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G7115 G7165 DAD MWD UseMa en SD 29000218

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0% found this document useful (0 votes)
73 views284 pages

G7115 G7165 DAD MWD UseMa en SD 29000218

Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Diode Array Detector WR and Multiple

Wavelength Detector
Agilent InfinityLab LC Series

User Manual

Agilent InfinityLab LC Series DAD WR and MWD User Manual


Notices
Document Information Warranty Safety Notices
Document No: SD-29000218 Rev. E The material contained in this document
Edition: 03/2021 is provided “as is,” and is subject to being C AU T I O N
changed, without notice, in future edi-
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Copyright tions. Further, to the maximum extent
permitted by applicable law, Agilent dis- hazard. It calls attention to an
© Agilent Technologies, Inc. 2016-2021 claims all warranties, either express or operating procedure, practice, or
No part of this manual may be repro- implied, with regard to this manual and the like that, if not correctly per-
duced in any form or by any means any information contained herein, includ- formed or adhered to, could result
(including electronic storage and retrieval ing but not limited to the implied warran- in damage to the product or loss
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sent from Agilent Technologies, Inc. as ble for errors or for incidental or conse- beyond a CAUTION notice until
governed by United States and interna- quential damages in connection with the the indicated conditions are fully
tional copyright laws. furnishing, use, or performance of this understood and met.
document or of any information con-
tained herein. Should Agilent and the user WAR N IN G
Agilent Technologies have a separate written agreement with
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76337 Waldbronn, Germany this document that conflict with these hazard. It calls attention to an
terms, the warranty terms in the separate operating procedure, practice, or
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the like that, if not correctly per-
Technology Licenses formed or adhered to, could
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The hardware and/or software described Do not proceed beyond a WARN-
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Software Documentation).

Agilent InfinityLab LC Series DAD WR and MWD User Manual


In This Guide...

In This Guide...

This manual covers the Agilent 1260 Infinity II Diode Array Detector WR and the
Agilent 1260 Infinity II Multiple Wavelength Detector modules:
• G7115A - 1260 Infinity II DAD WR
• G7165A - 1260 Infinity II MWD

1 Introduction
This chapter gives an introduction to the module.

2 Site Requirements and Specifications


This chapter provides information on environmental requirements, physical and
performance specifications.

3 Using the Module


This chapter explains the essential operational parameters of the module.

4 Preparing the Detector


This chapter provides information on how to set up the module for an analysis
and explains the basic settings.

5 Optimizing the Detector


This chapter provides information on how to optimize the detector.

6 Troubleshooting and Diagnostics


This chapter gives an overview about the troubleshooting and diagnostic
features.

7 Error Information
This chapter describes the meaning of error messages, and provides information
on probable causes and suggested actions how to recover from error conditions.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 3


In This Guide...

8 Test Functions and Calibration


This chapter describes the tests for the module.

9 Maintenance
This chapter describes the maintenance of the detector.

10 Parts for Maintenance


This chapter provides information on parts for maintenance and repair.

11 Identifying Cables
This chapter provides information on cables used with the Agilent 1200 Infinity
Series modules.

12 Hardware Information
This chapter describes the detector in more detail on hardware and electronics.

13 LAN Configuration
This chapter provides information on connecting the module to the Agilent
ChemStation PC.

14 Appendix
This chapter provides addition information on safety, legal and web.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 4


Contents

1 Introduction 9
Introduction to the Detector 10
G7115A Diode Array Detector WR 11
G7165A Multiple Wavelength Detector 13
Optical System 15
Leak and Waste Handling 17
Bio-inert Materials 22

2 Site Requirements and Specifications 24


Site Requirements 25
Physical Specifications 28
Performance Specifications 29

3 Using the Module 36


Magnets 37
Turn on/off 38
Status Indicators 40
Instrument Configuration 41
Set up the Detector with Agilent Open Lab ChemStation 42
The Detector User Interface 43
Detector Control Settings 45
Method Parameter Settings 46
Agilent Local Control Modules 50

4 Preparing the Detector 51


Leak and Waste Handling 52
Setting up an Analysis 54
Solvent Information 61

Agilent InfinityLab LC Series DAD WR and MWD User Manual 5


5 Optimizing the Detector 67
Optimizing the Detector Performance 68
Optimization Overview 69
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion 71
Optimizing Selectivity 81
Optimizing the Detector Regarding to the System 83
Warm up of the Detector 89

6 Troubleshooting and Diagnostics 91


Available Tests vs User Interfaces 92
Agilent Lab Advisor Software 93
Available Diagnostic Functions vs. Product Level 94

7 Error Information 97
What Are Error Messages 98
General Error Messages 99
Detector Error Messages 107

8 Test Functions and Calibration 115


Introduction 116
Conditions of Detector 120
Failing a Test 121
Self-Test 122
Intensity Test 124
Cell Test 127
Filter Test 129
Holmium Oxide Test 131
ASTM Drift and Noise Test 134
Slit Test 138
Wavelength Verification Test 141
Wavelength Calibration 143
D/A Converter (DAC) Test 146
Dark-Current Test 148
Spectral Scan 150
Other Lab Advisor Functions 151

Agilent InfinityLab LC Series DAD WR and MWD User Manual 6


9 Maintenance 152
Introduction to Maintenance 153
Cautions and Warnings 154
Overview of Maintenance 156
Cleaning the Module 157
Remove and Install Doors 158
Replace a Lamp 160
Remove and Install a Flow Cell 163
Maintenance of Standard, Semi-Micro or Micro Flow Cell 167
Maintenance of High Pressure Flow Cell 170
Replacing Capillaries on a Standard Flow Cell 172
Replacing Capillaries on a Semi-Micro and Micro Flow Cell 177
Nano Flow Cell - Replacing or Cleaning 181
Cleaning or Exchanging the Holmium Oxide Filter 185
Correcting Leaks 188
Replacing Leak Handling System Parts 190
Replacing the Module’s Firmware 192
Information from Module’s Assemblies 194

10 Parts for Maintenance 195


Overview of Maintenance Parts 196
Standard Flow Cell 198
Standard Flow Cell Bio-inert 200
Semi-Micro Flow Cell 202
Micro Flow Cell 204
High Pressure Flow Cell 206
Prep Flow Cell - SST 208
Prep Flow Cell - Quartz 210
Nano Flow Cells 212
Accessory Kits 215
Holmium Oxide Filter 216
Leak Handling Parts 217

Agilent InfinityLab LC Series DAD WR and MWD User Manual 7


11 Identifying Cables 218
Cable Overview 219
Analog Cables 221
Remote Cables 223
BCD Cables 226
CAN/LAN Cables 228
Agilent 1200 module to PC 229

12 Hardware Information 230


Firmware Description 231
Electrical Connections 234
Interfaces 236
Setting the 6-bit Configuration Switch 243
Instrument Layout 247
Early Maintenance Feedback (EMF) 248

13 LAN Configuration 250


What You Have to Do First 251
TCP/IP parameter configuration 252
Configuration Switches 253
Initialization Mode Selection 254
Dynamic Host Configuration Protocol (DHCP) 256
Manual Configuration 259

14 Appendix 264
General Safety Information 265
Waste Electrical and Electronic Equipment (WEEE) Directive 271
Radio Interference 272
Sound Emission 273
UV-Radiation 274
Solvent Information 275
Declaration of Conformity for HOX2 Filter 276
Installation of Stainless Steel Cladded PEEK Capillaries 277
Agilent Technologies on Internet 283

Agilent InfinityLab LC Series DAD WR and MWD User Manual 8


1 Introduction

Introduction to the Detector 10


G7115A Diode Array Detector WR 11
Product Description 11
Features 12
G7165A Multiple Wavelength Detector 13
Product Description 13
Features 14
Optical System 15
Leak and Waste Handling 17
Leak Sensor 21
Waste Concept 21
Bio-inert Materials 22

This chapter gives an introduction to the module.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 9


1 Introduction
Introduction to the Detector

Introduction to the Detector

The detector is designed for highest optical performance, GLP compliance and
easy maintenance. It includes the following features:
• 120 Hz data acquisition rate for (ultra-) fast LC applications,
• RFID tags for all flow cells and UV-lamps provides traceable information
about these assemblies,
• long-life deuterium with RFID tag and tungsten lamps for highest intensity and
lowest detection limit over a wavelength range of 190 – 950 nm,
• no loss in sensitivity for up to eight wavelengths simultaneous,
• programmable slit from 1 – 16 nm for complete optimization of sensitivity,
linearity and spectral resolution,
• optional flow-cell cartridges with RFID tag (standard 10 mm13 µL, semi-micro
6 mm5 µL, micro 3 mm2 µL, 80 nL, 500 nL, 10 mm, high pressure
10 mm1.7 µL and prep-cells) are available and can be used depending on the
application needs,
• easy front access to lamps and flow cell for fast replacement, and
• built-in holmium oxide filter for fast wavelength accuracy verification,
• built-in temperature control for improved baseline stability,
• additional diagnostic signals for temperature and lamp voltage monitoring,
For specifications, see “Specifications” on page 29.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 10


1 Introduction
G7115A Diode Array Detector WR

G7115A Diode Array Detector WR

Product Description
The 1260 Infinity II DAD WR detector is designed for highest optical performance,
GLP compliance, and easy maintenance. With its 120 Hz data acquisition rate the
detector is perfectly suited for fast LC applications. The long –life deuterium
lamps allow highest intensity and lowest detection limits over a wavelength
range of 190 – 950 nm. The use of RFID tags for all flow cells and UV-lamps
provides traceable information about these assemblies.
The built-in holmium oxide filter features the fast wavelength accuracy
verification, while the built-in temperature controls improves the baseline
stability. Additional diagnostic signals for temperature and lamp voltage
monitoring are available.

Status indicator

Flow cell

Power switch

Leak drain

Figure 1 Overview of the detector

Agilent InfinityLab LC Series DAD WR and MWD User Manual 11


1 Introduction
G7115A Diode Array Detector WR

Features
• Higher sensitivity and selectivity - simultaneous detection of up to eight
compound-specific wavelengths.
• Low detection limits - low noise front-end electronics and the patented flow
cell design delivers very low detection limits thanks to the minimization of
short-term noise (< ± 7 µAU).
• Up to 100 % resolution gain in fast LC - using an 120 Hz data acquisition rate.
• Maximum baseline stability - electronic temperature control (ETC) reduces
baseline drift under fluctuating ambient temperature and humidity conditions.
• Wide linear range - for reliable, simultaneous quantification of primary
compounds, by-products, and impurities.
• Programmable slit (1 – 16 nm) for rapid optimization of sensitivity and
linearity.
• Excellent data traceability - radio frequency identification (RFID) tags on cells
and source lamps improve traceability of data.
• Automatic wavelength verification by built-in holmium oxide filter.
• Nine analytical and preparative flow cells provide you with maximum
application flexibility and choice.
• Extensive diagnostics, error detection and display with Instant Pilot controller
and Lab Advisor software.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 12


1 Introduction
G7165A Multiple Wavelength Detector

G7165A Multiple Wavelength Detector

Product Description
The 1260 Infinity II Multiple Wavelength Detector is designed for highest optical
performance, GLP compliance, and easy maintenance. With its 120 Hz data
acquisition rate, the detector is perfectly suited for fast LC applications. The
long-life deuterium lamps allows highest intensity and lowest detection limits
over a wavelength range of 190 – 950 nm. The use of RFID tags for all flow cells
and UV-lamps provides traceable information about these assemblies.
The built-in holmium oxide filter features the fast wavelength accuracy
verification, while the built-in temperature controls improves the baseline
stability. Additional diagnostic signals for temperature and lamp voltage
monitoring are available.

Status indicator

Flow cell

Power switch

Leak drain

Figure 2 Overview of the detector

Agilent InfinityLab LC Series DAD WR and MWD User Manual 13


1 Introduction
G7165A Multiple Wavelength Detector

Features
• Higher sensitivity and selectivity - simultaneous detection of up to eight
compound-specific wavelengths.
• Low detection limits - low noise front-end electronics and the patented flow
cell design delivers very low detection limits thanks to the minimization of
short-term noise (< ± 7 µAU).
• Up to 100 % resolution gain in fast LC - using a 120 Hz data acquisition rate.
• Maximum baseline stability - electronic temperature control (ETC) reduces
baseline drift under fluctuating ambient temperature and humidity conditions.
• Wide linear range - for reliable, simultaneous quantification of primary
compounds, by-products and impurities.
• Programmable slit (1 – 16 nm) for rapid optimization of sensitivity and
linearity.
• Excellent data traceability - radio frequency identification (RFID) tags on cells
and source lamps improve traceability of data.
• Automatic wavelength verification by built-in holmium oxide filter.
• Nine analytical and preparative flow cells provide you with maximum
application flexibility and choice.
• Extensive diagnostics, error detection and display with Instant Pilot controller
and Lab Advisor software.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 14


1 Introduction
Optical System

Optical System

The optical system of the detector is shown in Figure below. Its illumination
source is a combination of a deuterium-arc-discharge lamp for the ultraviolet
(UV) wavelength range and a tungsten lamp for the visible (VIS) and short-wave
near-infrared (SWNIR) wavelength range. The image of the filament of the
tungsten lamp is focused on the discharge aperture of the deuterium lamp by
means of a special rear-access lamp design which allows both light sources to
be optically combined and share a common axis to the source lens. The
achromat (source lens) forms a single, focused beam of light through the flow
cell. Each cell room and lamp are separated by a quartz window which can be
cleaned or replaced. In the spectrograph, light is being dispersed onto the diode
array by a holographic grating. This allows simultaneous access to all
wavelength information.

Cell support window


Tungsten lamp

Coupling lens
Deuterium lamp

Achromat (source lens)

Holmium oxide filter

Flow cell

Spectro lens
Slit
Grating
Diode array
Figure 3 Optical System of the Detector

Lamps The light source for the UV-wavelength range is a deuterium lamp with a
shine-through aperture. As a result of plasma discharge in low-pressure
deuterium gas, the lamp emits light over the 190 nm to approximately 800 nm
wavelength range. The light source for the visible and SWNIR wavelength range
is a low noise tungsten lamp. This lamp emits light over the wavelength range
470 – 950 nm.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 15


1 Introduction
Optical System

Achromat The achromat receives the light from both lamps and focuses it so that the beam
(Source Lens) passes through the flow cell.
Holmium The holmium oxide filter is electromechanically actuated. During the holmium
Oxide Filter filter test it moves into the light path.
Cell Support The cell support window assembly separates the holmium filter area from the
Window flow cell area.
Flow Cell The optical unit has a flow cell compartment for easy access to flow cells. A
Compartment variety of optional flow cells can be inserted using the same quick, simple
mounting system. The flow cell can be removed to check the optical and
electronic performance of the detector without having influences from the flow
cell.
Spectrograph The spectrograph material is ceramic to reduce thermal effects to a minimum.
The spectrograph consists of the spectrograph lens, the variable entrance slit,
the grating and the photodiode array with front-end electronics. The
spectrograph lens refocuses the light beam after it has passed through the flow
cell. The sampling interval of the diode array is < 1 nm over the wavelength range
190 – 950 nm. Depending on the wavelength this varies from 1.0 to 1.25 diodes
per nanometer (for example a diode every 0.8 to 1 nm).
For a small wavelength range, the small non-linearity could be neglected. With
the wavelength range from 190 – 950 nm a new approach is required to achieve
wavelength accuracy over the full range. Each spectrograph is calibrated
individually. The calibration data is stored in the spectrograph on an EEPROM.
Based on these data, the built-in processors calculate absorbance data with
linear intervals (1.0, 2.0, …) between data points. This results in an excellent
wavelength accuracy and instrument-to-instrument reproducibility.
Variable The micro-slit system makes use of the mechanical properties of silicon
Entrance Slit combined with the precise structuring capabilities of bulk micro-machining. It
System combines the required optical functions — slit and shutter — in a simple and
compact component. The slit width is directly controlled by the micro-processor
of the instrument and can be set as method parameter.
Grating The combination of dispersion and spectral imaging is accomplished by using a
concave holographic grating. The grating separates the light beam into all its
component wavelengths and reflects the light onto the photodiode array.
Diode Array The diode array is a series of 1024 individual photodiodes and control circuits
located on a ceramic carrier. With a wavelength range from 190 – 950 nm the
sampling interval is < 1 nm.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 16


1 Introduction
Leak and Waste Handling

Leak and Waste Handling

The Agilent InfinityLab LC Series has been designed for safe leak and waste
handling. It is important that all security concepts are understood and
instructions are carefully followed.
The solvent cabinet is designed to store a maximum volume of 8 L solvent. The
maximum volume for an individual bottle stored in the solvent cabinet should not
exceed 2 L. For details, see the usage guideline for the Agilent Infinity II Solvent
Cabinets (a printed copy of the guideline has been shipped with the solvent
cabinet, electronic copies are available on the Internet).
All leak plane outlets are situated in a consistent position so that all Infinity and
Infinity II modules can be stacked on top of each other. Waste tubes are guided
through a channel on the right hand side of the instrument, keeping the front
access clear from tubes.
The leak plane provides leak management by catching all internal liquid leaks,
guiding them to the leak sensor for leak detection, and passing them on to the
next module below, if the leak sensor fails. The leak sensor in the leak plane
stops the running system as soon as the leak detection level is reached.
Solvent and condensate is guided through the waste channel into the waste
container:
• from the detector's flow cell outlet
• from the Multisampler needle wash port
• from the Sample Cooler or Sample Thermostat (condensate)
• from the pump's Seal Wash Sensor (if applicable)
• from the pump's Purge Valve or Multipurpose Valve

Agilent InfinityLab LC Series DAD WR and MWD User Manual 17


1 Introduction
Leak and Waste Handling

Figure 4 Infinity II Leak Waste Concept (Flex Bench installation)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 18


1 Introduction
Leak and Waste Handling

Figure 5 Infinity II Single Stack Leak Waste Concept (bench installation)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 19


1 Introduction
Leak and Waste Handling

Figure 6 Infinity II Two Stack Leak Waste Concept (bench installation)

The waste tube connected to the leak plane outlet on each of the bottom
instruments guides the solvent to a suitable waste container.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 20


1 Introduction
Leak and Waste Handling

Leak Sensor
Solvent incompatibility
C AU T I O N
The solvent DMF (dimethylformamide) leads to corrosion of the leak sensor.
The material of the leak sensor, PVDF (polyvinylidene fluoride), is incompatible
with DMF.
 Do not use DMF as mobile phase.
 Check the leak sensor regularly for corrosion.

Waste Concept
1 Agilent recommends using the 6 L waste can with 1 Stay Safe cap GL45 with
4 ports (5043-1221) for optimal and safe waste disposal. If you decide to use
your own waste solution, make sure that the tubes don't immerse in the liquid.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 21


1 Introduction
Bio-inert Materials

Bio-inert Materials

For the Bio-inert LC system, Agilent Technologies uses highest quality materials
in the flow path (also referred to as wetted parts), which are widely accepted by
life science scientists, as they are known for optimum inertness to biological
samples and ensure best compatibility with common samples and solvents over
a wide pH range. Explicitly, the complete flow path is free of stainless steel and
free of other alloys containing metals such as iron, nickel, cobalt, chromium,
molybdenum or copper, which can interfere with biological samples. The flow
downstream of the sample introduction contains no metals whatsoever.
Table 1 Used Bio-inert materials

Module Materials

Agilent 1260 Infinity II Bio-inert Pump Titanium, gold, platinum-iridium, ceramic,


(G5654A) ruby, PTFE, PEEK

Agilent 1260 Infinity II Bio-inert Multisampler Upstream of sample introduction:


(G5668A) • Titanium, gold, PTFE, PEEK, ceramic
Downstream of sample introduction:
• PEEK, ceramic

Agilent 1260 Infinity II Bio-inert Manual Injector PEEK, ceramic


(G5628A)

Agilent 1260 Infinity II Bio-inert Analytical Fraction Collector PEEK, ceramic, PTFE
(G5664B)

Bio-inert Flow Cells:

Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar ( 12 MPa) for MWD/DAD, PEEK, ceramic, sapphire, PTFE
includes 0890-1763 – 0.18 x 1500 mm PEEK capillary and 5063-6591 – PEEK
fittings (G5615-60022)
(for Agilent 1260 Infinity II DAD G7115A, and MWD G7165A)

Bio-inert flow cell, 8 µL, 20 bar (pH 1–12), includes 0890-1763 – 0.18 x 1500 mm PEEK, fused silica, PTFE
PEEK capillary and 5063-6591 – PEEK fittings (G5615-60005)
(for Agilent 1260 Infinity II FLD G7121A/B)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 22


1 Introduction
Bio-inert Materials

Table 1 Used Bio-inert materials

Module Materials

Bio-inert Heat Exchangers, Valves and Capillaries:

Quick Connect Heat Exchanger Bio-inert (G7116-60041) PEEK (steel-cladded)


(for Agilent 1260 Infinity II Multicolumn Thermostat G7116A)

Bio-inert Valve heads (G4235A, G5631A, G5632A, G5639A) PEEK, ceramic (Al2O3 based)

Bio-inert Connection capillaries Upstream of sample introduction:


• Titanium
Downstream of sample introduction:
• Agilent uses stainless-steel-cladded
PEEK capillaries, which keep the flow
path free of steel and provide pressure
stability up to 600 bar.

