate Test Peaks diagnostic function ..................................................... 5-13
General troubleshooting ...............................................................................
Power surges ..................................................................................................
Detector troubleshooting ...............................................................................
Power-on confidence check error messages ..................................................
Operational error messages ..........................................................................
5-13
5-13
5-14
5-16
5-17
Chromatography troubleshooting .............................................................. 5-21
Abnormal baseline ......................................................................................... 5-22
Erratic or incorrect retention times.............................................................. 5-27
6 Optimizing Detection and Preparing Solvents ............................... 6-1
Optimizing detector performance ................................................................
Optimizing the mobile phase ..........................................................................
Sample pretreatment.......................................................................................
Column treatment ...........................................................................................
6-2
6-2
6-2
6-2
Selecting a solvent ............................................................................................ 6-2
Table of Contents
xiii
Solvent degassing ............................................................................................. 6-7
Solvent degassing methods ............................................................................. 6-7
Solvent degassing considerations ................................................................... 6-8
Optimization protocol ...................................................................................... 6-9
Nebulizer gas pressure .................................................................................... 6-9
Nebulizer temperature .................................................................................... 6-9
Drift tube temperature .................................................................................. 6-10
Selecting the optimum temperature ............................................................. 6-10
A Safety Advisories .................................................................................. A-1
Warning symbols ............................................................................................... A-2
Task-specific hazard warnings........................................................................ A-2
Specific warnings ............................................................................................. A-3
Caution symbol .................................................................................................. A-5
Warnings that apply to all Waters instruments ......................................... A-5
Electrical and handling symbols ................................................................. A-12
Electrical symbols .......................................................................................... A-12
Handling symbols .......................................................................................... A-13
B Specifications ........................................................................................ B-1
2424 ELS detector specifications ................................................................. B-1
Index ..................................................................................................... Index-1
xiv
Table of Contents
1
2424 ELS Detector Optics
Principles
To use the 2424 ELS detector effectively, you must understand the principles
that underlie operation of the detector’s optics and electronics.
Contents:
Topic
Page
Principles of evaporative light scattering detection
1-2
Detector description
1-7
References
1-13
1-1
Principles of evaporative light scattering detection
Overview
Evaporative light scattering (ELS) detection works by nebulizing the solvent
flow from a liquid chromatography (LC) system and entraining the resultant
droplets in a gas stream. Mobile phase is then evaporated from the droplets.
When an analyte is less volatile than the mobile phase, it remains in the gas
stream as a “dry” solute particle and flows to the ELS detector. Once there,
the particles scatter the light beam. The amount of scattered light is measured
and bears a relationship to the concentration of material eluting.
Capabilities
The 2424 ELS detector is compatible with virtually all modes of
chromatography including flow injection analysis. The detector responds to all
compounds that are, relative to their mobile phase, sufficiently nonvolatile at
the conditions of analysis. Applications for ELS detection include
combinatorial libraries of small molecules, natural product extracts and
libraries, food products, and related materials. For detecting compounds that
exhibit little to no UV/Vis response and do not ionize well for mass
spectrometry, the ELS detector complements HPLC for analyzing sugars,
antibiotics, antivirals, lipids, phospholipids, biomolecules, and natural
products. You can use ELS detection in a system that includes a mass
spectrometer and absorbance detector, applying it as a qualitative tool to
demonstrate the purity or complexity of a sample. Quantitation can be
achieved by carrying out a calibration plot, as explained later in this guide.
Note, however, that the curve will not be linear because ELS detectors give a
non-linear response.
ELS detection performs well in isocratic or gradient elution with a wide
variety of mobile phases and additives. Waters recommends using mass
spectrometry-compatible volatile mobile-phase modifiers.
ELS detection process
The three separate regions of an ELS detector are nebulization, desolvation,
and detection. In all ELS detectors, these three regions are positioned so that
the chromatographic effluent is nebulized and mobile phase is evaporated so
1-2
2424 ELS Detector Optics Principles
that dry solute particles, consisting only of analytes, reach the light source for
scattering.
Low temperature nebulization
In the detector’s nebulization region, the chromatographic effluent is
transformed into a fine aerosol. A concentric tube, or flow-type nebulizer,
mixes chromatographic effluent with a carrier gas (usually nitrogen)
developing a series of droplets that forms the aerosol that enters a
narrow-orifice drift tube.
Nebulization region and drift tube (representative)
Nebulization region
Drift tube
The concentric flow nebulizer allows you to control the carrier gas flow versus
the chromatographic effluent flow rate. High gas flow produces small droplets,
requiring less heat to evaporate the solvent. Conversely, low gas flow produces
large droplets, requiring more heat to evaporate the solvent.
Desolvation
In the desolvation region, the mobile phase evaporates, leaving dried solute
particles in the drift tube.
As the aerosol drops exiting the nebulizer pass through the drift tube, they
become smaller. The carrier gas sweeps the dried, aerosolized solute particles
along to the instrument’s detection region.
Evaporation occurs as a function of time, temperature, and pressure of the
carrier gas. It is therefore important to use HPLC mobile phases that easily
and quickly evaporate and desolvate. Solvents of fairly low boiling point and
low viscosity are best. They include the more commonly used HPLC mobile
phases: water, acetonitrile, methanol, ethanol, and THF. Viscous and
high-boiling solvents might fail to fully separate from the analyte molecules or
Principles of evaporative light scattering detection
1-3
species before the detection step. This adds to the background noise and
decreases the analyte signal response, which causes low sensitivity (slope of
the calibration plot) and high limits of detection (LOD). The evaporated HPLC
solvents are condensed and captured in the recommended solvent trap and
exhaust routing. Nevertheless, small amounts of residual can persist, and
these should be exhausted into a fume hood to prevent their escape into the
laboratory.
Detection
The analyte particles enter the detection region where a light source impinges
on the particles. The light is thus scattered and focused onto a photomultiplier
tube (PMT) where its intensity is measured.
The size (diameter) of the analyte particles determines how the light is
scattered. The detector measures the intensity of the scattered light at 60°
relative to the excitation beam to minimize polarization effects and stray
light. Particles of different sizes exhibit different angular distributions of the
scattered light, and particles whose sizes and shapes vary have different
light-scattering cross sections. In general, larger particles scatter more light,
yielding more intense signals and peak responses.
A photomultiplier tube (PMT) converts the scattered light signal to a voltage
that can be recorded and analyzed. The stronger the scattering, the more
intense the final signal on the ELS detection chromatogram. The scattered
light is a rough measure of the mass of material represented by a
chromatographic peak. To some degree, this “mass” response can be
compound-independent. However, many factors can also affect the mass
response, particularly the density of the analyte in a small dried particle. For
example, a popped kernel of corn has a lower density than the unpopped
kernel from which it originated. Yet, because it is larger, in most cases it
would scatter more light. You should also remember that the output of an ELS
detector has no direct relation to the molecular weight of an analyte.
Types of light scattering
The three possible regimes of light scattering are
1-4
•
Rayleigh
•
Mie
•
refraction-reflection
2424 ELS Detector Optics Principles
Light scattering direction
Rayleigh scattering
Mie scattering
Refraction-reflection scattering
Direction of incident light
For a nebulizer that produces an average droplet diameter of D0, the diameter
of an average, resulting dry analyte particle is
D = D 0 ( c ⁄ p ) 1 / 3 where
D0 = Average liquid droplet diameter
c = Concentration of the analyte
p = Density of the dry analyte
For any given analyte peak, the response of an ELS detector can be that of all
three light scattering regimes. The light-scattering type depends on the size of
the particles going through the light beam. The ratio of particle diameter, D,
---- , defines the type of scattering that results.
to the incident wavelength, λ, or D
λ
•
---- <0.1. The
Rayleigh scattering occurs for the smallest particles where D
λ
6
scattered light from a particle is proportional to D , and consequently
2
the scattered signal is proportional to c .
•
---- >0.1, but <1.0. The scattered
Mie scattering occurs for particles where D
λ
4
4/3
light is proportional to D , and the scattered signal is proportional to c .
Principles of evaporative light scattering detection
1-5
•
---- >1.0. The
Refraction-reflection scattering occurs for particles where D
λ
2
scattered light is proportional to D , and the scattered signal is
2/3
proportional to c .
•
As a chromatographic peak elutes from a column, the concentration of
the analyte it represents changes. Concentration goes from near-zero at
the baseline to a maximum that corresponds to column efficiency,
injection volume, retention time, and concentration of the sample when
injected. From the maximum level, the concentration then returns to
near-zero. If the concentration is high enough, the diameter of a dry
analyte particle can vary through all three scattering regimes—
Rayleigh, Mie, and refraction-reflection scattering. It is this variance
that prevents linearity in ELS detection calibration plots over more than
one order of magnitude.
ELS detection limitations
Consider these limitations when implementing global ELS detection
separation methods:
1-6
•
ELS detection lacks linearity over wide concentration ranges. When you
use the detector for assays, you may need to experiment with a variety of
“best fits” using linear, quadratic, and log-log responses for the
compounds of interest. You might also need to establish groupings for
expected concentration ranges.
•
ELS detection is a destructive technique; the analyte is sacrificed to
generate the scattering particles. Ideally, therefore, the ELS detector
should be the final detector in a series. Alternatively, you can place the
ELS detector upstream of others, provided you split the column effluent
so that the ELS detector receives its own stream from the LC.
•
Any particle can interfere with the sample signal, including particulates
in poor-grade chromatographic solvents because the detector responds
equally to all particulates. This lack of selectivity can cause problematic
background noise.
•
The detector’s sensitivity to the particulates increases noise and,
consequently, signal-to-noise variation for a given method arising from
differences in the quality of mobile phases. Moreover, stationary phase
components can leach from the column and contribute particulates to
the sample flow.
2424 ELS Detector Optics Principles
•
You can reduce the load of unwanted particulates by filtering LC
effluent and the instrument’s carrier gas.
•
ELS detection cannot detect compounds whose volatility resembles that
of the mobile phase. When the analyte and mobile phase have similar
volatility, it is impossible to evaporate the mobile phase from droplets
without also evaporating the analyte.
•
In many cases the detector is minimally sensitive to baseline drift
caused by gradient changes in an LC separation. However, its
performance is not completely independent of the effects of changing
solvent composition, which affects the nebulizer’s ability to form droplets
and influence their size.
Detector description
The detection of a sample peak occurs as follows:
1.
Eluent from the column flows into the nebulizer where a steady supply
of gas converts it into a fine aerosol. Carefully controlled gas flow and
flow rates determine the size of eluent droplets found in the aerosol.
Warning: Fire and explosion hazard. Do not use air as the carrier
gas when the mobile phase contains flammable components.
2.
Droplets are vaporized in the evaporation drift tube, leaving a rising
column of particles, suspended in gas and vaporized solvent, to pass into
the center of the light scattering chamber.
3.
Two condensing lenses, L1 and L2, focus light from the lamp through a
slit.
2424 ELS detection process (representative)
Light trap
Photodiode
and light
trap
Scattering
chamber
Lens 4
M1 mirror
Snout
Condensing lenses
L1 and L2
Stray light
baffle
Relay
lens L3
Slit
Lamp
filament
PMT
Detector description
1-7
4.
Lens L3 relays the light from the slit to the center of the scattering
chamber. A baffle between the slit and relay lens minimizes stray light
reaching the scattering chamber.
5.
Only light scattered at a 60° angle relative to the incident light is
channeled through the snout and collector lens, L4. The positioning and
design of the snout, together with the aid of two light traps, minimize
stray light that can be detected. The first light trap houses a photodiode
to intercept a portion of the stray incident light by monitoring lamp
intensity variations. The second light trap minimizes stray light
opposite the collection optics.
6.
The collector lens focuses light onto the M1 mirror to change the
direction of light before reflecting it onto the photomultiplier tube.
7.
The PMT converts the light to an electrical signal.
8.
Remaining gaseous effluent is vented.
Signal processing and noise calculations
Power source fluctuations can introduce noise in the detector output and be a
major source of noise at high signal levels. To offset their effect, a reference
signal tracks lamp fluctuations and corrects the sample (PMT) signal
accordingly.
Calibrating the photomultiplier tube (PMT)
The full scale sensitivity of the instrument is controlled by the gain setting,
which increases the voltage to the PMT to amplify response. The instrument
gain is achieved by controlling the high voltage supply to the PMT. However,
the PMT response is not linear, so each unit must be individually calibrated to
determine the required voltage settings for each gain value. PMT calibration
is performed by Waters after the assembly and alignment of the detector and
whenever the PMT or any PC boards are replaced.
Filtering noise
In the General tab of the ELS Instrument Method Editor (for details, refer to
the Empower or MassLynx online Help), you can apply an optional noise filter
(the Time Constant parameter) to the data acquired.
1-8
2424 ELS Detector Optics Principles
Electronics and data acquisition
The detector's electronics consist of the following components:
•
DC power supply – Provides all DC voltages required for the analog and
digital circuitries.
•
Preamplifier board – Collects and processes the analog input signals
from the PMT and photodiode to the microprocessor for further signal
conditioning. Sample and reference signals are integrated and A/D
conversion is performed simultaneously. This ensures the best rejection
of common mode noise in the two beams, leading to a very quiet
baseline.
•
Controller board – Provides the drive circuitry for all modules in the
system such as the lamp, heaters, cooler, keypad, display, PMT, fans,
external column heater, etc. It provides power to the CPU board and the
preamplifier board. It also interfaces between the Preamplifier board
and the CPU board.
•
CPU board – Contains the microprocessor, serial RS232 and Ethernet
communications, battery backed nonvolatile RAM (in which the user
parameters and calibration values are saved), and Flash RAM (in which
the firmware resides).
•
Display and Keypad – Provides the user with direct control of the system
when it is used in standalone mode. The keypad allows the user to
access the control system, program methods, calibrate, and troubleshoot
the detector, while the display shows the status of many functions.
Nebulizer
Both high-flow and low-flow nebulizers are available. The high-flow nebulizer
is standard in the 2424 ELS detector and is designed for flow rates ranging
from 300 to 3000 μL/min. The low-flow nebulizer is designed for 50 to 500
μL/min and gives the highest sensitivity performance.
Optics bench
The detector’s optics bench consists of three major systems:
•
Illumination
•
Light scattering chamber
•
Collections
Detector description
1-9
Illumination system
The illumination system uses these components to direct broadband light
from the lamp into the light scattering chamber:
•
Tungsten halogen lamp
•
Entrance mask
•
Two convex lenses, L1 and L2, acting as a condenser
•
Slit
•
Baffle
•
Convex relay lens L3
Light scattering chamber
The light scattering chamber is the equivalent of a flow cell in other detectors.
It provides an environment where the sample in the gas stream and the
incident light beam can interact. The chamber contains these components:
•
Two light traps
•
Reference photodiode
To prevent the solvent and analyte from condensing on the chamber walls or
optical surfaces, the chamber is heated to 50 °C (122 °F) and cannot be varied.
A thermistor for temperature regulation and an over-temperature switch are
included in its heating circuit.
Collections system
The collections system collects scattered light from the scattering chamber
and directs it to the PMT for conversion to an electrical signal. It consists of
these components:
•
Snout
•
Biconvex collector lens, L4
•
Mirror M1
•
PMT
Temperature control
To vaporize and evaporate the solvent, the nebulizer and drift tube have
temperature control.
1-10
2424 ELS Detector Optics Principles
Nebulizer
The nebulizer can be heated using a variable control heater. This heater,
represented as a power function, can heat the sample solution to improve
mass flow into the drift tube. The power function indicates the power
available to the nebulizer heater circuit. In certain cases, the nebulization
process of the mobile phase can be endothermic, as with 100% organic solvents
such as methanol and acetonitrile. These require more power than other
eluents.
The nebulizer can also be cooled when faster equilibration times are required.
This reduces the amount of solvent that is sprayed into the drift tube in the
vaporization process and allows the drift tube temperature to run lower,
therefore increasing the sensitivity of semi-volatile samples.
Drift Tube
You can set the drift tube heater up to 100° C to evaporate any residual
solvent. RTD (resistance temperature detector) sensors provide temperature
feedback to the heater control to ensure the desired temperature is
maintained. The RTD is placed at the end of the drift tube, where the
temperature is hottest, so it can give accurate feedback of the most extreme
temperature the particles will be exposed to. This is particularly important for
semivolatile substances.
Startup diagnostics
On starting the detector, the presence of many electronic devices and
components is verified. Some can self calibrate, a process that takes place at
this time. The startup diagnostics include these tests:
•
Central processing unit (CPU) test
•
Serial communication interface (SCI) test
•
Electrically erasable programmable read-only memory (EEProm) test
•
RAM test
•
Display test pattern
•
Application program checksum verification (firmware)
•
Lamp test
•
Photodiode test
•
PMT test
Detector description
1-11
The signal of the lamp is measured, and the normalization constant is
adjusted accordingly to compensate for lamp intensity variations. This
minimizes the influence of lamp intensity changes on detected signal levels.
All settings are restored to the values present when the unit was shut down,
except for the heater setpoints and gas flow, which must be specified.
Recommendation: Turn the power off and on once a week to compensate for
lamp aging.
Lamp energy and performance
In conventional designs of ELS detectors, the signal-to-noise performance of
the instrument is directly proportional to the lamp energy input to the
instrument. Lamp energy input to the detector can be affected by these
factors:
•
Age and efficiency of the lamp
•
Improperly maintained optics
•
Normal degradation of optical components (including the
photomultiplier tube)
Optical components degrade slowly. In conventional ELS detectors, response
increases by incrementally increasing the gain. However, a sample’s response
varies with energy throughput. If the lamp energy is degraded, peak response
degrades accordingly. If lamp intensity diminishes, peak response decreases
and noise increases. During normal operation, lamps are usually replaced
when the reference energy falls below a user-set threshold. The useful lamp
life depends on the method’s specific requirements for noise performance.
Eventually, the detector’s performance becomes unacceptable and the lamp
replacement is necessary.
Tip: It is good practice to inspect the detector’s general condition when lamps
are replaced.
Predicting when the detector’s performance degrades to an unacceptable level
based solely on reference energy is unsatisfactory. Each user’s analyses
require different levels of sensitivity. Determining reference energy alone to
evaluate performance assumes that lamps exhibit the same longevity and
degradation patterns. Waters therefore designed the detector to operate as
independently of lamp output as possible. Ultimately, the detector’s
performance is a function of unique application requirements.
Signal-to-noise measurements are the best way to evaluate performance and
set boundaries for acceptable operational sensitivity limits. Waters
1-12
2424 ELS Detector Optics Principles
guarantees 2000 hours of lamp life, or one year since date of purchase,
whichever comes first.
Rear panel
The following figure shows the rear panel locations of the connectors used to
operate the detector with external devices.
2424 ELS detector rear panel
Gas inlet fitting
GAS
6.9 Bar (100psi)
Maximum
EXHAUST
Inputs and
outputs
Out
1
2
Inject Start
3
Ground
4
Auxiliary
Out
Lamp On
In
Stop Flow
Out
3
4
5
6
Chart Mark
In
1
2
5
6
Column
heater
7
8
Ground
9
Switch
10
EXT 1
Signal
Out
7
8
9
10
In
Ground
ACN 065444751
Ground
Auto Zero
In
EXHAUST - 15cm (6 inch) CLEARANCE REQUIRED
Serial #
Made in USA
For service
use only
RS 232
ETHERNET
!
V ~ 100 - 240
Hz 50 - 60
VA 200
F 5A/250V
Fuse holder
Power input
receptacle
TP02730
References
J.R. Rubinson and K.A. Rubinson, Contemporary Chemical Analysis, Simon &
Schuster, Prentice-Hall, Inc., New Jersey, 1998.
K.A. Rubinson and J.R. Rubinson, Contemporary Instrumental Analysis,
Simon & Schuster, Prentice-Hall, Inc., New Jersey, 2000.
G.D. Christian, Analytical Chemistry, Sixth Edition, John Wiley & Sons, Inc.
New York, 2003.
References
1-13
C.G. Enke, The Art and Science of Chemical Analysis, John Wiley & Sons,
Inc., New York, 2001.
Handbook of Instrumental Techniques for Analytical Chemistry, Edited by F.
Settle, Prentice Hall Publishers, Upper Saddle River, NJ, 1997.
HPLC Methods for Pharmaceutical Analysis, Edited by G. Lunn and N.
Schmuff, Wiley-Interscience Publishers, J. Wiley & Sons, New York, 1997.
(CD-ROM)
C.A. Poole and S.K. Poole, Chromatography Today, Elsevier Science
Publishing Co., Amsterdam and New York, 2001.
High Performance Liquid Chromatography, Edited by P.R. Brown and R.A.
Hartwick, Wiley-Interscience, New York, 1989.
A Century of Separation Science, Edited by H. Issaq, Marcel Dekker, Inc., New
York, Chapter 44, pp. 693-709, 2001.
Detectors for Liquid Chromatography, Edited by E. Yeung, J. Wiley & Sons,
New York, 1986.
B.A. Bidlingmeyer, Practical HPLC Methodology and Applications, Wiley &
Sons, NY, 1992.
U. Neue, HPLC Columns, Theory, Technology, and Practice. Wiley-VCH
Publishers, New York, 1997.
L. Snyder, J.J. Kirkland, and J. Glajch, Practical HPLC Method Development,
Second Edition, Wiley-Interscience Publishers, New York, 1997.
Reaction Detection in Liquid Chromatography, Edited by I.S. Krull, Marcel
Dekker, New York, 1986.
Liquid Chromatography Detectors, Edited by T.M. Vickrey, Marcel Dekker,
New York, 1983.
S. Ahuja, Selectivity and Detectability in HPLC. J. Wiley & Sons, New York,
1989.
R.P.W. Scott, Liquid Chromatography Detectors, Elsevier Scientific
Publishing Company, Amsterdam, The Netherlands, 1977.
HPLC Detection-Newer Methods, Edited by G. Patonay, VCH Publishers,
Weinheim, Germany, 1992.
Element-Specific Chromatographic Detection, Edited by P.C. Uden, ACS
Symposium Series 179, American Chemical Society, Washington, DC, 1992.
1-14
2424 ELS Detector Optics Principles
M. Dreux and M. Lafosse, “Evaporative light scattering detection of
carbohydrates in HPLC.” In Carbohydrate Analysis, High Performance Liquid
Chromatography and Capillary Electrophoresis, Edited by Z. El Rassi,
Journal of Chromatography Library, Volume 58, Elsevier Science Publishers,
Amsterdam, The Netherlands, 1995, Chapter 13. Second Edition, 2002.
A. Stolyhwo, H. Colin, and G. Guiochon, “Use of light scattering as a detector
principle in liquid chromatography.” J. Chromatogr., 265, 1 (1983).
G. Guiochon, A. Moysan, and C. Holley, “Influence of various parameters on
the response factors of the evaporative light scattering detector for a number
of nonvolatile compounds.” J. Liquid Chromatogr., 11(12), 2547 (1988).
J.A. Koropchak, L.E Magnusson, M. Heybroek, S. Sadain, X. Yang, and M.P.
Anisimov, “Fundamental aspects of aerosol-based light-scattering detectors
for separations.” Advances in Chromatography, Volume 40, Edited by P.R.
Brown, E. Grushka, and Marcel Dekker, New York, 1998, Chapter 5.