To ensure optimum bio-compatibility of your Agilent 1260 Infinity II Bio-inert LC


NOTE system, do not include non-inert standard modules or parts to the flow path. Do
not use any parts that are not labeled as Agilent “Bio-inert”. For solvent
compatibility of these materials, see “General Information about Solvent/Material
Compatibility” on page 61.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 23


2 Site Requirements and Specifications

Site Requirements 25
Physical Specifications 28
Performance Specifications 29
Specifications 29
Specification Conditions 35

This chapter provides information on environmental requirements, physical and


performance specifications.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 24


2 Site Requirements and Specifications
Site Requirements

Site Requirements
A suitable environment is important to ensure optimal performance of the
instrument.

Power Considerations
The module power supply has wide ranging capability. It accepts any line voltage
in the range described in Table 2 on page 28. Consequently there is no voltage
selector in the rear of the module. There are also no externally accessible fuses,
because automatic electronic fuses are implemented in the power supply.

Hazard of electrical shock or damage of your instrumentation


WAR N IN G
can result, if the devices are connected to a line voltage higher than
specified.
 Connect your instrument to the specified line voltage only.

Electrical shock hazard


WAR N IN G
The module is partially energized when switched off, as long as the power
cord is plugged in.
The cover protects users from personal injuries, for example electrical
shock.
 Do not open the cover.
 Do not operate the instrument and disconnect the power cable in case
the cover has any signs of damage.
 Contact Agilent for support and request an instrument repair service.

Inaccessible power plug.


WAR N IN G
In case of emergency it must be possible to disconnect the instrument
from the power line at any time.
 Make sure the power connector of the instrument can be easily reached
and unplugged.
 Provide sufficient space behind the power socket of the instrument to
unplug the cable.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 25


2 Site Requirements and Specifications
Site Requirements

Power Cords
Country-specific power cords are available for the module. The female end of all
power cords is identical. It plugs into the power-input socket at the rear. The male
end of each power cord is different and designed to match the wall socket of a
particular country or region.
Agilent makes sure that your instrument is shipped with the power cord that is
suitable for your particular country or region.

Unintended use of power cords


WAR N IN G
Using power cords for unintended purposes can lead to personal injury or
damage of electronic equipment.
 Never use a power cord other than the one that Agilent shipped with this
instrument.
 Never use the power cords that Agilent Technologies supplies with this
instrument for any other equipment.
 Never use cables other than the ones supplied by Agilent Technologies
to ensure proper functionality and compliance with safety or EMC
regulations.

Absence of ground connection


WAR N IN G
The absence of ground connection can lead to electric shock or short
circuit.
 Never operate your instrumentation from a power outlet that has no
ground connection.

Electrical shock hazard


WAR N IN G
Solvents may damage electrical cables.
 Prevent electrical cables from getting in contact with solvents.
 Exchange electrical cables after contact with solvents.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 26


2 Site Requirements and Specifications
Site Requirements

Bench Space
The module dimensions and weight (see Table 2 on page 28) allow you to place
the module on almost any desk or laboratory bench. It needs an additional
2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches)
in the rear for air circulation and electric connections.
If the bench shall carry a complete HPLC system, make sure that the bench is
designed to bear the weight of all modules.
The module should be operated in a horizontal position.

Agilent recommends that you install the HPLC instrument in the InfinityLab Flex
NOTE Bench rack. This option helps to save bench space as all modules can be placed
into one single stack. It also allows to easily relocate the instrument to another lab.

Environment
Your detector will work within the specifications at ambient temperatures and
relative humidity described in Table 2 on page 28.
ASTM drift tests require a temperature change below 2 °C/hour (3.6 °F/hour)
over one hour period. Our published drift specification (refer also to “Performance
Specifications G7115A” on page 29 and “Performance Specifications
G7165A” on page 32) is based on these conditions. Larger ambient temperature
changes will result in larger drift.
Better drift performance depends on better control of the temperature
fluctuations. To realize the highest performance, minimize the frequency and the
amplitude of the temperature changes to below 1 °C/hour (1.8 °F/hour).
Turbulences around one minute or less can be ignored.

The module is designed to operate in a typical electromagnetic environment


NOTE (EN61326-1) where RF transmitters, such as mobile phones, should not be used
in close proximity.

Condensation within the module


C AU T I O N
Condensation can damage the system electronics.
 Do not store, ship or use your module under conditions where temperature
fluctuations could cause condensation within the module.
 If your module was shipped in cold weather, leave it in its box and allow it to
warm slowly to room temperature to avoid condensation.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 27


2 Site Requirements and Specifications
Physical Specifications

Physical Specifications

Table 2 Physical Specifications

Type Specification Comments

Weight 12 kg (26.5 lbs)

Dimensions 140 x 396 x 436 mm


(height × width × depth) (5.5 x 15.6 x 17 inches)

Line voltage 100 – 240 V~, ± 10 % Wide-ranging capability

Line frequency 50 or 60 Hz, ± 5 %

Power consumption 110 VA / 100 W

Ambient operating 4–55 °C (39–131 °F)


temperature

Ambient non-operating -40 – 70 °C (-40 – 158 °F)


temperature

Humidity < 95 % r.h. at 40 °C (104 °F) Non-condensing

Operating altitude Up to 3000 m (9842 ft)

Safety standards: IEC, EN, Overvoltage category II, Pollution degree 2 For indoor use only.
CSA, UL

ISM Classification ISM Group 1 Class B According to CISPR 11

Agilent InfinityLab LC Series DAD WR and MWD User Manual 28


2 Site Requirements and Specifications
Performance Specifications

Performance Specifications

Specifications
Performance Specifications G7115A
Table 3 Performance Specifications G7115A

Type Specification

Detection type 1024-element photodiode array

Light source Deuterium and tungsten lamps

Number of signals 8

Maximum data rate 120 Hz

Short term signal noise < ± 0.7·10-5 AU at 254 and 750 nm


(ASTM)

Drift < 0.9·10-3 AU/h at 254 nm and 750 nm

Linear absorbance range > 2 AU (5 %) at 265 nm

Wavelength range 190 – 950 nm

Wavelength accuracy ± 1 nm, self-calibration with deuterium lines, verification with


holmium oxide filter

Wavelength bunching 1 – 400 nm, programmable in 1 nm steps

Slit width 1, 2, 4 , 8, 16 nm

Diode width ~1 nm

Time programmable Wavelength, polarity, peak width, lamp bandwidth, auto balance,
wavelength range, threshold, spectra storage mode

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2 Site Requirements and Specifications
Performance Specifications

Table 3 Performance Specifications G7115A

Type Specification

Flow cells Standard: 13 µL volume, 10 mm cell path length and 120 bar
(1740 psi) pressure maximum
Standard bio-inert: 13 µL volume, 10 mm cell path length and 120 bar
(1740 psi) pressure maximum
Semi-micro: 5 µL volume, 6 mm cell path length and 120 bar
(1740 psi) pressure maximum
Micro: 2 µL volume, 3 mm cell path length, 120 bar (1740 psi)
pressure maximum
Semi-nano: 500 nL volume, 10 mm cell path length and 40 bar
(580 psi) pressure maximum
Nano: 80 nL volume, 6 mm cell path length and 40 bar (580 psi)
pressure maximum
High pressure: 1.7 µL volume, 6 mm cell path length and 400 bar
(5800 psi) pressure maximum
Prep SST: 3 mm cell path length and 120 bar (1740 psi) pressure
maximum
Prep Quartz: 3 mm cell path length and 50 bar (1740 psi) pressure
maximum
Prep Quartz:0.3 mm cell path length and 50 or 20 bar (290 psi)
pressure maximum
Prep Quartz: 0.06 mm cell path length and 50 or 20 bar (290 psi)
pressure maximum
SFC Flow Cell: 13 μL volume, 10 mm cell path length and 400 bar
(5800 psi) pressure maximum
SFC Flow Cell LD: 2 μL volume, 3 mm cell path length and 400 bar
(5800 psi) pressure maximum

Spectral tools Data analysis software for spectra evaluation, including spectral
libraries and peak purity functions

Analog output Recorder/integrator: 100 mV or 1 V, output range 0.001 – 2 AU, one


output

Instrument control Lab Advisor B.02.08 or above


LC and CE Drivers A.02.14 or above
For details about supported software versions refer to the
compatibility matrix of your version of the LC and CE Drivers.

Local control Agilent Instant Pilot (G4208A) B.02.20 or above

Communication LAN, Controller-Area Network (CAN), USB


Extended Remote Interface (ERI): ready, start, stop and shut-down
signals

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2 Site Requirements and Specifications
Performance Specifications

Table 3 Performance Specifications G7115A

Type Specification

GLP RFID for electronics records of flow cell and UV lamp conditions (path
length, volume, product number, serial number, test passed, usage)
Early maintenance feedback (EMF) for continuous tracking of
instrument usage in terms of lamp burn time with user-setable limits
and feedback messages. Electronic records of maintenance and
errors. Verification of wavelength accuracy with built-in holmium
oxide filter.

Safety and maintenance Extensive diagnostics, error detection and display through Agilent
Instant Pilot and Agilent Lab Advisor software. Leak detection, safe
leak handling, leak output signal for shutdown of pumping system.
Low voltages in major maintenance areas.

Housing All materials recyclable.

Others Second generation of Electronic temperature control (ETC) for the


complete optical unit

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2 Site Requirements and Specifications
Performance Specifications

Performance Specifications G7165A


Table 4 Performance Specifications G7165A

Type Specification

Detection type 1024-element photodiode array

Light source Deuterium and tungsten lamps

Number of signals 8

Maximum data rate 120 Hz

Short term signal noise < ± 0.7·10-5 AU at 254 nm and 750 nm


(ASTM)

Drift < 0.9·10-3 AU/h at 254 nm

Linear absorbance range > 2 AU (5 %) at 265 nm

Wavelength range 190 – 950 nm

Wavelength accuracy ± 1 nm, self-calibration with deuterium lines, verification with


holmium oxide filter
Wavelength bunching 1 – 400 nm

Slit width 1, 2, 4 , 8, 16 nm

Diode width < 1 nm


Time programmable Wavelength, polarity, peak width, lamp bandwidth, auto balance,
wavelength range, threshold, spectra storage mode

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2 Site Requirements and Specifications
Performance Specifications

Table 4 Performance Specifications G7165A

Type Specification

Flow cells Standard: 13 µL volume, 10 mm cell path length and 120 bar
(1740 psi) pressure maximum
Standard bio-inert: 13 µL volume, 10 mm cell path length and 120 bar
(1740 psi) pressure maximum
Semi-micro: 5 µL volume, 6 mm cell path length and 120 bar
(1740 psi) pressure maximum
Micro: 2 µL volume, 3 mm cell path length, 120 bar (1740 psi)
pressure maximum
Semi-nano: 500 nL volume, 10 mm cell path length and 40 bar
(580 psi) pressure maximum
Nano: 80 nL volume, 6 mm cell path length and 40 bar (580 psi)
pressure maximum
High pressure: 1.7 µL volume, 6 mm cell path length and 400 bar
(5800 psi) pressure maximum
Prep SST: 3 mm cell path length and 120 bar (1740 psi) pressure
maximum
Prep Quartz:0.3 mm cell path length and 50 or 20 bar (290 psi)
pressure maximum
Prep Quartz: 0.06 mm cell path length and 50 or 20 bar (290 psi)
pressure maximum
SFC Flow Cell: 13 μL volume, 10 mm cell path length and 400 bar
(5800 psi) pressure maximum
SFC Flow Cell LD: 2 μL volume, 3 mm cell path length and 400 bar
(5800 psi) pressure maximum

Analog output Recorder/integrator: 100 mV or 1 V, output range 0.001 – 2 AU, one


output
Instrument control Lab Advisor B.02.08 or above
LC and CE Drivers A.02.14 or above
For details about supported software versions refer to the
compatibility matrix of your version of the LC and CE Drivers.

Local control Agilent Instant Pilot (G4208A) B.02.20 or above

Communication LAN, Controller Area Network (CAN), USB


Extended Remote Interface (ERI): ready, start, stop and shut-down
signals

GLP RFID for electronics records of flow cell and UV lamp conditions (path
length, volume, product number, serial number, test passed, usage)
Early maintenance feedback (EMF) for continuous tracking of
instrument usage in terms of lamp burn time with user-setable limits
and feedback messages. Electronic records of maintenance and
errors. Verification of wavelength accuracy with built-in holmium
oxide filter.

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2 Site Requirements and Specifications
Performance Specifications

Table 4 Performance Specifications G7165A

Type Specification

Safety and maintenance Extensive diagnostics, error detection and display through Agilent
Instant Pilot and Agilent Lab Advisor software. Leak detection, safe
leak handling, leak output signal for shutdown of pumping system.
Low voltages in major maintenance areas. Tracking of flow cells and
lamps with RFID (radio frequency identification) tags.

Housing All materials recyclable.


Others Second generation of Electronic temperature control (ETC) for the
complete optical unit

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2 Site Requirements and Specifications
Performance Specifications

Specification Conditions
ASTM: “Standard Practice for Variable Wavelength Photometric Detectors Used
in Liquid Chromatography”.
Reference conditions: cell path length 10 mm, wavelength 254 and 750 nm with
reference wavelength 360 nm/100 nm, slit width 4 nm, time constant 2 s (equal
to response time 4 s), flow 1 mL/min LC-grade Methanol.
Linearity: Linearity is measured with caffeine at 265 nm/4 nm with slit width 4 nm
and TC 2 s (or with RT 4 s) with 10 mm pathlength.
For environmental conditions refer to "Environment".

The specifications are based on the standard RFID tag lamp (2140-0820) and
NOTE may be not achieved when other lamp types or aged lamps are used.

Mobile devices used close to the intstrument could affect the detector's short
NOTE term noise level.

ASTM drift tests require a temperature change below 2 °C/hour (3.6 °F/hour)
over one hour period. Our published drift specification is based on these
conditions. Larger ambient temperature changes will result in larger drift. Better
drift performance depends on better control of the temperature fluctuations. To
realize the highest performance, minimize the frequency and the amplitude of the
temperature changes to below 1 °C/hour (1.8 °F/hour). Turbulences around one
minute or less can be ignored.
Performance tests should be done with a completely warmed up optical unit (>
two hours). ASTM measurements require that the detector should be turned on
at least 24 h before start of testing.

Time Constant versus Response Time


According to ASTM E1657-98 „Standard Practice of Testing Variable-Wavelength
Photometric Detectors Used in Liquid Chromatography” the time constant is
converted to response time by multiplying by the factor 2.2.

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3 Using the Module

Magnets 37
Turn on/off 38
Status Indicators 40
Instrument Configuration 41
Set up the Detector with Agilent Open Lab ChemStation 42
The Detector User Interface 43
Detector Control Settings 45
Method Parameter Settings 46
Agilent Local Control Modules 50

This chapter explains the essential operational parameters of the module.

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3 Using the Module
Magnets

Magnets

1 Magnets in doors of pumps, autosamplers, detectors, and fraction collectors.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 37


3 Using the Module
Turn on/off

Turn on/off

This procedure exemplarily shows an arbitrary LC stack configuration.

1 2

Power switch: On

Agilent InfinityLab LC Series DAD WR and MWD User Manual 38


3 Using the Module
Turn on/off

3 Turn instrument On/Off with the control software. 4

Power switch: Off


5

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3 Using the Module
Status Indicators

Status Indicators

This procedure exemplarily shows an arbitrary LC stack configuration.


1 The module status indicator indicates one of six possible module conditions:

Status indicators
1. Idle
2. Run mode
3. Not-ready. Waiting for a specific pre-run condition to be reached or
completed.
4. Error mode - interrupts the analysis and requires attention (for example, a
leak or defective internal components).
5. Resident mode (blinking) - for example, during update of main firmware.
6. Bootloader mode (fast blinking). Try to re-boot the module or try a
cold-start. Then try a firmware update.

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3 Using the Module
Instrument Configuration

Instrument Configuration

1 Set the switches of the Configuration switch at the rear of the module:
a All switches DOWN: module uses the default IP address 192.168.254.11.

b Switch 4 UP and others DOWN: module uses DHCP.


c Switch 5 UP and others DOWN: modules uses STORED address.
2 Enter the setup information (MAC / IP address and/or Instrument Name).
a Agilent OpenLab ChemStation (Configure Instrument):
b Lab Advisor (Instrument Overview - Add Instrument):

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3 Using the Module
Set up the Detector with Agilent Open Lab ChemStation

Set up the Detector with Agilent Open Lab


ChemStation

The setup of the detector is shown with the Agilent OpenLab ChemStation
C.01.07 and Driver A.02.14.

This section describes the detector settings only. For information on the Agilent
NOTE OpenLab ChemStation or other 1200 Infinity modules refer to the corresponding
documentation.

Figure 7 ChemStation Method and Run Control (just detector is shown)

After successful load of the OpenLab ChemStation, you should see the module
as an active item in the graphical user interface (GUI).

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3 Using the Module
The Detector User Interface

The Detector User Interface

Within the detector GUI, there are active areas. If you move the
mouse cursor across the icons the cursor will change.
1 Lamp: turn on and off of UV-lamp
2 EMF status
3 Detector status
4 Detector balance status
5 Lamp status (on/off)
6 Lamp information (RFID tag)
7 Flow Cell information (RFID tag)

RFID tag information is displayed when moving with the


mouse cursor on to the tag attached to the flow cell or lamp.
The information provides flow cell and lamp related
information like
• Part number
• Production date
• Serial number
and other details.

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3 Using the Module
The Detector User Interface

EMF Status shows Run / Ready / Error state and “Not Ready
text” or “Error text”
• Offline (gray)
• Ok. No Maintenance required (green)
• EMF warning. Maintenance might be required (yellow)
• EMF warning. Maintenance required (red)
Important: The EMF settings can be accessed via Agilent Lab
Advisor. The limit(s) can be changed. Based on the limit, the
User Interface displays the above status.

Module Status shows Run / Ready / Error state and “Not


Ready text” or “Error text”
• Error (red)
• Not ready (yellow)
• Ready (green)
• Pre run, Post run (purple)
• Run (blue)
• Idle (green)
• Offline (dark gray)
• Standby (light gray)

A right-click into the Active Area will open a menu to


• Show the Control Interface (special module settings)
• Show the Method interface (similar as via menu
Instrument > Setup Instrument Method)
• Set Error Method
• Identify Module (Status LED will blink)
• Perform a Balance
• Switch the UV-lamp on/off (same as click on button
“Make Device Ready/Turn device off (standby)”)
• Switch the Vis-lamp on/off

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3 Using the Module
Detector Control Settings

Detector Control Settings

The figure shows the default settings.


• Lamps: can be turned ON/OFF.
• At Power On: automatic lamp-on at power on.
• Analog Output Range: can be set to either 100 mV or 1 V
full scale, for additional settings see Analog Output (under
“Method Parameter Settings” on page 46).
• Temperature Control: can be turned ON/OFF. The optical
unit is kept on constant temperature and improves the
baseline stability in unstable environments. See also note
below. ON it will keep the optical unit stabilized.
• UV Lamp Tag
• Use lamp only if lamp tag is available detects a lamp
with RFID tag. If no RFID tag lamp is used, “UV lamp
not ready” is displayed and it cannot be ignited. A
compatible mode has to be selected based on the
used lamp; see Non-RFID-tag lamp information below.
• Always use lamp: In case a non-RFID-tag lamp is used,
the user interface will show this when selecting a
compatible mode. You may operate the detector
outside of the guaranteed specification. The correct
selection is important for optimal performance and
lifetime.
• Cell Tag
• Use cell only if cell tag is available detects a cell with
RFID tag. If no RFID tag cell is used, “cell tag not
ready” is displayed and it cannot be ignited and
analysis is disabled.
• Always use cell: In case a non-RFID-tag cell is used,
the user interface will show this when selecting a
compatible mode.
• Automatic Turn On: automatic detector power on.

If the flow cell temperature is critical for your chromatography, you may set the
NOTE Temperature Control to off. This will lower the optical unit and flow cell
temperature by some degree C.

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3 Using the Module
Method Parameter Settings

Method Parameter Settings

These settings are available via Menu > Instrument > Set up Instrument Method or
via right click into the module’s active area (does not show the Instrument Curves
tab).

Figure 8 Method parameter settings

For additional help and support: Highlight the desired cell and press F1. A help
NOTE screen will open with additional information and documentation about the topic.

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3 Using the Module
Method Parameter Settings

Table 5 Method Parameter Settings


Signals
Up to 8 individual signals can be set. For each of the signals,
the wavelength and bandwidth can be set for sample and
reference.
Limits:
• Wavelength: 190.0 to 950.0 nm in steps of 0.1 nm
• Bandwidth: 1.0 to 400.0 nm in steps of 0.1 nm
Setting an appropriate reference wavelength could improve
the baseline behavior.

Peakwidth (Responsetime, Data Rate)


Peakwidth enables you to select the peak width (response
time) for your analysis. The peak width is defined as the width
of a peak, in minutes, at half the peak height. Set the peak
width to the narrowest expected peak in your chromatogram.
The peak width sets the optimum response time for your
detector. The peak detector ignores any peaks that are
considerably narrower, or wider, than the peak width setting.
The response time is the time between 10 % and 90 % of the
output signal in response to an input step function. When the
All spectrum storage option is selected, then spectra are
acquired continuously depending on the setting of the peak
width. The time specified by the peak width is used as a factor
in the acquisition of spectra. The acquisition time for one
spectrum is slightly less than the peak width divided by 8,
which is the acquisition time.
Limits: When you set the peak width (in minutes), the
corresponding response time is set automatically and the
appropriate data rate for signal and spectra acquisition is
selected.
Do not use peak width shorter than necessary.
For details see “Peak width (response time)” on page 73.

Stoptime/Posttime
The stoptime is the time where either the complete system
stops (As Pump/Injector) or the module (if different from
system stop time). The data collection is stopped at this time.
A posttime period can be used to allow module’s items to
equilibrate (e.g. after gradient change or temperature change).

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3 Using the Module
Method Parameter Settings

Table 5 Method Parameter Settings


Spectrum Settings (DAD only)
• Store: None / All
ALL spectra are taken continuously depending on the
setting of the Peakwidth. Eight spectra are acquired per
Peakwidth. The acquisition time for one spectrum is
slightly less than the Peakwidth divided by 8, that is,
greater than or equal to 0.01 s and less than or equal to
2.55 s.
• Range defines the wavelength range for spectral storage.
Limits: 190 – 950 nm in steps of 1 nm for both low and
high values. The high value must be greater than the low
value by at least 2 nm.
• Step defines the wavelength resolution for spectral
storage.
Limits: 0.10 – 100.00 nm in steps of 0.1 nm.

Analog Output
The range can be set to either 100 mV or 1 V full scale, see
“Detector Control Settings” on page 45.
• Zero Offset: 1 – 99 % in steps of 1 % (5 % equal to 50 mV).
• Attenuation: 0.98 – 2000 mAU at discrete values for either
100 mV or 1 V full scale.

Margin for negative Absorbance


Use this field to modify the detector’s signal handling to
increase the margin for negative absorbance. Use this option
if, for example, your solvent gradient produces a decreasing
baseline absorbance, and for GPC analyses.
Limits: 100 to 4000 mAU.
The higher the value the greater the baseline noise. Set this
value only if you expect negative absorbance greater than
-100 mAU.
Slitwidth: You can select the optical bandwidth (1, 2, 4, 8 or
16 nm) of the detector; the narrower the slit, the smaller the
optical bandwidth of the instrument, but the lower its
sensitivity. The smaller the optical bandwidth the higher the
spectral resolution.

Autobalance
Defines, whether a balance is performed prior to a run and/or
after a run has finished.
Lamp on required for acquisition:
If unchecked, the lamp will be turned off after the analysis has
finished. Note that the lamp on requires at least one hour
warm-up time, see “Warm up of the Detector” on page 89.

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3 Using the Module
Method Parameter Settings

Table 5 Method Parameter Settings


Timetable
You may set up time events to change functions with their
parameters over the run time. Add lines as required.
Time Limits: 0.00 to 99999.00 min in steps of 0.01 min.
Via the buttons in the bottom area, time table lines can be
added, removed, cut copied, pasted or completely cleared.
Based on the chosen function, a certain parameter can be
selected.

Instrument Curves
The detector has several signals (internal temperatures,
voltages of lamps) that can be used for diagnosing problems.
These can be baseline problems deriving from deuterium
lamps wander / drift problems due to temperature changes.
These signals can be used in addition to the normal baseline
signal to determine whether correlation to temperature or
voltage/current of the lamp.
These signals are available via the Agilent ChemStation Online
Plot/Data Signal and/or Agilent Lab Advisor Software.

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3 Using the Module
Agilent Local Control Modules

Agilent Local Control Modules

Agilent InfinityLab Companion G7108AA


The Agilent InfinityLab Companion gives you complete control, system
monitoring, signal plotting, and diagnostic capabilities for a wide range of LC
system modules.
The instrument control solution is available as full package including all hardware
and accessories, but can also be used on your own mobile devices like tablets,
mobile phones and other electronic equipment.
Combining the conveniences of the Agilent Instant Pilot features with
state-of-the-art mobile technology, the Agilent InfinityLab Companion gives you
maximum flexibility and ease of use to control and monitor your LC system
modules.
Features:
• Complete local control and monitoring of Agilent Infinity II LC modules
• Excellent usability and ease of use through a user interface specifically
tailored for mobile devices - simple, intuitive touch-enabled, and visual
controllable.
• High flexibility through a modern “Bring your own device” approach.
Connection between LC module and mobile device either wireless via Wi-Fi or
wired over USB cable (with full package).
• Convenient, ergonomic operation either handheld or attached to a module at
the stack with newly developed, secure tablet holder (included in the full
package).
• Preconfigured tablet with all required software already installed (included in
the full package).
• Centerpiece of the solution is a USB dongle that activates the complete
intelligence of the InfinityLab Companion on the instrument stack.
The InfinityLab Companion provides:
• fast and direct control in front of the instrument
• a clear overview of the system status
• control functionalities
• access to method parameters and sequences
• a logbook showing events from the modules
• diagnostic tests

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4 Preparing the Detector

Leak and Waste Handling 52


Waste Concept 53
Setting up an Analysis 54
Before Using the System 55
Requirements and Conditions 56
Preparing the Detector 58
Preparing the HPLC System 58
Running the Sample and Verifying the Results 60
Solvent Information 61

This chapter provides information on how to set up the module for an analysis
and explains the basic settings.

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4 Preparing the Detector
Leak and Waste Handling

Leak and Waste Handling

Toxic, flammable and hazardous solvents, samples and reagents


WAR N IN G
The handling of solvents, samples and reagents can hold health and safety
risks.
 When working with these substances observe appropriate safety
procedures (for example by wearing goggles, safety gloves and
protective clothing) as described in the material handling and safety
data sheet supplied by the vendor, and follow good laboratory practice.
 Do not use solvents with an auto-ignition temperature below 200 °C
(392 °F). Do not use solvents with a boiling point below 56 °C (133 °F).
 Avoid high vapor concentrations. Keep the solvent temperature at least
40 °C (72 °F) below the boiling point of the solvent used. This includes
the solvent temperature in the sample compartment. For the solvents
methanol and ethanol keep the solvent temperature at least 25 °C
(45 °F) below the boiling point.
 Do not operate the instrument in an explosive atmosphere.
 Do not use solvents of ignition Class IIC according IEC 60079-20-1 (for
example, carbon disulfide).
 Reduce the volume of substances to the minimum required for the
analysis.
 Never exceed the maximum permissible volume of solvents (8 L) in the
solvent cabinet. Do not use bottles that exceed the maximum
permissible volume as specified in the usage guideline for solvent
cabinet.
 Ground the waste container.
 Regularly check the filling level of the waste container. The residual free
volume in the waste container must be large enough to collect the waste
liquid.
 To achieve maximal safety, regularly check the tubing for correct
installation.

For details, see the usage guideline for the solvent cabinet. A printed copy of the
NOTE guideline has been shipped with the solvent cabinet, electronic copies are
available in the Agilent Information Center or via the Internet.

For details on correct installation, see separate installation documentation.

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4 Preparing the Detector
Leak and Waste Handling

Waste Concept
1 Agilent recommends using the 6 L waste can with 1 Stay Safe cap GL45 with
4 ports (5043-1221) for optimal and safe waste disposal. If you decide to use
your own waste solution, make sure that the tubes don't immerse in the liquid.

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4 Preparing the Detector
Setting up an Analysis

Setting up an Analysis

This chapter may be used to


• Prepare the system,
• Get to know the set up of an HPLC analysis and
• Use it as an instrument check to demonstrate that all modules of the system
are correctly installed and connected. It is not a test of the instrument
performance.
• Learn about special settings

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4 Preparing the Detector
Setting up an Analysis

Before Using the System


Solvent Information
Observe recommendations on the use of solvents in chapter “Solvents” in the
pump’s reference manual.

Priming and Purging the System


When the solvents have been exchanged or the pumping system has been turned
off for a certain time (for example, overnight) oxygen will re-diffuse into the
solvent channel between the solvent reservoir, vacuum degasser (when available
in the system) and the pump. Solvents containing volatile ingredients will slightly
lose these. Therefore priming of the pumping system is required before starting
an application.
Table 6 Choice of Priming Solvents for Different Purposes

Activity Solvent Comments


After an installation Isopropanol Best solvent to flush air out of the system

When switching between reverse phase and Isopropanol Best solvent to flush air out of the system
normal phase (both times)

After an installation Ethanol or Methanol Alternative to Isopropanol (second choice) if no


Isopropanol is available
To clean the system when using buffers Bidistilled water Best solvent to re-dissolve buffer crystals

After a solvent change Bidistilled water Best solvent to re-dissolve buffer crystals

After the installation of normal phase seals Hexane + 5% Isopropanol Good wetting properties
(P/N 0905-1420)

The pump should never be used for priming empty tubings (never let the pump
NOTE run dry). Use a syringe to draw enough solvent for completely filling the tubings
to the pump inlet before continuing to prime with the pump.

1 Open the purge valve of your pump (by turning it counterclockwise) and set
flow rate to 3 – 5 mL/min.
2 Flush all tubes with at least 30 mL of solvent.
3 Set flow to required value of your application and close the purge valve.

Pump for approximately 10minutes before starting your application.


NOTE

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4 Preparing the Detector
Setting up an Analysis

Requirements and Conditions


What You Will Need
The table below lists the items you need to have for the set up of the analysis.
Some of these are optional (not required for the basic system).
Table 7 What you will need

Agilent 1200 Infinity Series system Pump (plus degassing)

Autosampler

Detector, standard flow cell installed

Degasser (optional)

Column Compartment (optional)

Agilent CDS

System should be correctly set up for LAN


communication with the Agilent ChemStation

Column: Zorbax Eclipse XDB-C18, 4.6 x 150 mm, 5 µm


(993967-902) or an equivalent column

Standard: Agilent isocratic checkout sample (01080-68704)

Conditions
A single injection of the isocratic test standard is made under the conditions
given in Table 8 on page 56:
Table 8 Conditions

Flow 1.5 mL/min

Stoptime 8 min

Solvent 100% (30% water/70% Acetonitrile)

Temperature Ambient

Wavelength sample 254 nm

Injection Volume 1 µL

Column Temperature (optional): 25 °C or ambient

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4 Preparing the Detector
Setting up an Analysis

Typical Chromatogram
A typical chromatogram for this analysis is shown in Figure 9 on page 57. The
exact profile of the chromatogram will depend on the chromatographic
conditions. Variations in solvent quality, column packing, standard concentration
and column temperature will all have a potential effect on peak retention and
response.

Figure 9 Typical Chromatogram with UV-detector

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4 Preparing the Detector
Setting up an Analysis

Preparing the Detector


For best performance of the detector
• Let the lamp warm-up and stabilize for at least one hour (initial turn on of the
module requires a longer time depending on the environment and the
application needs); refer to “Specification Conditions” on page 35.
• For high sensitivity measurements, a stable environment is required; refer to
“Environment” on page 27. Prevent drafts from air condition systems.
• Setting an appropriate reference wavelength could improve the baseline
behavior.
• Do not work with removed/open front panels/doors. When the system
includes a G1316 TCC (typically located below the detector) and its front
panel is removed while the TCC is set to high temperatures, the up-streaming
air could influence the stability of the detector baseline.

Preparing the HPLC System


1 Turn on the control software and the monitor.
2 Turn on the modules.
3 Start the control software. The screen should show all modules and the
system status is Not Ready.
4 Turn on the modules that require conditioning:
a Detector lamp (warm-up for at least 60 min to get a stable baseline).
b Column compartment (set temperature as required).
c Pump (purge).
d Sampler (prepare the standard isocratic sample into a vial).
e Solvents (fill water and Acetontrile into the solvent bottles).
5 Load the default method.
6 Pump the water/acetonitrile (30/70 %) mobile phase through the column for
10 min for equilibration.

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4 Preparing the Detector
Setting up an Analysis

7 Select the menu item Run Control > Sample Info and enter information about
this application. Click OK to leave this screen.

Figure 10 Sample Info

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4 Preparing the Detector
Setting up an Analysis

Running the Sample and Verifying the Results


1 To start a run select the menu item RunControl > Run Method.
2 This will start the modules and the online plot on the Agilent ChemStation will
show the resulting chromatogram.

Figure 11 Chromatogram with Isocratic Test Sample

Information about using the Data Analysis functions can be obtained from the
NOTE Using your ChemStation manual supplied with your system.

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4 Preparing the Detector
Solvent Information

Solvent Information

Observe the following recommendations on the use of solvents.


• Follow the recommendations for avoiding the growth of algae, see the pump
manuals.
• Small particles can permanently block capillaries and valves. Therefore,
always filter solvents through 0.22 µm filters.
• Avoid or minimize the use of solvents that may corrode parts in the flow path.
Consider specifications for the pH range given for different materials such as
flow cells, valve materials etc. and recommendations in subsequent sections.

General Information about Solvent/Material


Compatibility
Materials in the flow path are carefully selected based on Agilent’s experiences in
developing highest-quality instruments for HPLC analysis over several decades.
These materials exhibit excellent robustness under typical HPLC conditions. For
any special condition, please consult the material information section or contact
Agilent.

Disclaimer
Subsequent data was collected from external resources and is meant as a
reference. Agilent cannot guarantee the correctness and completeness of such
information. Data is based on compatibility libraries, which are not specific for
estimating the long-term life time under specific but highly variable conditions of
UHPLC systems, solvents, solvent mixtures and samples. Information can also
not be generalized due to catalytic effects of impurities like metal ions,
complexing agents, oxygen etc. Apart from pure chemical corrosion, other
effects like electro corrosion, electrostatic charging (especially for
non-conductive organic solvents), swelling of polymer parts etc. need to be
considered. Most data available refers to room temperature (typically 20 – 25 °C,
68 – 77 °F). If corrosion is possible, it usually accelerates at higher temperatures.
If in doubt, please consult technical literature on chemical compatibility of
materials.

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4 Preparing the Detector
Solvent Information

MP35N
MP35N is a nonmagnetic, nickel-cobalt-chromium-molybdenum alloy
demonstrating excellent corrosion resistance (for example, against nitric and
sulfuric acids, sodium hydroxide, and seawater) over a wide range of
concentrations and temperatures. In addition, this alloy shows exceptional
resistance to high-temperature oxidation. Due to excellent chemical resistance
and toughness, the alloy is used in diverse applications: dental products, medical
devices, nonmagnetic electrical components, chemical and food processing
equipment, marine equipment. Treatment of MP35N alloy samples with 10 %
NaCl in HCl (pH 2.0) does not reveal any detectable corrosion. MP35N also
demonstrates excellent corrosion resistance in a humid environment. Although
the influence of a broad variety of solvents and conditions has been tested, users
should keep in mind that multiple factors can affect corrosion rates, such as
temperature, concentration, pH, impurities, stress, surface finish, and dissimilar
metal contacts.

Polyphenylene Sulfide (PPS)


Polyphenylene sulfide has outstanding stability even at elevated temperatures. It
is resistant to dilute solutions of most inorganic acids, but it can be attacked by
some organic compounds and oxidizing reagents. Nonoxidizing inorganic acids,
such as sulfuric acid and phosphoric acid, have little effect on polyphenylene
sulfide, but at high concentrations and temperatures, they can still cause material
damage. Nonoxidizing organic chemicals generally have little effect on
polyphenylene sulfide stability, but amines, aromatic compounds, and
halogenated compounds may cause some swelling and softening over extended
periods of time at elevated temperatures. Strong oxidizing acids, such as nitric
acid (> 0.1 %), hydrogen halides (> 0.1 %), peroxy acids (> 1 %), or chlorosulfuric
acid degrade polyphenylene sulfide. It is not recommended to use polyphenylene
sulfide with oxidizing material, such as sodium hypochlorite and hydrogen
peroxide. However, under mild environmental conditions, at low concentrations
and for short exposure times, polyphenylene sulfide can withstand these
chemicals, for example, as ingredients of common disinfectant solutions.

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4 Preparing the Detector
Solvent Information

PEEK
PEEK (Polyether-Ether Ketones) combines excellent properties regarding
biocompatibility, chemical resistance, mechanical and thermal stability. PEEK is
therefore the material of choice for UHPLC and biochemical instrumentation.
It is stable in the specified pH range (for the Bio-Inert LC system: pH 1 – 13, see
bio-inert module manuals for details), and inert to many common solvents.
There is still a number of known incompatibilities with chemicals such as
chloroform, methylene chloride, THF, DMSO, strong acids (nitric acid > 10 %,
sulfuric acid > 10 %, sulfonic acids, trichloroacetic acid), halogens or aqueous
halogen solutions, phenol and derivatives (cresols, salicylic acid, and so on).
When used above room temperature, PEEK is sensitive to bases and various
organic solvents, which can cause it to swell. Under such conditions, normal
PEEK capillaries are sensitive to high pressure. Therefore, Agilent uses stainless
steel cladded PEEK capillaries in bio-inert systems. The use of stainless steel
cladded PEEK capillaries keeps the flow path free of steel and ensures pressure
stability up to 600 bar. If in doubt, consult the available literature about the
chemical compatibility of PEEK.

Polyimide
Agilent uses semi-crystalline polyimide for rotor seals in valves and needle seats
in autosamplers. One supplier of polyimide is DuPont, which brands polyimide as
Vespel, which is also used by Agilent.
Polyimide is stable in a pH range between 1 and 10 and in most organic solvents.
It is incompatible with concentrated mineral acids (e.g. sulphuric acid), glacial
acetic acid, DMSO and THF. It is also degraded by nucleophilic substances like
ammonia (e.g. ammonium salts in basic conditions) or acetates.

Polyethylene (PE)
Agilent uses UHMW (ultra-high molecular weight)-PE/PTFE blends for yellow
piston and wash seals, which are used in 1290 Infinity pumps, 1290 Infinity II
pumps, the G7104C and for normal phase applications in 1260 Infinity pumps.
Polyethylene has a good stability for most common inorganic solvents including
acids and bases in a pH range of 1 to 12.5. It is compatible with many organic
solvents used in chromatographic systems like methanol, acetonitrile and
isopropanol. It has limited stability with aliphatic, aromatic and halogenated
hydrocarbons, THF, phenol and derivatives, concentrated acids and bases. For
normal phase applications, the maximum pressure should be limited to 200 bar.

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4 Preparing the Detector
Solvent Information

Tantalum (Ta)
Tantalum is inert to most common HPLC solvents and almost all acids except
fluoric acid and acids with free sulfur trioxide. It can be corroded by strong bases
(e.g. hydroxide solutions > 10 %, diethylamine). It is not recommended for the use
with fluoric acid and fluorides.

Stainless Steel (SST)


Stainless steel is inert against many common solvents. It is stable in the
presence of acids and bases in a pH range of 1 to 12.5. It can be corroded by
acids below pH 2.3. It can also corrode in following solvents:
• Solutions of alkali halides, their respective acids (for example, lithium iodide,
potassium chloride, and so on) and aqueous solutions of halogens.
• High concentrations of inorganic acids like nitric acid, sulfuric acid and
organic solvents especially at higher temperatures (replace, if your
chromatography method allows, by phosphoric acid or phosphate buffer
which are less corrosive against stainless steel).
• Halogenated solvents or mixtures which form radicals and/or acids, for
example:
2 CHCl3 + O2→ 2 COCl2 + 2 HCl
This reaction, in which stainless steel probably acts as a catalyst, occurs
quickly with dried chloroform if the drying process removes the stabilizing
alcohol.
• Chromatographic grade ethers, which can contain peroxides (for example,
THF, dioxane, diisopropylether). Such ethers should be filtered through dry
aluminium oxide which adsorbs the peroxides.
• Solutions of organic acids (acetic acid, formic acid, and so on) in organic
solvents. For example, a 1 % solution of acetic acid in methanol will attack
steel.
• Solutions containing strong complexing agents (for example, EDTA, ethylene
diamine tetra-acetic acid).
• Mixtures of carbon tetrachloride with isopropanol or THF.