References
1-15
1-16
2424 ELS Detector Optics Principles
2
Setting up the Detector
Contents:
Topic
Page
Introduction
2-2
Before you begin
2-2
Unpacking and inspecting
2-3
Selecting a site within a laboratory
2-3
Making the gas supply connection
2-7
Venting the exhaust hose
2-8
Connecting to the electricity source
2-11
Installing the nebulizer assembly
2-12
Connecting the siphon drain tubing
2-14
Connecting the drip tray
2-18
Connecting the nebulization gas to the nebulizer
2-19
Connecting a column or second detector
2-19
Making signal connections
2-20
2-1
Introduction
The following figure shows the major steps in installing the detector.
Major steps in installing the detector
Start installation
procedure
Select
appropriate
site
Unpack and
inspect
Place 2424 ELS
detector in desired
location
Make gas
connections
Make waste and
venting connections
Make power
connections
Install nebulizer
Make liquid line
connections
Make signal
Make Signal
connections to
Connections to
other devices
Fill siphon with
mobile phase
Installation
complete
Before you begin
Requirement: To install the detector, you should know how, in general, to set
up and operate laboratory instruments and computer-controlled devices and
also how to handle solvents.
2-2
Setting up the Detector
Before installing the detector, ensure that
•
it is not situated under a heating or cooling vent
•
the required components are present
•
none of the shipping containers or unpacked items are damaged
Unpacking and inspecting
The shipping carton contains these items:
•
2424 ELS detector
•
Waters 2424 Evaporative Light Scattering Detector Operator’s Guide
•
Startup kit
•
Release notes
To unpack the detector and nebulizer:
1.
Check the contents of the shipping cartons against the packing lists to
ensure that you received all items.
2.
Save the shipping cartons for future transport or shipment.
If you discover any damage or discrepancy when you inspect the contents of
the cartons, immediately contact the shipping agent and your local Waters
representative.
Customers in the USA and Canada should report damage and discrepancies to
Waters Technical Service (800 252-4752). Others should phone their local
Waters subsidiary or Waters corporate headquarters in Milford,
Massachusetts (USA), or they may visit http://www.waters.com.
For complete information on reporting shipping damages and submitting
claims, see Waters Licenses, Warranties, and Support Services.
Selecting a site within a laboratory
The reliable operation of your detector depends on a proper installation site
and suitable power supply.
Unpacking and inspecting
2-3
Site selection requirements
Install the detector in an area that meets the requirements in the table at the
end of this section.
The detector is a stackable unit and does not require bench space beyond the
dimensions shown in the figure on page 2-5.
Caution: To avoid damaging the detector, the amount of weight stacked
on top of it should not exceed 18 kg (40 pounds).
Place the detector close to the column outlet to minimize band broadening,
which reduces the resolution of a chromatogram.
Tip: If your system includes more than one detector, connect the ELS detector
so that it is the final detector in the series because it nebulizes column effluent
and exhausts it as gas vapor.
Installation site requirements
2-4
Parameter
Requirement
Operating temperature
range
4 to 30 °C (39.2 to 86 °F); avoid direct exposure
to sunlight and heating and cooling vents
Storage temperature
range
-30 to 60 °C (-22 to 140 °F))
Relative humidity
20 to 95%, noncondensing
Storage humidity range
0 to 95%, noncondensing
Bench space
At least 33.53 cm (13.2 inches) wide × 66.04 cm
(26 inches) deep × 20.8 cm (8.2 inches) high
(includes 15.0 cm [6 inches] clearance at the
rear and 5 cm [2 inches] clearance on the left for
ventilation)
At least 5 cm (2 inches) clearance is needed on
the left side of the detector to allow venting for
nebulizer cooling. Blocking this vent could
adversely affect nebulizer cooling.
Power
Grounded AC, 100 to 240 VAC,
50 to 60 Hz nominal 200 VA
Setting up the Detector
Installation site requirements (Continued)
Parameter
Requirement
Gas supply
450 to 690 kPa (4.5 to 6.9 bar, 65 to 100 psi), at
the regulator, of dry, oil-free, filtered nitrogen
or zero grade oil-free, filtered air
Ventilation
Locate near fume hood or exhaust system for
proper venting of detector exhaust
Surface orientation
Level (ensures proper nebulizer drip tray
function)
Altitude limitations
None
Detector dimensions
The following figure shows the dimensions of the detector.
Detector dimensions
52.1 cm
(20.5 inches)
20.3 cm
(8.0 inches)
28.5 cm
(11.2 inches)
TP02723
Tip: Access to the instrument inside the top cover is not required. All required
access is through the left-front panel where the liquid line connections are
located.
Selecting a site within a laboratory
2-5
Power requirements
The detector, which operates over the range 100 to 240 VAC, is shipped from
the factory with two 5.00 A, 250 V fuses.
Warning: To avoid electrical shock, observe these precautions:
• Use power cord SVT-type in the United States and HAR-type (or
better) in Europe. For other countries, contact your local Waters
distributor.
• Power-off and unplug the detector before performing any
maintenance on the instrument.
• Connect all components of the HPLC system to a common ground.
Warning: For continued protection against fire, replace fuses only with
those of the same type and rating.
The detector’s two fuses are located above the power input receptacle on its
rear panel.
2424 ELS detector rear panel
Gas inlet fitting
GAS
6.9 Bar (100psi)
Maximum
EXHAUST
Inputs and
outputs
1
2
Auxiliary
Out
Stop Flow
Out
6
7
8
Ground
9
Switch
10
EXT 1
Out
Ground
4
5
Column
heater
Signal
3
Out
1
2
3
4
5
6
7
8
9
10
Inject Start
In
Ground
Lamp On
In
Chart Mark
In
ACN 065444751
Ground
Auto Zero
In
EXHAUST - 15cm (6 inch) CLEARANCE REQUIRED
Serial #
Made in USA
For service
use only
RS 232
ETHERNET
!
V ~ 100 - 240
Hz 50 - 60
VA 200
F 5A/250V
Fuse holder
Power input
To replace a fuse in the detector, see page 4-14.
2-6
Setting up the Detector
TP02730
Gas requirements
Use a constant supply of dry, oil-free, filtered nitrogen (or zero-grade, oil-free,
filtered air) to operate the detector. Other inert gases can also be used. Use an
operating pressure, at the regulator, of between 450 to 690 kPa (4.5 to 6.9 bar,
65 to 100 psi).
Warning: Do not use gases that are not inert. In particular, avoid those
that would allow the combustion of combustible solvents and/or the
oxidation of samples.
Caution:
• A pressure relief valve vents gas to protect the detector when the
input pressure is too high. If you can hear gas leaking from the relief
valve, lower the input pressure to avoid wasting gas.
• Gas cylinders are not recommended for extended operation of the
detector due to the rapid consumption of gas. For example, a
standard tank of nitrogen running a standard flow nebulizer at
170 kPa (1.7 bar, 25 psi) would last approximately 40 hours.
Making the gas supply connection
The detector is connected to the gas supply via 6-mm plastic tubing (supplied
in startup kit). The tubing attaches to the detector via a fitting on the back of
the unit.
To make the gas supply connection
1.
Cut the 6-mm tubing squarely (that is, perpendicular to the tubing’s
horizontal axis).
Making the gas supply connection
2-7
2.
Insert the tubing into the fitting until it bottoms.
Inserting the gas supply tube
Fitting
Gas supply tubing
3.
Pull the tubing to check engagement of the grab ring.
4.
Two pieces of tubing are provided in the startup kit. If you are using the
system with an external filter, first connect the gas source to the filter,
and then connect the filter to the back of the unit.
Venting the exhaust hose
To properly vent the exhaust vapor to waste, a vapor trap exhaust bottle is
provided (startup kit). The vessel traps condensates that form from vented
vapor exiting the detector.
2-8
Setting up the Detector
Vapor trap bottle
Barbed fittings
Bottle cap
Vapor trap bottle
Caution:
• Failure to use the vapor trap could result in too strong a vacuum,
which could adversely affect the vapor flow through the drift tube.
This could cause loss of sensitivity and excessive high-frequency
noise in the baseline.
• To avoid condensate flowing backward into the detector and thus
damaging it, run at least 61 cm (24 inches) of the instrument’s
exhaust hose vertically toward the bench top.
Exhaust Venting Requirements
Requirement: Ensure the instrument’s exhaust hose runs straight down,
toward the bench top, a minimum of 61 cm (24 inches).
•
Attach the vapor trap bottle to the end of the exhaust hose.
•
Place the vapor trap bottle’s exit hose close to an evacuation source, but
do not apply a vacuum.
Venting the exhaust hose
2-9
•
Direct the exhaust from the detector into a fume hood or exhaust vent.
•
Ensure both hoses are free of restrictions.
Warning: Inhalation risk. Do not allow detector exhaust to enter the
laboratory atmosphere.
To vent the exhaust hose
1.
Connect one end of the exhaust hose exiting from the rear of the detector
directly onto one of the barbed fittings on the vapor trap bottle.
Vapor trap bottle and exhaust hose
Exhaust hose from ELS detector
Outlet to laboratory
exhaust vent
Vapor trap bottle
Caution:
• To avoid excessive electronic noise, do not kink the exhaust
hose, which creates an unintended trap. The hose must slope
downward, without sharply bending, when exiting the detector.
• To avoid operational problems, do not cut the exhaust hose.
2-10
Setting up the Detector
2.
Using the 1.5 meter (5-foot) hose, attach one end of the tubing to the
remaining fitting on the bottle cap.
3.
Position the other end of the tubing at a perpendicular angle to a
laboratory exhaust system that applies gentle vacuum. There should be
a minimum negative pressure of −0.2 kPa (0 bar, −0.03 psi) between the
detector and the laboratory exhaust system.
Caution: Avoid placing the tubing end inside the exhaust vent.
Doing so will create a stronger vacuum on the gas exiting the
detector and likely carry away valuable sample.
Exhaust system flow example
To exhaust vent
Exhaust hose
Connecting to the electricity source
The 2424 ELS detector requires a separate, grounded electricity source. The
ground connection in the electrical outlet must be common and connected near
the chromatographic system.
Connecting to the electricity source
2-11
To connect to the electricity source
Recommendation: Use a line conditioner or an uninterruptible power supply
(UPS) for optimum long-term input voltage stability.
1.
Place the On/Off switch in the Off position.
2.
Connect the female end of the power cord to the receptacle on the rear
panel of the detector.
3.
Connect the male end of the power cord to a suitable wall outlet.
4.
Do not turn the detector on at this time.
Installing the nebulizer assembly
Waters offers two nebulizers for the 2424 ELS detector: a low-flow (for flow
rates from 50 to 500 μL/min) and a high-flow (for flow rates from 300 to
3000 μL/min). The high-flow nebulizer is provided as standard equipment.
To install the nebulizer assembly
2-12
1.
Remove the nebulizer assembly from the shipping container.
2.
Slide the packing ring onto the assembly.
3.
Remove the protective cap from the assembly.
4.
Remove the protective cap from the end of the nebulizer tube.
Setting up the Detector
5.
Align the two pins inside the nebulization chamber with the grooves in
the nebulizer.
Pins inside the nebulization chamber
The quick-disconnect tubing fitting will be at the twelve o’clock position.
Installing the nebulizer
Quick-disconnect tubing
fitting at twelve o’clock
position
6.
Push the nebulizer into the nebulization chamber, and turn it clockwise
until it snaps into place.
See also: “Selecting the type of nebulizer” on page 3-29.
Installing the nebulizer assembly
2-13
Connecting the siphon drain tubing
Siphon waste is routed down the front or to the rear of the detector via one of
two different siphon drain tubes supplied in the startup kit.
Tip: At initial setup, Waters recommends that you fill the siphon with water
or mobile phase. Omitting this step delays satisfactory detector performance.
Routing the siphon drain tubing down the front of the detector
Required materials
•
Front siphon drain tubing (in startup kit)
•
Hose clamp, to secure front siphon drain tubing to siphon (in startup kit)
To route the siphon drain tubing down the front of the detector
1.
Slide the 0.68 × 0.74 cm (.269 × .291 inches) hose clamp onto the end of
the siphon drain tubing.
Hose clamp on end of siphon drain tubing
End of siphon
drain tubing
Hose clamp
2-14
Setting up the Detector
2.
Attach the front siphon drain tubing to the stainless steel siphon drain
on the front of the detector and pinch the clamp so that it is snug.
Front siphon drain tubing installation
Siphon drain tubing
Hose clamp
3.
Ensure that the siphon drain tubing is routed to a collection bottle in
such a way that condensed solvent can flow freely from the condenser
and the end of the tubing is not immersed in the collected liquid.
Warning: To avoid flooding the detector, ensure the siphon drain
tubing is not kinked or submerged in the collection bottle.
Routing the siphon drain tubing to the rear of the detector
Tip: The rear siphon drain tubing is intended for use with the optional Waters
Alliance bottle tray kit.
Required material
•
Rear siphon drain tubing (in startup kit)
•
Convoluted tubing (in startup kit)
•
Plastic hose clamp (in startup kit)
•
Siphon drain tubing bracket (in startup kit)
•
Phillips® screwdriver
Connecting the siphon drain tubing
2-15
To route the siphon drain tubing to the rear of the detector
1.
Using a Phillips screwdriver, remove the front left-hand screw that
secures the detector cover.
2.
Insert the screw through the hole in the siphon drain tubing bracket,
and align the screw and bracket with the hole that you removed the
cover screw from.
3.
Using a Phillips screwdriver, secure the bracket to the front, left side of
the detector.
Siphon drain tubing bracket installation
Siphon drain
tubing bracket
Left front side
of detector
4.
2-16
Route the rear siphon drain tubing through the siphon drain tubing
bracket to the rear of the unit.
Setting up the Detector
5.
Attach the rear siphon drain tubing to the stainless steel siphon drain
on the front of the detector.
Rear siphon drain tubing installation
Siphon drain
tubing bracket
Rear siphon
drain tubing
6.
Route the other end of the rear siphon drain tubing through the opening
in the rear left corner of the detector tray.
7.
Attach the convoluted tubing to the rear siphon drain tubing using the
plastic hose clamp.
Convoluted tubing attached to rear siphon drain tubing
Rear siphon
drain tubing
Plastic hose
clamp
Convoluted
tubing
Connecting the siphon drain tubing
2-17
8.
Ensure that the siphon waste tube is routed to a collection bottle in such
a way that condensed solvent can flow freely from the condenser and the
end of the tube is not immersed in the collected liquid.
Warning: To avoid flooding the detector, ensure the siphon drain
tubing is not kinked or submerged in the collection bottle.
Connecting the drip tray
The detector uses a drip tray underneath the nebulizer on the front panel to
direct solvent to the front of the unit in the event of a leak.
Required materials
•
Tubing (not supplied)
•
Sharp knife (not supplied)
To connect the drip tray
1.
Cut a length of tubing sufficient to reach between the drip tray and the
waste container.
2.
Connect the tubing to the white plastic fitting located under the
nebulizer on the front of the detector.
White plastic fitting under nebulizer
White plastic fitting
3.
2-18
Insert the other end of the tubing into the waste container.
Setting up the Detector
Connecting the nebulization gas to the nebulizer
Caution: To avoid contaminating the detector, connect the
chromatography system during operation. Gas flow in the nebulizer
creates a slight vacuum that can attract solvent or dust from the
detector's inlet port.
Insert the gas inlet tubing into the quick-disconnect tubing fitting on the
right-hand side of the nebulizer.
Connecting a column or second detector
Tips:
•
If your system includes more than one detector, connect the ELS
detector so that it is the final detector in the series because it nebulizes
the column effluent and exhausts it as gas vapor.
•
Do not allow solvent flow to continue if no gas flow is present.
Caution: In order to avoid particulate contamination, you should flush
any columns you are connecting to the detector before connecting them.
Required materials
•
Sample inlet tubing assembly
•
5/16-inch open-end wrench
To connect a column or second detector
1.
Use the sample inlet tubing assembly supplied in the startup kit.
Connecting the nebulization gas to the nebulizer
2-19
2.
Insert one end of the inlet tubing assembly into the fluid fitting on the
front of the nebulizer.
Sample inlet tubing connection
Compression screw
Sample inlet tubing
3.
Tighten the compression screw 1/4-turn past finger tight.
4.
Repeat step 2, inserting the other end of the inlet tubing assembly into
the outlet fitting of the column or another detector.
Making signal connections
Tip: Connect the detector to other HPLC system components through an
Ethernet connection.
The figure on page 2-6 shows the rear panel locations of the connectors used to
operate the detector with external devices.
The signal connections you need to make to your detector depend on the signal
connections available on the other instruments in your HPLC system.
The following figure provides an overview of the steps to follow to connect the
detector to other instruments in your HPLC system.
2-20
Setting up the Detector
Connecting components to the detector overview
Start signal
connection
Connect to
Ethernet bus?
Yes
Install Ethernet
cable
Yes
Install event and
I/O cable(s)
Yes
Install event and
I/O cable(s)
No
Connect integrator
or chart recorder?
No
Connect event
inputs or outputs?
No
Connect stop
flow outputs?
Yes
Install event and
I/O cable(s)
No
Signal connection
complete
Making signal connections
2-21
Connecting the Ethernet cable
A Waters instrument communicates with the acquisition computer through
the dedicated local area network (LAN). At the acquisition computer, the
instrument network card provides the interface that makes communication
possible.
You must install the Waters instrument software driver in the acquisition
computer so that the computer can control the instrument. See the software
installation instructions that accompany the instrument control software.
Single Waters instrument connection
In a single Waters instrument system configuration, the connection hardware
requires only one standard, shielded Ethernet cable. This cable is contained in
the startup kit.
Single Waters instrument connection
Instrument LAN
network card
Waters
instrument
Acquisition computer
Straight-through
Ethernet cable
Multiple Waters instrument connections
In a system configuration with many Waters Ethernet instruments, an
Ethernet switch is required to communicate multiple signals between Waters
instruments and the acquisition computer.
Connection hardware requires one standard 100 base-T Ethernet cable per
Waters instrument and a standard 100 base-T Ethernet cable to connect
between the network switch and the acquisition computer.
You must install the Waters instrument control software in the acquisition
computer so that the computer can control the Waters instrument. See the
software installation instructions that accompany the software instrument
driver disk.
2-22
Setting up the Detector
Network installation guidelines
Configurations for multiple Waters instruments use a dedicated LAN, which
requires a design based on the following guidelines:
•
100 base-T, 100-Mbps shielded twisted-pair (STP) cable
•
A maximum distance of 100 meters (328 feet)
Requirement: You must use a network switch for multiple Ethernet
instruments. Use of a network hub in place of a network switch is not
supported.
Multiple Waters Ethernet instrument connections
Network switch
Instrument
network card
TP02075
Workstation
100 Base-T
Ethernet cable
eSAT/IN module
Mass
spectrometer
ELS detector
Analog input
Analog input
Connecting to a Waters MassLynx system using Ethernet
When connecting to a MassLynx system using Ethernet, the various
components should be connected as shown in the figure below.
Making signal connections
2-23
MassLynx system connections
IEEE card
Network switch
Instrument LAN
network card
TP02075
IEEE-488
cable
Chromatography
manager
IEEE-488 cable
HPLC pump
PDA detector
ELS detector
Mass
spectrometer
Making inject start signal connections
When you are using an Ethernet data system with the detector, the data
system or controller must receive an inject-start signal from the autosampler
or manual injector to initiate the data collection and time-based programs.
The following table summarizes the inject start connections for different
system configurations.
Detector inject start connections
Inject start output source
Inject start input connection (on the
2424 ELS detector, connector II)
Waters 700-series
Inject Start In + / –
Waters Alliance Separations Module Inject Start In
Waters 712 Autosampler
Inject Start In + / –
Waters manual injector, or
third-party manual injector or
autosampler
Inject Start In + / –
Tip: For pinout connections to the detector, see page 2-26.
2-24
Setting up the Detector
Note: If the injector is an e2695 separations module running in Ethernet mode
or a 2707 autosampler, then the inject start cable should not be connected.
However, if the injector is an e2695 separations module running in IEEE
mode, then the inject start cable should be connected.
Connecting to a manual injector
If you are using a manual injector with your system, connect the signal cables
from the rear panel connector on the detector to the injector as shown in the
following table.
Detector connections to a manual injector
2424 ELS detector (connector II)
Manual injector
Inject Start In + (red)
One set of spade lug Inject Start
terminals
Inject Start In – (black)
For information on injection trigger signals from a manual injector, see
page 2-31.
Connecting to other instruments
To connect the detector to other instruments, use the two analog-out/event-in
(I/O) connectors and their corresponding pin-outs on the rear panel.
This section describes signal connections between the detector’s rear panel
and these items:
•
Waters Alliance Separations Module
•
Waters 1500-series pump
•
Waters SAT/IN™ Module
•
Waters, or other, manual injector
•
Waters autopurification system
•
Other manufacturer’s integrator or A/D interface device
Warning: To avoid electrical shock, power-off the detector before making
any electrical connections.
Requirement: To meet the regulatory requirements of immunity from
external electrical disturbances that can affect the performance of this
Making signal connections
2-25
instrument, do not use cables longer than 3 meters (9.8 feet) when you make
connections to the I/O connectors. In addition, ensure you connect the shield of
the cable to ground at one instrument only.
2424 rear panel analog-out/event-in connectors
Connector I (outputs)
Connector II (inputs)
1
2
3
4
5
6
7
8
9
10
+ Signal Out
− Signal Out
Ground
+ Auxiliary Out
− Auxiliary Out
+ Stop Flow
− Stop Flow
Ground
+ Switch Out
− Switch Out
1
2
3
4
5
6
7
8
9
10
+ Inject Start In
− Inject Start In
Ground
+ Lamp On
− Lamp On
+ Chart Mark In
− Chart Mark In
Ground
+ Auto Zero In
− Auto Zero In
The following table describes the detector I/O connections.
Detector analog-out/event-in connections
Signal
connections
2-26
Description
Inject start in
Activates timed events by triggering the run-time clock
to start.
Lamp on
Enables and disables the lamp. When the input is
active, the lamp is on.
Chart mark in
Adds a chart mark (at 10% of full scale) to either or
both analog output channels (Signal Out 1 and Signal
Out 2) and is configurable.
Auto zero in
Calculates an offset value that, when added to the
sample signal, makes the resulting baseline signal
zero.
Setting up the Detector
Detector analog-out/event-in connections (Continued)
Signal
connections
Description
Signal out
Provides a high resolution analog output for the
sample signal.
Output voltage range: –0.1 to 2.1 VDC (selectable
maximum data rates are 10, 20, 40, or 80 Hz).
Auxiliary out
Monitors the nebulizer, drift tube, column heater
temperature, or gas pressure and is programmable.
Output voltage range: –0.1 to 2.1 VDC (fixed maximum
data rate is 10 Hz).
Stop flow
Stops the flow to the chromatographic system when a
low input gas pressure condition, temperature control
error condition, or lamp failure occurs.
Switch out
Controls a timed event or threshold level and is a
user-programmable auxiliary output.
Generating inject start
To generate the inject start function on the detector at the start of an injection
from the Alliance Separations Module, make the connections shown in the
following table and figure.
Tip: The firmware defaults to auto zero on inject.
Detector connections to an Alliance separations module
Alliance separations module
(connector B)
2424 ELS detector (connector II)
Pin 1 inject start (red)
Pin 1 inject start in + (red)
Pin 2 inject start (black)
Pin 2 inject start in − (black)
Making signal connections
2-27
Inject start connections between the Alliance separations module and the
detector
2424 ELS detector connector II
Alliance connector B
Red
Inject Start
Inject Start
Ground
Stop Flow +
Stop Flow −
Hold Inject 1 +
Hold Inject 1 −
Hold Inject 2 +
Hold Inject 2 −
Ground
Chart Out +
Chart Out −
1
2
3
4
5
6
7
8
9
10
11
12
Black
1
2
3
4
5
6
7
8
9
10
+ Inject Start In
− Inject Start In
Ground
+ Lamp On
− Lamp On
+ Chart Mark In
− Chart Mark In
Ground
+ Auto Zero In
− Auto Zero In
Generating stop flow
The detector has a dedicated switch output, called “stop flow” that becomes
active when a heater, gas flow, or lamp failure occurs.
To use the stop flow function, make the connections shown in the following
table and figure.
Warning: Fire and explosion hazard. Failure to connect the stop flow
output could cause the detector to flood.
2-28
Setting up the Detector
Requirement: To automatically stop the chromatographic flow to the system
in the event of an error condition or hardware failure, the Stop Flow signal
must be connected to the chromatographic pump.
Detector connections to an Alliance separations module
Alliance separations module
(connector B)
2424 ELS detector (connector I)
Pin 4 stop flow + (red)
Pin 6 stop flow + (red)
Pin 5 stop flow – (black)
Pin 7 stop flow – (black)
Stop flow connections between the Alliance separations module and the
detector
2424 ELS detector connector I
Alliance connector B
Inject Start
Inject Start
Ground
Stop Flow +
Stop Flow −
Hold Inject 1 +
Hold Inject 1 −
Hold Inject 2 +
Hold Inject 2 −
Ground
Chart Out +
Chart Out −
1
2
3
4
5
6
7
8
9
10
11
12
Red
Blacki
1 +
2 −
3
4 +
5 −
6 +
7 −
8
9 +
10 −
Signal Out
Signal Out
Ground
Auxiliary Out
Auxiliary Out
Stop Flow
Stop Flow
Ground
Switch Out
Switch Out
Making signal connections
2-29
Connecting to a chart recorder or external analog data collection
device
To send an analog output signal from the detector to a chart recorder, make
the connections shown in the following table and figure.
Analog output connections to a chart recorder
Chart recorder connectors
2424 ELS detector (connector I)
Pen 1 +
Pin 1 signal out + (red)
Pen 1 –
Pin 2 signal out – (black)
Tip: For this connection, do not use the cable shield. Tape back the shield.
Tape back the shield to prevent it from causing a short circuit.
Analog output connections to a chart recorder
2424 ELS detector connector I
Red
Black
+ – + –
Y2
Y1
Chart recorder connectors
2-30
Setting up the Detector
1
2
3
4
5
6
7
8
9
10
+ Signal Out
− Signal Out
Ground
+ Auxiliary Out
− Auxiliary Out
+ Stop Flow
− Stop Flow
Ground
+ Switch Out
− Switch Out
Connecting to a Millennium data system using a busSAT/IN module
To send an integrator analog output signal (–0.1 to +2.1 V) from the detector
to a Millennium System (through a two-channel SAT/IN Module), make the
connections shown in the following table and figure.
Detector connections to the busSAT/IN module
SAT/IN module connector
2424 ELS detector (connector I)
CHANNEL 1
Pin 1 signal out + (white)
Pin 2 signal out – (black)
Analog output connections to the busSAT/IN module
2424 ELS detector connector I
Bus SAT/IN Module
Red
Black
Shield
1
2
3
4
5
6
7
8
9
10
+ Signal Out
− Signal Out
Ground
+ Auxiliary Out
− Auxiliary Out
+ Stop Flow
− Stop Flow
Ground
+ Switch Out
− Switch Out
Connecting injection trigger signals
The detector accepts the following injection trigger signals from a manual
injector:
•
Inject start signal from a contact closure signal with each injection
•
Auto zero signal to adjust the zero offset of the detector each time the
injector makes an injection
Each time the detector receives a signal from an injector, it performs the
corresponding auto zero or Inject Start function.
Making signal connections
2-31
To send an auto zero or chart mark signal from an injector to the detector,
make the connections shown in the following tables and figures.
Tip: The firmware defaults to auto zero on inject.
Inject start connections to an injector (pulse duration 0 to 10 seconds)
2424 ELS detector (connector II)
Injector connector
Pin 1, inject start in + (red)
Two spade lug terminal connectors
(both cables may be functionally
identical) or similar connectors.
Pin 2, inject start in – (black)
Inject start connections to an injector
2424 ELS detector connector II
1
2
3
4
5
6
7
8
9
10
2-32
Setting up the Detector
+ Inject Start In
− Inject Start
Ground
+ Lamp On
− Lamp On
+ Chart Mark In
− Chart Mark In
Ground
+ Auto Zero In
− Auto Zero In
Injector
Connecting the Waters column heater module
The detector can control one Waters column heater module through the EXT
port on the rear panel of the detector. The port is a standard, 9-pin, D-type
connector.
Waters column heater module
Making signal connections
2-33
2-34
Setting up the Detector
3
Operating the Detector
Contents:
Topic
Page
Starting up the detector
3-2
Using the keypad
3-7
Navigating the user interface
3-13
Preparing to start a run
3-15
Setting up a run
3-17
Configuring the detector
3-26
Operating the detector
3-30
Programming methods and events
3-34
Conserving lamp life
3-41
Changing chromatographic conditions
3-43
Shutting down the detector
3-44
Periodic maintenance
3-45
3-1
After you install the detector, you are ready to set it up and operate it either
as a standalone instrument or as part of a data system.
•
As a standalone instrument – Use the detector as a standalone detector
within a system, such as the Waters Alliance system, or with any
fluid-handling unit, injector, integrator, or data system. You can
program the front panel of the detector for standalone operation (see
page 3-31).
•
As part of an Empower System – Use the detector configured with an
Empower system to control and collect digital data. To configure the
detector with this system, follow the instructions in the Empower online
Help to specify parameters and control the detector.
•
As part of a MassLynx System – Use the detector configured with a
MassLynx system. To configure the detector with a MassLynx system,
follow the instructions in the MassLynx documentation to set the
parameters and control the detector.
Starting up the detector
Initializing the detector
Before you power-on the detector, turn the gas supply on. Ensure the power
cord connector that runs from the detector’s rear panel to the power source is
properly installed.
Tip: If you do not turn the gas supply on before you turn the detector power on,
the detector will display an error message.
To power-on the detector, press the On/Off switch located on the front
lower-right corner of the detector.
At startup, the detector beeps three times, displays the message “Booting
System... Please Wait,” and runs a series of startup confidence tests. The
initialization screens appear in the order shown in the following figure.
3-2
Operating the Detector
Detector startup screens
Tip: Service keypad inputs are coded for use only by Waters Service Engineers
for troubleshooting.
When initialization is complete, the detector displays the Home screen (see
page 3-7 and page 3-13).
Detector Home screen
Tip: For normal use, allow the detector to warm up at least 60 minutes before
operating.
Starting up the detector
3-3
If confidence tests fail
If one or more of the confidence tests fail during initial startup, the detector
behaves as follows:
•
Beeps
•
Displays an error message
•
For serious errors, displays the word “Error” in brackets (<Error>) in
place of the runtime light scattering units on the Home screen.
See “Startup error messages” on page 5-2, for a list of startup confidence tests
failures, error messages, and recommended recovery actions. Error messages
that can appear as you operate the detector and suggested corrective actions
are described in the table on page 5-17. See page 5-14 for hardware-related
causes of confidence tests failure during startup and their corrective actions.
Using the display
The detector employs a 128 × 64 bitmap graphic display and a 24-key
membrane keypad for the operator interface. After the startup confidence
tests have run successfully, the detector displays the Home screen.
Detector Home screen
Gas pressure
Light scattering
units
Lamp on/off
Shift on/off
Error or additional
function modes
Keypad lock/unlock
Gain
Local method
number/remote control
Nebulizer
temperature
display
Run time (minutes)
Next screen
Drift tube
temperature
display
Sticky diagnostics
on/off
You can recall the Home screen at any time by pressing HOME. At the first
use of the detector, the Home screen shows the default settings for the gain
and pressure.
3-4
Operating the Detector
The detector monitors performance in units of light scattering in real time,
allowing you to modify all the parameters discussed in the table in the next
section.
Detector Home and Message screen icons
The detector Home and Message screens display the icons or fields shown in
the previous figure. For a list of the ranges and defaults for these icons and
fields, see the following table.
Detector Home and Message screen icons
Icon or field Icon/field name
Function
Gain
Selects the gain setting. Regular field.
PSI
Gas pressure
Displays the current gas pressure and
allows you to enter a new gas pressure
value.
Neb °C
Nebulizer
temperature
Displays the current temperature of the
nebulizer.
Tube °C
Drift tube
temperature
Displays the current temperature of the
drift tube.
0.0
LS units
Displays the current light scattering
units.
Lamp on
Indicates the lamp is on.
Lamp off
Indicates the lamp is off.
Shift off
Blank = Shift off
Shift on
Indicates shift is on for one key press.
Starting up the detector
3-5
Detector Home and Message screen icons (Continued)
Icon or field Icon/field name
0.00
3-6
Function
Keypad unlock
Indicates unrestricted keypad entry.
Keypad lock
Indicates parameter changes are not
allowed; instrument is running a
method.
Sticky diagnostic
on
Indicates a sticky diagnostic is active
(see page 5-2).
Local method
number
Indicates that the detector is not
controlled by a data system. It displays
either a cursive “m” and the current
method number or an asterisk (*), which
indicates current conditions are not
stored as a method.
Remote control
Indicates that the detector is controlled
by a data system, and displays a remote
control icon.
Run time
Displays how many minutes elapsed
since you pressed Run or since an inject
start signal was received.
Next
Indicates that pressing Next brings you
to additional screens.
Message screen
icon
Indicates an error message.
Message screen
icon
Indicates a question.
Message screen
icon
Indicates a warning message.
Operating the Detector
Detector Home and Message screen icons (Continued)
Icon or field Icon/field name
Function
Message screen
icon
Indicates information is being displayed.
Message screen
icon
Indicates that you should standby.
Using the keypad
The detector’s 24 keys carry out these functions:
•
Full numeric entry – 10 digits plus a decimal point.
•
Global functions – Enter, Shift, CE (Clear Entry), Next, and ? (Help).
•
Navigation – and
move you to the left,
•
Direct access to specific screens – HOME, TEMP ×C, METHOD,
CONFIG (Configure), DIAG (Diagnostics), and TRACE.
•
Primary function keys – Chart Mark, Auto Zero, Run/Stop, and Next.
Primary function keys take effect immediately, with no further entry
required.
•
Secondary function keys – Reset, Lamp, Lock, System Information,
Contrast, Previous, Cancel, +/–, and Clear Field. You must enter
information into parameter fields and then press Enter.
(used for navigation only; pressing
to the right).
may also
Using the keypad
3-7
Detector keypad
?
Reset
HOME
Chart Mark
METHOD
Lamp
TEMP °C
CONFIG
Auto Zero
Run/Stop
1
2
3
System Info
Lock
Contrast
Previous
4
5
6
Next
7
8
9
Cancel
+/−
DIAG
Scale
TRACE
Shift
0
.
Clear Field
CE
Enter
Keys labeled in an all-capital-letter style (HOME, METHOD, TEMP °C,
CONFIG, DIAG, and TRACE) take you directly to a function from most
screens.
Select a numeric entry on a choice list or menu as follows:
•
For numeric entries from 1 to 9 (inclusive) on choice lists or menus,
specify the number corresponding to the desired item, then press Enter.
•
For the number 10, select 0, and then press Enter.
•
To go to the end of a choice list, press •.
•
For entries numbered 11 or 12, press the or key to scroll to the
desired item on the choice list, and then press Enter.
Tip: The and keys do not increase or decrease the values in numeric
fields. To change field entries, use the numeric keypad.
3-8
Operating the Detector
The following table explains the functions of the primary and secondary keys
on the detector keypad.
Keypad description
Description
Key
?
HOME
Chart Mark
Auto Zero
Reset
Run/Stop
Unshifted
Shifted
HOME – Displays the Home
screen containing icons and
the gas pressure, Gain,
Nebulizer, Drift Tube, and
Light Scattering fields.
? – Displays context-sensitive
Help when available.
Chart Mark – Causes a
momentary pulse to the
analog output and digital
data.
Auto Zero – Sets the light
scattering offset so that the
signal light scattering output
reads 0 LSU.
Run/Stop – Starts or stops
(pauses) the run clock. The
elapsed time appears near the
lower, right-hand corner of
the Home screen.
Reset – Resets the detector
run clock to zero minutes and
returns the detector to initial
conditions for the current
method.
and – Displays the active field, displaying a heavy border
on screens with entry fields (edit, check box, or choice list).
The arrow keys make a different field active. ( moves up or
leftward; moves down or rightward.) On screens with a
scrollable list, these keys move the highlight upward (toward
the beginning of the list) or downward (toward the end). Other
screens can have special instructions for using the and
keys (for example, the Display Contrast screen).
Using the keypad
3-9
Keypad description (Continued)
Description
Key
Previous
Next
METHOD
TEMP °C
CONFIG
DIAG
Scale
TRACE
Shift
3-10
Unshifted
Shifted
Next – Displays a screen with
additional options related to
the current screen. Repeated
pressing of this key returns
you to where you started. On
most screens where this key is
active, the NEXT arrow
appears in the lower,
right-hand corner of the
display.
Previous – Navigates through
the screens in reverse order
when the Next key is
available.
TEMP °C – Displays the
Temp °C screen, with which
you set the nebulizer power
factor for heating, turn
cooling on, and specify the
drift tube temperature.
METHOD – Displays the list
of options for creating and
clearing timed and threshold
events and storing, retrieving,
and resetting methods.
DIAG – Displays the list of
diagnostic routines.
CONFIG – Displays the first
Configuration screen.
TRACE – Displays the light
scattering monitor trace for
the channel.
Scale – Provides you with the
means to modify the display
range in the X (time) and Y
(LSU) dimensions when the
light scattering trace is
visible.
Shift – Enables the shifted functions (identified by the text at
the top of most keys). The shifted state is temporary (for one
keystroke only) and resets after the next keystroke.
Operating the Detector
Keypad description (Continued)
Description
Key
0-9
Unshifted
Shifted
0-9 – Enters the
corresponding number into a
current field.
Also positions the cursor at
the corresponding entry in a
list (0 = tenth item). Selects
the corresponding number
from a choice list.
0-9 – See descriptions for
specific, shifted numeric keys.
1 – See 0-9 above.
Lamp – Displays the lamp use
statistics for a currently
installed lamp, and provides
the means to turn the lamp on
or off. The current state of the
lamp is indicated by an icon
on the Home screen.
4 – See 0-9 above.
System Info – Displays
system information including
software version, checksum,
and instrument serial
number.
5 – See 0-9 above.
Lock – Enables or disables the
keypad lock feature when you
are on the Home screen. Use
the lock to prevent
inadvertent changes to
detector settings. The current
lock state is indicated by an
icon on the Home screen.
6 – See 0-9 above.
Contrast – Permits
adjustment of contrast
(viewing angle) of the liquid
crystal display.
Lamp
1
System Info
4
Lock
5
Contrast
6
Using the keypad
3-11
Keypad description (Continued)
Description
Key
Unshifted
Shifted
0 – See 0-9 above.
Cancel – Backs out of a
prompt without completing
the task. The word “Cancel”
appears as a cue in the lower,
right-hand border of the
message.
• – Enters a decimal point.
Also positions the cursor at
the last entry in a list.
+/– – Enters a
positive/negative sign. Use
this function to invert the sign
of the number in the active
field.
Cancel
0
.
+/−
Clear Field
CE
Enter
CE – Clears an editing change Clear Field – Blanks the
and returns the contents of a current entry field before you
field to its previous value.
enter the desired values.
Sets the value to a unique
word for some fields. For
example, in the voltage offset
diagnostic, you may either
enter a numeric offset value
or press CE to change it to
Off.
Enter – Completes the entry in an edit field. Also advances the
active field as if had been pressed (except after you edit the
wavelength on the Home screen). Press Enter to acknowledge
error messages and other prompts; the word “Enter” appears
as a cue in the lower, right-hand border of the message.
Tip: The detector does not have a polarity setting because the detector signal
measures and outputs either concentration/mass or temperature, which are
always positive numeric values.
3-12
Operating the Detector
Navigating the user interface
When operating the detector:
1.
Press Enter or and to navigate among editable fields. A heavy
border appears around the active field after you complete an entry.
2.
Press Enter to advance to the next active field.
3.
If you make an error, press CE (Clear Entry) to undo any changes and
return to the active entry field.
4.
An active field containing a choice list has a number to the right of the
field within the thick border. To display a choice list, press Enter, and
then take one of these actions:
•
Press the corresponding number key to select an item immediately.
•
Use
and
to scroll through the list, and then press Enter.
Tips:
•
If you know the number corresponding to the desired choice, you can
press that number without pressing Enter first.
•
The and keys do not increase or decrease numeric fields. To change
field entries, use the numeric keypad.
Navigating to and from the Home screen
Pressing HOME brings you to the Home screen from most screens. From the
Home screen, you can access the following secondary functions by pressing
Next:
•
Data rate and filter time constant
•
Enable/disable auxiliary switch output
•
LSU offset (data offset)
•
Maximum voltage output
•
Voltage offset
•
Enable/disable and select the auto zero function
Tip: The parameters you enter into the secondary function fields become part
of the current method conditions and are stored when you store the method.
See also: “Programming methods and events” on page 3-34.
Navigating the user interface
3-13
When you press Next, the detector displays four additional Home screens,
labeled 2 of 5, 3 of 5, 4 of 5, and 5 of 5.
Secondary functions of the Home screen
Press Next.
Light scattering Home screen
Press Next.
Auto zero on inject and gain;
enable keypad and event-in for
auto zero and chart mark
Data rate and time constant
Press Next.
Analog out
Press Next.
Press Next.
Data offset and voltage offset
3-14
Operating the Detector
Preparing to start a run
You must set up the detector before you can start a run to make light
scattering measurements with a detector. To start a run, you can press
Run/Stop or trigger the detector by means of the inject start terminals on the
rear panel. When you start a run, the detector performs an auto zero function
(if enabled).
Tip: The auto zero on inject function must be enabled (default) for the detector
to perform an auto zero.
Primary and secondary functions
Access the primary and secondary functions via the Home screen or by
pressing Next.
Caution: Changing the sensitivity (LSU-FS) setting affects only the 2-V
output. The digital output at the Ethernet connector remains
unchanged.
Gain – Controls the full-scale sensitivity of the detector by defining the gain
factor from 1 to 1000. Each gain setting has a linear relationship with the
actual light scattering signal.
Gas pressure – Gas pressure is controlled at the nebulizer by a pressure
regulator. This function monitors the condition of gas flow through the
nebulizer. For the high-flow and low-flow nebulizers, the maximum gas
pressure is 410 kPa (4.1 bar, 60 psi).
Filter time constant – Allows you to adjust the noise filter (time constant) to
achieve the optimum signal-to-noise ratio.
Primary and secondary function (method) parameters
Function
Units
Range
Default
Data rate
Hz
10, 20, 40, or 80 Hz
10 Hz
0 to 1000
0
Gain
Filter time
constant
sec
0 to 5.0 sec
1.0 sec
Sample
full-scale
LSU
0.1 to 2000.0 LSU
2000 LSU
Preparing to start a run
3-15
Primary and secondary function (method) parameters (Continued)
Function
Units
Range
Default
Sample
offset
mVDC
±2000 mVDC
0 mVDC
On, off
On
Lamp state
Gas
pressure
PSI
Off, 140 to 400 kPa (1.4 to
4.0 bar, 20 to 60 psi)
Off
LSU-FS
LSU-FS
10 to 2000
2000 LSU
Analog out
mV
10 to 2000
2000 mV
Auto zero on
inject
YES, NO
YES
Auto zero on
gain change
Disable, Zero, Maintain
Baseline
Maintain Baseline
Nebulizer
heater level
% Heating,
Cool, Off
Heater level, 0 to 100 or
Cool
Cool
Drift tube
heater
set-temp
°C
Off, 5 to 100 °C
Off
Drift tube
heater
alarm band
°C
±5 to 25 °C
±20 °C
Column
heater
set-temp
°C
Off, 5 to 150 °C
Off
Column
heater
alarm band
°C
±5 to 25 °C
±20 °C
Drift Tube, Nebulizer,
Column
Nebulizer
±2000 mV
0 mV
Off, 0 to 2000
Off
Temperatur
e source
Temp
output
offset
mV
Threshold
level
3-16
Operating the Detector
Primary and secondary function (method) parameters (Continued)
Function
Units
Range
Default
Threshold
switch mode
On, Off, Pulse,
Rectangular Wave
On
PULSE
sec
switch mode
period
0.1 to 60.0 sec
0.1 sec
RECT
sec
WAVE
switch mode
period
0.1 to 60.0 sec
0.2 sec
Number of
timed
events
0 to 50
0
Setting up a run
Start a run by pressing the Run/Stop key. Before starting a run, you must set
the detector operating parameters before data can be acquired.
To set up a run
1.
Press HOME to return to the Home screen.
2.
Set the drift tube heater temperature (see page 3-18).
3.
Set the gain and gas pressure (see page 3-19).
4.
Equilibrate the detector for about an hour.
5.
Make sure the stop flow output switch is reset (see page 3-21).
You need to program several other parameters, depending on the functions
you want to perform during a run. See page 3-15 for function descriptions,
fields, screen number, type of function, display units, allowable ranges, and
default settings for the Home screen and the secondary function screens. You
can view the properties of common chromatographic solvents in the table on
page 6-4.
Setting up a run
3-17
Setting the nebulizer and drift tube temperature
The nebulizer cooler cools the nebulizer tube wall providing a cold surface for
mobile phase eluent droplets to condense and flow to waste. This reduces the
amount of solvent that is sprayed into the drift tube in the vaporization
process and allows the drift tube temperature to run lower, therefore
increasing the sensitivity of semi-volatile samples.
The nebulizer heater, which is regulated by a heater power level setting, is
located in the same oven as the drift tube heater. The nebulizer heater allows
preheating of the sample solution to the set heater power level via a resistive
heat wrap that surrounds the nebulizer tube.
From the Nebulizer and Drift Tube Temperature Control Home screen, you
control the nebulizer heater, nebulizer cooler, and drift tube heater
temperature independently.
Tips:
•
The drift tube temperature must be sufficiently high to remove all
solvent; otherwise, detector noise occurs.
•
Too high a drift tube temperature can vaporize the sample and cause
loss of sensitivity.
•
The nebulizer temperature must be at least 5 °C below the drift tube
temperature.
To set the nebulizer and drift tube temperature
1.
Press Temp °C.
Result: The Nebulizer Heater/Cooler and Drift Tube Heater
Temperature Control Home screen appears.
Nebulizer and Drift Tube Temperature Control Home screen
3-18
Operating the Detector
2.
To toggle between Heating %, Cool, and Off, press CE when the “set”
field is active:
a.
If you selected Heating %, you must specify the nebulizer heater
power level setting in the set field. You can now view any nebulizer
temperature changes in the “cur. temp” field.
b.
If you selected Cool, thereby turning on the nebulizer cooler, you
cannot enter any values in the “set” field. However, you can view
any nebulizer temperature changes in the “cur. temp” field.