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4 Preparing the Detector
Solvent Information

Titanium (Ti)
Titanium is highly resistant to oxidizing acids (for example, nitric, perchloric and
hypochlorous acid) over a wide range of concentrations and temperatures. This
is due to a thin oxide layer on the surface, which is stabilized by oxidizing
compounds. Non-oxidizing acids (for example, hydrochloric, sulfuric and
phosphoric acid) can cause slight corrosion, which increases with acid
concentration and temperature. For example, the corrosion rate with 3 % HCl
(about pH 0.1) at room temperature is about 13 μm/year. At room temperature,
titanium is resistant to concentrations of about 5 % sulfuric acid (about pH 0.3).
Addition of nitric acid to hydrochloric or sulfuric acids significantly reduces
corrosion rates. Titanium is sensitive to acidic metal chlorides like FeCl3 or CuCl2.
Titanium is subject to corrosion in anhydrous methanol, which can be avoided by
adding a small amount of water (about 3 %). Slight corrosion is possible with
ammonia > 10 %.

Diamond-Like Carbon (DLC)


Diamond-Like Carbon is inert to almost all common acids, bases and solvents.
There are no documented incompatibilities for HPLC applications.

Fused silica and Quartz (SiO2)


Fused silica is used in Max Light Cartridges. Quartz is used for classical flow cell
windows. It is inert against all common solvents and acids except hydrofluoric
acid and acidic solvents containing fluorides. It is corroded by strong bases and
should not be used above pH 12 at room temperature. The corrosion of flow cell
windows can negatively affect measurement results. For a pH greater than 12,
the use of flow cells with sapphire windows is recommended.

Gold
Gold is inert to all common HPLC solvents, acids and bases within the specified
pH range. It can be corroded by complexing cyanides and concentrated acids like
aqua regia.

Zirconium Oxide (ZrO2)


Zirconium Oxide is inert to almost all common acids, bases and solvents. There
are no documented incompatibilities for HPLC applications.

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4 Preparing the Detector
Solvent Information

Platinum/Iridium
Platinum/Iridium is inert to almost all common acids, bases and solvents. There
are no documented incompatibilities for HPLC applications.

Fluorinated polymers (PTFE, PFA, FEP, FFKM, PVDF)


Fluorinated polymers like PTFE (polytetrafluorethylene), PFA (perfluoroalkoxy),
and FEP (fluorinated ethylene propylene) are inert to almost all common acids,
bases, and solvents. FFKM is perfluorinated rubber, which is also resistant to
most chemicals. As an elastomer, it may swell in some organic solvents like
halogenated hydrocarbons.
TFE/PDD copolymer tubings, which are used in all Agilent degassers except
G1322A/G7122A, are not compatible with fluorinated solvents like Freon,
Fluorinert, or Vertrel. They have limited life time in the presence of
hexafluoroisopropanol (HFIP). To ensure the longest possible life with HFIP, it is
best to dedicate a particular chamber to this solvent, not to switch solvents, and
not to let dry out the chamber. For optimizing the life of the pressure sensor, do
not leave HFIP in the chamber when the unit is off.
The tubing of the leak sensor is made of PVDF (polyvinylidene fluoride), which is
incompatible with the solvent DMF (dimethyl formamide).

Sapphire, Ruby and Al2O3-based ceramics


Sapphire, ruby and ceramics based on aluminum oxide Al2O3 are inert to almost
all common acids, bases and solvents. There are no documented
incompatibilities for HPLC applications.

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5 Optimizing the Detector

Optimizing the Detector Performance 68


Optimization Overview 69
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion 71
Flow Cell Path Length 71
Peak width (response time) 73
Sample and Reference Wavelength and Bandwidth 74
Slit Width 78
Optimizing Spectral Acquisition (DAD only) 79
Margin for Negative Absorbance 80
Optimizing Selectivity 81
Quantifying Coeluting Peaks by Peak Suppression 81
Optimizing the Detector Regarding to the System 83
Delay Volume and Extra-Column Volume 83
How to Configure the Optimum Delay Volume 83
How to Achieve Higher Sensitivity 84
Warm up of the Detector 89

This chapter provides information on how to optimize the detector.

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5 Optimizing the Detector
Optimizing the Detector Performance

Optimizing the Detector Performance

The detector has a variety of parameters that can be used to optimize


performance. Depending on whether signal or spectral data need to be
optimized, different settings are recommended. The following sections describe
optimization for:
• signal sensitivity, selectivity and linearity,
• spectral sensitivity and resolution (DAD only), and
• disk space required for storing data.

The information in this chapter should be seen as a basic introduction to diode


NOTE array detector techniques. Some of these techniques may not be available in the
instrument software controlling the detector.

How to Get the Best Detector Performance


The information below will guide you on how to get the best detector
performance. Follow these rules as a start for new applications. It gives
rules-of-thumb for optimizing detector parameters.

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5 Optimizing the Detector
Optimization Overview

Optimization Overview

Table 9 Optimization Overview

Parameter Impact

1 Selection of flow cell • peak resolution versus sensitivity

• Choose flow cell according to used column, see Figure 12 on page 70.

2 Connection of flow cell • chromatographic resolution

• For flow rates from 0.5 mL/min connect column using the
zero-dead-volume fittings of the detector.
• For small column i.d. (e.g 1 mm) the inlet capillary of the micro flow cell can
be connected directly to the column.

3 Setting the peak width (response time) • peak resolution versus sensitivity
versus disk space

• Use peak width according Figure 12 on page 70 as starting point.


• Set the peak-width close to the width of a narrow peak of interest in your
chromatogram.

4 Setting wavelength and bandwidth

• Sample wavelength:
• Never miss a peak by the use of a browser wavelength like 250 nm with • sensitivity versus selectivity
100 nm bandwidth.
• Select specific wavelength with reduced bandwidth if you need • sensitivity versus linearity
selectivity, e.g. 250,10 nm and 360,100 nm as reference wavelength.
• Set the sample wavelength to a peak or valley in the spectrum to get
best linearity for high concentrations.

• Reference wavelength:
• Select the reference wavelength with broad bandwidth (30...100 nm) • baseline drift due to RI effects.
wavelength range where your analytes have little or no absorbance (e.g.
sample at 254 nm, reference at 320 nm).

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5 Optimizing the Detector
Optimization Overview

Table 9 Optimization Overview

Parameter Impact

5 Setting the slit width

• Use 4 nm slit for normal applications. • spectral resolution, sensitivity and


• Use narrow slit (e.g 1 nm) if your analytes have narrow absorbance bands linearity.
and for high concentrations.
• Use a wide slit (e.g. 16 nm) to detect very low concentrations.
• Optimizing spectral acquisition (DAD only)
• Select spectra acquisition mode according to your needs.
• Set the spectral wavelength range (for colorless samples 190...400 nm is
sufficient).
• Set step to 4 nm for normal use; set small step (and slit width) if high
resolution of spectra with fine structure is wanted.

Typical column Typical peak Recommended flow cell


length width

T <= 5 cm 0.025 min Micro or


Semi-nano

10 cm 0.05 min Semi-micro


flow cell High pressure
flow cell for
20 cm 0.1 min Standard pressures
flow cell above 100bar

>= 40 cm 0.2 min

Typical flow 0.01 ... 0.2 0.2 ... 0.4 0.4 ... 0.4 1 ... 5 0.01 ... 5
rate ml/min ml/min ml/min ml/min ml/min

Internal column diameter 0.5 ... 1 mm 2.1 mm 3.0 mm 4.6 mm

Figure 12 Choosing a Flow Cell in HPLC

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Optimizing for Sensitivity, Selectivity, Linearity


and Dispersion

Flow Cell Path Length


Lambert-Beer’s law shows a linear relationship between the flow cell path length
and absorbance.

where
T is the transmission, defined as the quotient of the intensity of the transmitted
light I divided by the intensity of the incident light, I0,

 is the extinction coefficient, which is a characteristic of a given substance under


a precisely-defined set of conditions of wavelength, solvent, temperature and
other parameters,
C [mol/L] is the concentration of the absorbing species, and
d [m] is the path length of the cell used for the measurement.
Therefore, flow cells with longer path lengths yield higher signals. Although noise
usually increases little with increasing path length, there is a gain in
signal-to-noise ratio. For example, in Figure 13 on page 72 the noise increased by
less than 10 % but a 70 % increase in signal intensity was achieved by increasing
the path length from 6 – 10 mm.
When increasing the path length, the cell volume usually increases — in our
example from 5 – 13 µL. Typically, this causes more peak dispersion. As
Figure 13 on page 72 demonstrates, this did not affect the resolution in the
gradient separation in our example.
As a rule-of-thumb the flow cell volume should be about 1/3 of the peak volume
at half height. To determine the volume of your peaks, take the peak width as
reported in the integration results multiply it by the flow rate and divide it by 3).

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Analysis of pesticide standard

6-mm optical path length


10-mm optical path length
Absorbance

Time (min)
Figure 13 Influence of Cell Path Length on Signal Height

Traditionally LC analysis with UV detectors is based on comparing


measurements with internal or external standards. To check photometric
accuracy of the detector it is necessary to have more precise information on path
lengths of the flow cells.
The correct response is:
expected response * correction factor
Please find below the details of the flow cells:
Table 10 Correction factors for flow cells

Flow cell Path length (actual) Correction factor

Standard flow cell, 10 mm, 13 µL, 120 bar ( 12 MPa) 9.80±0.07 mm 10/9.8
(G1315-60022)

Semi-micro flow cell, 6 mm, 5 µL, 120 bar ( 12 MPa) 5.80±0.07 mm 6/5.8
(G1315-60025)

Micro flow cell, 3 mm, 2 µL, 120 bar ( 12 MPa) (G1315-60024) 3.00+0.05 mm/-0.07 mm 3/3

Semi-nano flow cell kit, 10 mm, 500 nL, 5 MPa (G1315-68724) 10.00±0.02 mm 10/10

Nano flow cell kit, 6 mm, 80 nL, 5 MPa ( G1315-68716) 6.00±0.02 mm 6/6

Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar ( 12 MPa) for 9.80±0.07 mm 10/9.8
MWD/DAD, includes 0890-1763 – 0.18 x 1500 mm PEEK
capillary and 5063-6591 – PEEK fittings (G5615-60022)

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Peak width (response time)


Response time describes how fast the detector signal follows a sudden change
of absorbance in the flow cell. The detector uses digital filters to adapt response
time to the width of the peaks in your chromatogram. These filters do not affect
peak area nor peak symmetry. When set correctly, such filters reduce baseline
noise significantly ( Figure 14 on page 73), but reduce peak height only slightly. In
addition, these filters reduce the data rate to allow optimum integration and
display of your peaks and to minimize disk space required to store
chromatograms and spectra.

Unfiltered

Response time
0.05 min

Response time
0.1 min

Figure 14 Influence of Response Time on Signal and Noise

Table 11 on page 74 list the filter choices of the detector. To get optimum results,
set peak width as close as possible to a narrow peak of interest in your
chromatogram. Response time will the be approximately 1/3 of the peak width,
resulting in less than 5 % peak-height reduction and less than 5 % additional peak
dispersion. Decreasing the peak width setting in the detector will result in less
than 5 % gain in peak height but baseline noise will increase by a factor of 1.4 for
a factor of 2 response-time reduction. Increasing peak width (response time) by
factor of two from the recommended setting (over-filtering) will reduce peak
height by about 20 % and reduce baseline noise by a factor of 1.4. This gives you
the best possible signal-to-noise ratio, but may affect peak resolution.

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Table 11 Peak Width — Response Time — Data Rate (G7115A/G7165A)

Peak width at half Response [s] Scan data Scan data Scan data
height [min]1 rate[Hz] ≤251 rate[Hz] ≤501 rate[Hz] > 501
pts/scan pts/scan pts/scan

< 0.0015625 0.015625 120 120 40 20

> 0.0015625 0.03125 120 120 40 20

> 0.003125 0.0625 80 80 40 20

> 0.00625 0.125 40 40 40 20

> 0.0125 0.25 20 20 20 20

> 0.025 0.5 10 10 10 10

> 0.05 1 5 5 5 5

> 0.1 2 2.5 2.5 2.5 2.5

> 0.2 4 1.25 1.25 1.25 1.25

> 0.4 8 0.625 0.625 0.625 0.625

> 0.85 16 0.3125 0.3125 0.3125 0.3125

1 Values in the User Interface may be rounded.

Sample and Reference Wavelength and Bandwidth


The detector measures absorbance simultaneously at wavelengths from 190 to
950 nm. Two lamps provide good sensitivity over the whole wavelength range.
The deuterium discharge lamp provides the energy for the UV range (190 to
400 nm) and the tungsten lamp emits light from 400 to 950 nm for the visible
and short wave near infrared.
If you know little about the analytes in your sample, use both lamps and store all
spectra over the full wavelength range. This provides full information but fills up
your disk space rather quickly. Spectra can be used to check a peak’s purity and
identity. Spectral information is also useful to optimize wavelength settings for
your chromatographic signal.

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

The detector can compute and store at run time up to 8 signals with these
properties:
• sample wavelength, the center of a wavelength band with the width of sample
bandwidth (BW), and optionally
• reference wavelength, the center of a wavelength band with the width of
reference bandwidth.
The signals comprises a series of data points over time, with the average
absorbance in the sample wavelength band minus the average absorbance of
the reference wavelength band.
Signal A in the detector default method is set to sample 250,100, reference
360,100, that is, the average absorbance from 200 – 300 nm minus the average
absorbance from 300 – 400 nm. As all analytes show higher absorbance at
200 – 300 nm than at 300 – 400 nm, this signal will show you virtually every
compound which can be detected by UV absorbance.
Many compounds show absorbance bands in the spectrum. Figure 15 on
page 76 shows the spectrum of anisic acid as an example.
To optimize for lowest possible detectable concentrations of anisic acid, set the
sample wavelength to the peak of the absorbance band (that is, 252 nm) and the
sample bandwidth to the width of the absorbance band (that is, 30 nm). A
reference of 360,100 is adequate. Anisic acid does not absorb in this range.
If you work with high concentrations, you may get better linearity above 1.5 AU by
setting the sample wavelength to a valley in the spectrum, like 225 nm for anisic
acid.

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

sample wavelength 252 nm Anisic acid

Absorbance (mAU) Reference bandwidth 100 nm

30 nm
bandwidth
Reference wavelength 360

Wavelength (nm)

Figure 15 Optimization of Wavelength Setting

A wide bandwidth has the advantage of reducing noise by averaging over a


wavelength range — compared to a 4 nm bandwidth, the baseline noise is
reduced by a factor of approximately 2.5, whereas the signal is about 75 % of a 4
nm wide band. The signal-to-noise ratio for a 30 nm bandwidth is twice that for a
4 nm bandwidth in our example.

Bandwidth

30 nm
12 nm

4 nm

Figure 16 Influence of Bandwidth on Signal and Noise

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Because the detector averages absorbance values that are calculated for each
wavelength, using a wide bandwidth does not negatively impact linearity.
The use of a reference wavelength is highly recommended to further reduce
baseline drift and wander induced by room temperature fluctuations or refractive
index changes during a gradient.
An example of the reduction of baseline drifts is shown in Figure 17 on page 77
for PTH-amino acids. Without a reference wavelength, the chromatogram drifts
downwards due to refractive index changes induced by the gradient. This is
almost completely eliminated by using a reference wavelength. With this
technique, PTH-amino acids can be quantified in the low picomole range even in
a gradient analysis.
PTH-ASN

PTH-PHE
PTH-ALA

PTH-PRO
PTH-ARG

1pmol each

Wavelength
267 nm
Reference 380nm

Wavelength
267nm
No reference

Time (min)

Grad.: 0.02 m KH2 PO4 /ACN from 12% ACN to 45% ACN in 12 min

Figure 17 Gradient Analysis of PTH-Amino Acids (1 pmol each), with and without Reference

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Slit Width
The detector has a variable slit at the entrance of the spectrograph. This is an
effective tool to adapt the detector to changing demand of different analytical
problems.
A narrow slit provides spectral resolution for analytes with very fine structures in
the absorbance spectrum. An example of such a spectrum is benzene. The five
main absorbance bands (fingers) are only 2.5 nm wide and just 6 nm apart from
each other.

16 nm

4 nm

1 nm

Figure 18 Benzene at 1, 4 and 16 nm slit width (principle)

A wide slit uses more of the light shining through the flow cell. This gives lower
baseline noise as shown in Figure 19 on page 78.

Slit width 1 nm

Slit width 4 nm

Slit width 16 nm

Figure 19 Influence of the Slit Width on Baseline Noise

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

However, with a wider slit, the spectrograph’s optical resolution (its ability to
distinguish between different wavelengths) diminishes. Any photodiode receives
light within a range of wavelength determined by the slit width. This explains why
the fine spectral structure of benzene disappears when using a 16-nm wide slit.
Furthermore, the absorbance is no longer strictly linear with concentration for
wavelengths at a steep slope of a compound’s spectrum.
Substances with fine structures and steep slopes like benzene are very rare.
In most cases the width of absorbance bands in the spectrum is more like 30 nm
as with anisic acid (Figure 15 on page 76).
In most situations, a slit width of 4 nm will give the best results.
Use a narrow slit (1 or 2 nm) if you want to identify compounds with fine spectral
structures or if you need to quantify at high concentrations (> 1000 mAU) with a
wavelength at the slope of the spectrum. Signals with a wide bandwidth can be
used to reduce baseline noise. Because (digital) bandwidth is computed as
average of absorbance, there is no impact on linearity.
Use a wide (8 or 16 nm) slit when your sample contains very small
concentrations. Always use signals with bandwidth at least as wide as the slit
width.

Optimizing Spectral Acquisition (DAD only)


Storage of all spectra consumes a lot of disk space. It is very useful to have all
spectra available during optimization of a method or when analyzing unique
samples. However when running many samples of the same type, the large size
of data files with all spectra may become a burden. The detector provides
functions to reduce the amount of data, yet retaining the relevant spectral
information.
Range
Only the wavelength range where the compounds in your sample absorb
contains information that is useful for purity checks and library searches.
Reducing the spectrum storage range saves disk space.
Step
Most substances have broad absorbance bands. Display of spectra, peak purity
and library search works best if a spectrum contains 5 to 10 data points per
width of the absorbance bands. For anisic acid (the example used before) a step
of 4 nm would be sufficient. However a step of 2 nm gives a more optimal
display of the spectrum.

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5 Optimizing the Detector
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion

Margin for Negative Absorbance


The detector adjusts its gain during balance such that the baseline may drift
slightly negative (about -100 mAU). In some special case, for example, when
gradient with absorbing solvents are used, the baseline may drift to more
negative values.
Only for such cases, increase the margin for negative absorbance to avoid
overflow of the analog-to-digital converter.

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5 Optimizing the Detector
Optimizing Selectivity

Optimizing Selectivity

Quantifying Coeluting Peaks by Peak Suppression


In chromatography, two compounds may often elute together. A conventional
dual-signal detector can only detect and quantify both compounds independently
from each other if their spectra do not overlap. However, in most cases this is
highly unlikely.
With a dual-channel detector based on diode-array technology, quantifying two
compounds is possible even when both compounds absorb over the whole
wavelength range. The procedure is called peak suppression or signal
subtraction. As an example, the analysis of hydrochlorothiazide in the presence
of caffeine is described. If hydrochlorothiazide is analyzed in biological samples,
there is always a risk that caffeine is present which might interfere
chromatographically with hydrochlorothiazide. As the spectra in Figure 20 on
page 81 shows, hydrochlorothiazide is best detected at 222 nm, where caffeine
also shows significant absorbance. It would therefore be impossible, with a
conventional variable wavelength detector, to detect hydrochlorothiazide
quantitatively when caffeine is present.