Tip: The Cool setting is the default.
c.
3.
If you selected Off, both the nebulizer heater and cooler are turned
off.
Specify the drift tube heater temperature in the “set” field.
Warning: The flash point is the lowest temperature at which a
flame can propagate through the vapor of a combustible material
to its liquid surface. A chemical’s flash point is determined by the
vapor pressure of the liquid. Only when a sufficiently high
concentration is reached, can a solvent vapor support combustion
(see page 6-4 for the flash points of common solvents).
Setting the gain and gas pressure
The gain setting controls the full-scale sensitivity of the detector by defining
the gain factor from 1 to 1000. Each gain setting relates linearly with the
actual light-scattering signal. The gas pressure setting monitors the condition
of gas flow through the nebulizer. For the high-flow and low-flow nebulizers,
the maximum gas pressure to 410 kPa (4.1 bar, 60 psi).
Caution: To avoid flooding the nebulizer and detector, Waters
recommends leaving the nebulizer gas flowing, at full or reduced rate,
when the mobile phase pump is shut down or the solvent flow is set to
zero.
Setting up a run
3-19
Tips:
•
Gas pressure should be high enough to prevent extended exposure time
of the sample in the drift tube area. Gas pressure that is too low could
cause higher-than-desired dispersion of particles and, consequently, loss
of sensitivity.
•
Gas pressure should be high enough to prevent the formation of large
particles that could cause detector noise.
To set the gain and gas pressure
1.
Press Home. The Gain and Gas Pressure Home screen appears.
Gain and Gas Pressure Home screen
2.
Enter the gain amount in the Gain field. Once you enter a gain amount,
the photomultiplier tube (PMT) is activated.
3.
To turn off the PMT, enter 0 in the Gain field.
4.
Specify a gas pressure of at least 450 kPa (4.5 bar, 65 psi) in the PSI
field to activate the gas valve.
Recommendation: When operating the instrument with an unlimited
gas source, such as a nitrogen generator, use a low gas flow when the
instrument is idle.
5.
To shut off the gas valve, enter 0 in the PSI field.
Caution: To prevent the detector from flooding, ensure that no
liquid is flowing into it when you specify a gas value of 0.
3-20
Operating the Detector
Setting the column heater module temperature
In the Column Heater Temperature Control Home screen, you control the
temperature of the column heater module (see page 2-33).
To set the column heater module temperature
1.
Press Temp °C, Next. The Column Heater Temperature Control Home
screen appears.
Column Heater Temperature Control Home screen
2.
Specify the column heater temperature in the “set” field.
Result: You can now view any changes in the current field.
Resetting the stop flow output switch
Warning: Fire and explosion hazard. Failure to connect the stop flow
output could cause the detector to flood.
A dedicated switch, “stop flow,” becomes active when a heater, gas flow, or
lamp failure occurs. Once the cause of the error is corrected, the stop flow
output switch can be reset by reactivating the faulty detector function or
pressing DIAG 1, Reset Flow & Diags.
Requirement: To automatically stop the chromatographic flow to the system
in the event of an error condition or hardware failure, the Stop Flow signal
must be connected to the chromatographic pump.
Setting up a run
3-21
Operating the trace and scale functions
The trace function allows you to display an LSU signal for the last n minutes
(up to 60) of detector operation.
•
Press TRACE to display the LSU signal acquired over the last 30
minutes by default. The LSU signal updates once every 20 seconds.
•
Press Scale (press Shift, TRACE) to display the scaled trace with T1
(ending time) displayed (-30 for the last 30 minutes) by default.
Change the ending time parameter to any number from 3 to 60. You can
use the Scale function to zoom in on a particular section of the trace.
To display the Scale parameters
1.
Press Scale.
2.
Press Next to display T2 (starting time). The default is 0.
3.
Press Next again to display LSU1 (starting or low light-scattering
signal). The default is auto-scaled.
4.
Press Next again to display LSU2 (ending or high light-scattering
signal). The default is auto-scaled.
By entering appropriate times and light scattering numbers in the four
scaling parameter boxes, you can zoom in on one section of the current
light scattering trace.
3-22
•
For LSU1 and LSU2, press CE to reset to auto-scaled.
•
T1 represents the left-hand side of the trace, or ending time, to be
displayed. The default is -30.
•
T2 represents the right side of the trace, or starting time. The
default is 0.
Operating the Detector
The following screen shows a 30-minute trace of simulated peaks.
30-minute scaled trace of continuous, simulated peaks, with T1 changed
to -30
LSU2
LSU1
T1
T2
The following screen shows a 5-minute, scaled trace (or zoom) of the 30 screen
shown above. T1 is changed to -5. T2 is changed to 0. LSU1, and LSU2 remain
as auto-scaled.
Scaled trace for 5 minutes changing T1 to -5
LSU2
LSU1
T1
T2
The following screen shows a 30-minute, scaled trace similar to that shown in
the first screen, with the starting light scattering or LSU1 changed from
auto-scaled to -10. T1 remains at -30, T2 at 0.
Scaled trace for 30 minutes changing LSU1 to -10
LSU2
LSU1
T1
T2
Setting up a run
3-23
The following screens show a 60-minute trace on Channel A scaled to the last
15 minutes of data. T1 is changed to -15.
Scaled trace changing T1 to -15
As you modify the output using the scale function, the trace function
continues to display the detector output in real time on either or both
channels.
Setting the data rate
This function allows you to set the data rate to 10, 20, 40, or 80 Hz.
To set the data rate
1.
From the Home screen, press Next. The data rate and time constant
function screen appears.
Data rate and time constant function screen
2.
Use Enter and the numeric keypad or
data rate.
and
to select the appropriate
Setting the filter time constant
This function allows you to adjust the noise filter (time constant) to achieve
the optimum signal-to-noise ratio. The detector uses a Hamming filter to
process the sample’s signal. The filter time constant can be adjusted from 0 to
5.0 seconds in 0.1 increments. When the time constant value is set to zero, the
Hamming filter is disabled.
3-24
Operating the Detector
Setting the switch output
The detector has a general purpose switch output that can be controlled
manually, by run time, or by sample level. On the third Home screen, it
displays the current setting of the method and the switch output. Changing
the initial value, On or Off, also changes the current state of the switch
output.
For information on programming the switch output by time or by level, see
page 3-37.
Setting the analog signal output
The fourth Home screen contains the sample signal analog output
parameters, the units full scale value, the analog output full-scale value, and
its offset. These settings only affect the sample signal’s analog output, not the
digital data processed by the data system using the Ethernet communications
data link.
The units full scale value defines the maximum signal value that can be
represented using the analog output. Likewise, the analog output full-scale
value defines the maximum output voltage value that will be used to
represent the units full-scale value. For example, using the default values, the
units full-scale value of 2000 is represented as a 2000-mV output on the
analog outputs. Reducing the units full-scale value to 1000 means that the
2000-mV analog output will represent a 1000-LSU signal. This also increases
the analog output sensitivity from 1 LSU/mV to 0.5 LSU/mV.
Changing the analog output full-scale value reduces the sensitivity of the
analog output. For example, changing the analog output full-scale value to
1000 mV reduces the analog output sensitivity from 1 LSU/mV to 2 LSU/mV.
The analog output sensitivity can be improved by also reducing the units
full-scale value to 1000 LSU to obtain a 1 LSU/mV sensitivity.
The offset data field provides a way to raise the analog output signal to meet
the detection signal requirements of some data loggers.
Setting auto zero options
The fifth Home screen contains options for setting various auto zero options,
either when the gain is changed or at the start of a run (on inject).
Setting up a run
3-25
When the gain amount is modified from the front panel, a downloaded
method, or a timed event, the following can occur:
•
The auto zero adjustment can be recalculated. This can be done based on
the detector’s baseline signal, or to no signal (zero).
•
The auto zero adjustment can be reset to zero.
Based on the setting of the On Inject check box at the start of a run, the
detector either evaluates the auto zero adjustment based on no signal (zero),
or it resets the auto zero adjustment to zero.
Configuring the detector
Press CONFIGURE (press Shift, DIAG). The first of four Configuration
screens appears.
Tip: Other functions, such as specifying event inputs and enabling pulse
periods, are also available in the Configuration screens.
Configuration screens
3-26
Configuration screen 1 of 4
Configuration screen 2 of 4
Configuration screen 3 of 4
Configuration screen 4 of 4
Operating the Detector
Configuring event inputs
You can also use CONFIGURE to edit event input settings and specify
switched output settings.
Four editable entry fields appear on the first Configuration screen: Inject,
Chart mark, Auto zero, and Lamp.
•
Inject – You can specify the Inject input to signal the start of a run. This
event resets the runtime clock and applies initial method conditions
immediately:
–
High – Start run when contact closure changes from Off (open) to
On (closed).
–
Low – Start run when contact closure changes from on (closed) to off
(open).
–
Ignore – Do not respond to inject-start input.
Use Enter and the numeric keypad or
entry.
•
to select the appropriate
Chart mark – You can specify the input to create a chart mark on signal
output. To determine the response of the channel, use the chart mark
function.
–
High – Create chart mark(s) when contact closure changes from Off
(open) to On (closed).
–
Low – Create chart mark(s) when contact closure changes from On
(closed) to Off (open).
–
Ignore – Do not respond to chart mark input.
Use Enter and the numeric keypad or
entry.
•
and
and
to select the appropriate
Auto zero – You can configure the auto-zero input to auto zero light
scattering readings on signal output. To determine the response of the
channel, use the auto zero function.
–
High – Auto zero the channel when contact closure changes from Off
(open) to On (closed).
–
Low – Auto zero the channel when contact closure changes from On
(closed) to Off (open).
–
Ignore – Do not respond to auto-zero input.
Configuring the detector
3-27
Use Enter and the numeric keypad or
entry.
•
and
to select the appropriate
Lamp – You can configure the lamp input level to ignite or extinguish
the tungsten lamp on or off from an external device as follows:
–
High – Ignite the lamp on when contact closure is On (closed).
–
Low – Ignite the lamp on when contact closure is Off (open).
–
Ignore – Do not respond to lamp input.
Use Enter and the numeric keypad or
entry.
and
to select the appropriate
The default for Inject, Chart mark, and Auto zero is low; the default for the
Lamp parameter is Ignore.
Tip: Controlling the lamp state by the event input overrides keypad control.
Configuring stop flow output
Warning: Fire and explosion hazard. Failure to connect the stop flow
output could cause the detector to flood.
The stop flow output is an output switch. Its default active state is On, which
can be changed to Off on the second configuration screen.
When the active state is Off, the stop flow output is normally On, until a stop
flow error condition occurs. At that point, the stop flow output is changed to
the Off state.
Requirement: To automatically stop the chromatographic flow to the system
in the event of an error condition or hardware failure, the Stop Flow signal
must be connected to the chromatographic pump.
Setting pulse periods
You use the third configuration screen to set pulse width or to activate a
rectangular wave on the switch.
3-28
•
Single pulse (in seconds) – If the switch is programmed to generate a
pulse as a timed or threshold event, then the period of the signal (single
pulse width) is as specified in this field (range is 0.1 to 60 seconds).
•
Rectangular wave (in seconds) – If the switch is programmed to initiate
a rectangular wave as a timed or threshold event, then the period of the
Operating the Detector
signal (the width of one pulse period in a rectangular wave or pulse
train) is as specified in this field (range is 0.1 to 60 seconds).
The following figure shows the difference between a single pulse and a
rectangular wave.
Setting the pulse period or signal width on the switch
n seconds
Single pulse
n seconds
Rectangular wave
Selecting the type of nebulizer
You use the fourth configuration screen to select the appropriate nebulizer for
your flow rate range:
•
High flow – 0.3 to 3 mL/minute
•
Low flow – .05 to .5 mL/minute
Setting the display contrast
Adjust the contrast of a displayed screen using the Display Contrast function.
When you press Contrast (press Shift, 6), the Display Contrast screen
appears.
Display Contrast screen
Press
and
to adjust the contrast of the display, and then press Enter.
Configuring the detector
3-29
Displaying system information
Press System Info (press Shift, 4) to display information about the detector,
including the serial number, the software version number with checksum, and
the version date, if applicable.
Press Enter to return to the Home screen.
Example of a system information screen
Tip: See the detector release notes for the actual checksum and version.
Using help
The detector offers limited context-sensitive Help. When you press ? (press
Shift, HOME) from a point in the program with which a Help screen is
associated, the screen appears. If Help is unavailable for the function you are
working on, you do not receive a response.
Example of a Help screen
Press Enter to return to the previous screen.
Operating the detector
Tip: If you are operating the detector under the control of an external data
system, you can program any parameters not controlled by the external data
system at the front panel of the detector, before the external system takes
control.
3-30
Operating the Detector
Standalone operation
When using the detector as a standalone instrument, you can store as many
as 10 methods containing up to 50 timed events each. An asterisk in the
method number field on the detector Home screen indicates current
conditions, not a stored method. See page 3-34 for information on how to store
a method.
Auto-optimizing gain and LSU-FS
You must select a gain setting for the photomultiplier tube before a
chromatographic injection. The proper setting maximizes the signal on the
internal analog-to-digital converter without exceeding the signal’s maximum
potential limit. If the gain is too high, the signal can overload the signal
collection electronics. If the gain is too low, sensitivity is reduced, and the
signal-to-noise ratios are degraded.
Using the Auto Gain diagnostic, you run a single, trial chromatogram after
which the detector suggests ideal gain values. If you run timed-event gain
changes, the detector adjusts the values to determine the ideal gain setting for
each critical timed-event region. At the end of the run, a report of the ideal
gain values appears on screen. The report is based on a computation that
maximizes use of one-half the range of the electronics, so a 2× margin
accommodates any variations in signal intensity. Based on this report, you
adjust the gain values in the method, including its timed event table, to
optimize the performance of the method.
Besides the ideal gain settings, the detector also monitors the maximum
signal level throughout the entire run. It recommends a minimum LSU-FS
value, which applies to the entire chromatogram and is displayed when you
use the analog outputs during data collection. This value is also computed
assuming a 2× margin for error.
Method optimization
Before using the Auto-Optimize diagnostic, a chromatogram of the sample
should be run to establish the approximate retention time of the peaks of
interest. A timed event table should be constructed, consisting of gain-change
timed events at times corresponding to sections of baseline between the peaks.
For example, if the RT of peak 1 is 0.9 minutes, and the RT of peak 2 is 1.75
minutes, a gain change timed event should be entered at 1.5 minutes. The
goal is to provide retention time demarcation points at which a gain change
could be tolerated without disrupting the integration of peaks in the
Operating the detector
3-31
chromatogram. The minimum requirement for the Auto Gain diagnostic to
function is for you to set the initial conditions. No timed events are necessary.
This means, however, that the detector recommends only one gain value
setting for all of the peaks in the chromatogram, with no segregated peak
region optimization.
Gain optimized chromatograph
LSU
Region 1
0.0
Gain: 10
Region 2
1.5
Gain: 1000
Region 3
2.0
Gain: 5
Time
4.0
Recommended method development approach
You should use a method with two timed event changes to optimize this
chromatogram. The first gain setting change could occur at 1.5 minutes, just
before the small peak best detected at a gain of 1000. The next change would
occur at 2.0 minutes. You need not to be concerned with the initial gain
setting. The only requirement for the first timed event is that some gain
3-32
Operating the Detector
setting takes place. An initial method table could resemble what is shown in
the following table.
Method development
Event time
Event
Initial (0.0)
Gain = 10
1.5
Gain = 100
2.0
Gain = 10
You can develop methods by entering the method information into the
detector using the keypad or by retrieving a previously created method from a
stored memory location.
If you are using Empower software, you must enter the method into the
detector’s Instrument Method Editor. Under Empower control, the method is
downloaded to the detector when you make an injection or if the method is set
up.
Once you program the method into the detector (or Empower editor), press
DIAG, and then press 3 Enable Auto Gain. The Auto Gain enabled screen
appears.
Selecting the Auto Gain diagnostic
The diagnostic will run during the next injection. The sticky diagnostic
(wrench) icon appears on the front panel, and <Auto Gain> appears in the
emission field.
Operating the detector
3-33
Auto Gain diagnostic screen
Auto Gain diagnostic
Sticky diagnostic icon
You can start the injection via a trigger from an injector input to the Inject
Start event input on the rear panel. You can also press Run/Stop on the front
panel while the sample is injected into the fluid stream.
Requirement: Synchronize the start trigger with the chromatography so that
the timed events occur at the proper times relative to the peaks.
Select Make Injection if you are running under Empower control, or start the
injection through other devices (such as the Alliance 2695 Separations
Module).
When the run is completed, press Run/Stop, Reset. The detector displays a
recommended LSU-FS value and a table of gain values.
Gain values
Event time
Best gain
0
10
1.5
1000
2.0
5
Programming methods and events
Overview of methods
The detector allows the storage and retrieval of up to 10 methods. The
detector refers to the stored methods as 1 through 10. If you are operating
using a stored method, the method number appears on the Home screen. An
asterisk in the method number icon indicates that the current conditions are
not stored.
If you edit a parameter, you are editing the current conditions (Method *). You
may store the method in one of the 10 available method storage slots, or you
3-34
Operating the Detector
can replace the current method with one of the methods previously stored.
When you retrieve a previously stored method, you replace the existing
method conditions with those of the stored method.
The method number displayed on the Home screen is that of the retrieved
method until you make a change. Any parameter change alters the current
conditions so that the original recalled method is no longer in effect, causing
the method number to change to an asterisk.
The operating parameters at the time of system shutdown are restored on
startup. However, any timed events or thresholds associated with the method
are deactivated when power is restored. On startup, you always see an
asterisk inside the method icon on the Home screen.
When the detector is operating under remote control, the remote icon appears.
Programming timed events
You can program up to 50 timed events, to the nearest 0.01 minute. As you
enter timed events, each new event appends to the end of the timed event list.
You can enter a time that is not in sequence with the events entered
previously, and the timed event list is sorted when you press Next. The
detector allows programming of the timed events listed in the following table.
Timed event parameters
Number
Event
Range
Default
1.
Gain
0 to 1000
Off
4.
Chart mark
5.
Auto zero
6.
Lamp
On, Off
Off
7.
Auxiliary
switch
On, Off, Pulse, Rect wave
Off
8.
Gas
pressure
140 to 410 kPa (1.4 to
4.1 bar, 20 to 60 psi)
Off
9.
Threshold
0 to 2000 LSU
Off
Programming methods and events
3-35
To program a new timed event
1.
Press METHOD (press Shift, TEMP °C). The Method choice list appears.
Method choice list
2.
Press 1 Timed events. An active field for entering the time of the event
appears.
3.
Enter the time for the event. When you begin entering the time,
additional fields appear.
Timed events screen
4.
Press Enter to enter the time. To advance to the “set” field (Events
choice list), press .
5.
Press Enter again to display the choice list, or, if you know the event
number, press the number for the event you are programming.
6.
Enter the appropriate selection in the “to” field, if the field appears.
7.
Press Next to advance to a new timed event.
8.
To delete a timed event, press CE when the time field is active to change
it to Off.
9.
Press HOME to return to the Home screen, and then press Run/Stop to
start the method.
10. Press Reset (press Shift, Run/Stop) to reset the run clock to 0.
3-36
Operating the Detector
If the detector is configured with the 700 Series Autosampler or another
external device, the inject start signal programmed from that device
starts the method.
Tip: If you are working in real time under current conditions (method *),
and a power failure or shutdown occurs, you lose all timed or threshold
events if you did not store them as a method (see page 3-38).
Programming threshold events
You can program threshold events to control the auxiliary switch.
Below the specified threshold, the switch is set as shown in the table, below.
You can program the switch parameters listed in the table.
Threshold events “to” parameters
Number
Set to
Below threshold
switch state
1.
On
Off
10.
Off
Off
11.
Pulse
Off
12.
Rect wave (rectangular
wave)
Off
To define the pulse period, or the frequency of a wave, see page 3-26.
To program a threshold event
1.
Press METHOD (press Shift, TEMP °C) on the detector keypad. The
Method choice list appears.
2.
Press 2 Threshold events. An active field (LSU) for entering the
threshold appears. When you begin to enter a number in the LSU field,
additional fields appear.
Tip: The threshold selection provides the means to modify this initial
Threshold value as a timed event.
Programming methods and events
3-37
3.
Press Enter to advance to the “set” field, or press
among the three fields.
and
to move
Threshold events screen
4.
When the “set” field is active, press Enter to display the threshold events
choice list, or press the number corresponding to the event you are
programming.
5.
When the “to” field is active, press Enter to display the switch state
options, or press the number corresponding to the threshold parameter
you are programming.
Storing a method
A method consists of all programmable parameters on the Home and
associated screens, as well as timed and threshold events. You can store the
current method by selecting a location from 1 to 10.
To store a method
1.
Press METHOD. The Method choice list appears.
2.
Press 4 Store method *. A method number field appears.
Tip: No warning message appears when the method number you select is
already used by a previously stored method. When you enter a number
and press Enter, the current method conditions are stored, overwriting
any previous method stored in the same slot.
Method number field
3-38
Operating the Detector
3.
Enter a number from 1 to 10 (inclusive), and press Enter. A brief
message (“Storing * as method n”) appears. When the display returns to
the Method choice list, the method number you selected appears within
the method icon. That method remains active until you retrieve another
method or reset the detector to default conditions (Method *).
Retrieving a method
To retrieve a previously stored method
1.
Return to the Method choice list by pressing METHOD.
2.
Press 3 Retrieve a method. The last method number stored or retrieved
appears in the method number slot box.
3.
Specify the number of the method you wish to retrieve and press Enter.
Result: A brief message (“Retrieving method n”) appears.
4.
When the display returns to the Method choice list, the method number
you specified appears within the method number icon.
Viewing events within a method
To view timed and threshold events that make up a stored method
1.
Retrieve the method. Once you enter the method number to retrieve, the
Method choice list appears with the method number displayed within
the method number icon.
2.
Press 1 to view the timed events or 2 to view the threshold events of the
method.
3.
If you change a timed or threshold event within a method, the asterisk
appears (Method *) indicating that the method (*) is no longer the same
as the stored method you retrieved in step 1. You can then store the
method containing the altered event(s) in the same storage slot.
Resetting a method
Resetting a stored method is a two-step process. First, you reset the current
conditions to the defaults; and then you save the defaults in one of the storage
locations. The table on page 3-15 lists the parameter default settings.
Programming methods and events
3-39
To reset one or more methods
1.
Press METHOD. The Method choice list appears.
2.
Press 5 Reset method *. A message screen appears.
Reset method message
3.
If you press Enter
•
all timed events are deleted.
•
all threshold events are disabled.
•
all other operating parameters of the method (LSU-FS, etc.) are set
to defaults.
If you press Cancel (press Shift, 0), the Method choice list appears.
Tip: To prevent losing the current conditions before you clear the
method, store them in one of the available storage slots. When you clear
the storage slots, you can restore the previous conditions.
4.
Press 4 Store method, and enter a storage location number.
5.
To clear other stored methods, repeat step 4.
6.
When you return to the Home screen by pressing HOME, the method
number icon displays an asterisk.
Clearing events
You may want to clear only timed and threshold events without resetting any
other operating parameters.
To clear active events
1.
3-40
Return to the Method choice list by pressing METHOD.
Operating the Detector
2.
Press 6 Clear events. A message screen appears.
Clear events message
3.
If you press Enter
•
all timed and threshold events in the method are cleared.
•
all other operating parameters of the method (LSU-FS, etc.) are
unaffected.
If you press Cancel (press Shift, 0), the Method choice list appears.
4.
When you return to the Home screen by pressing HOME, the method
number icon displays an asterisk.
Conserving lamp life
To conserve the tungsten lamp, extinguish it while allowing the detector to
remain powered-on. You can do this in three ways:
•
Manually
•
By programming a timed event
•
By programming the lamp itself via the external contact closure
Tip: If you are operating the detector remotely, you can program the controller
to extinguish the lamp without using the detector’s front panel.
Recommendation: Regardless of whether you program the lamp to shut off or
extinguish it manually, ensure that the “lamp off time” value is greater than 4
hours.
To manually extinguish and reignite the lamp, use the Lamp key. When the
lamp is extinguished, the Home screen displays the words “Lamp off” and the
lamp icon appears with an X through it.
Conserving lamp life
3-41
Press the Lamp key (press Shift, 1) for these purposes:
•
Extinguish the lamp or ignite it manually
•
Display the number of times the lamp has ignited
•
Display the hours and minutes the lamp has been ignited
–
during the current run
–
since installation
To turn off the lamp manually from the detector front panel
1.
Press Lamp (press Shift, 1). The lamp control screen displays this
information:
•
The amount of time, in hours and minutes, the lamp has been
ignited since the most recent startup
•
The total time the lamp has been ignited since its installation
•
The number of times the lamp has been ignited
Lamp control screen
2.
Press Lamp (press Shift, 1) again to extinguish the lamp. The Home
screen appears with an X through the lamp indicator icon and the words
“Lamp off”.
Lamp off/on sequence
Lamp off indicator
3-42
Operating the Detector
Lamp on indicator
To ignite the lamp manually (when the lamp icon on the Home screen
has an X)
1.
Press Lamp (press Shift, 1). The lamp control screen appears again with
0 hours and 00 minutes in the “Lamp has been on” field.
2.
Press Lamp (press Shift, 1) again to turn the lamp on. Once the lamp is
ignited, the Home screen appears with the X removed from the lamp
icon.
You can conserve lamp life by programming its automatic operation via a
timed event method.
To program the lamp to turn on or turn off, select the Timed events option in
the Method choice list, or program the lamp through one of the external
contact closures.
•
See page 3-15 and page 3-34 for more information on programming lamp
operation using a timed event.
•
See page 3-27 for more information on programming the lamp through
the external contact closure.
Changing chromatographic conditions
Requirement: When the detector is plumbed to the chromatographic system,
and the buffer type or pH of the mobile phase is changed, you must remove the
previous buffered mobile phase from the fluid path.
Caution: Failure to remove all traces of buffered mobile phase from the
fluid path before changing new conditions could result in buffer
precipitation and consequent clogging of the nebulizer.
To change chromatographic conditions
1.
Set the drift tube temperature at the appropriate desolvation
temperature setting.
Tip: 50 °C (122 °F) is an appropriate desolvation temperature for most
solvents.
2.
To remove mobile phase from the fluid path of the detector, replace the
buffered mobile phase with 100% HPLC-quality water, and flush the
system for 10 minutes at 3 mL/min.
Changing chromatographic conditions
3-43
3.
If the new mobile phase is miscible with water, replace the 100%
HPLC-quality water with new mobile phase, and equilibrate the system
for 10 minutes at 3 mL/min.
Shutting down the detector
Before you power-off the detector, you must remove any buffered mobile phase
present in the fluid path.
Caution: To avoid damaging the column, remove all buffers from it
before you shut down the detector.
To shut down the detector
1.
Remove all buffers from the column and detector.
2.
Flow nonbuffered mobile phase through the system.
3.
Turn off the pump.
4.
Allow the nebulization gas to flow through the detector for a few
minutes to drain the evaporation tube and detection chamber.
5.
Stop the gas flow.
6.
Power-off the power to the detector.
Tips:
3-44
•
The last set of selected parameters is retained in memory and becomes
the default condition when the detector is powered-on again.
•
It is not harmful to leave the detector powered-on overnight when the
instrument is not in use. To increase the life of the lamp, extinguish it.
•
Do not allow solvent flow to continue if no gas flow is present. However,
you may let the nebulizer gas flow at full or reduced rate even in the
absence of solvent flow (that is, when the mobile phase pump is turned
off or the flow rate is set to zero).
Operating the Detector
Periodic maintenance
To maintain the best performance from your detector, remove the mobile
phase from the fluid path once each week.
To perform periodic maintenance
Tip: To avoid damaging the column, remove it before you remove the
mobile phase from the fluid path.
1.
Set the drift tube temperature at the appropriate desolvation
temperature setting.
Tip: 50 °C (122 °F) is an appropriate desolvation temperature for most
solvents.
2.
Replace the buffered mobile phase with 100% HPLC-quality water, and
flush the system for 10 minutes at 3 mL/min.
Periodic maintenance
3-45
3-46
Operating the Detector
4
Maintaining the Detector
Contents:
Topic
Page
Contacting Waters technical service
4-2
Maintenance considerations
4-2
Replacing the lamp cartridge
4-3
Replacing the nebulizer
4-6
Cleaning the nebulizer ultrasonically
4-9
Cleaning the drift tube
4-12
Servicing the vapor trap
4-13
Replacing fuses
4-14
Cleaning the instrument’s exterior
4-15
4-1
Contacting Waters technical service
If you are located in the USA or Canada, report malfunctions or other
problems to Waters Technical Service (800 252-4752). Otherwise, phone the
Waters corporate headquarters in Milford, Massachusetts (USA), or contact
your local Waters subsidiary. The Waters’ Web site includes phone numbers
and e-mail addresses for Waters locations worldwide. Visit www.waters.com.
When you contact Waters, be prepared to provide this information:
•
Detector serial number
•
Problem symptom(s)
•
Nebulizer and drift tube temperatures
•
Heater set points and levels
•
Flow rate
•
Filter setting
•
System operating pressure
•
Gas pressure
•
Solvent(s)
•
System configuration (other components)
For complete information on reporting shipping damages and submitting
claims, see the document Waters Licenses, Warranties, and Support Services.
Maintenance considerations
Perform the procedures in this chapter when you discover a problem with a
25X5 QGM component or during preventive maintenance. For information
about isolating problems in the 25X5 QGM, consult the console’s online Help.
Safety and handling
Observe these warning and caution advisories when you perform maintenance
operations on your 25X5 QGM.
4-2
Maintaining the Detector
Warning: To prevent injury, always observe Good Laboratory Practices
when you handle solvents, change tubing, or operate the system. Know
the physical and chemical properties of the solvents you use. See the
Material Safety Data Sheets for the solvents in use.
Warning: Avoid electric shock:
• Do not open the detector cover. The components within are not
user-serviceable.
• Power-off and unplug the detector before performing any
maintenance operation on the instrument.
Caution: To avoid damaging electrical parts, never disconnect an
electrical assembly while power is applied to the detector. To completely
interrupt power, set the module’s power switch to “off”, and then unplug
the power cord from the AC outlet. Wait 10 seconds thereafter before
you disconnect an assembly.
Spare parts
Replace only parts mentioned in this document. For spare parts details, see
the Waters Quality Parts Locator on the Waters Web site’s Services & Support
page.
Replacing the lamp cartridge
Recommendation: Because lamp alignment is critical to proper detector
operation, it is recommended that only Waters pre-aligned lamp cartridges be
used.
Required Materials
•
#2 Phillips screwdriver
•
Lamp cartridge
To replace the lamp cartridge
1.
Power-off the detector, and disconnect the power cable from the rear
panel.
Replacing the lamp cartridge
4-3
Alternative: To save time, leave the detector powered on for 15 minutes
after you power-off the lamp. Doing so will allow the fan to blow cool air
on the lamp, cooling it faster.
Warning: The lamp and lamp housing can be hot. Wait 30 minutes
(or 15 minutes with the fan running) after powering-off the
detector for these components to cool before touching them.
2.
Allow the lamp to cool for 30 minutes (or 15 minutes with the fan
running), and then remove the left-front panel cover.
3.
Using a Phillips screwdriver, completely loosen the two captive screws
and pull the assembly out slightly to relieve stress on the lamp
connector wires.
Captive screws
Lamp connector
wires
Lamp connector
TP02726
4-4
Maintaining the Detector
Warning: To avoid electric shock, power-off and unplug the
detector before detaching the lamp power connector from the
detector.
Caution: To avoid damaging the detector’s electronics, power-off
and unplug the detector before detaching the lamp power
connector from the detector.
4.
Disconnect the lamp connector from the front panel.
Lamp connector
5.
Remove the lamp cartridge assembly and replace it with a new one.
6.
Reconnect the lamp connector.
Caution:
• Do not touch the new lamp with your bare fingers. Skin oils can
greatly reduce the lifetime of the lamp. If fingerprints do get on
the lamp, remove them with a lint-free tissue saturated with
ethanol.
• To avoid misaligning the lamp, do not touch the bulb height
adjustment lever.
7.
Push the assembly back in, and tighten the two captive screws with a
Phillips screwdriver.
Replacing the lamp cartridge
4-5
8.
Replace the left-hand, front panel cover.
9.
Power-on the detector, and enter the new lamp information (see
page 5-8).
Replacing the nebulizer
Required material
Nebulizer
To replace the nebulizer
1.
Stop the liquid flow.
2.
Power-off the detector, and disconnect the power cable from the rear
panel.
Warning: To avoid burn injuries, do not touch the nebulizer until
its temperature cools to less than 30 °C, as displayed on the
detector home screen. If its temperature exceeds 30 °C, let the
nebulizer cool in one of two ways before touching it:
• Wait 30 minutes after powering-off the detector.
• Wait 10 minutes after specifying Cool in the Nebulizer and
Drift Tube Temperature Control Home screen (see page 3-18).
3.
4-6
Remove the left-hand, front panel cover.
Maintaining the Detector
4.
If a column or second detector is connected to the system, disconnect the
solvent inlet tubing from the front of the nebulizer as follows:
a.
Use a 5/16-inch wrench to loosen the compression screw that holds
the inlet tubing in place.
5/16-inch wrench
Compression screw
b.
5.
Remove the solvent inlet tubing from nebulizer.
Push in the quick-disconnect tubing fitting on the right-hand side of the
nebulizer, and pull out the gas inlet tubing.
Quick disconnect fitting
Gas inlet tube
Replacing the nebulizer
4-7
6.
Push in and turn the nebulizer counterclockwise so that the
quick-disconnect tubing fitting is at the twelve o’clock position. Then
remove it from the nebulization chamber.
Quick-disconnect tubing fitting
at twelve o’clock position
7.
4-8
Remove the packing ring from the old nebulizer, and slide it onto the
new nebulizer. If the old packing ring is damaged, replace it with a new
one.
Maintaining the Detector
8.
Align the two pins inside the desolvation chamber with the grooves in
the new nebulizer. The quick-disconnect tubing fitting will be at the
twelve o’clock position.
Pins inside the desolvation chamber
Pins
9.
Push the nebulizer into the nebulization chamber, and turn it clockwise
until it snaps into place.
10. Insert the gas inlet tubing into the quick disconnect-tubing fitting on the
right side of the nebulizer.
11. Reconnect the solvent inlet tubing.
12. Power-on the detector.
See also: “Selecting the type of nebulizer” on page 3-29.
Cleaning the nebulizer ultrasonically
To clean the nebulizer
1.
Stop the liquid flow, and remove the solvent inlet line.
Cleaning the nebulizer ultrasonically
4-9
2.
Power-off the detector, and disconnect the power cable from the rear
panel.
Warning: To avoid burn injuries, do not touch the nebulizer until
its temperature cools to less than 30 °C, as displayed on the
detector home screen. If its temperature exceeds 30 °C, let the
nebulizer cool in one of two ways before touching it:
• Wait 30 minutes after powering-off the detector.
• Wait 10 minutes after specifying Cool in the Nebulizer and
Drift Tube Temperature Control Home screen (see page 3-18).
3.
Remove the left-hand, front panel cover.
4.
If a column or second detector is connected to the system, disconnect the
solvent inlet tubing from the front of the nebulizer as follows:
a.
Use a 5/16-inch wrench to loosen the compression screw that holds
the inlet tubing in place.
5/16-inch wrench
Compression screw
b.
4-10
Remove the solvent inlet tubing from the nebulizer.
Maintaining the Detector
5.
Push in the quick-disconnect tubing fitting on the right-hand side of the
nebulizer, and pull out the gas inlet tubing.
Quick disconnect fitting
Gas inlet tube
6.
Push in and turn the nebulizer counterclockwise so that the
quick-disconnect tubing fitting is at the twelve o’clock position. Then
remove it from the nebulization chamber.
Quick-disconnect tubing fitting
at twelve o’clock position
7.
Remove the packing ring from the nebulizer.
8.
Place the nebulizer upright in a beaker so that it stands up.
Cleaning the nebulizer ultrasonically
4-11
9.
Pour 100% HPLC-grade water or a mixture of organic solvent
compatible with your mobile phase into the beaker, but do not submerge
the gas inlet fitting or solvent inlet fitting in the liquid.
Solvent inlet fitting
Gas inlet fitting
Do not fill past here
10. Place the beaker in an ultrasonic bath for 10 to 15 minutes.
11. Remove the beaker from the bath.
12. Remove the nebulizer from the beaker.
13. Insert the gas inlet tubing into the quick-disconnect tubing fitting on the
right side of the nebulizer, and place the nebulizer in a dry beaker so
that it stands up.
14. Run gas at 410 kPa (4.1 bar, 60 psi) for 5 to 10 minutes through the
nebulizer to blow out any excess liquid.
15. Reinstall the nebulizer (see page 2-12).
16. Reset the system to operating conditions and evaluate chromatography.
Cleaning the drift tube
To clean the drift tube
4-12
1.
Increase the nebulizer power to 75%.
2.
Set the drift tube temperature to 100 °C.
Maintaining the Detector
3.
Remove the column.
4.
Flush the system with 100% HPLC-quality water for 60 minutes at 1
mL/min.
5.
Reassemble the detector for operation.
6.
Reset the system to operating conditions and evaluate chromatography.
Servicing the vapor trap
To service the vapor trap
1.
Unscrew the vapor trap bottle from the cover, and empty the contents of
the bottle into an appropriate waste container.
Cover
Vapor trap bottle
2.
Replace the vapor trap cover.
Servicing the vapor trap
4-13
Replacing fuses
Warning: To avoid electric shock, power-off and unplug the
detector before examining the fuses. For continued protection
against fire, replace fuses only with those of the same type and
rating indicated on the module.
The detector requires two 5.00 A, 250 V, 5 × 20 mm (IEC) fuses.
Suspect a fuse is open or otherwise defective when
•
the detector fails to power-on.
•
the display is blank.
•
the fan does not operate.
To replace the fuses
Requirement: Replace both fuses, even when only one is open or otherwise
defective.
1.
Power-off the detector and disconnect the power cord from the power
entry module.
2.
Pinch the sides of the spring-loaded fuse holder, which fits above the
power entry module on the rear panel of the detector. With minimum
pressure, withdraw the spring-loaded fuse holder.
Fuse holder
Fuse receptacle
Power entry module
4-14
3.
Remove and discard the fuses.
4.
Make sure that the new fuses are properly rated for your requirements.
Insert them into the holder and the holder into the power entry module,
gently pushing until the assembly locks into position.
Maintaining the Detector
5.
Reconnect the power cord to the power entry module.
Cleaning the instrument’s exterior
Use a soft cloth, dampened with water, to clean the outside of the detector.
Cleaning the instrument’s exterior
4-15
4-16
Maintaining the Detector
5
Diagnostic Functions and
Troubleshooting
Consult this chapter when troubleshooting problems with the ELS detector.
However, bear in mind that the detector measures only the bulk properties of
a system. Therefore, the cause of an apparent detector problem may actually
originate with the chromatography or other system instruments.
If you isolate a general chromatography problem, see “Chromatography
troubleshooting” on page 5-21. If you determine that a problem lies with the
detector, refer to “Error messages” on page 5-2.
Contents:
Topic
Page
Error messages
5-2
User-selectable diagnostic functions
5-2
General troubleshooting
5-13
Chromatography troubleshooting
5-21
5-1
Error messages
Startup error messages
Startup confidence tests are executed on detector startup. They run after the
detector is powered-on, and they determine whether the detector’s electronics
are performing properly.
If one or more of the startup confidence tests fail, the detector beeps and
displays an error message.
When you encounter an error message, use the Enter key to clear it and
continue operating the detector while following any recommended corrective
action.
Operational error messages
During initialization and operation, the detector might display an error
message screen. Errors described on this screen can be catastrophic in nature,
preventing further operation of the detector, suspending the light scattering
display and halting output. The error messages can also be informational,
advising you to take appropriate action.
When you encounter an informational error message, press Enter to clear the
message and continue operating the detector, following any recommended
corrective action.
When you encounter a catastrophic error, power-off and then power-on the
detector. If the error persists, review “General troubleshooting” on page 5-13.
If you cannot resolve the problem, contact Waters Technical Service.
User-selectable diagnostic functions
Overview
You can run diagnostic functions to troubleshoot the detector and verify that
its electronics and optics are working properly.
5-2
Diagnostic Functions and Troubleshooting
To perform user-selectable diagnostic functions
1.
Press DIAG on the detector’s front panel. The detector displays the
diagnostic functions.
Diagnostic functions menu
2.
To access a specific diagnostic function, press the or key to navigate
to the function you want to run and press Enter, or select a number
between 1 and 9 that corresponds to the number on the detector keypad.
Menu items that display further choices are accompanied by >>.
Diagnostic functions
Diagnostic function
Description
Reset flow & diags
Resets all diagnostic functions to
default values. Resets the Stop Flow
output. Removes sticky diagnostics
and the wrench icon.
Signal-to-Noise test
Runs the signal-to-noise test.
Auto gain
Determines the optimum gain
settings for a chromatogram.
Input & output
Lists diagnostic functions for contact
closure inputs and single switch
output:
1. Auto zero offset
2. Fix voltage
3. Contact closures & events
4. Previous choices
User-selectable diagnostic functions
5-3
Diagnostic functions (Continued)
Diagnostic function
Description
Lamp, display & keypad
Lists diagnostic functions for lamp,
display, and keypad:
1. Change lamp
5. Lamp history
6. Test keypad
7. Test display
8. Previous choices
Gas & temp control
Lists diagnostic functions for gas
and temperature control:
1. Gas control
9. Neb & drift heaters
10.Opt & col heaters
11.Previous choices
Sample & ref energy
Allows you to view the raw sample
signal and reference energy signal
information.
Service
Lists diagnostic functions used by
Waters service personnel.
“Sticky diagnostics” tests
The detector uses two types of user-selectable diagnostic tests: persistent and
nonpersistent. A persistent test, also called a “sticky diagnostic,” remains
enabled until you disable it. Nonpersistent tests end, and previous operating
conditions are restored as soon as you exit the test.
When a sticky diagnostic is active, the detector Home screen displays a
wrench icon.
•
You can disable a sticky diagnostic by resetting it to the default settings.
•
You can disable all active sticky diagnostics by pressing DIAG 1, Reset
Flow & Diags.
If no sticky diagnostics are active, the wrench icon does not appear in the
home screen.
5-4
Diagnostic Functions and Troubleshooting
Home screen with sticky diagnostics active
The user-selectable sticky diagnostics are Auto Gain and Simulate Peak.
To cancel a sticky diagnostic function, reselect it or select 1, Reset Flow &
Diags from the Diagnostics menu.
Running diagnostic tests
The detector employs both user-selectable and service diagnostics. You access
user diagnostics by pressing DIAG. Only qualified Waters service personnel
can access service diagnostics. To exit any diagnostic when completed, press
DIAG to return to the diagnostics menu or HOME to return to the Home
screen.
Running the Auto Gain diagnostic function
When enabled, Auto Gain determines the optimum gain settings for a
chromatogram. At the end of a run, the timed event table contains the
optimum gain setting, and the function is disabled.
Tip: To access the timed event table, press Shift > METHOD, and then press 1
Timed Events.
To enable the Auto Gain diagnostic test
Press DIAG 3, Enable Auto Gain. The Auto Gain enabled screen
appears.
Auto Gain enabled diagnostic test screen
User-selectable diagnostic functions
5-5
Tip: To disable the Auto Gain diagnostic test, press Enter.
To disable the Auto Gain diagnostic test after it was enabled
1.
Press DIAG on the detector front panel. The Diagnostic functions menu
appears.
2.
Press DIAG 3, Disable Auto Gain. The Auto Gain disabled diagnostic
tests screen appears.
Auto Gain disabled diagnostic test screen
Tip: To reenable the Auto Gain diagnostic, press Enter.
Input and output diagnostic functions
Use the input and output diagnostic functions for these purposes:
•
To view and reset the sample signal’s auto zero value
•
To fix (establish) voltage
•
To monitor two event output switches and four event input switches
To perform any of the input and output diagnostic functions, press DIAG 4,
Input & output. The Input & Output diagnostic functions menu appears.
Input & Output diagnostic functions menu
Displaying the Auto Zero offset
Using this diagnostic function, you view and reset the sample signal’s auto
zero offset value to zero.
5-6
Diagnostic Functions and Troubleshooting
To display the Auto Zero offset
1.
From the Input & Output diagnostic functions menu, press 1, Auto zero
offset. The Auto Zero Offset diagnostics screen appears.
Auto Zero Offset diagnostics screen
2.
Press Cancel to reset the sample signal’s auto zero value to zero.
Setting fixed voltage output
From the Input & Output diagnostic functions menu, press 2, Fix voltage, to
establish voltage levels for the detector output and auxiliary output. Both
must be fixed, but the values can be set independently. The valid range of
voltages is ±2000 mV for both channels. The voltage is driven on the selected
channel (Detector Out or Auxiliary Out).
Monitoring contact closures and events
To monitor contact closures and events
1.
From the Input & Output diagnostics menu, press 3, Contact closures &
events, to monitor the four contact closure inputs and to control the two
switch outputs.
Switch & events display diagnostic screen
The Input & Output diagnostic function allows real-time monitoring of
the state of the contact closure inputs. A solid circle indicates the contact
closure is closed (ON = High). An open circle indicates the contact
closure is open (OFF = Low).
User-selectable diagnostic functions
5-7
2.
For the outputs listed, you can take the following actions:
a.
Press Enter to display the active switch (surrounded by a
dotted-line border).
b.
Press any numerical key to change the status of the switch (from On
to Off, or vice-versa).
Lamp, display, and keypad diagnostic functions
To access the lamp, display, and keypad diagnostic functions, press DIAG 5.
Change Lamp diagnostic function
Use the Change Lamp diagnostic function to enter the serial number and
installation date of a new lamp.
To use the Change Lamp function
1.
From the Lamp, display & keypad menu, press 1, Change lamp. The
Change Lamp diagnostic screen appears.
Change Lamp diagnostic screen
2.
Enter the serial number of the new lamp and the date it was installed;
then press Enter. The second Change Lamp diagnostic screen appears.
Second Change Lamp diagnostic screen
5-8
Diagnostic Functions and Troubleshooting
3.
Confirm your entries, and then press Enter. The third Change Lamp
diagnostic screen appears.
Third Change Lamp diagnostic screen
4.
Press Enter to exit the Change Lamp function.
Lamp History diagnostic function
Use the Lamp History diagnostic function to view lamp use information.