WL1 (204 nm, caffeine)


WL2 (222 nm, hydrochlorothiazide)
WL3 (260 nm, reference to suppress)
hydrochlorothiazide)
WL4 (282 nm, reference to suppress caffeine)

WL3 WL4

WL1 WL2 Wavelength (nm)

Figure 20 Wavelength Selection for Peak Suppression

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5 Optimizing the Detector
Optimizing Selectivity

With a UV-visible detector based on a diode array and the correct choice of a
reference wavelength setting, quantitative detection is possible. To suppress
caffeine, the reference wavelength must be set to 282 nm. At this wavelength,
caffeine shows exactly the same absorbance as at 222 nm. When the
absorbance values are subtracted from each another, any indication of the
presence of caffeine is eliminated. In the same way, hydrochlorothiazide can be
suppressed if caffeine is to be quantified. In this case the wavelength is set to
204 nm and the reference wavelength to 260 nm. Figure 21 on page 82 shows
the chromatographic results of the peak suppression technique.
The trade-off for this procedure is a loss in sensitivity. The sample signal
decreases by the absorbance at the reference wavelength relative to the signal
wavelength. Sensitivity may be decreased by as much as 10–30 %.

Hydrochlorothiazide Hydrochlorothiazide
and caffeine and caffeine
Wavelength 204 nm Wavelength 222 nm
No reference No reference

Hydrochlorothiazides Caffeine suppressed


uppressed
Wavelength 204 nm Wavelength 222 nm
Reference 260 nm Reference 282 nm

Time (min) Time (min)

Figure 21 Peak Suppression Using Reference Wavelength

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

Optimizing the Detector Regarding to the


System

Delay Volume and Extra-Column Volume


The delay volume is defined as the system volume between the point of mixing in
the pump and the front of the column.
The extra-column volume is defined as the volume between the injection point
and the detection point, excluding the volume in the column.

Extra-Column Volume
Extra-column volume is a source of peak dispersion that will reduce the
resolution of the separation and so should be minimized. Smaller diameter
columns require proportionally smaller extra-column volumes to keep peak
dispersion at a minimum.
In a liquid chromatograph the extra-column volume will depend on the
connection tubing between the autosampler, column and detector; and on the
volume of the flow cell in the detector. The extra-column volume is minimized
with the Agilent InfinityLab LC Series system due to the narrow-bore (0.12 mm
i.d.) tubing, the low-volume heat exchangers in the column compartment and the
flow cell in the detector.

How to Configure the Optimum Delay Volume


To maintain resolution in the Agilent 1290 Infinity II DAD/Agilent 1290 Infinity
DAD FS the 10 mm Max-Light cartridge cell has a low dispersion volume (
volume 1.0 µL) and no further volume optimization is required. In situations
where the alternative 60 mm Max-Light high sensitivity cell is used to get higher
sensitivity the cell volume is optimized for the use with 3 mm and 4.6 mm inner
diameter columns.

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

How to Achieve Higher Sensitivity


The detector has a number of parameters that are used to optimize
performance. The following sections describe how the detector parameters
affect performance characteristics:
• Flow cell affects sensitivity,
• Wavelength and bandwidth affect sensitivity, selectivity and linearity,
• Slit width affects sensitivity, spectral resolution and linearity,
• Peak width affects sensitivity and resolution.

Flow Cell
The Max-Light cartridge flow cell has a standard 10 mm path length and is
optimized for minimal volume and dispersion ( volume 1.0 µL). It has high light
transmission minimizing noise to reduce noise due to the optofluidic waveguide.
It is suitable for use with a wide range of analytical columns from short
narrow-bore columns to long standard diameter (4.6 mm) columns. Generally the
peak dispersion volume (calculated from peak width x flow rate) should be
greater than about 2 µL for this cell (for example 0.02 min x 200 µL/min = 4 µL).
The Max-Light high sensitivity cell has a path length of 60 mm and this will give
between three and five times increase in signal-to-noise values depending on the
application conditions. The dispersion volume is fractionally increased compared
to the standard cell.

Wavelength and Bandwidth


The detector measures absorbance simultaneously at wavelengths from 190 nm
to 640 nm using diode-array detection. A UV-lamp provides good sensitivity over
the whole wavelength range. The diode-array detector (DAD) can simultaneously
compute and send to the data system up to eight chromatographic signals and
the full-range spectra at every time point.
A UV chromatogram or signal is a plot of absorbance data versus time and is
defined by its wavelength and bandwidth.
• The wavelength indicates the center of the detection band.
• The bandwidth defines the wavelength range over which the absorbance
values are averaged to give the result at each time point.

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

For example, a signal at wavelength 250 nm with a bandwidth of 16 nm will be an


average of the absorbance data from 242 nm to 258 nm. Additionally, a reference
wavelength and reference bandwidth can be defined for each signal. The average
absorbance from the reference bandwidth centered on the reference wavelength
will be subtracted from its equivalent value at the signal wavelength to produce
the output chromatogram.
The signal wavelength and bandwidth can be chosen so that they are optimized
for:
• Broad band universal detection
• Narrow band selective detection
• Sensitivity for a specific analyte.
Broad band or universal detection works by having a wide bandwidth to detect
any species with absorbance in that range. For example, to detect all absorbing
molecules between 200 nm and 300 nm set a signal at 250 nm with a bandwidth
of 100 nm. The disadvantage is that sensitivity will not be optimal for any one of
those molecules. Narrow band or selective detection is used most often. The UV
spectrum for a particular molecule is examined and an appropriate absorbance
maximum is selected. If possible, the range where solvents absorb strongly
should be avoided (below 220 nm for methanol, below 210 nm for acetonitrile).
For example, in Figure 22 on page 86, anisic acid has a suitable absorbance
maximum at 252 nm. A narrow bandwidth of 4 nm to 12 nm generally gives good
sensitivity and is specific for absorbance in a narrow range.
The narrow band can be optimized for sensitivity for a specific molecule. As the
bandwidth is increased the signal is reduced but so is the noise and there will be
an optimum for best S/N. As an approximate guide, this optimum is often close
to the natural bandwidth at half-height of the absorption band in the UV
spectrum. In the anisic acid example this is 30 nm.
The analytical wavelength is usually set at a wavelength maximum to increase
sensitivity to that molecule. The detector is linear up to 2 AU and beyond for
many applications. This offers a wide linear range for concentration. For high
concentration analysis the concentration linear range can be extended by setting
the wavelength to one with a lower absorbance such as a wavelength minimum
or by taking a wider bandwidth which usually includes lower absorbance values.
The use of wavelength maxima and minima for quantitation dates back to
conventional UV detectors which because of mechanical tolerances in moving
gratings needed to avoid steeply sloping parts of the spectrum. Diode-array
based detectors do not have this limitation but for reasons of convention
maxima and minima are chosen in preference to other parts of the spectrum.

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

The reference bandwidth is normally set on a region of the UV spectrum in which


the analyte has no absorbance. This is shown in the spectrum for anisic acid in
Figure 22 on page 86. This spectrum is typical of many small molecules
containing a UV chromophore. For best results the reference has been set so that
it is a wide band as close to the signal wavelength as possible but on a zero
absorbance region. Reference bandwidths of 60 nm to 100 nm are commonly
used. The default reference is 360 nm with a bandwidth of 100 nm. A wide
bandwidth is used because this reduces the noise in the reference signal (from
statistical theory, the error, i.e. noise in this case, is reduced by the square root of
the number of determinations). It is important that the reference bandwidth does
not extend to a part of the spectrum that has some absorbance as this would
then reduce the resulting signal and sensitivity would be reduced. The use of a
reference wavelength can help to reduce drift or wander in the chromatogram
caused by refractive index changes due to room temperature fluctuation or
gradient operation. The effect of a reference signal can be easily tested by setting
two otherwise identical signals, one with and one without a reference signal. If
there is no part of the spectrum with zero absorbance then it will be better to
have the reference signal turned off.

Figure 22 Spectrum of Anisic Acid

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

Peak Width, Response Time and Data Collection Rate


The peak width setting, response time and data rate in the detector are all linked.
The available settings are shown in Table 12 on page 88. It is important to set
this correctly for optimum sensitivity and to preserve the resolution achieved in
the separation.
The detector internally acquires data points faster than is needed for a
chromatogram and processes them to produce the signal seen by the data
system. Part of the processing reduces the data to an appropriate data rate
which allows the chromatographic peaks to be accurately drawn. As with most
analytical determinations groups of readings are effectively averaged to reduce
error in the result. The detector bunches raw data points and produces the output
signal data at the required data collection rate by an electronic filtering process. If
the resulting data rate is too slow (over filtering) the peak heights will be reduced
and the resolution between them reduced; too fast and the data is noisier than it
need be to accurately profile narrow peaks.
The peak width setting in the detector allows the user to correctly set these
parameters without needing any knowledge other than sight of the
chromatogram integration results to see how wide the peaks are. The peak width
setting should be set for the narrowest peak width observed in the
chromatogram. If it is set too wide it will make the peaks appear lower in height
and wider (and potentially less resolved) and if it is set too narrow it will increase
the baseline noise unnecessarily. Essentially the software uses this value to set
the data collection rate such that it collects enough data points over the
narrowest peaks and it is aiming for 15 to 25 points across a peak. The DAD can
collect at a maximum up to 120 Hz if required which would allow enough data
points to be collected over a peak that is only 0.1 s wide. The response time
setting is another way of indicating how this filtering is set. It is measured in
seconds and is about one-third of the peak width value (which is measured in
minutes). It effectively shows how quickly the plotted signal responds to a step
change in the input signal.

The full spectra is not available under all conditions.


NOTE
Based on the data points, the scan data rate is reduced, see Table 12 on page 88.

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5 Optimizing the Detector
Optimizing the Detector Regarding to the System

Table 12 Peak Width — Response Time — Data Rate (G7115A/G7165A)

Peak width at half Response [s] Scan data Scan data Scan data
height [min]1 rate[Hz] ≤251 rate[Hz] ≤501 rate[Hz] > 501
pts/scan pts/scan pts/scan

< 0.0015625 0.015625 120 120 40 20

> 0.0015625 0.03125 120 120 40 20

> 0.003125 0.0625 80 80 40 20

> 0.00625 0.125 40 40 40 20

> 0.0125 0.25 20 20 20 20

> 0.025 0.5 10 10 10 10

> 0.05 1 5 5 5 5

> 0.1 2 2.5 2.5 2.5 2.5

> 0.2 4 1.25 1.25 1.25 1.25

> 0.4 8 0.625 0.625 0.625 0.625

> 0.85 16 0.3125 0.3125 0.3125 0.3125

1 Values in the User Interface may be rounded.

The maximum spectra scan rate depends on the data points per scan, see
NOTE Table 12 on page 88.

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5 Optimizing the Detector
Warm up of the Detector

Warm up of the Detector

Give the optical unit enough time to warm-up and stabilize (> 60 minutes). The
detector is temperature controlled. After turn-on of the detector, it goes through a
cycle of different states:
• 0 to 0.5 minutes the heater control is OFF and the heater element runs at 0 %
duty cycle.
• 0.5 to 1 minutes the heater control is OFF and the heater element runs at 66%
duty cycle. This first minute is used as self-test of the heater functionality.
• 1 to 30 minutes the heater control is OFF and the heater element runs at 40%
duty cycle.
• After 30 minutes the heater control is ON and is working with optimized
parameters to get the optical unit into the optimal temperature window
stabilized.
This cycle starts
• when the detector is turned off/on
• when the lamp is turned off/on
to ensure that the temperature control operates in a defined control range.

The times to stabilize the baseline may vary from instrument to instrument and
NOTE depends on the environment. The example below was done under stable
environmental conditions.

The figures below show the first two hours of a detector warm-up phase. The
lamp was turned on immediately after turn on of the detector.

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5 Optimizing the Detector
Warm up of the Detector

Figure 23 Detector Warm-up – 1st hour

Figure 24 Detector Warm-up – 2nd hour

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6 Troubleshooting and Diagnostics

Available Tests vs User Interfaces 92


Agilent Lab Advisor Software 93
Available Diagnostic Functions vs. Product Level 94

This chapter gives an overview about the troubleshooting and diagnostic


features.

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6 Troubleshooting and Diagnostics
Available Tests vs User Interfaces

Available Tests vs User Interfaces

Depending on the used interface, the available tests and the screens/reports
NOTE may vary.
Preferred tool should be the Agilent Lab Advisor, see “Agilent Lab Advisor
Software” on page 93.
Agilent Lab Advisor B.02.08 or later is required.

Screenshots used within these procedures are based on the Agilent Lab Advisor
software.

Figure 25 Tests in the Agilent Lab Advisor

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6 Troubleshooting and Diagnostics
Agilent Lab Advisor Software

Agilent Lab Advisor Software

The Agilent Lab Advisor Software (basic license, shipped with an Agilent LC
pump) is a standalone product that can be used with or without a
chromatographic data system. Agilent Lab Advisor helps to manage the lab for
high-quality chromatographic results by providing a detailed system overview of
all connected analytical instruments with instrument status, Early Maintenance
Feedback counters (EMF), instrument configuration information, and diagnostic
tests. With the push of a button, a detailed diagnostic report can be generated.
Upon request, the user can send this report to Agilent for a significantly improved
troubleshooting and repair process.
The Agilent Lab Advisor software is available in two versions:
• Lab Advisor Basic
• Lab Advisor Advanced
Lab Advisor Basic is included with every Agilent 1200 Infinity Series and Agilent
InfinityLab LC Series instrument.
The Lab Advisor Advanced features can be unlocked by purchasing a license key,
and include real-time monitoring of instrument actuals, all various instrument
signals, and state machines. In addition, all diagnostic test results, calibration
results, and acquired signal data can be uploaded to a shared network folder. The
Review Client included in Lab Advisor Advanced allows to load and examine the
uploaded data no matter on which instrument it was generated. This makes Data
Sharing an ideal tool for internal support groups and users who want to track the
instrument history of their analytical systems.
The optional Agilent Maintenance Wizard Add-on provides an easy-to-use,
step-by-step multimedia guide for performing preventive maintenance on Agilent
1200 Infinity LC Series instrument.
The tests and diagnostic features that are provided by the Agilent Lab Advisor
software may differ from the descriptions in this manual. For details, refer to the
Agilent Lab Advisor software help files.

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6 Troubleshooting and Diagnostics
Available Diagnostic Functions vs. Product Level

Available Diagnostic Functions vs. Product Level

Table 13 Available Diagnostic Functions vs. Product Level

Product Level
Tests

-ASTM Drift and Noise Test Basic Advanced

-Cell Test Basic Advanced


-D/A Converter Test Basic Advanced

-Dark Current Test Basic Advanced

-Filter Test Basic Advanced

-Holmium Oxide Test Basic Advanced

-Intensity Test Basic Advanced

-Quick Noise Test Basic Advanced

-Self Test Basic Advanced


-Slit Test Basic Advanced

-Wavelength Verification Test Basic Advanced

Calibrations

-Wavelength Calibration Basic Advanced

Tools

-Diagnostic Buffers Basic Advanced


-Module Info Basic Advanced

-Test Chromatogram Basic Advanced

-Spectral Scan Basic Advanced


Controls

-Advanced Method Parameters

-Vis lamp required Advanced

-Analog Output 1 Offset [% Full Advanced


Scale]

-D2 lamp required Advanced

-Analog Output 1 Attenuation Advanced

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6 Troubleshooting and Diagnostics
Available Diagnostic Functions vs. Product Level

Table 13 Available Diagnostic Functions vs. Product Level

Product Level

-Configuration
-Analog Output 1 Range Advanced

-Remote Pulse Duration [s]* Basic Advanced

-Control
-Vis lamp Basic Advanced

-Balance Detector Advanced

-UV Lamp Basic Advanced


-Method Parameters

-Set Signal A Advanced

-Set Signal C Advanced

-Set Data Rate [HZ] Advanced

-Set Signal B Advanced

-Module Information

-Identify Module Basic Advanced


-Special Commands

-Lamp tag required Basic Advanced

-Cell tag required Basic Advanced


-Detector Reset Basic Advanced

-Clear Error Basic Advanced

Statemachines
-UV Lamp Basic Advanced

-Vis Lamp Advanced

Signals

-Signal A [mAU] Advanced

-Lamp Voltage [V] Advanced

-Board Temperature [°C] Advanced


-Optical Temperature [°C] Advanced

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6 Troubleshooting and Diagnostics
Available Diagnostic Functions vs. Product Level

Table 13 Available Diagnostic Functions vs. Product Level

Product Level

EMF Counters
-Accumulated UV Lamp Basic Advanced
On-Time
-Number of UV Lamp Ignitions Basic Advanced

-Accumulated Tungsten Lamp Basic Advanced


On-Time

-Number of Tungsten Lamp Basic Advanced


Ignitions

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7 Error Information

What Are Error Messages 98


General Error Messages 99
Timeout 99
Shutdown 100
Remote Timeout 101
Lost CAN Partner 101
Leak Sensor Short 102
Leak Sensor Open 102
Compensation Sensor Open 103
Compensation Sensor Short 103
Fan Failed 104
Leak 104
Open Cover 105
Cover Violation 105
ERI Messages 106
Detector Error Messages 107
Visible Lamp Current 107
Visible Lamp Voltage 107
Diode Current Leakage 108
UV Lamp Current 108
UV Lamp Voltage 109
UV Ignition Failed 109
UV Heater Current 110
Calibration Values Invalid 110
Holmium Oxide Test Failed 111
Illegal Temperature Value from Sensor on Main Board 111
Illegal Temperature Value from Sensor at Air Inlet 112
Wavelength Recalibration Lost 112
Heater at fan assembly failed 113
Heater Power At Limit 113
DSP Not Running 114

This chapter describes the meaning of error messages, and provides information
on probable causes and suggested actions how to recover from error conditions.

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7 Error Information
What Are Error Messages

What Are Error Messages

Error messages are displayed in the user interface when an electronic,


mechanical, or hydraulic (flow path) failure occurs which requires attention
before the analysis can be continued (for example, repair, or exchange of
consumables is necessary). In the event of such a failure, the red status indicator
at the front of the module is switched on, and an entry is written into the module
logbook.
If an error occurs outside a method run, other modules will not be informed about
this error. If it occurs within a method run, all connected modules will get a
notification, all LEDs get red and the run will be stopped. Depending on the
module type, this stop is implemented differently. For example, for a pump the
flow will be stopped for safety reasons. For a detector, the lamp will stay on in
order to avoid equilibration time. Depending on the error type, the next run can
only be started, if the error has been resolved, for example liquid from a leak has
been dried. Errors for presumably single time events can be recovered by
switching on the system in the user interface.
Special handling is done in case of a leak. As a leak is a potential safety issue and
may have occurred at a different module from where it has been observed, a leak
always causes a shutdown of all modules, even outside a method run.
In all cases, error propagation is done via the CAN bus or via an APG/ERI remote
cable (see documentation for the APG/ERI interface).

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7 Error Information
General Error Messages

General Error Messages

General error messages are generic to all Agilent series HPLC modules and may
show up on other modules as well.

Timeout
Error ID: 0062
The timeout threshold was exceeded.

Probable cause Suggested actions

1 The analysis was completed successfully, Check the logbook for the occurrence and source
and the timeout function switched off the of a not-ready condition. Restart the analysis
module as requested. where required.

2 A not-ready condition was present during a Check the logbook for the occurrence and source
sequence or multiple-injection run for a of a not-ready condition. Restart the analysis
period longer than the timeout threshold. where required.

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7 Error Information
General Error Messages

Shutdown
Error ID: 0063
An external instrument has generated a shutdown signal on the remote line.
The module continually monitors the remote input connectors for status signals.
A LOW signal input on pin 4 of the remote connector generates the error
message.

Probable cause Suggested actions

1 Leak detected in another module with a CAN Fix the leak in the external instrument before
connection to the system. restarting the module.

2 Leak detected in an external instrument with Fix the leak in the external instrument before
a remote connection to the system. restarting the module.

3 Shut-down in an external instrument with a Check external instruments for a shut-down


remote connection to the system. condition.

4 The degasser failed to generate sufficient Check the vacuum degasser for an error
vacuum for solvent degassing. condition. Refer to the Service Manual for the
degasser or the pump that has the degasser
built-in.

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7 Error Information
General Error Messages

Remote Timeout
Error ID: 0070
A not-ready condition is still present on the remote input. When an analysis is
started, the system expects all not-ready conditions (for example, a not-ready
condition during detector balance) to switch to run conditions within one minute
of starting the analysis. If a not-ready condition is still present on the remote line
after one minute the error message is generated.

Probable cause Suggested actions

1 Not-ready condition in one of the Ensure the instrument showing the not-ready
instruments connected to the remote line. condition is installed correctly, and is set up
correctly for analysis.

2 Defective remote cable. Exchange the remote cable.

3 Defective components in the instrument Check the instrument for defects (refer to the
showing the not-ready condition. instrument’s documentation).

Lost CAN Partner


Error ID: 0071
During an analysis, the internal synchronization or communication between one
or more of the modules in the system has failed.
The system processors continually monitor the system configuration. If one or
more of the modules is no longer recognized as being connected to the system,
the error message is generated.

Probable cause Suggested actions

1 CAN cable disconnected. • Ensure all the CAN cables are connected
correctly.
• Ensure all CAN cables are installed correctly.

2 Defective CAN cable. Exchange the CAN cable.

3 Defective mainboard in another module. Switch off the system. Restart the system, and
determine which module or modules are not
recognized by the system.

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7 Error Information
General Error Messages

Leak Sensor Short


Error ID: 0082
The leak sensor in the module has failed (short circuit).
The current through the leak sensor is dependent on temperature. A leak is
detected when solvent cools the leak sensor, causing the leak sensor current to
change within defined limits. If the current increases above the upper limit, the
error message is generated.

Probable cause Suggested actions

1 Defective leak sensor. Please contact your Agilent service representative.

2 Leak sensor incorrectly routed, being Please contact your Agilent service representative.
pinched by a metal component.

3 Power switch assembly defective Please contact your Agilent service representative.

4 Cable or contact problem. Please contact your Agilent service representative.

Leak Sensor Open


Error ID: 0083
The leak sensor in the module has failed (open circuit).
The current through the leak sensor is dependent on temperature. A leak is
detected when solvent cools the leak sensor, causing the leak sensor current to
change within defined limits. If the current falls outside the lower limit, the error
message is generated.

Probable cause Suggested actions


1 Leak sensor not connected to the Please contact your Agilent service representative.
power switch board.

2 Defective leak sensor. Please contact your Agilent service representative.

3 Leak sensor incorrectly routed, Please contact your Agilent service representative.
being pinched by a metal
component.

4 Power switch assembly defective Please contact your Agilent service representative.

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7 Error Information
General Error Messages

Compensation Sensor Open


Error ID: 0081
The ambient-compensation sensor (NTC) on the power switch board in the
module has failed (open circuit).
The resistance across the temperature compensation sensor (NTC) on the
power switch board is dependent on ambient temperature. The change in
resistance is used by the leak circuit to compensate for ambient temperature
changes. If the resistance across the sensor increases above the upper limit, the
error message is generated.

Probable cause Suggested actions

1 Loose connection between the power switch Please contact your Agilent service
board and the mainboard representative.

2 Defective power switch assembly Please contact your Agilent service


representative.

Compensation Sensor Short


Error ID: 0080
The ambient-compensation sensor (NTC) on the power switch board in the
module has failed (open circuit).
The resistance across the temperature compensation sensor (NTC) on the
power switch board is dependent on ambient temperature. The change in
resistance is used by the leak circuit to compensate for ambient temperature
changes. If the resistance across the sensor falls below the lower limit, the error
message is generated.

Probable cause Suggested actions

1 Defective power switch assembly Please contact your Agilent service


representative.

2 Loose connection between the power switch Please contact your Agilent service
board and the mainboard representative.

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7 Error Information
General Error Messages

Fan Failed
Error ID: 0068
The cooling fan in the module has failed.
The hall sensor on the fan shaft is used by the mainboard to monitor the fan
speed. If the fan speed falls below a certain limit for a certain length of time, the
error message is generated.
This limit is given by 2 revolutions/second for longer than 5 seconds.
Depending on the module, assemblies (e.g. the lamp in the detector) are turned
off to assure that the module does not overheat inside.

Probable cause Suggested actions

1 Fan cable disconnected. Please contact your Agilent service


representative.

2 Defective fan. Please contact your Agilent service


representative.

3 Defective mainboard. Please contact your Agilent service


representative.

Leak
Error ID: 0064
A leak was detected in the module.
The signals from the two temperature sensors (leak sensor and board-mounted
temperature-compensation sensor) are used by the leak algorithm to determine
whether a leak is present. When a leak occurs, the leak sensor is cooled by the
solvent. This changes the resistance of the leak sensor which is sensed by the
leak sensor circuit on the main board.

Probable cause Suggested actions

1 Loose fittings. Ensure all fittings are tight.

2 Broken capillary. Exchange defective capillaries.

3 Leaking flow cell. Exchange flow cell components.

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7 Error Information
General Error Messages

Open Cover
Error ID: 0205
The top foam has been removed.
The sensor on the main board detects when the top foam is in place. If the foam
is removed, the fan is switched off, and the error message is generated.

Probable cause Suggested actions

1 The top foam was removed during operation. Please contact your Agilent service
representative.

2 Foam not activating the sensor. Please contact your Agilent service
representative.

3 Defective sensor or main board. Please contact your Agilent service


representative.

Cover Violation
Error ID: 7461
The top foam has been removed.
The sensor on the main board detects when the top foam is in place. If the foam
is removed while the lamps are on (or if an attempt is made to switch on for
example the lamps with the foam removed), the lamps are switched off, and the
error message is generated.

Probable cause Suggested actions

1 The top foam was removed during operation. Please contact your Agilent service
representative.

2 Foam not activating the sensor. Please contact your Agilent service
representative.

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7 Error Information
General Error Messages

ERI Messages
Error ID: 11120 (+5 V) , 11121 (+25 V)
The ERI (Enhanced Remote Interface) provides two error events related to over
current situations on the +5 V and +24 V lines.

Probable cause Suggested actions

1 The load on the ERI is too high. Reduce the load.

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7 Error Information
Detector Error Messages

Detector Error Messages

These errors are detector specific.

Visible Lamp Current


The visible lamp current is missing.
The processor continually monitors the lamp current during operation. If the
current falls below the lower current limit, the error message is generated.

Probable cause Suggested actions

1 Lamp disconnected. Ensure the visible lamp connector is seated


firmly.

2 Defective visible lamp. Exchange the visible lamp.

3 Defective connector or cable. Please contact your Agilent service


representative.

4 Defective power supply. Please contact your Agilent service


representative.

Visible Lamp Voltage


The visible lamp voltage is missing.
The processor continually monitors the voltage across the lamp during
operation. If the lamp voltage falls below the lower limit, the error message is
generated.

Probable cause Suggested actions

1 Defective connector or cable. Please contact your Agilent service


representative.

2 Defective power supply. Please contact your Agilent service


representative.

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7 Error Information
Detector Error Messages

Diode Current Leakage


Error ID: 1041
When the detector is switched on, the processor checks the leakage current of
each of the optical diodes. If the leakage current exceeds the upper limit, the error
message is generated.

Probable cause Suggested actions

1 Defective PDA/optical unit. Please contact your Agilent service


representative.

2 Defective connector or cable. Please contact your Agilent service


representative.

UV Lamp Current
Error ID: 7450
The UV lamp current is missing.
The processor continually monitors the anode current drawn by the lamp during
operation. If the anode current falls below the lower current limit, the error
message is generated.

Probable cause Suggested actions

1 Lamp disconnected. Ensure the UV lamp connector is seated firmly.

2 Defective UV lamp or non-Agilent lamp. Exchange the UV lamp.

3 Defective detector main board. Please contact your Agilent service


representative.

4 Defective power supply. Please contact your Agilent service


representative.

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7 Error Information
Detector Error Messages

UV Lamp Voltage
Error ID: 7451
The UV lamp anode voltage is missing.
The processor continually monitors the anode voltage across the lamp during
operation. If the anode voltage falls below the lower limit, the error message is
generated.

Probable cause Suggested actions

1 Defective UV lamp or non-Agilent lamp. Exchange the UV lamp.

2 Defective detector main board. Please contact your Agilent service


representative.

3 Defective power supply. Please contact your Agilent service


representative.

UV Ignition Failed
Error ID: 7452
The UV lamp failed to ignite.
The processor monitors the UV lamp current during the ignition cycle. If the lamp
current does not rise above the lower limit within 2 – 5 seconds, the error
message is generated.

Probable cause Suggested actions

1 Lamp too hot. Hot gas discharge lamps may Switch off the lamp and allow it to cool down for
not ignite as easily as cold lamps. at least 15 minutes.

2 Lamp disconnected. Ensure the lamp is connected.

3 Defective UV lamp or non-Agilent lamp. Exchange the UV lamp.

4 Defective detector main board. Please contact your Agilent service


representative.

5 Defective power supply. Please contact your Agilent service


representative.

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7 Error Information
Detector Error Messages

UV Heater Current
Error ID: 7453
The UV lamp heater current is missing.
During UV lamp ignition, the processor monitors the heater current. If the current
does not rise above the lower limit within one second, the error message is
generated.

Probable cause Suggested actions

1 Lamp disconnected. Ensure the UV lamp is connected.

2 Ignition started without the top foam in Please contact your Agilent service
place. representative.

3 Defective UV lamp or non-Agilent lamp. Exchange the UV lamp.

4 Defective detector main board. Please contact your Agilent service


representative.

5 Defective power supply. Please contact your Agilent service


representative.

Calibration Values Invalid


Error ID: 1036
The calibration values read from the spectrometer ROM are invalid.
After recalibration, the calibration values are stored in ROM. The processor
periodically checks if the calibration data are valid. If the data are invalid or
cannot be read from the spectrometer ROM, the error message is generated.

Probable cause Suggested actions

1 Defective connector or cable. Please contact your Agilent service


representative.

2 Defective PDA/optical unit. Please contact your Agilent service


representative.

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7 Error Information
Detector Error Messages

Holmium Oxide Test Failed

Probable cause Suggested actions

1 Lamps switched off. Ensure the lamps are switched on.

2 Defective or dirty flow cell. Ensure the flow cell is inserted correctly, and is
free from contamination (cell windows, buffers
etc.).

3 Defective filter assembly. Please contact your Agilent service


representative.

4 Defective achromat assembly. Please contact your Agilent service


representative.

5 Defective PDA/optical unit. Please contact your Agilent service


representative.

Illegal Temperature Value from Sensor on Main


Board
Error ID: 1071
This temperature sensor (located on the detector main board) delivered a value
outside the allowed range. The parameter of this event equals the measured
temperature in 1/100 centigrade. As a result the temperature control is switched
off.

Probable cause Suggested actions

1 Defective sensor or main board. Please contact your Agilent service


representative.

2 Detector is exposed to illegal ambient Verify that the ambient conditions are within the
conditions. allowed range.

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7 Error Information
Detector Error Messages

Illegal Temperature Value from Sensor at Air Inlet


Error ID: 1072
This temperature sensor delivered a value outside the allowed range. The
parameter of this event equals the measured temperature in 1/100 centigrade.
As a result the temperature control is switched off.

Probable cause Suggested actions

1 The temperature sensor is defect. • Replace the cable to the main board.
• Please contact your Agilent service
representative.

2 Detector is exposed to illegal ambient Verify that the ambient conditions are within the
conditions. allowed range.

Wavelength Recalibration Lost


Error ID: 1037
The calibration information needed for your detector to operate correctly has
been lost.
During calibration of the detector the calibration values are stored in ROM. If no
data is available in the spectrometer ROM, the error message is generated.

Probable cause Suggested actions

1 The detector is new. Recalibrate the detector.

2 The detector has been repaired. Please contact your Agilent service
representative.

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7 Error Information
Detector Error Messages

Heater at fan assembly failed


Error ID: 1073
Every time the deuterium lamp or the tungsten lamp (DAD only) is switched on or
off a heater self-test is performed. If the test fails an error event is created. As a
result the temperature control is switched off.

Probable cause Suggested actions

1 Defective connector or cable. Please contact your Agilent service


representative.

2 Defective heater. Please contact your Agilent service


representative.

Heater Power At Limit


Error ID: 1074
The available power of the heater reached either the upper or lower limit. This
event is sent only once per run. The parameter determines which limit has been
hit:
0 means upper power limit hit (excessive ambient temperature drop).
1 means lower power limit hit (excessive ambient temperature increase).

Probable cause Suggested actions

1 Excessive ambient temperature change. Wait until temperature control equilibrates.

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7 Error Information
Detector Error Messages

DSP Not Running


This error message comes up when the communication between the optical unit
and the main board has a problem.

Probable cause Suggested actions

1 Random communication error. • Switch the detector off and on again at the
power switch. If the error reoccurs:
• Please contact your Agilent service
representative.

2 Defective detector main board. Please contact your Agilent service


representative.

3 Defective PDA/optical unit. Please contact your Agilent service


representative.

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8 Test Functions and Calibration

Introduction 116
Conditions of Detector 120
Failing a Test 121
Self-Test 122
Intensity Test 124
Test Failed 126
Cell Test 127
Test Failed (low ratio value) 128
Filter Test 129
Test Evaluation 130
Holmium Oxide Test 131
Test Evaluation 131
ASTM Drift and Noise Test 134
Test Failed 137
Slit Test 138
Test Failed 140
Wavelength Verification Test 141
Wavelength Calibration 143
Wavelength Recalibration Fails 145
D/A Converter (DAC) Test 146
Test Evaluation 147
Dark-Current Test 148
Test Failed 149
Spectral Scan 150
Other Lab Advisor Functions 151
EMFs - Early Maintenance Feature 151

This chapter describes the tests for the module.

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8 Test Functions and Calibration
Introduction

Introduction

All tests are described based on the Agilent Lab Advisor Software B.02.08. Other
user interfaces may not provide any test or just a few.
For details on the use of the interface refer to the interface documentation.
The Lab Advisor shows the available test under Service & Diagnostics.
Table 14 Available Diagnostic Functions vs. Product Level

Product Level

Tests

-ASTM Drift and Noise Test Basic Advanced

-Cell Test Basic Advanced

-D/A Converter Test Basic Advanced

-Dark Current Test Basic Advanced

-Filter Test Basic Advanced

-Holmium Oxide Test Basic Advanced

-Intensity Test Basic Advanced

-Quick Noise Test Basic Advanced

-Self Test Basic Advanced

-Slit Test Basic Advanced

-Wavelength Verification Test Basic Advanced

Calibrations

-Wavelength Calibration Basic Advanced

Tools

-Diagnostic Buffers Basic Advanced

-Module Info Basic Advanced

-Test Chromatogram Basic Advanced

-Spectral Scan Basic Advanced

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8 Test Functions and Calibration
Introduction

Table 14 Available Diagnostic Functions vs. Product Level

Product Level

Controls

-Advanced Method Parameters

-Vis lamp required Advanced

-Analog Output 1 Offset [% Full Advanced


Scale]

-D2 lamp required Advanced

-Analog Output 1 Attenuation Advanced

-Configuration

-Analog Output 1 Range Advanced

-Remote Pulse Duration [s]* Basic Advanced

-Control

-Vis lamp Basic Advanced

-Balance Detector Advanced

-UV Lamp Basic Advanced

-Method Parameters

-Set Signal A Advanced

-Set Signal C Advanced

-Set Data Rate [HZ] Advanced

-Set Signal B Advanced

-Module Information

-Identify Module Basic Advanced

-Special Commands

-Lamp tag required Basic Advanced

-Cell tag required Basic Advanced

-Detector Reset Basic Advanced

-Clear Error Basic Advanced

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8 Test Functions and Calibration
Introduction

Table 14 Available Diagnostic Functions vs. Product Level

Product Level

Statemachines

-UV Lamp Basic Advanced

-Vis Lamp Advanced

Signals

-Signal A [mAU] Advanced

-Lamp Voltage [V] Advanced

-Board Temperature [°C] Advanced

-Optical Temperature [°C] Advanced

EMF Counters

-Accumulated UV Lamp Basic Advanced


On-Time

-Number of UV Lamp Ignitions Basic Advanced

-Accumulated Tungsten Lamp Basic Advanced


On-Time

-Number of Tungsten Lamp Basic Advanced


Ignitions

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8 Test Functions and Calibration
Introduction

Figure 26 The Lab Advisor shows the available tests

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8 Test Functions and Calibration
Conditions of Detector

Conditions of Detector

The test usually should be performed with a detector turned on for at least one
hour, so that the temperature regulation of the optical unit is working (not active
during the first 30 minutes after turn on). If the detector is on, tests can be
performed usually 10 minutes after the UV-lamp has been turned on.

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8 Test Functions and Calibration
Failing a Test

Failing a Test

If a test fails with the flow cell installed, repeat the test with removed flow cell and
compare. If the test fails also, then start with proposed actions mentioned in the
details of the tests.

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8 Test Functions and Calibration
Self-Test

Self-Test

The self-test runs a series of individual tests (described on the next pages), and
evaluates the results automatically. The following tests are run:
• Filter Test
• Slit Test
• Dark Current Test
• Intensity Test
• Wavelength Verification Test
• Holmium Oxide Test
• Spectral Flatness Test
• ASTM Noise Test (without testing the Drift)

When For complete detector check.

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Lamp must be on for at least 10 min.


• For noise test a longer warm-up time may be required (> 2 h).

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8 Test Functions and Calibration
Self-Test

1 Run the Self Test with Agilent Lab Advisor (for further information see
Online-Help of user interface).

Figure 27 Self Test – Results

Under the tab Signals you can find the detailed signals from the tests.

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8 Test Functions and Calibration
Intensity Test

Intensity Test

The intensity test measures the intensity of the UV-lamp over the full wavelength
range (190 - 950 nm). Four spectral ranges are used to evaluate the intensity
spectrum. The test is used to determine the performance of the lamp and optics
(see also “Cell Test” on page 127). When the test is started, the 1 nm slit is moved
into the light path automatically. To eliminate effects due to absorbing solvents,
the test should be done with water in the flow cell or with the flow cell removed.
The shape of the intensity spectrum is primarily dependent on the lamp, grating,
and diode array characteristics. Therefore, intensity spectra will differ slightly
between instruments.

When In case of UV-lamp problem (drift, noise).

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Lamp must be on for at least 10 min.


• When using a flow cell a flow rate of 1 mL/min with water is required.

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8 Test Functions and Calibration
Intensity Test

1 Run the Intensity Test with Agilent Lab Advisor (for further information see
Online-Help of user interface).

Figure 28 Intensity Test – Results (w/o flow cell)

Figure 29 Intensity Test – Signals (w/o flow cell)

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8 Test Functions and Calibration
Intensity Test

Test Failed
Intensity Test Evaluation

Probable cause Suggested actions

1 Absorbing solvent or air bubble in flow cell. • Ensure the flow cell is filled with water, and
free from air bubbles.
• Repeat test without flow cell and compare
results.

2 Incorrect calibration Recalibrate and repeat the test.

3 Dirty or contaminated flow cell. Run the cell test. If the test fails, flush the flow
cell. See also “Maintenance of Standard,
Semi-Micro or Micro Flow Cell” on page 167.

4 Dirty or contaminated optical components. Please contact your Agilent service


representative.

5 Old UV-lamp. Exchange the UV-lamp.

6 Defect optical unit. If the test fails with flow cell and new UV-lamp,
please contact your Agilent service
representative.

If only one range fails and the application does not require this range, the lamp
NOTE may not be changed.

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8 Test Functions and Calibration
Cell Test

Cell Test

The cell test measures the intensity of the UV- and tungsten lamps over the full
wavelength range (190 - 950 nm), once with the flow cell installed, and once with
the flow cell removed. The resulting intensity ratio is a measure of the amount of
light absorbed by the flow cell. The test can be used to check for dirty or
contaminated flow cell windows. When the test is started, the 1 nm slit is moved
into the light path automatically.
This test should be performed initially with a new detector/flow cell. The values
should be kept for later reference/comparison.

When In case of low intensity or noise and drift problem.

Parts required Description


Flow Cell (filled with water)

Preparations • Lamp must be on for at least 10 min.


• When using a flow cell a flow rate of 1 mL/min with water is required.

1 Run the Cell-Test with Agilent Lab Advisor (for further information see
Online-Help of user interface).

Figure 30 Cell Test – Results

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8 Test Functions and Calibration
Cell Test

Figure 31 Cell Test – Signals (example shows low intensity for flow cell)

Test Failed (low ratio value)


Cell Test Evaluation

Probable cause Suggested actions

1 Absorbing solvent or air bubble in flow cell. Ensure the flow cell is filled with water, and free
from air bubbles.

2 Dirty or contaminated flow cell. Clean the flow cell as described in “Maintenance
of Standard, Semi-Micro or Micro Flow Cell” on
page 167.

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8 Test Functions and Calibration
Filter Test

Filter Test

The filter test checks the correct operation of the filter assembly. When the test is
started, the holmium oxide filter is moved into position. During filter movement,
the absorbance signal is monitored. As the edge of the filter passes through the
light path, an absorbance maximum is seen. Once the filter is in position, the
absorbance maximum (of holmium oxide) is determined. Finally, the filter is
moved out of the light path. During movement, an additional absorbance
maximum is expected as the edge of the filter passes through the light path. The
test passes successfully, if the two maxima resulting from the edge of the filter
assembly (during filter movement) are seen, and the absorbance maximum of
holmium oxide is within the limits.