To use the Lamp History function
From the Lamp, display & keypad menu, press 2, Lamp history. The
Lamp History diagnostic screen appears.
Lamp History diagnostic screen
Test Keypad diagnostic function
To use the Test Keypad diagnostic function
1.
From the Lamp, display & keypad menu, press 3, Test keypad. A
representation of the keypad appears.
2.
Press any key to begin the test, and then press each key until you try all
of them. If the keypad is operating properly, each key location is filled in
User-selectable diagnostic functions
5-9
then cleared with another press of the key. If any key does not respond
when pressed, contact your Waters service representative.
Tip: You must press Enter twice to exit the keypad diagnostic.
Test Keypad diagnostic screen
Test Display diagnostic function
To use the Test Display function
1.
From the Lamp, display & keypad menu, press 4, Test display. The
display fills from top to bottom and right to left. It then returns to the
Lamp, display & keypad menu. If the display does not completely fill,
either horizontally or vertically, contact your Waters service
representative.
2.
From the Lamp, display & keypad menu, press 5 to return to the
Diagnostics menu.
Gas and temperature control diagnostic functions
To access the gas and temperature control tests, press DIAG 6.
5-10
Diagnostic Functions and Troubleshooting
Viewing the nebulizer and drift tube temperature
To view the nebulizer and drift tube temperature
From the Gas & temp control menu, press 2, Neb & drift heaters, to run
the nebulizer and drift tube heater temperature control test. The
Nebulizer & Tube Heater Temperature Control screen appears.
Nebulizer and drift tube temperature control diagnostic screen
Using the gas control diagnostic
With the Gas Control diagnostic function, you can control the gas pressure
regulator and gas solenoid valve independently. The diagnostic screen
displays the state of the gas pressure switch and the value of the pressure
transducer. When the function ends, the original state of the gas regulator
and gas solenoid valve is restored.
Tips:
•
Gas Pressure should be high enough to prevent extended exposure time
of the sample in the drift tube area. Gas pressure that is too low could
cause higher-than-desired dispersion of particles and, consequently, loss
of sensitivity.
•
Gas pressure should be high enough to prevent the formation of large
particles that could cause detector noise.
User-selectable diagnostic functions
5-11
To use the gas control diagnostic
1.
From the Gas & temp control menu, press 1, Gas control, to run the gas
control diagnostic. The Gas Control diagnostic screen appears.
Gas Control diagnostic screen
Pressure transducer
reading
2.
Enter the gas pressure, in psi, in the set point field.
Requirement: Use at least 450 kPa (4.5 bar, 65 psi), to run the gas
control diagnostic.
3.
To stop gas flow, enter 0 in the set point field.
Sample and reference energy diagnostic function
With the sample and reference energy diagnostic function, you view raw
sample, signal, and reference energy information, and you change the state of
the lamp and gain.
To use the sample and reference energy diagnostic function
1.
Press DIAG 7, Sample & ref energy. The sample and reference energy
diagnostic screen appears.
Sample and reference energy diagnostic screen
PMT signal level
Lamp energy
2.
5-12
Enter the gain value to view the difference between the raw sample
signal and reference energy information.
Diagnostic Functions and Troubleshooting
Generate Test Peaks diagnostic function
The Generate Test Peaks diagnostic function allows you to override sample
signal input with a simulated Gaussian peak.
To use the generate test peaks function
1.
Press DIAG 8, Generate test peaks. If the Generate Test Peaks
diagnostic function is disabled, the Test peaks enabled diagnostic screen
appears.
Test peaks enabled diagnostic screen
2.
To disable the Generate Test Peaks function, press Enter.
General troubleshooting
This section suggests possible causes of errors and recommends
troubleshooting actions. Keep in mind that the source of apparent detector
problems can actually be the chromatography, or it can involve other system
instruments.
Most detector problems are relatively easy to correct. If, after running the
diagnostic functions applicable to your problem and troubleshooting the
detector, you cannot correct an error condition, contact Waters’ Technical
Service department.
Power surges
Power surges, line spikes, and transient energy sources can adversely affect
detector operations. Be sure that the electrical supply used for the detector is
properly grounded and free from any of these conditions.
General troubleshooting
5-13
Detector troubleshooting
The following table contains general hardware troubleshooting for the
detector.
Detector troubleshooting
Symptom
Possible cause
Corrective action
Analog output
incorrect
LSU or maximum
output setting
changed
Reset the LSU or maximum
output setting.
Column heater
module not
functioning
Column heater
module is not
powered on
Power-on the column heater
module.
Column heater
module is not
connected to the
detector
Connect the column heater
module to detector.
Fuse blown
Check that the front panel
display is operational; if it is
not, check or replace the AC
rear panel fuse.
No power at outlet
Check the outlet by connecting
another electrical unit known
to be in working order and see
if it operates.
Bad internal power
supply or circuit
board
Call Waters Technical Service
(see page 4-2).
Broken electrical
connection
Check power connections.
Fuse blown
Check and, if necessary,
replace fuse(s).
Bad LCD or control
board
Call Waters Technical Service
(see page 4-2).
Detector inoperative
Front panel display
fails to illuminate
Front panel displays Faulty EPROMs
odd characters
Bad LCD control
board
5-14
Diagnostic Functions and Troubleshooting
Call Waters Technical Service
(see page 4-2).
Detector troubleshooting (Continued)
Symptom
Possible cause
Corrective action
Fumes detected in
lab
Exhaust is restricted Ensure the exhaust hose from
the detector runs downward,
toward the floor, and is
unobstructed.
Waste tube is not
properly connected
to the siphon drain,
causing solvent to
collect in the drip
tray
Properly attach and route the
waste tube.
Keypad not
functioning
Keypad defective
1. Power-off and then
power-on the detector.
2. Run the keypad diagnostic
(see page 5-9).
3. If the problem persists, call
Waters Technical Service
(see page 4-2).
Lamp not
functioning
Lamp burned out
1. Power-off and then
power-on the detector.
2. If the problem persists,
replace the lamp cartridge
(see page 4-3).
General troubleshooting
5-15
Power-on confidence check error messages
The following table contains power-on confidence check error messages, along
with their descriptions, for the detector.
Power-on confidence check error messages
Error message
Possible cause
HW communications Cable loose or
failure, multiplexed intermittent
ADC
connector contact.
HW communications Personality board
problem.
failure, reference
photodiode ADC
Corrective action
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
HW communications
failure, sample ADC
Lamp or PMT signal Weak lamp or bad
too low
alignment.
5-16
1. Replace the lamp (see
page 5-8).
2. Power the detector off, and
then on.
3. If the problem persists, call
Waters Technical Service
(see page 4-2).
PMT dark current
too high
Light entering the
1. Power-off and then
optics bench.
power-on the detector.
Problem with PMT
2. If the problem persists, call
or personality board.
Waters Technical Service
(see page 4-2).
PMT dark current
too low
Problem with PMT
1. Power-off and then
or personality board.
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
PMT not calibrated
Memory was reset
and previous
normalization
information was
reset.
Diagnostic Functions and Troubleshooting
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Power-on confidence check error messages (Continued)
Error message
Possible cause
Corrective action
Reference dark
current too high
Light entering optics 1. Power-off and then
bench.
power-on the detector.
Problem with PMT
2. If the problem persists, call
or personality board.
Waters Technical Service
(see page 4-2).
Reference dark
current too low
Problem with PMT
1. Power-off and then
or personality board.
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Signal too high. Bad
PMT or light leak in
bench.
Light entering optics 1. Power-off and then
bench.
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
System not
normalized. Run
diagnostic.
Memory was reset
and previous
normalization
information was
reset.
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Operational error messages
The following table contains operational error messages, along with their
descriptions, for the detector.
Operational error messages
Error message
Probable cause
Corrective action
Column heater fell
below its set
temperature
Heater failure (short 1. Power-off and then
circuit).
power-on the detector.
Cable or connector
2. If the problem persists, call
short.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
General troubleshooting
5-17
Operational error messages (Continued)
5-18
Error message
Probable cause
Corrective action
Column heater has
been disconnected
The heater’s
connection is not
connected or loose.
1. Check Column Heater
connection and connector.
2. Power-off and then
power-on the detector.
3. If the problem persists, call
Waters Technical Service
(see page 4-2).
Column heater has
not reached its set
temperature
A run was started
before the heater’s
temperature was
within its alarm
limits.
Allow the heaters to reach
their set temperatures before
starting a run.
Column heater rose
above its set
temperature
Heater failure (short 1. Power-off and then
circuit).
power-on the detector.
Cable or connector
2. If the problem persists, call
short.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
Column heater
temperature probe
failure
The heater’s
1. Power-off and then
temperature probe is
power-on the detector.
not connected or has 2. If the problem persists, call
a loose connection.
Waters Technical Service
Problem with
(see page 4-2).
personality board.
Configuration not
found
A memory failure
was detected, and it
was reset to its
default value.
Diagnostic Functions and Troubleshooting
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Operational error messages (Continued)
Error message
Probable cause
Corrective action
Drift tube heater fell Heater failure (short 1. Power-off and then
power-on the detector.
below its set
circuit).
temperature
2. If the problem persists, call
Cable or connector
Waters Technical Service
short.
(see page 4-2).
Problem with
personality board.
Drift Tube heater
has not reached its
set temperature
A run was started
before the heater’s
temperature was
within its alarm
limits.
Drift tube heater
rose above its set
temperature
Heater failure (short 1. Power-off and then
circuit).
power-on the detector.
Cable or connector
2. If the problem persists, call
short.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
Drift tube heater
temperature probe
failure
The heater’s
1. Power-off and then
temperature probe is
power-on the detector.
not connected or has 2. If the problem persists, call
a loose connection.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
Lamp failure
Weak lamp or bad
alignment.
Allow the heaters to reach
their set temperatures before
starting a run.
1. Replace the lamp (see
page 5-8).
2. Power-off and then
power-on the detector.
3. If the problem persists, call
Waters Technical Service
(see page 4-2).
General troubleshooting
5-19
Operational error messages (Continued)
5-20
Error message
Probable cause
Corrective action
Low input gas
pressure
The gas input is
below 450 kPa
(4.5 bar, 65 psi).
Defective low gas
pressure limit
switch.
1. Check gas source.
2. Power-off and then
power-on the detector.
3. If the problem persists, call
Waters Technical Service
(see page 4-2).
Method not found
A memory failure
was detected, and it
was reset to its
default value.
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Nebulizer heater
rose above its set
temperature
Heater failure (short 1. Power-off and then
circuit).
power-on the detector.
Cable or connector
2. If the problem persists, call
short.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
Nebulizer heater
temperature probe
failure
The heater’s
1. Power-off and then
temperature probe is
power-on the detector.
not connected or has 2. If the problem persists, call
a loose connection.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
NV-RAM bad
A memory failure
was detected, and it
was reset to its
default value.
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Optics heater has
been disconnected
The heater’s
connection is not
connected or loose.
1. Power-off and then
power-on the detector.
2. If the problem persists, call
Waters Technical Service
(see page 4-2).
Diagnostic Functions and Troubleshooting
Operational error messages (Continued)
Error message
Probable cause
Corrective action
Optics heater rose
above its set
temperature
Heater failure (short 1. Power-off and then
power-on the detector.
circuit).
2. If the problem persists, call
Cable or connector
Waters Technical Service
short.
(see page 4-2).
Problem with
personality board.
Optics heater
temperature probe
failure
1. Power-off and then
The heater’s
power-on the detector.
temperature probe is
not connected or has 2. If the problem persists, call
a loose connection.
Waters Technical Service
(see page 4-2).
Problem with
personality board.
Chromatography troubleshooting
This section contains chromatography troubleshooting tables that include
symptoms, possible causes, and suggested corrective actions. These tables can
help you isolate the possible causes of problems related to these factors:
•
Abnormal baseline (drift, noise, or cycling) (see the table titled
“Abnormal baseline troubleshooting” on page 5-22).
•
Erratic or incorrect retention times (see the table titled “Troubleshooting
general chromatography problems” on page 5-27).
•
Poor peak resolution (see the table titled “Peak resolution
troubleshooting” on page 5-30).
•
Incorrect qualitative/quantitative results (see the table titled “Incorrect
results troubleshooting” on page 5-31).
Warning: To avoid chemical hazards, always observe safe laboratory
practices when operating your system. Refer to the Material Safety Data
Sheets shipped with solvents for handling information.
If your system exhibits symptoms not addressed in one of the tables, refer to
“General troubleshooting” on page 5-13. If you need further help, contact
Waters Technical Service.
Chromatography troubleshooting
5-21
Abnormal baseline
Drift, noise, and cycling are common symptoms of an abnormal baseline.
Cycling
If the baseline is cycling, determine the period of the cycle and whether it is
related to the flow rate or fluctuations in ambient temperature or pressure.
Refer to the following table to troubleshoot problems with your baseline.
Abnormal baseline troubleshooting
Symptom
Possible cause
Corrective action
Baseline drift
Mobile phase mixing
problem causing
improper
evaporation.
Correct mobile phase
composition. Use high-quality
HPLC water and organic
solvents.
Drift tube
temperature not
optimized correctly.
Recalculate temperature for
least volatile mobile phase
during a gradient run. Reset
temperature as necessary (see
page 3-18).
Column shedding
particles during
gradient run.
Recalculate temperature for
least volatile mobile phase
during a gradient run. Reset
temperature as necessary (see
page 3-18).
Air in mobile phase
or pump.
Degas mobile phase. Purge
pump to remove air.
Pump pulsations.
Incorporate pulse dampener
into system.
Correct pump check valve or
pump seal problems.
Baseline noise
(regular)
5-22
Diagnostic Functions and Troubleshooting
Abnormal baseline troubleshooting (Continued)
Symptom
Possible cause
Corrective action
Baseline noise
(irregular)
Improper
volatilization of
mobile phase.
Check drift tube temperature
setting, optimize temperature
(see page 3-18).
Dirty nebulizer
and/or drift tube.
Clean nebulizer and/or drift
tube (see page 4-9) or call
Waters Technical Service (see
page 4-2).
Varying or low gas
flow.
Check gas flow setting.
Optimize gas flow. Reset gas
flow as necessary. Check
source gas.
Obstructed or full
exhaust trap.
Check for kinks in exhaust line
or empty condensate flask.
Column leaking
silica or packing
material.
Replace column and flush it
thoroughly before connecting it
to the detector.
Air trapped in
system.
Flush system with strong
solvent.
Leaks.
Check system for loose fittings.
Check pump for leaks or
unusual noise. Change pump
seals if necessary.
Leak (especially
between the column
and detector).
Check for loose fittings.
Tubing between
column and detector
too long or too large
of an ID.
Use short piece of 0.005 to-0.010-inch ID tubing.
Broad peaks
Chromatography troubleshooting
5-23
Abnormal baseline troubleshooting (Continued)
Symptom
Possible cause
Corrective action
Change in peak
height or loss in
sensitivity
Nebulizer blocked.
Clean nebulizer and/or drift
tube (see page 4-9).
Dirty nebulizer
and/or drift tube.
Clean nebulizer and/or drift
tube (see page 4-9) or call
Waters Technical Service (see
page 4-2).
Detector/recorder
setting changed.
Check drift tube temperature
and gas flow settings.
Detector exhaust too Move exhaust hose further
strong.
away from vacuum. See the
figure “Exhaust system flow
example” on page 2-11.
Detector is making a Detector exhaust too Move exhaust hose further
gurgling sound
strong.
away from vacuum. See the
figure “Exhaust system flow
example” on page 2-11.
Drift tube not
heating
Drift tube
overheating
High solvent
pressure
5-24
Tube temperature
not set correctly.
Adjust tube setting to correct
temperature (see page 3-18).
Oven temperature
switch defect.
Contact Waters Technical
Service.
Tube temperature
not set correctly.
Adjust tube setting to correct
temperature.
Temperature sensor
malfunctioning.
Contact Waters Technical
Service.
Blocked nebulizer.
1. Clean the nebulizer (see
page 4-9).
2. Replace nebulizer (see
page 4-6).
Diagnostic Functions and Troubleshooting
Abnormal baseline troubleshooting (Continued)
Symptom
Possible cause
Corrective action
Nebulizer cooler not
functioning
Nebulizer cooler
malfunctioning.
1. Ensure there is 5 cm
(2 inches) clearance on the
left side of the detector to
allow venting for nebulizer
cooling.
2. Power-off and then
power-on the detector.
3. Allow 30 to 60 minutes for
the detector to equilibrate.
4. If the problem persists, call
Waters Technical Service
(see page 4-2).
No mobile phase
flow
Detector went into
error and shut off
pump.
Determine and fix the error,
then restart the pump.
Flow interrupted or
obstructed.
Check mobile phase level in
reservoirs. Check flow
throughout system. Make sure
mobile phase inlet filter is
clean.
Leak.
Check system for loose fittings.
Check for leak or unusual
noises. Change pump seals, if
necessary.
Air in pump head.
Prime the pump. Consult the
operator’s guide that
accompanied the pump for
more information.
Gas source valve
closed.
Open gas valve and set to
desired rate.
Blocked nebulizer.
Clean or replace nebulizer (see
page 4-9 and page 4-6).
Source gas pressure
too low.
Check gas source.
No gas flow
Chromatography troubleshooting
5-25
Abnormal baseline troubleshooting (Continued)
Symptom
Possible cause
Corrective action
No gas flow
(continued)
Clogged inlet gas
filter.
Contact Waters Technical
Service to replace filter.
No power
Line unplugged.
Plug in power line.
Blown fuse.
Replace fuse (see page 4-14).
No LCD display
Electrical problem.
Contact Waters Technical
Service.
No peaks detected
Sample is volatile at
detector conditions.
Modify method to use a more
volatile mobile phase.
Sample being
retained on column.
Remove column. Connect
injection valve directly to
detector and inject into mobile
phase. Peak should be seen
immediately.
Detector output
signal not zeroed.
Press the Auto Zero key.
No gain set.
Set gain (see page 3-19).
Detector exhaust too Move exhaust hose further
strong.
away from vacuum. See the
figure “Exhaust system flow
example” on page 2-11.
5-26
Drift tube
temperature too
high.
Decrease drift tube
temperature (see page 3-18).
Rounded peaks
Detector time
constants set too
high.
Reduce setting to lowest value
or value at which no further
improvements are seen.
Spiking
Gas source
contaminated or of
low purity.
Use clean, dry, inert gas,
usually 99.9% pure nitrogen.
Drift tube dirty.
Clean drift tube. Contact
Waters Technical Service.
Diagnostic Functions and Troubleshooting
Abnormal baseline troubleshooting (Continued)
Symptom
Possible cause
Corrective action
Spiking (continued)
Mobile phase
contaminated or
made of low quality
material.
Check make up of mobile
phase.
Gas flow set too low.
Increase gas flow.
Erratic or incorrect retention times
When you troubleshoot retention time problems, determine whether the
retention times:
•
Change from run to run or are constant from run to run but outside the
allowable range for the assay
•
Vary due to pressure fluctuations that are short-term (with each pump
cycle) or long-term (over the course of several minutes)
•
Are associated with an absolute pressure change, that is, if the pressure
is constant but higher or lower than the normal operating pressure
•
Change suddenly at the end of a series of runs, which may indicate that
air is dissolving in the mobile phase, that the mobile phase is degrading,
or that the column is contaminated
•
Change early in a series of runs and tend to become constant or fall
within range after a few minutes, which can indicate that the column
was not equilibrated or that the solvent is not properly degassed and
sparged
Troubleshooting general chromatography problems
Symptom
Possible cause
Corrective action
Erratic retention
times
Air bubble in pump
head
Degas all solvents, prime
pump (see page 6-7).
Malfunctioning
pump check valves
Clean, replace, or rebuild
pump check valves.
Leaking pump seals
Replace pump seals.
Separation
chemistry
Check mobile phase and
column.
Chromatography troubleshooting
5-27
Troubleshooting general chromatography problems (Continued)
Symptom
Possible cause
Corrective action
Erratic retention
times (continued)
Clogged solvent
filters
Replace filters.
Increased retention
times
Incorrect flow rate
Verify flow rate.
Incorrect solvent
composition
Change solvent composition.
Column heater
module not
operating
Power-on column heater
module.
Column not
equilibrated
Equilibrate column.
Incorrect column or
guard column
Use correct column or guard
column.
Air bubble in pump
head
Prime pump to remove bubble.
Malfunctioning
pump check valve(s)
Clean, replace, or rebuild
pump check valve(s).
Broken pump
plunger
Replace the plunger.
Incorrect flow rate
Verify flow rate.
Incorrect solvent
composition
Change composition.
High column
temperature
Reduce column temperature
(see page 3-21).
Incorrect column
pretreatment
See column manual.
Column
contaminated
Clean or replace column.
Incorrect column or
guard column
Use correct column or guard
column.
Doubled retention
times
Reduced retention
times
5-28
Diagnostic Functions and Troubleshooting
Troubleshooting general chromatography problems (Continued)
Symptom
Possible cause
Corrective action
Reproducibility
errors
Solvent not properly
degassed/sparged
Degas or sparge solvent (see
page 6-7).
Incorrect chemistry
or integration
Check chemistry or
integration.
Column not
equilibrated
Equilibrate column.
Injector problem
Troubleshoot injector.
Poor peak resolution
Before you address problems with peak resolution, be certain that peaks elute
at the correct retention time. The most common causes of poor peak resolution
can also appear as retention time problems.
If peak retention times are correct, determine whether poor resolution occurs
throughout the chromatogram or at a single peak pair.
If efficiency of early peaks is poor, extra-column band broadening, such as
auto injector or guard column failure, can be at fault. If peak efficiency is poor
throughout the chromatogram, post-column band-broadening or loss of
column efficiency can be the cause.
If only one peak in a chromatogram is badly-shaped, the peak component may
be interacting with the column through a chemical mechanism different from
the components in the other peaks. To troubleshoot this resolution problem,
you need to understand the separation chemistry.
Chromatography troubleshooting
5-29
Use the following table to troubleshoot peak resolution problems that may be
affecting your results.
Peak resolution troubleshooting
Symptom
Possible cause
Straight baseline, no No pump flow
peaks
Lamp not operating
Detector not zeroed
Corrective action
Set pump flow rate.
Check method. Lamp might be
turned off.
Call Waters Technical Service.
Auto zero detector baseline.
Check cables between unit and
recorder.
Improper connection Auto zero detector baseline.
between the detector Check cables between unit and
and the recorder
recorder.
No sample injected
Check injector.
Leak in solvent path Check fittings and drip tray.
Bad column
Clean or flush or replace
column.
Call Waters Technical Service.
Detector gas flow set Turn gas flow back on.
to off
Flat-topped peaks
5-30
No gain set
Set gain (see page 3-19).
Detector not zeroed
Auto zero detector baseline.
Incorrect recorder
input voltage
Adjust recorder input voltage,
or connect cable to correct port
on recorder.
Sample
concentration or
injection volume
exceeds voltage
output of detector
Decrease sample concentration
or injection volume.
Diagnostic Functions and Troubleshooting
Incorrect qualitative and quantitative results
If a peak is incorrectly identified by a data system or integrator, ensure that
the retention time is correct. If retention times are correct, and peak
resolution is good, the cause of qualitative and quantitative errors is not likely
to be chromatographic; it is more likely due to inadequate sample preparation
or faulty processing of the data (integration).
Refer to the following table to troubleshoot problems with qualitation and/or
quantitation.
Incorrect results troubleshooting
Symptom
Possible cause
Corrective action
Decreased peak
height
Leak in injector.
Troubleshoot injector.
Increased noise
Degraded,
Use fresh sample.
contaminated, or
improperly prepared
sample.
Column
contaminated.
Clean or replace column.
Loss of column
efficiency.
Clean or replace column.
Change in mobile
phase composition.
Correct mobile phase pH or
ionic composition.
Incorrect flow rate.
Change flow rate.
Drift tube
temperature too
high.
Decrease drift tube
temperature (see page 3-18).
Nebulizer not
spraying properly.
Clean/replace nebulizer.
Air bubble in flow
path.
Replace column with union
and purge flow path at 10
mL/min.
Mobile phase not
degassed.
Degas or sparge mobile phase.
Contaminated
mobile phase.
Use fresh mobile phase.
Chromatography troubleshooting
5-31
Incorrect results troubleshooting (Continued)
5-32
Symptom
Possible cause
Corrective action
Increased noise
(continued)
Drift tube
Increase drift tube
temperature too low. temperature (see page 3-18).
Drift tube
temperature too
high.
Decrease drift tube
temperature (see page 3-18).
Nebulizer
temperature too
high.
Decrease nebulizer power level
(see page 3-18).
Diagnostic Functions and Troubleshooting
6
Optimizing Detection and
Preparing Solvents
Proper solvent selection and preparation are critical in differential
evaporative light scattering detection to prevent baseline changes such as
drift, noise, or an erratic baseline. This chapter presents information on
•
detector performance
•
common solvent problems
•
solvent selection
•
degassing a solvent
Warning: To avoid chemical hazards, always observe safe laboratory
practices when handling solvents. Refer to the Material Safety Data
Sheets shipped with solvents for handling information.
Contents:
Topic
Page
Optimizing detector performance
6-2
Selecting a solvent
6-2
Solvent degassing
6-7
Optimization protocol
6-9
6-1
Optimizing detector performance
Optimizing the mobile phase
Particulate matter in the mobile phase increases the background and noise. In
most cases, distilled water and HPLC-grade solvents are sufficient. When
comparing solvents, the most critical parameter is the amount of residue after
evaporation, which should be less than 1 ppm. For that reason, the mobile
phase should contain volatile solvent modifiers, not nonvolatile ones, such as
ammonium acetate, ammonium bicarbonate, formic acid, phosphoric acids,
sulfuric acid, phosphates, and sulfates. MS-compatible, volatile solvent
modifiers, such as CF3COOH (Trifluoroacetic Acid) and CH3COOH (Acetic
Acid), can be used with the ELS detector.
Sample pretreatment
If the sample contains any particulate matter, filter it through a 0.2-μm or
0.45-μm filter before injection.
Column treatment
The chromatographic column contains microparticles to separate the
compounds being analyzed. Under certain circumstances, the column packing
undergoes chemical and/or mechanical breakdown, which can introduce
particulate matter into the detector, increasing noise.
Column breakdown depends on particle size, the type of column used, column
manufacturer, and the nature of the mobile phase. For example, high pH
degrades silica-based columns.
Caution: To avoid damaging the nebulizer, flush columns with at least
10 column volumes of clean mobile phase before connecting them to the
nebulizer. For example, flush a 2.1 × 50 column for 10 minutes at
0.5 ml/minute.
Selecting a solvent
An ideal solvent for your analysis has good solubility characteristics for your
application, and gives satisfactory baseline noise performance.
6-2
Optimizing Detection and Preparing Solvents
Solvent quality
Use spectral-grade or HPLC-grade solvents to ensure reproducible results and
minimal instrument maintenance.
A dirty or impure solvent can cause these problems:
•
Baseline noise and drift
•
Plugged columns
•
Blockages in the fluid path
Preparation checklist
The following solvent preparation guidelines help to ensure stable baselines
and good resolution:
•
Filter solvents with a 0.45-µm filter.
•
Degas and/or sparge the solvent.
•
Protect solvents from shock and drafts.
Water
Use water only from a high-quality water purification system. If the water
system does not provide filtered water, filter it through a 0.45-µm membrane
filter before use. The total organic carbon reading should be as low as possible
(<5 ppb).
Buffer compatibility
The detector cannot be used with nonvolatile solvents such as salt-buffer
solutions. Volatile modifiers, such as acetic acid and ammonium formate, may
be used successfully.
Mobile phase modifiers that are suitable for mass spectrometry (for example,
ammonium acetate, ammonium bicarbonate, ammonium formate) can be used
for evaporative light scattering detection in concentrations of less than 0.01
M, or 0.1% (v/v %). Higher concentrations of nonvolatile materials in the
mobile phase cause greater baseline noise, lower sensitivity, and nebulizer
and small bore tubing blockages. High purity mobile phases with low boiling
points are recommended.
Caution: Nonvolatile buffers are not recommended for use with the
detector. They cause noise and block fluid pathways.
Selecting a solvent
6-3
Organic solvent compatibility
The ELS detector is fully compatible with standard chromatographic solvents
including both reversed phase and normal phase organic solvents. The
limitations of detector solvent compatibility are limits imposed by the
chromatographic system in use.
Tetrahydrofuran (THF)
When you use unstabilized THF, ensure that your solvent is fresh. Previously
opened bottles of THF contain peroxide contaminants, which cause baseline
drift.
Warning: THF contaminants (peroxides) can explode when concentrated
or evaporated to dryness.
Warning: Do not use flammable solvents with air as the gas.
Properties of common solvents
The following table lists the properties for some common chromatographic
solvents.
Properties of common solvents
6-4
Solvent
Vapor Pressure
mm Hg (Torr)
Boiling
Point (°C)
Flash
Point (°C)
Acetone
184.5 at 20 °C
56.29
-20
Acetonitrile
88.8 at 25 °C
81.6
6
n-butyl acetate
7.8 at 20 °C
126.11
22
n-butyl alcohol
4.4 at 20 °C
117.5
37
n-butyl chloride
80.1 at 20 °C
78.44
-9
Chlorobenzene
8.8 at 20 °C
131.69
28
Chloroform
158.4 at 20 °C
61.15
Cyclohexane
77.5 at 20 °C
80.72
-20
Cyclopentane
400 at 20 °C
49.26
-7
o-Dichlorobenzene
1.2 at 20 °C
180.48
66
Dichloromethane
350 at 20 °C
39.75
Optimizing Detection and Preparing Solvents
Properties of common solvents (Continued)
Solvent
Vapor Pressure
mm Hg (Torr)
Boiling
Point (°C)
Flash
Point (°C)
Dimethyl acetamide
1.3 at 25 °C
166.1
70
N,N-Dimethylformamide
2.7 at 20 °C
153.0
58
Dimethyl sulfoxide
0.6 at 25 °C
189.0
88
1,4-Dioxane
29 at 20 °C
101.32
12
Ethyl acetate
73 at 20 °C
77.11
-4
Ethyl alcohol
43.9 at 20 °C
78.32
15
Ethyl ether
442 at 20 °C
34.55
-45
Ethylene dichloride
83.35 at 20 °C
83.48
13
Heptane
35.5 at 20 °C
98.43
-4
Hexane
124 at 20 °C
68.7
-22
Iso-octane
41 at 20 °C
99.24
-12
Isobutyl alcohol
8.8 at 20 °C
107.7
28
Isopropyl alcohol
32.4 at 20 °C
82.26
12
Isopropyl myristate
<1 at 20 °C
192.6
164
Methanol
97 at 20 °C
64.7
11
Methyl t-butyl ether
240 at 20 °C
55.2
-28
Methyl ethyl ketone
74 at 20 °C
79.64
-9
Methyl isobutyl ketone
16 at 20 °C
117.4
18
N-Methylpyrrolidone
0.33 at 25 °C
202.0
86
Pentane
420 at 20 °C
36.07
-49
n-Propyl alcohol
15 at 20 °C
97.2
23
241.7
135
Propylene carbonate
Pyridine
18 at 25 °C
115.25
20
Tetrahydrofuran
142 at 20 °C
66.0
-14
Toluene
28.5 at 20 °C
110.62
4
1,2,4-Trichlorobenzene
1 at 20 °C
213.5
106
Triethylamine
57 at 25 °C
89.5
-9
Trifluoroacetic acid
71.8
Selecting a solvent
6-5
Properties of common solvents (Continued)
Solvent
Vapor Pressure
mm Hg (Torr)
Boiling
Point (°C)
Water
17.54 at 20 °C
100.0
o-xylene
6 at 20 °C
144.41
Flash
Point (°C)
17
Properties of volatile mobile phase modifiers
The following table lists the properties for volatile mobile phase modifiers.
Properties of volatile mobile phase modifiers
pH range
Boiling
Point (°C)
pKa
pKb
Acetic Acid
4.75
9.25
Carbonic Acid
6.37
7.63
Formic Acid
3.75
10.25
100.70
Trifuoroacetic
Acid
0.30
13.70
71.80
Ammonia
9.25
4.75
-33.35
Ethylamine
10.81
3.19
16.60
Methylamine
10.66
3.34
-6.30
Triethylamine
11.01
2.99
89.30
Acids
116.00
Bases
Buffers
6-6
Ammonium
Acetate
3.8 to 5.8
Ammonium
Carbonate
5.5 to 7.5
and 9.3 to
11.3
Ammonium
Formate
3.0 to 5.0
Optimizing Detection and Preparing Solvents
Solvent degassing
Using degassed solvents is one of the most important steps in solvent
preparation. Degassing provides
•
stable baselines and enhanced sensitivity
•
reproducible retention times
•
stable pump or solvent delivery system operation
This section presents information on the solubility of gases, solvent degassing
methods, and solvent degassing considerations.
Solvent degassing methods
Solvent degassing helps you attain a stable baseline and also improves
reproducibility and pump performance.
Three common methods used to degas solvents are
•
sparging with helium
•
reducing pressure by vacuum
•
using sonication
These methods may be used individually or in combination.
Vacuum-ultrasound followed by sparging is the most effective technique for
most solvents.
Sparging
Sparging removes gases from solution by displacing dissolved gases in the
solvent with a less soluble gas, usually helium. Well-sparged solvent improves
pump performance. Helium sparging brings the solvent to a state of
equilibrium, which may be maintained by slow sparging or by keeping a
blanket of helium over the solvent. Blanketing inhibits reabsorption of
atmospheric gases.
Tip: Sparging may change the composition of mixed solvents.
Vacuum degassing
The inline vacuum degasser operates on the principle of Henry’s law to
remove dissolved gases from the solvent. Henry’s law states that the mole
fraction of a gas dissolved in liquid is proportional to the partial pressure of
Solvent degassing
6-7
that gas in the vapor phase above the liquid. If the partial pressure of a gas on
the surface of the liquid is reduced, for example, by evacuation, then a
proportional amount of that gas comes out of solution.
Tip: Vacuum degassing can change the composition of mixed solvents.
Ultrasonic agitation
High energy ultrasonic agitation drives energy into the solvent and causes the
submicron-sized “bubbles” of gas to aggregate. As the gas bubbles aggregate,
they become large enough to float out of the solvent and dissipate. Used alone,
ultrasonic agitation degasses 4 liters of solvent in approximately 22 minutes.
Solvent degassing considerations
Select the most efficient degassing operation for your application. To remove
dissolved gas quickly, consider the following.
Vacuum degassing
The longer a solvent is exposed to the vacuum, the more dissolved gases are
removed. Two factors affect the amount of time the solvent is exposed to the
vacuum:
•
Flow rate – At low flow rates, most of the dissolved gas is removed as the
solvent passes through the vacuum chamber. At higher flow rates, lesser
amounts of gas per unit volume of solvent are removed.
•
Surface area of the degassing membrane – The length of the degassing
membrane is fixed in each vacuum chamber. To increase the length of
membrane, you can connect two or more vacuum chambers in series.
The inline degasser is available as an option or factory-installed in the Waters
Alliance Separations Module, XE model. Standalone inline degassers are also
available.
Sparging
Helium sparging prevents reabsorption of atmospheric gases. Use this method
to retard oxidation when you are using THF or other peroxide-forming
solvents.
6-8
Optimizing Detection and Preparing Solvents
Ultrasound plus vacuum
Ultrasonic agitation combined with vacuum degasses solvent very quickly.
This technique is less likely to change the composition of mixed solvents than
vacuum alone because the mixed solvents are held under vacuum for only a
short time (less than a minute is usually sufficient).
Warning: Do not apply vacuum to the brown glass bottles in which
solvent is shipped. There is a high risk of implosion under these
conditions. Use a thick-walled container designed for vacuum
applications.
Optimization protocol
You must select the appropriate application operating parameters to obtain
the best performance from your detector. Nebulizer gas flow rate, nebulizer
temperature, and drift tube temperature must all be optimized for the best
results.
Nebulizer gas pressure
Increased nebulizer gas flow rate causes a decreased signal response because
of the resulting formation of smaller droplets that scatter less light. Lower gas
flow rates tend to be more favorable because less gas is consumed and a better
sensitivity is achieved. However, at some point this benefit is offset by an
increase in baseline noise from the inefficient nebulization of the eluent,
resulting in large droplets. The particle size of these droplets results in
complex scattering mechanisms and poor detector performance. If you reduce
the eluent flow, you must also reduce the nebulizer gas flow rate to maintain
the optimum nebulized droplet size. Never decrease the nitrogen flow rate
below 170 kPa (1.7 bar, 25 psi).
Nebulizer temperature
Note: Setting the nebulizer temperature high enough to boil the solvent can
cause excessive baseline noise.
The detector starts more quickly when you decrease the temperature of the
nebulizer chamber. The cooling option was added to effect faster equilibration.
Optimization protocol
6-9
Using the heater to increase the nebulizer temperature reduces solvent
viscosity and the surface tension of sample droplets. It also increases the
amount of analyte vapor in the drift tube, increasing signal levels. However, a
heated nebulizer chamber can require a higher drift tube temperature, which
can adversely affect temperature-sensitive samples. If your samples are
temperature-sensitive, cooling the nebulizer increases sensitivity and permits
a lower drift tube temperature, which can increase sensitivity even more.
Recommendation: In general, set as low a nebulizer temperature as possible.
Drift tube temperature
The effects of modifying the drift tube temperature are not as significant as
those that result from changing the nebulizer gas flow rate. However, the
evaporator temperature must be high enough to evaporate the solvent and
sufficiently dry the particle plume without adversely affecting the sample. If
the evaporator temperature is too low, the solvent can saturate the diffuser,
resulting in high noise and spikes. If the drift tube temperature is too high,
the sample may be volatilized, resulting in a small response.
Selecting the optimum temperature
When setting up a system, set the temperature of the drift tube to 50 °C if you
are using reversed-phase chromatography. You can adjust these values during
method optimization.
If you think your compound is thermally labile, you can use a lower
temperature to improve detector sensitivity to minimize thermal loss.
However, for a given solvent and flow rate, there is a point at which the noise
in the chromatogram dramatically increases because all of the eluent is not
vaporized. At higher flow rates, higher temperatures are required to minimize
the noise level.
6-10
Optimizing Detection and Preparing Solvents
A
Safety Advisories
Waters instruments display hazard symbols designed to alert you to the
hidden dangers of operating and maintaining the instruments. Their
corresponding user guides also include the hazard symbols, with
accompanying text statements describing the hazards and telling you
how to avoid them. This appendix presents all the safety symbols and
statements that apply to the entire line of Waters products.
Contents
Topic
Page
Warning symbols
A-2
Caution symbol
A-5
Warnings that apply to all Waters instruments
A-5
Electrical and handling symbols
A-12
A-1
Warning symbols
Warning symbols alert you to the risk of death, injury, or seriously adverse
physiological reactions associated with an instrument’s use or misuse. Heed
all warnings when you install, repair, and operate Waters instruments.
Waters assumes no liability for the failure of those who install, repair, or
operate its instruments to comply with any safety precaution.
Task-specific hazard warnings
The following warning symbols alert you to risks that can arise when you
operate or maintain an instrument or instrument component. Such risks
include burn injuries, electric shocks, ultraviolet radiation exposures, and
others.
When the following symbols appear in a manual’s narratives or procedures,
their accompanying text identifies the specific risk and explains how to avoid
it.
Warning: (General risk of danger. When this symbol appears on an
instrument, consult the instrument’s user documentation for important
safety-related information before you use the instrument.)
Warning: (Risk of burn injury from contacting hot surfaces.)
Warning: (Risk of electric shock.)
Warning: (Risk of fire.)
Warning: (Risk of needle puncture.)
Warning: (Risk of injury caused by moving machinery.)
Warning: (Risk of exposure to ultraviolet radiation.)
Warning: (Risk of contacting corrosive substances.)
Warning: (Risk of exposure to a toxic substance.)
A-2
Safety Advisories
Warning: (Risk of personal exposure to laser radiation.)
Warning: (Risk of exposure to biological agents that can pose a serious
health threat.)
Specific warnings
The following warnings can appear in the user manuals of particular
instruments and on labels affixed to them or their component parts.
Burst warning
This warning applies to Waters instruments fitted with nonmetallic tubing.
Warning: Pressurized nonmetallic, or polymer, tubing can burst.
Observe these precautions when working around such tubing:
• Wear eye protection.
• Extinguish all nearby flames.
• Do not use tubing that is, or has been, stressed or kinked.
• Do not expose nonmetallic tubing to incompatible compounds like
tetrahydrofuran (THF) and nitric or sulfuric acids.
• Be aware that some compounds, like methylene chloride and
dimethyl sulfoxide, can cause nonmetallic tubing to swell, which
significantly reduces the pressure at which the tubing can rupture.
Mass spectrometer flammable solvents warning
This warning applies to instruments operated with flammable solvents.
Warning: Where significant quantities of flammable solvents are
involved, a continuous flow of nitrogen into the ion source is required to
prevent possible ignition in that enclosed space.
Ensure that the nitrogen supply pressure never falls below 690 kPa
(6.9 bar, 100 psi) during an analysis in which flammable solvents are
used. Also ensure a gas-fail connection is connected to the LC system so
that the LC solvent flow stops if the nitrogen supply fails.
Warning symbols
A-3
Mass spectrometer shock hazard
This warning applies to all Waters mass spectrometers.
Warning: To avoid electric shock, do not remove the mass spectrometer’s
protective panels. The components they cover are not user-serviceable.
This warning applies to certain instruments when they are in Operate mode.
Warning: High voltages can be present at certain external surfaces of
the mass spectrometer when the instrument is in Operate mode. To
avoid non-lethal electric shock, make sure the instrument is in Standby
mode before touching areas marked with this high voltage warning
symbol.
Biohazard warning
This warning applies to Waters instruments that can be used to process
material that might contain biohazards: substances that contain biological
agents capable of producing harmful effects in humans.
Warning: Waters instruments and software can be used to analyze or
process potentially infectious human-sourced products, inactivated
microorganisms, and other biological materials. To avoid infection with
these agents, assume that all biological fluids are infectious, observe
Good Laboratory Practices, and consult your organization’s biohazard
safety representative regarding their proper use and handling. Specific
precautions appear in the latest edition of the US National Institutes of
Health (NIH) publication, Biosafety in Microbiological and Biomedical
Laboratories (BMBL).
A-4
Safety Advisories
Chemical hazard warning
This warning applies to Waters instruments that can process corrosive, toxic,
flammable, or other types of hazardous material.
Warning: Waters instruments can be used to analyze or
process potentially hazardous substances. To avoid injury
with any of these materials, familiarize yourself with the
materials and their hazards, observe Good Laboratory
Practices (GLP), and consult your organization’s safety
representative regarding proper use and handling.
Guidelines are provided in the latest edition of the National
Research Council's publication, Prudent Practices in the
Laboratory: Handling and Disposal of Chemicals.
Caution symbol
The caution symbol signifies that an instrument’s use or misuse can damage
the instrument or compromise a sample’s integrity. The following symbol and
its associated statement are typical of the kind that alert you to the risk of
damaging the instrument or sample.
Caution: To avoid damage, do not use abrasives or solvents to clean the
instrument’s case.
Warnings that apply to all Waters instruments
When operating this device, follow standard quality control procedures and
the equipment guidelines in this section.
Caution symbol
A-5
Attention: Changes or modifications to this unit not expressly approved by the
party responsible for compliance could void the user’s authority to operate the
equipment.
Important: Toute modification sur cette unité n’ayant pas été expressément
approuvée par l’autorité responsable de la conformité à la réglementation peut
annuler le droit de l’utilisateur à exploiter l’équipement.
Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die
ausdrückliche Genehmigung der für die ordnungsgemäße Funktionstüchtigkeit
verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des
Systems führen.
Avvertenza: qualsiasi modifica o alterazione apportata a questa unità e non
espressamente autorizzata dai responsabili per la conformità fa decadere il
diritto all'utilizzo dell'apparecchiatura da parte dell'utente.
Atencion: cualquier cambio o modificación efectuado en esta unidad que no
haya sido expresamente aprobado por la parte responsable del cumplimiento
puede anular la autorización del usuario para utilizar el equipo.
注意:未經有關法規認證部門允許對本設備進行的改變或修改,可能會使使用者喪失操作該設
備的權利。
注意:未经有关法规认证部门明确允许对本设备进行的改变或改装,可能会使使用者丧失操
作该设备的合法性。
주의: 규정 준수를 책임지는 당사자의 명백한 승인 없이 이 장치를 개조 또는 변경할 경우,
이 장치를 운용할 수 있는 사용자 권한의 효력을 상실할 수 있습니다.
注意:規制機関から明確な承認を受けずに本装置の変更や改造を行うと、本装置のユー
ザーとしての承認が無効になる可能性があります。
A-6
Safety Advisories
Warning: Use caution when working with any polymer tubing under pressure:
• Always wear eye protection when near pressurized polymer tubing.
• Extinguish all nearby flames.
• Do not use tubing that has been severely stressed or kinked.
• Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated
nitric or sulfuric acids.
• Be aware that methylene chloride and dimethyl sulfoxide cause nonmetallic
tubing to swell, which greatly reduces the rupture pressure of the tubing.
Attention: Manipulez les tubes en polymère sous pression avec precaution:
• Portez systématiquement des lunettes de protection lorsque vous vous
trouvez à proximité de tubes en polymère pressurisés.
• Eteignez toute flamme se trouvant à proximité de l’instrument.
• Evitez d'utiliser des tubes sévèrement déformés ou endommagés.
• Evitez d'utiliser des tubes non métalliques avec du tétrahydrofurane (THF)
ou de l'acide sulfurique ou nitrique concentré.
• Sachez que le chlorure de méthylène et le diméthylesulfoxyde entraînent le
gonflement des tuyaux non métalliques, ce qui réduit considérablement leur
pression de rupture.
Vorsicht: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere
Vorsicht angebracht:
• In der Nähe von unter Druck stehenden Polymerschläuchen stets
Schutzbrille tragen.
• Alle offenen Flammen in der Nähe löschen.
• Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind.
• Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder
konzentrierte Salpeter- oder Schwefelsäure verwenden.
• Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische
Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich
reduziert.
Warnings that apply to all Waters instruments
A-7
Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico
sotto pressione:
• Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
• Spegnere tutte le fiamme vive nell'ambiente circostante.
• Non utilizzare tubi eccessivamente logorati o piegati.
• Non utilizzare tubi non metallici con tetraidrofurano (THF) o acido solforico
o nitrico concentrati.
• Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamenti nei tubi non metallici, riducendo notevolmente la pressione di
rottura dei tubi stessi.
Advertencia: se recomienda precaución cuando se trabaje con tubos de
polímero sometidos a presión:
• El usuario deberá protegerse siempre los ojos cuando trabaje cerca de tubos
de polímero sometidos a presión.
• Si hubiera alguna llama las proximidades.
• No se debe trabajar con tubos que se hayan doblado o sometido a altas
presiones.
• Es necesario utilizar tubos de metal cuando se trabaje con tetrahidrofurano
(THF) o ácidos nítrico o sulfúrico concentrados.
• Hay que tener en cuenta que el cloruro de metileno y el sulfóxido de dimetilo
dilatan los tubos no metálicos, lo que reduce la presión de ruptura de los
tubos.
警告:當在有壓力的情況下使用聚合物管線時,小心注意以下幾點。
•
•
•
•
•
A-8
當接近有壓力的聚合物管線時一定要戴防護眼鏡。
熄滅附近所有的火焰。
不要使用已經被壓癟或嚴重彎曲管線。
不要在非金屬管線中使用四氫呋喃或濃硝酸或濃硫酸。
要了解使用二氯甲烷及二甲基亞楓會導致非金屬管線膨脹,大大降低管線的耐壓能力。
Safety Advisories
警告:当有压力的情况下使用管线时,小心注意以下几点:
• 当接近有压力的聚合物管线时一定要戴防护眼镜。
• 熄灭附近所有的火焰。
• 不要使用已经被压瘪或严重弯曲的管线。
• 不要在非金属管线中使用四氢呋喃或浓硝酸或浓硫酸。
• 要了解使用二氯甲烷及二甲基亚枫会导致非金属管线膨胀,大大降低管线的耐压能力。
경고: 가압 폴리머 튜브로 작업할 경우에는 주의하십시오.
• 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오.
• 근처의 화기를 모두 끄십시오.
• 심하게 변형되거나 꼬인 튜브는 사용하지 마십시오.
• 비금속(Nonmetallic) 튜브를 테트라히드로푸란(Tetrahydrofuran: THF) 또는
농축 질산 또는 황산과 함께 사용하지 마십시오.
• 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는
비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오.
警告:圧力のかかったポリマーチューブを扱うときは、注意してください。
• 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。
• 近くにある火を消してください。
• 著しく変形した、または折れ曲がったチューブは使用しないでください。
• 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流
さないでください。
• 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が
あり、その場合、チューブは極めて低い圧力で破裂します。
Warnings that apply to all Waters instruments
A-9
Warning: The user shall be made aware that if the equipment is used in a
manner not specified by the manufacturer, the protection provided by the
equipment may be impaired.
Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une
façon non spécifiée par le fabricant, la protection assurée par le matériel risque
d’être défectueuses.
Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei
unsachgemäßer Verwenddung des Gerätes die eingebauten
Sicherheitseinrichtungen unter Umständen nicht ordnungsgemäß
funktionieren.
Attenzione: si rende noto all'utente che l'eventuale utilizzo
dell'apparecchiatura secondo modalità non previste dal produttore può
compromettere la protezione offerta dall'apparecchiatura.
Advertencia: el usuario deberá saber que si el equipo se utiliza de forma
distinta a la especificada por el fabricante, las medidas de protección del equipo
podrían ser insuficientes.
警告:使用者必須非常清楚如果設備不是按照製造廠商指定的方式使用,那麼該設備所提供
的保護將被消弱。
警告:使用者必须非常清楚如果设备不是按照制造厂商指定的方式使用,那么该设备所提供
的保护将被削弱。
경고: 제조업체가 명시하지 않은 방식으로 장비를 사용할 경우 장비가 제공하는 보호 수단이
제대로 작동하지 않을 수 있다는 점을 사용자에게 반드시 인식시켜야 합니다.
警告: ユーザーは、製造元により指定されていない方法で機器を使用すると、機器が提供
している保証が無効になる可能性があることに注意して下さい。
A-10
Safety Advisories
Warning: To protect against fire, replace fuses with those of the type
and rating printed on panels adjacent to instrument fuse covers.
Attention: pour éviter tout risque d'incendie, remplacez toujours les
fusibles par d'autres du type et de la puissance indiqués sur le panneau
à proximité du couvercle de la boite à fusible de l'instrument.
Vorsicht: Zum Schutz gegen Feuer die Sicherungen nur mit
Sicherungen ersetzen, deren Typ und Nennwert auf den Tafeln neben
den Sicherungsabdeckungen des Geräts gedruckt sind.
Attenzione: per garantire protezione contro gli incendi, sostituire i
fusibili con altri dello stesso tipo aventi le caratteristiche indicate sui
pannelli adiacenti alla copertura fusibili dello strumento.
Advertencia: Para evitar incendios, sustituir los fusibles por aquellos
del tipo y características impresos en los paneles adyacentes a las
cubiertas de los fusibles del instrumento.
警告 : 為了避免火災,更換保險絲時,請使用與儀器保險絲蓋旁面板上所印刷之相同類
型與規格的保險絲。
警告 : 为了避免火灾,应更换与仪器保险丝盖旁边面板上印刷的类型和规格相同的
保险丝。
경고: 화재의 위험을 막으려면 기기 퓨즈 커버에 가까운 패널에 인쇄된 것과 동일한
타입 및 정격의 제품으로 퓨즈를 교체하십시오.
警告 : 火災予防のために、ヒューズ交換では機器ヒューズカバー脇のパネルに記
載されているタイプおよび定格のヒューズをご使用ください。
Warnings that apply to all Waters instruments
A-11
Electrical and handling symbols
Electrical symbols
These can appear in instrument user manuals and on the instrument’s front
or rear panels.
Electrical power on
Electrical power off
Standby
Direct current
Alternating current
Protective conductor terminal
Frame, or chassis, terminal
Fuse
Recycle symbol: Do not dispose in municipal waste.
A-12
Safety Advisories
Handling symbols
These handling symbols and their associated text can appear on labels affixed
to the outer packaging of Waters instrument and component shipments.
Keep upright!
Keep dry!
Fragile!
Use no hooks!
Electrical and handling symbols
A-13
A-14
Safety Advisories
B
Specifications
2424 ELS detector specifications
Physical specifications
Attribute
Specification
Height
20.3 cm (8.0 inches)
Depth
52.1 cm (20.5 inches)
Width
28.4 cm (11.2 inches)
Weight
14.7 kg (32.5 pounds)
Environmental specifications
Attribute
Specification
Operating temperature
4 to 30 °C (39.2 to 86 °F)
Operating humidity
20 to 95%, noncondensing
Shipping and storage temperature
-30 to 60 °C (-22 to 140 °F)
Shipping and storage humidity
0 to 95%, noncondensing
Acoustic noise (instrument
generated)
<65 dBA
Electrical specifications
Attribute
Specification
Protection classa
Class I
b
Overvoltage category
II
2424 ELS detector specifications
B-1
Electrical specifications (Continued)
Attribute
Specification
Pollution degree
2
Moisture protectiond
Normal (IPXO)
c
Line voltages, nominal
Grounded AC
Voltage range
100 to 240 VAC nominal
Frequency
50 to 60 Hz
Fuse
5.00 A
Power consumption
200 VA
a. Protection Class I – The insulating scheme used in the instrument to protect from electrical shock. Class I identifies a single level of insulation between live parts (wires) and
exposed conductive parts (metal panels), in which the exposed conductive parts are connected to a grounding system. In turn, this grounding system is connected to the third pin
(ground pin) on the electrical power cord plug.
b. Overvoltage Category II – Pertains to instruments that receive their electrical power
from a local level such as an electrical wall outlet.
c. Pollution Degree 2 – A measure of pollution on electrical circuits, which may produce a
reduction of dielectric strength or surface resistivity. Degree 2 refers only to normally
nonconductive pollution. Occasionally, however, expect a temporary conductivity caused
by condensation.
d. Moisture Protection – Normal (IPXO) – IPXO means that no Ingress Protection
against any type of dripping or sprayed water exists. The X is a placeholder that identifies protection against dust, if applicable.
Operational specifications
Attribute
Nebulizer:
• High-flow rate (standard with
detector)
• Low-flow rate
B-2
Specification
300 to 3000 μL/min, 1.80 standard liters
per minute (Ls/min) at 170 kPa (1.7 bar,
25 psi)
50 to 500 μL/min, 0.77 Ls/min at 170 kPa
(1.7 bar, 25 psi)
Gas
140 kPa (1.4 bar, 20 psi) to 410 kPa
(4.1 bar, 60 psi)
Gain settings
0 to 1000
Time constant filter settings
0.0 to 5.0 seconds (Hamming)
Specifications
Operational specifications (Continued)
Attribute
Specification
a
Two analog outputs
b
Four event inputs
Channel 1 = -0.1 to 2.1 VDC (selectable
maximum data rates are 10, 20, 40, or 80
Hz)
Channel 2 = -0.1 to 2.1 VDC (fixed
maximum data rate is 10 Hz)
Input voltage: ±30 Volts max
Low input voltage: <1.7 V
High input voltage: >3.2 V
Two event outputs
Type: Contact closure
Voltage: ±30 Volts max
Current, switching: 0.5 A
Current, carry: 1.2 A
Temperature control
Nebulizer heater power: 0 to 100%
Nebulizer cooler: Cooling/Off
Drift tube heater: Ambient to 100 °C
(212 °F)
c
a. Signal and Auxiliary.
b. Inject Start, Lamp On, Chart Mark, and Auto Zero.
c. One event output is dedicated to Stop Flow.
Optical specifications
Attribute
Specification
Evaporative light
scattering optics
Lens relay system
Evaporative light
scattering angle, θ
60 degrees
Photodiode
Energy reference
Photo detector
Evaporative light scattering signal;
photomultiplier tube
2424 ELS detector specifications
B-3
B-4
Specifications
Index
Symbols
+/− key 3-12
? key 3-9, 3-30
• key 3-12
A
abnormal baseline 5-22
accessing secondary functions 3-13
activating a pulse or rectangular wave
3-28
active method 3-39
adjusting contrast 3-29
advancing to the next field 3-12
analog signal output, setting 3-25
analog signals 2-25, 2-30
audience and purpose v
auto zero
configuring 3-27
disabling 3-13
enabling 3-13
function 3-9
key 3-9
options, setting 3-25
selecting 3-13
timed event parameter 3-35
auto-optimizing
gain 3-31
LSU-FS 3-31
auxiliary switch timed event
parameter 3-35
B
baseline, troubleshooting 5-30
biohazard warning A-4
burst warning A-3
C
calibration
photomultiplier tube 1-8
PMT 1-8
Cancel key 3-12
caution symbol A-5
CE key 3-12
changing
contrast 3-11
data rate 3-13
filter time constant 3-13
scale on a light scattering trace
3-10
chart mark
configuring event inputs 3-27
generating 3-9
timed event parameter 3-35
Chart Mark key 3-9
chart recorder, connecting 2-30
chemical hazard warning A-5
CHM 3-21
chromatography troubleshooting 5-21
cleaning drift tube 4-12
Clear Field key 3-12
clearing
editing changes 3-12
events 3-40
collections system 1-10
column heater module
temperature, setting 3-21
column heater module, connecting 2-33
column, connecting 2-19
confidence tests, failure 3-4
CONFIGURE key 3-10, 3-26, 3-27
configuring
auto zero event input 3-27
Index-1
detector 3-10, 3-26
event inputs 3-27
stop flow output 3-28
connecting
chart recorder 2-30
column 2-19
column heater module 2-33
drip tray 2-18
electricity source 2-12
Ethernet cable 2-22
external analog data collection
device 2-30
inject start 2-24
injection trigger signals 2-31
input and output 2-26
manual injector 2-25
Millennium data system 2-31
multiple Waters instruments 2-22
nebulization gas 2-19
single Waters instrument 2-22
siphon drain tubing
rear 2-16
siphon drain tubing, front 2-14
conserving lamp life 3-41
contacting Waters Technical Service
2-3, 4-2
context-sensitive Help 3-30
contrast
adjusting 3-29
changing 3-11
function 3-29
key 3-11
controller board 1-9
controlling
from Empower system 3-2
from MassLynx system 3-2
CPU board 1-9
current method conditions 3-13, 3-34,
3-40
Index-2
D
damage, reporting 2-3, 4-2
data acquisition 1-9
data rate
changing 3-13
setting 3-24
DC power supply 1-9
decimal point key 3-12
degassing
considerations 6-8
solvent 6-7
deleting a timed event 3-36
desolvation 1-3
detection 1-4
detector
access to 2-5
dimensions 2-5
operating under remote control
3-35
specifications B-1
DIAG key 3-10
diagnostics
failure 5-2
key 3-10
procedure 5-3
startup 1-11, 3-2
sticky 3-6
user-selected 5-2
dimensions 2-5
disabling
auto zero function 3-13
auxiliary switch output 3-13
display 1-9
lamp use statistics 3-11
light scattering trace 3-10
options 3-10
system information 3-30
drift tube
cleaning 4-12
temperature
overview 6-10
temperature, setting 3-18
drift tube temperature, icon 3-5
drip tray, connecting 2-18
E
EC Authorized Representative vii
electrical specifications B-1
electrical symbols A-12
electricity source, connecting 2-12
electronics 1-9
Empower system control 3-2
enabling
auto zero function 3-13
auxiliary switch output 3-13
chart mark event inputs 3-27
Enter key 3-12
entering negative numbers 3-12
environmental specifications B-1
equipment guidelines v, A-5
error messages 5-1
Ethernet cable, connecting 2-22
evaporative light scattering
detection process 1-2
limitations 1-6
event inputs
auto zero 3-27
chart mark 3-27
configuring 3-27
default 3-28
inject start 3-27
lamp 3-28
exhaust
venting requirements 2-9
external analog data collection device,
connecting 2-30
F
failure of startup confidence tests 3-4
filter time constant
changing 3-13
function 3-15
setting 3-24
filtering noise 1-8
filters, time constant 3-15
flammable solvents A-3
fluorescence, trace 3-10
functions
filter time constant 3-15
gain 3-15
gas pressure 3-15
primary 3-15
secondary 3-15
zoom 3-22
fuses
installing 2-6
replacing 4-14
I
G
gain
auto-optimizing 3-31
function 3-15
icon 3-5
setting 3-19
gas
pressure
function 3-15
icon 3-5
setting 3-19
timed event parameter 3-35
requirements 2-7
supply connection, making 2-7
generating
chart mark 3-9
inject start 2-27
stop flow 2-28
H
handling symbols A-13
Index-3
hardware, preparing 3-1
Help key 3-9, 3-30
HOME key 3-4, 3-9, 3-13
Home screen 3-3, 3-4
navigating from 3-13
secondary pages 3-17
fuses 2-6
major steps 2-2
network guidelines 2-23
procedure 2-2
intended use v
ISM classification vi
I
K
icons
drift tube temperature 3-5
gain 3-5
gas pressure 3-5
keypad lock 3-6
keypad unlock 3-6
lamp 3-5
light scattering unit 3-5
local/remote control 3-6
method number 3-6, 3-35
nebulizer temperature 3-5
next 3-6
run time 3-6
shift 3-5
sticky diagnostics 3-6
table of 3-5
wrench 3-6
illumination system 1-10
initial method conditions 3-9, 3-27,
3-39
initializing the detector 3-2
initiating a scan 3-9
inject signal 3-27
inject start
connection 2-24
generating 2-27
signal 2-24
injection trigger signals, connecting
2-31
input and output connectors 2-26
installing
Index-4
keypad 1-9
+/− key 3-12
? key 3-9, 3-30
• key 3-12
auto zero key 3-9
Cancel key 3-12
CE key 3-12
Chart Mark key 3-9
Clear Field key 3-12
CONFIGURE key 3-10, 3-27
contrast key 3-11
decimal point key 3-12
description 3-9
DIAG key 3-10
Enter key 3-12
functions 3-7, 3-9
Help key 3-9, 3-30
HOME key 3-9
illustration 3-8
Lamp key 3-11
Lock key 3-11
locking 3-11
METHOD key 3-10, 3-36
Next key 3-10
numeric keys 3-11
Previous key 3-10
Reset key 3-9
Run/Stop key 3-9
Scale key 3-10, 3-22
Shift key 3-10
System Info key 3-11
TEMP C key 3-10
TRACE key 3-10, 3-22
up/down arrow keys 3-9
using 3-7
keypad lock icon 3-6
keypad unlock icon 3-6
L
lamp
configuring lamp event inputs 3-28
conserving lamp life 3-41
energy 1-12
icon 3-5
performance 1-12
timed event parameter 3-35
turning off 3-41–3-43
turning on or off 3-11
use statistics 3-11
Lamp key 3-11
light scattering
chamber 1-10
types
Mie 1-4
Rayleigh 1-4
refraction-reflection 1-4
light scattering unit, icon 3-5
line spikes 5-13
local/remote control icon 3-6
lock icon 3-6
Lock key 3-11
locking the keypad 3-11
loss of current method conditions 3-40
LSU, offset parameter 3-13
LSU-FS, auto-optimizing 3-31
M
maintenance considerations 4-2
mass spectrometer shock hazard A-4
MassLynx system control 3-2
maximum voltage outputs, function
3-13
method
active 3-39
I
choice list 3-10
current conditions 3-13
initial conditions 3-27, 3-39
method * 3-34, 3-39
preventing loss of current
conditions 3-40
programming 3-34–3-41
resetting a stored 3-39
retrieving 3-39
storing 3-34, 3-38
viewing events within 3-39
METHOD key 3-10, 3-36
method number icon 3-6, 3-35
Millennium data system, connecting
2-31
mobile phase modifiers, properties 6-6
moving to the last entry in a list 3-12
multiple Waters instruments,
connecting 2-22
N
navigating
from the Home screen 3-13
in reverse order 3-10
the user interface 3-13
nebulization 1-3
nebulization gas, connecting 2-19
nebulizer 1-9
gas flow rate 6-9
replacing 4-6
selecting 3-29
temperature
icon 3-5
overview 6-9
setting 3-18
Index-5
negative number entry 3-12
network, installation guidelines 2-23
new timed event 3-36
Next arrow 3-10
Next icon 3-6
Next key 3-10
noise
calculations 1-8
filtering 1-8
increased peak 5-31
numeric keys 3-11
O
offset
LSU 3-13
voltage 3-13
operating
as a standalone instrument 3-31
under remote control 3-35
operational specifications B-2
optical specifications B-3
optics bench 1-9
optimization 6-9
optimum temperature, selecting 6-10
outputs
disabling 3-13
enabling 3-13
voltage 3-13
P
parameters
auto zero timed event 3-35
auxiliary switch timed event 3-35
chart mark timed event 3-35
gas pressure timed event 3-35
lamp timed event 3-35
threshold timed event 3-35
peak
identification 5-31
resolution 5-29
Index-6
troubleshooting 5-30
photomultiplier tube calibration 1-8
physical specifications B-1
plus/minus key 3-12
PMT calibration 1-8
power requirements 2-6
power supply, DC 1-9
power surges 5-13
powering off 3-44
preamplifier board 1-9
pressure changes 5-27
preventing loss of current method
conditions 3-40
Previous key 3-10
primary functions 3-15
programming
switches 3-28
threshold events 3-37
timed events and methods
3-34–3-41
pulse periods, setting 3-28
purpose and audience v
R
rear panel 1-13, 2-6
recalling the Home screen 3-4
rectangular wave signal 3-28
remote control 3-35
replacing
fuses 4-14
nebulizer 4-6
reproducibility errors 5-29
requirements
exhaust venting 2-9
gas 2-7
Reset key 3-9
resetting
run clock 3-9
stop flow output switch 3-21
stored method 3-39
results
troubleshooting 5-31
retention times, troubleshooting 5-28
retrieving a method 3-39
returning to initial conditions 3-9
run
setting up 3-17
run clock, stopping 3-9
run time icon 3-6
Run/Stop key 3-9
S
safety advisories A-1
safety considerations, maintenance 4-2
scale function, operating- 3-22
Scale key 3-10, 3-22
scaling factor 3-10
scanning, initiating 3-9
screen
display 3-9
Home 3-3
icons 3-5
startup 3-3, 3-4
secondary functions 3-13, 3-15
secondary pages 3-17
selecting
auto zero function 3-13
nebulizer 3-29
setting
analog signal output 3-25
auto zero options 3-25
column heater module temperature
3-21
data rate 3-24
drift tube temperature 3-18
filter time constant 3-24
gain 3-19
gas pressure 3-19
nebulizer temperature 3-18
pulse periods 3-28
switch output 3-25
setting up a run 3-17
shift icon 3-5
I
Shift key 3-10
shutting down the detector 3-44
signal connections
inject start 2-24
injection trigger 2-31
input and output 2-26
manual injector 2-25
Millennium data system 2-31
signal processing 1-8
signal, start of run 3-27
single pulse signal 3-28
single Waters instrument, connecting
2-22
siphon drain tubing, connecting
front 2-14
siphon waste tube, connecting rear
2-16
solvent
common properties 6-4
degassing 6-7
ideal 6-2
preparation 6-1
selection 6-1
spare parts 4-3
sparging 6-7, 6-8
specifications
electrical B-1
environmental B-1
operational B-2
optical B-3
physical B-1
standalone operation 3-2, 3-31
start up procedures 3-2
starting
detector 3-2
Index-7
run 3-27
run clock 3-9
startup
confidence tests failure 3-4
diagnostics 1-11, 3-2
screens 3-3, 3-4
sticky diagnostics 3-6
stop flow
generating 2-28
output switch, resetting 3-21
output, configuring 3-28
stopping the run clock 3-9
storing methods 3-34, 3-38
switch output, setting 3-25
switches, programming 3-28
symbols
caution A-5
electrical A-12
handling A-13
warning A-2
system
displaying information 3-11
information 3-30
setup 2-3
System Info key 3-11
T
TEMP C key 3-10
temperature
control 1-10
drift tube 6-10
nebulizer 6-9
threshold events
clearing 3-40
programming 3-37
threshold timed event parameter 3-35
timed events
and methods 3-34–3-41
auxiliary switch parameters 3-35
Index-8
clearing 3-40
deleting 3-36
description 3-35
gas pressure parameters 3-35
lamp parameters 3-35
parameters
auto zero 3-35
chart mark 3-35
programming 3-34–3-41
programming a new event 3-36
threshold parameters 3-35
trace function, operating 3-22
TRACE key 3-10, 3-22
transient energy 5-13
troubleshooting
abnormal baseline, cycling 5-22
chromatography 5-21
contacting Waters 5-13
detector 5-14
diagnostic functions 5-1
peak shapes 5-29, 5-30, 5-31
pressure changes 5-27
reproducibility errors 5-29
resolution 5-29
results 5-31
retention times 5-28
turning lamp on or off
from an external device 3-28
from front panel 3-11
to conserve lamp life 3-41–3-43
U
ultrasonic agitation 6-8
unlock icon 3-6
up/down arrow keys 3-9
user interface 3-13
user-selected diagnostics 5-2
using
diagnostic functions 5-1
keypad 3-7
scale function to zoom 3-22
V
vacuum degassing 6-7, 6-8
vapor trap, servicing 4-13
viewing events within a method 3-39
voltage offset, function 3-13
I
W
warm up time 3-3
warning symbols A-2, A-5
Waters Technical Service, contacting
2-3, 4-2
wrench icon 3-6
Z
zoom function 3-22
Index-9
Index-10
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