Figure 32 Filter Test

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8 Test Functions and Calibration
Filter Test

Test Evaluation
Filter Test Failed

Test Failed

Probable cause Suggested actions

1 Filter assembly (lever and filter) not installed. Install the filter assembly.

2 Defective filter motor. Please contact your Agilent service


representative.

Holmium Oxide Maximum out of Limits

Probable cause Suggested actions

1 Holmium oxide filter not installed. Install the holmium oxide filter.

2 Dirty or contaminated filter. Exchange the holmium oxide filter.

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8 Test Functions and Calibration
Holmium Oxide Test

Holmium Oxide Test

The holmium oxide test uses characteristic absorbance maxima of the built-in
holmium oxide filter to verify wavelength accuracy (see also “Wavelength
Verification Test” on page 141). When the test is started, the 1-nm slit is moved
into the light path automatically. To eliminate effects due to absorbing solvents,
the test should be done with water in the flow cell or with removed flow cell.

See also “Declaration of Conformity for HOX2 Filter” on page 276.


NOTE

Test Evaluation
Holmium Oxide Test Evaluation
Limits:

361.0 nm 360.0 - 362.0 nm (± 1nm)

418.9 nm 417.9 - 419.9 nm (± 1nm) (not with ChemStation)

453.7 nm 452.7 - 454.7 nm (± 1nm)

536.7 nm 535.7 - 537.7 nm (± 1nm)

The test is evaluated by the instrument, and the measured maxima are displayed
automatically. The test fails if one or more of the maxima lies outside of the
limits (see Figure 33 on page 132).

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8 Test Functions and Calibration
Holmium Oxide Test

Figure 33 Holmium Oxide Test

Figure 34 Holmium Oxide Test (Signal)

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8 Test Functions and Calibration
Holmium Oxide Test

Test Failed

Probable cause Suggested actions

1 Absorbing solvent or air bubble in flow cell. Ensure the flow cell is filled with water.

2 Incorrect calibration Recalibrate (see “Wavelength Calibration” on


page 143) and repeat the test.

3 Dirty or contaminated flow cell. Run the cell test (see “Cell Test” on page 127). If
the test fails, exchange the flow cell windows.

4 Dirty or contaminated optical components Clean optical components with alcohol and
(achromat, windows). lint-free cloth or replace the parts (see “Intensity
Test” on page 124).

5 Old or non-Agilent lamp. Exchange the UV lamp.

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8 Test Functions and Calibration
ASTM Drift and Noise Test

ASTM Drift and Noise Test

The ASTM noise test determines the detector noise over a period of 20 minutes.
The test is done with installed flow cell or flow cell removed.
This test also checks for the drift. It is also part of the Self Test (without checking
for the drift).
If the test is performed with the flow cell removed, the test results are not
influenced by solvent or pump effects.

When In case of noise and drift problem.

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Detector and UV-lamp must be on for at least 2 hours.


• ASTM measurements based on specifications may require longer stabilization times.
• When using a flow cell a flow rate of 1 mL/min with water is required.

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8 Test Functions and Calibration
ASTM Drift and Noise Test

1 Run the ASTM Drift and Noise Test with Agilent Lab Advisor (for further
information see Online-Help of user interface).

Figure 35 ASTM Drift and Noise Test – Results (with Flow Cell removed)

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8 Test Functions and Calibration
ASTM Drift and Noise Test

Figure 36 ASTM Drift and Noise Test – Signal (with Flow Cell removed)

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8 Test Functions and Calibration
ASTM Drift and Noise Test

Test Failed
ASTM Noise Test Evaluation

Probable cause Suggested actions

1 Insufficient lamp warm-up time. Allow detector and UV-lamp turned on for at least
2 hours.

2 Absorbing solvent or air bubble in flow cell. Ensure the flow cell is filled with water, and free
from air bubbles.

3 Dirty or contaminated flow cell. • Flush flow cell.


• Clean the flow cell as described in
“Maintenance of Standard, Semi-Micro or
Micro Flow Cell” on page 167.

4 Old UV-lamp. Exchange the UV-lamp.

5 Old Vis-lamp. Exchange the Vis-lamp.

6 Environment not according to specifications. Improve environment.

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8 Test Functions and Calibration
Slit Test

Slit Test

The slit test verifies correct operation of the micromechanical slit.


During the test, the slit is moved through all slit positions while the detector
monitors the lamp intensity change. When the slit position is changed, the
intensity drop (move to smaller slit) or intensity increase (move to larger slit)
must be within a defined range.
If the test is performed with the flow cell removed, the test results are not
influenced by solvent or pump effects.
If the intensity changes are outside the expected range, the test fails.

When In case of problems.

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Lamp must be on for at least 10 min.


• When using a flow cell a flow rate of 1 mL/min with water is required.

1 Run the Slit Test with the Agilent Lab Advisor (for further information see
Online-Help of user interface).

Figure 37 Slit Test – Results

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8 Test Functions and Calibration
Slit Test

Figure 38 Slit Test – Signal

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8 Test Functions and Calibration
Slit Test

Test Failed
Slit Test Evaluation

Probable cause Suggested actions

1 Air bubble in flow cell. Flush the flow cell or remove the flow cell.

2 Old lamp. Run the “Intensity Test”. Exchange the lamp if old
or defective.

3 Defective slit assembly. Please contact your Agilent service


representative.

4 Defective detector main board. Please contact your Agilent service


representative.

5 Defective optical unit. Please contact your Agilent service


representative.

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8 Test Functions and Calibration
Wavelength Verification Test

Wavelength Verification Test

The detector uses the alpha (656.1 nm) and beta (486 nm) emission lines of the
UV-lamp for wavelength calibration. The sharp emission lines enable accurate
calibration. When verification is started, the 1-nm slit is moved into the light path
automatically. The test is run with Flow Cell removed or with Flow Cell installed.
If the test is performed with the Flow Cell removed, the test results are not
influenced by solvent or pump effects.

When The detector is calibrated at the factory, and under normal operating conditions should not require
recalibration. However, it is advisable to recalibrate:
• after repair of components in the optical unit,
• after exchange of the optical unit or main board,
• after replacing the Flow Cell or UV-lamp,
• after significant environmental condition changes (temperature, humidity),
• at a regular interval, at least once per year (for example, prior to an Operational
Qualification/Performance Verification procedure), and
• when chromatographic results indicate the detector may require recalibration.

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Lamp must be on for at least 10 min.


• When using a Flow Cell a flow rate of 0.5 mL/min with water is required.

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8 Test Functions and Calibration
Wavelength Verification Test

1 Run the Wavelength Verification Test with the Agilent Lab Advisor (for further
information see Online-Help of user interface).

Figure 39 Wavelength Verification – Results

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8 Test Functions and Calibration
Wavelength Calibration

Wavelength Calibration

The detector uses the alpha (656.1 nm) and beta (486 nm) emission lines of the
deuterium lamp for wavelength calibration. The sharp emission lines enable
more accurate calibration than is possible with holmium oxide. When
recalibration is started, the 1 nm slit is moved into the light path automatically.
The gain is set to zero.
On completion of the scan, the alpha- and beta-line deviations (in nm) are
displayed. These values indicate how far the detector calibration deviates from
the actual positions of the alpha and beta emission lines. After calibration, the
deviation is zero.
To eliminate effects due to absorbing solvents, remove the flow cell before
starting the test.

When The detector is calibrated at the factory, and under normal operating conditions should not require
recalibration. However, it is advisable to recalibrate:
• after maintenance (flow cell or UV-lamp),
• after repair of components in the optical unit,
• after exchange of the optical unit or main board,
• after significant environmental condition changes (temperature, humidity),
• at a regular interval, at least once per year (for example, prior to an Operational
Qualification/Performance Verification procedure), and
• when chromatographic results indicate the detector may require recalibration.

Parts required Description


Removed Flow Cell or Flow Cell (filled with water)

Preparations • Detector/lamp must be on for more than 1 h.


• When using a Flow Cell a flow rate of 0.5 mL/min with water is required.

If the detector is operated in a lab environment that differs at average from the
NOTE final test environment (25 °C) then the detector should be recalibrated for this
temperature.

If the detector was repaired (opened covers), the wavelength calibration can be
NOTE done 10 minutes after lamp on. A final wavelength calibration should be
repeated after complete warm-up of the detector.

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8 Test Functions and Calibration
Wavelength Calibration

1 Run the Wavelength Calibration with the Agilent Lab Advisor (for further
information see Online-Help of user interface).

Figure 40 Wavelength Calibration - Results

If you select No, the test is aborted.


If you select Yes, the re-calibration is performed (the offset is corrected).

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8 Test Functions and Calibration
Wavelength Calibration

Wavelength Recalibration Fails

Probable cause Suggested actions

1 Absorbing solvent or air bubble in Flow Cell. Repeat calibration with Flow Cell and compare
results.

2 Dirty or contaminated Flow Cell. • Ensure the Flow Cell is filled with water.
• Recalibrate.

3 Old UV-lamp. Exchange the UV-lamp.

4 Dirty or contaminated optical components. Run the Cell Test. If the test fails, flush the flow
cell.

If the test fails with Flow Cell and new UV-lamp, the optical unit must be
NOTE checked/replaced.

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8 Test Functions and Calibration
D/A Converter (DAC) Test

D/A Converter (DAC) Test

The detector provides analog output of chromatographic signals for use with
integrators, chart recorders or data systems. The analog signal is converted from
the digital format by the digital-analog-converter (DAC).
The DAC test is used to verify correct operation of the digital-analog-converter by
applying a digital test signal to the DAC.
The DAC outputs an analog signal of approximately 50 mV (if the zero offset of
the analog output is set to the default value of 5 %) which can be plotted on an
integrator. A continuous square wave with an amplitude of 10 µV and a
frequency of approximately 1 cycle/24 seconds is applied to the signal.
The amplitude of the square wave and the peak-to-peak noise are used to
evaluate the DAC test.

When If the analog detector signal is noisy or missing.

Preparations Lamp must be on for at least 10 minutes. Connect integrator, chart recorder or data system to the
detector analog output.

1 Run the D/A Converter (DAC) Test with the Agilent Lab Advisor (for further
information see Online-Help of user interface).

Figure 41 D/A Converter (DAC) Test – Results

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8 Test Functions and Calibration
D/A Converter (DAC) Test

Test Evaluation
The noise on the step should be less than 3 µV.

Probable cause Suggested actions

1 Bad cable or grounding problem between Check or replace the cable.


detector and external device.

2 Defective detector main board. Please contact your Agilent service


representative.

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8 Test Functions and Calibration
Dark-Current Test

Dark-Current Test

The dark-current test measures the leakage current from each diode. The test is
used to check for leaking diodes which may cause non-linearity at specific
wavelengths. During the test, the slit assembly moves to the dark position,
cutting off all light falling onto the diode array. Next, the leakage current from
each diode is measured, and displayed graphically. The leakage current
(represented in counts) for each diode should fall within the limits.

When In case of problem.

1 Run the Dark Current Test with the recommended user interface (for further
information see Online-Help of user interface).

Figure 42 Dark Current Test – Results

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8 Test Functions and Calibration
Dark-Current Test

Figure 43 Dark Current Test – Signals

Test Failed

Probable cause Suggested actions

1 Defective slit assembly (stray light). Run the “Slit Test” on page 138 (part of the
“Self-Test” on page 122).

2 Defective detector main board. Please contact your Agilent service


representative.

3 Defective PDA/optical unit. Please contact your Agilent service


representative.

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8 Test Functions and Calibration
Spectral Scan

Spectral Scan

The Spectral Scan tool is available for diode-array and variable wavelength
detectors (DAD/MWD and VWD). It allows you to scan a spectrum over a
specified wavelength range and export the data to a csv (comma-separated
values) file that can be used in other applications (for example, Microsoft Excel).

Figure 44 Spectral Scan

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8 Test Functions and Calibration
Other Lab Advisor Functions

Other Lab Advisor Functions

EMFs - Early Maintenance Feature


The EMFs screen allows you to view and manage the EMF counters for all
modules in all systems.

Figure 45 Early Maintenance Feature

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9 Maintenance

Introduction to Maintenance 153


Cautions and Warnings 154
Overview of Maintenance 156
Cleaning the Module 157
Remove and Install Doors 158
Replace a Lamp 160
Remove and Install a Flow Cell 163
Maintenance of Standard, Semi-Micro or Micro Flow Cell 167
Maintenance of High Pressure Flow Cell 170
Replacing Capillaries on a Standard Flow Cell 172
Replacing Capillaries on a Semi-Micro and Micro Flow Cell 177
Nano Flow Cell - Replacing or Cleaning 181
Wrench plus Torque 184
Cleaning or Exchanging the Holmium Oxide Filter 185
Correcting Leaks 188
Replacing Leak Handling System Parts 190
Replacing the Module’s Firmware 192
Information from Module’s Assemblies 194

This chapter describes the maintenance of the detector.

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9 Maintenance
Introduction to Maintenance

Introduction to Maintenance

The module is designed for easy maintenance. Maintenance can be done from
the front with module in place in the system.

There are no serviceable parts inside.


NOTE
Do not open the module.

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9 Maintenance
Cautions and Warnings

Cautions and Warnings

Module is partially energized when switched off, as long as the power cord
WAR N IN G
is plugged in.
Risk of stroke and other personal injury. Repair work at the module can
lead to personal injuries, e. g. shock hazard, when the module cover is
opened and the instrument is connected to power.
 Never perform any adjustment, maintenance or repair of the module
with the top cover removed and with the power cord plugged in.
 The security lever at the power input socket prevents that the module
cover is taken off when line power is still connected. Never plug the
power line back in when cover is removed.

Sharp metal edges


WAR N IN G
Sharp-edged parts of the equipment may cause injuries.
 To prevent personal injury, be careful when getting in contact with sharp
metal areas.

Toxic, flammable and hazardous solvents, samples and reagents


WAR N IN G
The handling of solvents, samples and reagents can hold health and safety
risks.
 When working with these substances observe appropriate safety
procedures (for example by wearing goggles, safety gloves and
protective clothing) as described in the material handling and safety
data sheet supplied by the vendor, and follow good laboratory practice.
 The volume of substances should be reduced to the minimum required
for the analysis.
 Do not operate the instrument in an explosive atmosphere.

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9 Maintenance
Cautions and Warnings

Electronic boards and components are sensitive to electrostatic discharge


C AU T I O N (ESD).
ESD can damage electronic boards and components.
 Be sure to hold the board by the edges, and do not touch the electrical
components. Always use ESD protection (for example, an ESD wrist strap)
when handling electronic boards and components.

Eye damage by detector light


WAR N IN G
Eye damage may result from directly viewing the UV-light produced by the
lamp of the optical system used in this product.
 Always turn the lamp of the optical system off before removing it.

Safety standards for external equipment


C AU T I O N
 If you connect external equipment to the instrument, make sure that you
only use accessory units tested and approved according to the safety
standards appropriate for the type of external equipment.

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9 Maintenance
Overview of Maintenance

Overview of Maintenance

The following pages describe maintenance (simple repairs) of the detector that
can be carried out without opening the main cover.
Table 15 Overview of Maintenance

Procedure Typical Frequency Notes

Cleaning of module If required.

Deuterium lamp or If noise and/or drift exceeds your application limits or An intensity test should be performed
tungsten lamp lamp does not ignite. after replacement.
exchange

Flow cell exchange If application requires a different flow cell type. A holmium or wavelength calibration
test should be performed after
replacement.

Flow cell parts Cleaning If leaking or if intensity drops due to contaminated flow A pressure tightness test should be done
or exchange cell windows. after repair.

Holmium oxide filter If contaminated. A holmium or wavelength calibration


Cleaning or exchange test should be performed after
replacement.

Leak sensor drying If leak has occurred. Check for leaks.

Leak handling System If broken or corroded. Check for leaks.


replacement

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9 Maintenance
Cleaning the Module

Cleaning the Module

The module case should be kept clean. Cleaning should be done with a soft cloth
slightly dampened with water or a solution of water and mild detergent. Do not
use an excessively damp cloth allowing liquid to drip into the module.

Liquid dripping into the electronic compartment of your module can cause
WAR N IN G
shock hazard and damage the module
 Do not use an excessively damp cloth during cleaning.
 Drain all solvent lines before opening any connections in the flow path.

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9 Maintenance
Remove and Install Doors

Remove and Install Doors

Parts required p/n Description


5067-5737 Door left
5067-5736 Door right

The figures shown in this procedure exemplarily show the Infinity II Multisampler
NOTE module.
The principle of how to remove and/or install doors works in the same way for all
Infinity II modules.

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9 Maintenance
Remove and Install Doors

1 Press the release buttons and pull the front door out. 2 For the Installation of the front door. Insert the hinges
into their guides and move the door in until the release
buttons click into their final position.

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9 Maintenance
Replace a Lamp

Replace a Lamp

When If noise or drift exceeds application limits or lamp does not ignite

Tools required Description


Screwdriver, Pozidriv #1 PT3

Parts required # p/n Description


1 2140-0820 Longlife Deuterium lamp “C“ (with black cover and RFID tag)
1 G1103-60001 Tungsten lamp

Preparations Turn the lamp(s) off.

Eye damage by detector light


WAR N IN G

Eye damage may result from directly viewing the light produced by the
deuterium lamp used in this product.
 Always turn the deuterium lamp off before removing it.

Injury by touching hot lamp


WAR N IN G
If the detector has been in use, the lamp may be hot.
 If so, wait for lamp to cool down.

The lamp house cover includes a magnet.


NOTE

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9 Maintenance
Replace a Lamp

1 Open the doors. 2 Grab the lamp cover and pull it off (it is fixed by two
magnets in the center of the cover).

3 Unplug the lamp connector as required 4 Unscrew (do not remove) the two lamp screws
. (Pozidriv) as required.

5 Remove the deuterium lamp and place it on a clean 6 Remove the Vis-lamp and place it on a clean place.
place.

NOTE NOTE
Do not touch the glass bulb with your fingers. It may reduce Do not touch the glass bulb with your fingers. It may reduce
the light output. the light output.

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9 Maintenance
Replace a Lamp

7 Insert the deuterium lamp (RFID tag on the top side). 8 Insert the Vis-lamp (flat side to the right).

9 Reconnect the lamp connector as required. 10 Place the lamp cables in the lamp cover.

11 Slide the lamp cover into the top position of the metal 12 Close the doors.
front and press the lamp cover completely in until it
clicks.

1.

2.

Next Steps:

13 Perform a Wavelength Verification Test or a Holmium Oxide Test to check the correct positioning of the lamp
(“Wavelength Verification Test” on page 141, “Holmium Oxide Test” on page 131).
14 Perform an Intensity Test.

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9 Maintenance
Remove and Install a Flow Cell

Remove and Install a Flow Cell

For bio-inert modules use bio-inert parts only!

When If an application needs a different type of flow cell or the flow cell needs repair.

Tools required p/n Description


Wrench, 1/4 inch
for capillary connections
5043-0915 Fitting mounting tool

Parts required p/n Description


G1315-60022 Standard flow cell, 10 mm, 13 µL, 120 bar (12 MPa)
G1315-60025 Semi-micro flow cell, 6 mm, 5 µL, 120 bar (12 MPa)
G1315-60024 Micro flow cell, 3 mm, 2 µL, 120 bar (12 MPa)
G1315-60015 High pressure flow cell, 6 mm, 1.7 µL, 400 bar (40 MPa)
Nano flow cell
G5615-60022 Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar (12 MPa) for MWD/DAD,
includes 0890-1763 – 0.18 x 1500 mm PEEK capillary and 5063-6591 – PEEK
fittings

Preparations Turn the lamp(s) off.

Sample degradation and contamination of the instrument


C AU T I O N
Metal parts in the flow path can interact with the bio-molecules in the sample
leading to sample degradation and contamination.
 For bio applications, always use dedicated bio parts, which can be identified
by the bio-inert symbol or other markers described in this manual.
 Do not mix bio, and non-bio modules or parts in a bio system.

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9 Maintenance
Remove and Install a Flow Cell

The lamp house cover includes a magnet.


NOTE

1 Open the doors. 2 Grab the lamp cover and pull it off (it is fixed by two
magnets in the center of the cover).

3 Open the flow cell door. 4 Disconnect the flow cell inlet capillary (top) from the
union.

5 Disconnect the waste tubing (bottom) from the union. 6 Loosen the thumb screw (1.) and remove the flow cell
outlet capillary (bottom) with the union (2.).

2. 1.

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9 Maintenance
Remove and Install a Flow Cell

7 Remove the flow cell while pressing the flow cell holder. 8 Insert the flow cell while pressing the flow cell holder.

NOTE
The label attached to the flow cell provides information on
part number, path length, and maximum pressure.

If you want to replace flow cell parts, see “Maintenance of


Standard, Semi-Micro or Micro Flow Cell” on page 167 or
“Maintenance of High Pressure Flow Cell” on page 170.
9 Insert the flow cell capillaries into the union holder (top 10 Tighten the thumb screw.
is inlet, bottom is outlet).

1.

2. 3.

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9 Maintenance
Remove and Install a Flow Cell

11 Reconnect the waste tubing (bottom) to the union. 12 Close the flow cell door.
Establish a flow and check for leaks.

NOTE
To check for leaks, establish a flow and observe the flow
cell (outside of the cell compartment) and all capillary
connections.
13 Slide the lamp cover into the top position of the metal 14 Close the doors.
front and press the lamp cover completely in until it
clicks.

1.

2.

15 Perform a Wavelength Verification and Calibration or a Holmium Oxide Test to check the correct positioning of the flow
cell.

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9 Maintenance
Maintenance of Standard, Semi-Micro or Micro Flow Cell

Maintenance of Standard, Semi-Micro or Micro


Flow Cell

When If the flow cell needs repair due to leaks or contaminations (reduced light throughput)

Tools required p/n Description


Wrench, 1/4 inch
for capillary connections
5043-0915 Fitting mounting tool
Hexagonal key, 4 mm
Toothpick

Parts required Description


For parts, see “Standard Flow Cell” on page 198, “Semi-Micro Flow Cell” on page 202, “Micro Flow
Cell” on page 204.

Preparations • Turn the flow off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163

The gaskets used in the standard and semi-micro/micro flow cell are different.
NOTE

Sample degradation and contamination of the instrument


C AU T I O N
Metal parts in the flow path can interact with the bio-molecules in the sample
leading to sample degradation and contamination.
 For bio applications, always use dedicated bio parts, which can be identified
by the bio-inert symbol or other markers described in this manual.
 Do not mix bio, and non-bio modules or parts in a bio system.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 167


9 Maintenance
Maintenance of Standard, Semi-Micro or Micro Flow Cell

1 Use a 4 mm hex key to unscrew the window assembly 2 Use a tooth pick to remove the quartz window from the
(1) and remove the gasket (6,7) from the cell body. window assembly.

1 NOTE
7
If the washers fall out of the window assembly, they must
be inserted in the correct order with the PTFE ring to prevent
any leaks from the flow cell window.
6
1

NOTE
Carefully take one of the gaskets (#6 back or # 7 front) and
insert it into the cell body.

Do not mix the gasket #6 and # 7.

Gasket # 7 has the smaller hole and must be on the light


entrance side.

Verify that the gasket is positioned flat on the bottom and


the light path is not blocked.

If you removed all individual parts from the window


assembly refer to “Standard Flow Cell” on page 198 for the
correct orientation of the parts.
3 Orientation of Flow Cell Parts. 4 Assemble the washers and the window assembly in
correct order.

8
7

65
43 2
11
9 1

10

NOTE
Gaskets # 6 and #7 have different hole diameters.

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9 Maintenance
Maintenance of Standard, Semi-Micro or Micro Flow Cell

5 Correct orientation of spring washers (2) is required. 6 Press the PTFE ring into the window assembly.

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Quartz window
6 - Gasket

1 2 3 4 5 6

7 Press the window assembly onto the new or cleaned 8 Insert the window assembly (1) into the cell body.
quartz window.

1
7

6
1

NOTE
Do not mix the gasket #6 and #7 (different hole diameter).
Next Steps:

9 Using a 4-mm hex key, tighten the window screw hand tight plus a quarter turn.
10 Reconnect the capillaries, see “Remove and Install a Flow Cell” on page 163.
11 Perform a leak test.
12 Insert the flow cell.
13 Replace the front cover
14 Perform a Wavelength Verification Test or a Holmium Oxide Test to check the correct positioning of the lamp
(“Wavelength Verification Test” on page 141, “Holmium Oxide Test” on page 131).

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9 Maintenance
Maintenance of High Pressure Flow Cell

Maintenance of High Pressure Flow Cell

When If the flow cell needs repair due to leaks or contaminations (reduced light throughput)

Tools required p/n Description


Wrench, 1/4 inch
for capillary connections
OR 5043-0915 Fitting mounting tool
Hexagonal key, 4 mm
Toothpick

Parts required Description


For parts see “High Pressure Flow Cell” on page 206

Preparations • Turn the flow off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163

All descriptions in this procedure are based on the default orientation of the cell
NOTE (as it is manufactured). The heat exchanger/capillary and the cell body can be
fixed mirror symmetrically to have both capillaries routed to the bottom or to the
top (depending on the routing of the capillaries to the column).

1 Use a 4 mm hex key to unscrew the window assembly (1) and remove the
gasket (2) from the cell body.
1
2

2
1

If you want to replace the gasket only, reinsert the window assembly into the
cell body.

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9 Maintenance
Maintenance of High Pressure Flow Cell

2 Use a tooth pick to remove the quartz window from the window assembly.

If the washers fall out of the window assembly, they must be inserted in the
NOTE correct order with the PTFE ring to prevent any leaks from the flow cell window.

6
5
4
2
3 2

9
8

1 Window assembly (contains items 2, 3, 4, 5 and 6

2 Seal ring

3 Quartz window

4 Compression washer

5 Spring washers

6 Window screw

7 Inlet capillary

8 Outlet capillary

3 Follow the procedure “Maintenance of Standard, Semi-Micro or Micro Flow


Cell” on page 167 for reassembling.

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9 Maintenance
Replacing Capillaries on a Standard Flow Cell

Replacing Capillaries on a Standard Flow Cell

For bio-inert modules use bio-inert parts only!

When If the capillary is blocked

Tools required p/n Description


Wrench, 1/4 inch
for capillary connections
5043-0915 Fitting mounting tool
Wrench, 4 mm
(for capillary connections)
Screwdriver, Pozidriv #1 PT3

Parts required Description


For parts see “Standard Flow Cell” on page 198

Preparations • Turn the lamp(s) off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163.

All descriptions in this procedure are based on the default orientation of the cell
NOTE (as it is manufactured). The heat exchanger/capillary and the cell body can be
fixed mirror symmetrically to have both capillaries routed to the bottom or to the
top (depending on the routing of the capillaries to the column).

The fittings at the flow cell body are special types for low dead volumes and not
NOTE compatible with other fittings.
When retightening the fittings, make sure that they are carefully tightened
(handtight plus 1/4 turn with a wrench). Otherwise damage of the flow cell body
or blockage may result.

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9 Maintenance
Replacing Capillaries on a Standard Flow Cell

Sample degradation and contamination of the instrument


C AU T I O N
Metal parts in the flow path can interact with the bio-molecules in the sample
leading to sample degradation and contamination.
 For bio applications, always use dedicated bio parts, which can be identified
by the bio-inert symbol or other markers described in this manual.
 Do not mix bio, and non-bio modules or parts in a bio system.

1 Identify the inlet and outlet capillaries. To replace the 2 Remove the outlet capillary.
inlet capillary, continue with step "To replace the inlet
capillary, use a 4 mm wrench for the fitting."

Inlet

Outlet

3 To replace the inlet capillary, use a 4 mm wrench to 4 Unscrew the cell body from the heat exchanger.
open the fitting.

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9 Maintenance
Replacing Capillaries on a Standard Flow Cell

5 Remove the heat exchanger from the clamp unit. 6 Use a small flat screw driver to carefully lift off the I.D.
tag. Shown is the default orientation. See Note at the
beginning of this section.

7 Unscrew the fixing screw and unwrap the inlet capillary 8 Take the new inlet capillary and bend it 90° about 35
from the grove in the flow cell body. mm from its end.

35 cm
90°

9 Bend the capillary again by 90° as shown below. 10 Insert the capillary into the hole between fixing screw
and the inlet fitting.

90°

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9 Maintenance
Replacing Capillaries on a Standard Flow Cell

11 The capillary lays in the grove and should be tied around 12 Insert the fixing screw, so that the capillary cannot leave
the body (in the grove) 5 times. the grove.

13 Carefully insert the I.D. tag into the new heat exchanger. 14 Fix the heat exchanger to the clamp unit.
Shown is the default orientation. See Note at the
beginning of this section.

15 Fix the flow cell body to the heat exchanger. 16 Fix the inlet capillary to the flow cell body handtight first.
Then do a 1/4 turn with a 4 mm wrench.

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9 Maintenance
Replacing Capillaries on a Standard Flow Cell

17 After replacing the outlet capillary, fix it handtight first. 18 Check for a centered holder vs. hole. If required adjust
Then do a 1/4 turn with a 4 mm wrench. with the holder screws.

Next Steps:

19 Reconnect the capillaries, see “Remove and Install a Flow Cell” on page 163.
20 Perform a leak test.
21 Insert the flow cell.
22 Close the doors of the module.
23 Perform a Wavelength Verification Test or a Holmium Oxide Test to check the correct positioning of the lamp
(“Wavelength Verification Test” on page 141, “Holmium Oxide Test” on page 131).

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9 Maintenance
Replacing Capillaries on a Semi-Micro and Micro Flow Cell

Replacing Capillaries on a Semi-Micro and Micro


Flow Cell

When If the capillary is blocked

Tools required p/n Description


Wrench, 1/4 inch
for capillary connections
OR 5043-0915 Fitting mounting tool
Wrench, 4 mm
(for capillary connections)
Screwdriver, Pozidriv #1 PT3

Parts required Description


For parts see “Semi-Micro Flow Cell” on page 202 or “Micro Flow Cell” on page 204.

Preparations • Turn the lamp(s) off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163.

All descriptions in this procedure are based on the default orientation of the cell
NOTE (as it is manufactured). The heat exchanger/capillary and the cell body can be
fixed mirror symmetrically to have both capillaries routed to the bottom or to the
top (depending on the routing of the capillaries to the column).

The fittings at the flow cell body are special types for low dead volumes and not
NOTE compatible with other fittings. When retightening the fittings, make sure that they
are carefully tightened (handtight plus 1/4 turn with a wrench). Otherwise
damage of the flow cell body or blockage may result.

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9 Maintenance
Replacing Capillaries on a Semi-Micro and Micro Flow Cell

1 Identify the inlet and outlet capillaries. 2 Remove the outlet capillary.

Inlet

Outlet

3 To replace the inlet capillary, use a 4 mm wrench to 4 Unscrew the cell body from the heat exchanger.
open the fitting.

5 Remove the heat exchanger from the clamp unit. 6 Use a small flat screw driver to carefully lift off the I.D.
tag. Shown is the default orientation. See Note at the
beginning of this section.

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9 Maintenance
Replacing Capillaries on a Semi-Micro and Micro Flow Cell

7 Carefully insert the I.D. tag into the new heat exchanger. 8 Fix the heat exchanger to the clamp unit.
Shown is the default orientation. See Note at the
beginning of this section.

9 Fix the flow cell body to the heat exchanger. 10 Fix the inlet capillary to the flow cell body handtight first.
Then do a 1/4 turn with a 4 mm wrench.

11 After replacing the outlet capillary, fix it handtight first. 12 Check for a centered holder vs. hole. If required adjust
Then do a 1/4 turn with a 4 mm wrench. with the holder screws.

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9 Maintenance
Replacing Capillaries on a Semi-Micro and Micro Flow Cell

Next Steps:

13 Reconnect the capillaries, see “Remove and Install a Flow Cell” on page 163.
14 Perform a leak test.
15 Insert the flow cell.
16 Close the doors.
17 Perform a Wavelength Verification Test or a Holmium Oxide Test to check the correct positioning of the lamp
(“Wavelength Verification Test” on page 141, “Holmium Oxide Test” on page 131).

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9 Maintenance
Nano Flow Cell - Replacing or Cleaning

Nano Flow Cell - Replacing or Cleaning

When If parts are contaminated or leaky.

Tools required Description


Screwdriver, Pozidriv #1 PT3
Wrench, 1/4 inch
for capillary connections

Parts required Description


For parts identification refer to “Nano Flow Cells” on page 212 (80 nL and 500 nL).

Preparations • Turn the lamp(s) off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163.

For details refer to the technical note that comes with the nano-flow cell kit.
NOTE

The quartz block can be cleaned with alcohol. DO NOT touch the inlet and outlet
NOTE windows at the quartz block.

1 Disconnect the capillaries from the capillary holder and 2 Unscrew the cell body from the holder.
remove the flow cell, see “Remove and Install a Flow
Cell” on page 163.

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9 Maintenance
Nano Flow Cell - Replacing or Cleaning

3 Unscrew the capillaries from the flow cell. DO NOT use 4 Using for example a toothpick, press on the plastic part
the adapter at this time! and slide the quartz body out of the cell housing.

5 The quartz body and the cell seal assembly can be 6 This figure shows the correct holding of the quartz body
separated for cleaning purpose. and the cell seal assembly.

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9 Maintenance
Nano Flow Cell - Replacing or Cleaning

7 Replace the cell seal assembly onto the quartz body. 8 Slide the quartz body completely into the cell body to
Always use a new seal assembly to exclude damage the front stop (use for example a toothpick).
during disassembling.

9 Insert the flow cell capillaries and tighten them 10 Reassemble the flow cell body to the holder.
fingertight. Use the wrench and torque adapter as
described on Figure 46 on page 184 and tighten the
fittings alternately.

Next Steps:

11 Install the flow cell, see “Remove and Install a Flow Cell” on page 163.
12 Perform a leak test with the flow cell outside of the detector.
13 If no leak is observed, install the flow cell and you are ready to work.
14 Make sure that the flow cell assembly is inserted correctly and fits perfectly in the optical unit (especially when PEEK
capillaries are used).

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9 Maintenance
Nano Flow Cell - Replacing or Cleaning

Wrench plus Torque


The cell body can be fitted in two positions to allow the capillaries routed
NOTE upwards or downwards (depending on where the column is located). Route the
capillaries directly column (inlet) and waste assembly (outlet).

With the instrument accessory kit comes a 4-mm wrench and with the Sealing
NOTE Kit a special adapter. Both together work as a torque wrench with pre-defined
torque (maximum allowed torque for the cell fittings is 0.7 Nm). It can be used to
tight the capillary fittings at the flow cell body. The wrench has to be plugged into
the adapter as shown in Figure 46 on page 184.

Adapter

Wrench DO NOT press down


more than shown here

max
0.7 Nm

Figure 46 Wrench plus Torque Adapter

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9 Maintenance
Cleaning or Exchanging the Holmium Oxide Filter

Cleaning or Exchanging the Holmium Oxide Filter

When If holmium oxide filter is contaminated

Tools required Description


Screwdriver, Pozidriv #1 PT3
Screwdriver, flat blade
Wrench, 1/4 inch
for capillary connections
Pair of tweezers

Parts required # p/n Description


1 79880-22711 Holmium oxide filter

Preparations • Turn the lamp(s) off.


• Open the doors of the module.
• Remove the flow cell, see “Remove and Install a Flow Cell” on page 163.

See also “Declaration of Conformity for HOX2 Filter” on page 276.


NOTE
The glass tends to build a film on its surface even under normal environmental
conditions. This is a phenomenon, which can be found also on the surface of
several other glasses and has something to do with the composition of the
glass. There is no indication, that the film has an influence on the measurement.
Even in the case of a thick film, which scatters the light remarkably, no shift of
the peak positions is to be expected. A slight change in the absorbance might be
possible. Other components within the light path (lenses, windows, ...) are also
changing their behavior over the time.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 185


9 Maintenance
Cleaning or Exchanging the Holmium Oxide Filter

1 Unscrew the six screws and remove the flow cell cover. 2 If not already in this position, move the filter up.

3 Release the holder with a screw driver (at the top). 4 Remove the holmium oxide filter.

NOTE NOTE
Do not scratch the holmium oxide filter. The holmium oxide filter can be cleaned with alcohol and a
lint-free cloth.
5 Insert the holmium oxide filter. 6 Replace the flow cell cover and fix the six screws.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 186


9 Maintenance
Cleaning or Exchanging the Holmium Oxide Filter

7 Perform a holmium oxide test (see “Holmium Oxide 9 Close the doors.
Test” on page 131) to check the proper function of the
holmium oxide filter.
8 Install the flow cell, see “Remove and Install a Flow
Cell” on page 163.

10 Turn on the flow.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 187


9 Maintenance
Correcting Leaks

Correcting Leaks

When If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections

Tools required p/n Description


Tissue
Wrench, 1/4 inch
for capillary connections
5043-0915 Fitting mounting tool

Use tissue to dry the leak sensor area and the leak pan.
NOTE

1 Open the doors. 2 Grab the lamp cover and pull it off (it is fixed by two
magnets in the center of the cover).

Agilent InfinityLab LC Series DAD WR and MWD User Manual 188


9 Maintenance
Correcting Leaks

3 Open the flow cell door. 4 Observe the capillary connections and the flow cell area
for leaks and correct, if required.

NOTE
To check for leaks, establish a flow and observe the flow
cell (outside of the cell compartment) and all capillary
connections.

5 Check the Leak Sensor area for leaks and correct, if 6 Install the flow cell and close the flow cell door.
required.

7 Slide the lamp cover into the top position of the metal 8 Close the doors.
front and press the lamp cover completely in until it
clicks.

1.

2.

9 Perform a Wavelength Verification and Calibration or a Holmium Oxide Test to check the correct positioning of the flow
cell.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 189


9 Maintenance
Replacing Leak Handling System Parts

Replacing Leak Handling System Parts

When If the parts are corroded or broken

Parts required p/n Description


5043-0856 Leak Adapter
5063-6527 Tubing, Silicon Rubber, 1.2 m, ID/OD 6/9 mm

1 Open the doors. 2 Press the Leak Adapter down (1.) and remove it
together with the tubing (2.).

1.
2.

3 Install the Leak Adapter by pressing it into the Main 4 Insert the Tubing (approximately 85 mm required for
Cover. replacement) between Leak Adapter outlet and Leak
Panel.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 190


9 Maintenance
Replacing Leak Handling System Parts

5 Close the doors.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 191


9 Maintenance
Replacing the Module’s Firmware

Replacing the Module’s Firmware

When The installation of newer firmware might be necessary


• if a newer version solves problems of older versions or
• to keep all systems on the same (validated) revision.
The installation of older firmware might be necessary
• to keep all systems on the same (validated) revision or
• if a new module with newer firmware is added to a system or
• if third party control software requires a special version.

Tools required Description


Agilent Lab Advisor software

Parts required # Description


1 Firmware, tools and documentation from Agilent web site

Preparations Read update documentation provided with the Firmware Update Tool.

To upgrade/downgrade the module’s firmware carry out the following steps:


1 Download the required module firmware, the latest FW Update Tool and the
documentation from the Agilent web.
http://www.agilent.com/en-us/firmwareDownload?whid=69761
2 For loading the firmware into the module follow the instructions in the
documentation.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 192


9 Maintenance
Replacing the Module’s Firmware

Module Specific Information


Table 16 Module Specific Information (G7115A DAD/G7165A MWD)

G7115A DAD G7165A MWD

Initial firmware (main D.07.01 D.07.01


and resident)

Compatibility with When using the G7115A or G7165A in a system, all other modules must
1260/1290 Infinity have firmware revision from firmware set 7.00 or above (main and
modules resident).

Compatibility with When using the G7115A or G7165A in a system, all other modules must
1100/1200 Series have firmware revision from firmware set 7.00 or above (main and
modules resident). Otherwise the communication will not work.

Conversion to / • G7115A allows conversion to G1315C/D DAD, G1365C/D MWD


emulation of G1315D or • G7165A allows conversion to G1365C/D MWD
G1365D

Agilent InfinityLab LC Series DAD WR and MWD User Manual 193


9 Maintenance
Information from Module’s Assemblies

Information from Module’s Assemblies

Lamp and Flow Cell RFID Tag


The detector is equipped with a UV lamp and flow cell identification system using
RFID (radio frequency identification) tags attached to the assemblies and RFID
tag readers at the optical unit. The table below lists all parameters stored in the
RFID tag.
Table 17 RFID Tag Data

Lamp information Flow cell information

• product number • product number

• serial number • serial number

• production date • production date

• accumulated UV on time (in hours) • nominal path length of the cell (in mm)

• actual UV lamp on time (in hours) • cell volume () in µL

• number of ignitions • maximum pressure (in bar)

• date of last intensity test • date of last cell test

The pressure value is always displayed in bar, even if the user interface uses
NOTE other units, e.g. PSI.

Serial Number and Firmware Revision


The user interface provides module specific information that is stored in the
main board. These are for example the serial number, firmware revision.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 194


10 Parts for Maintenance

Overview of Maintenance Parts 196


Standard Flow Cell 198
Standard Flow Cell Bio-inert 200
Semi-Micro Flow Cell 202
Micro Flow Cell 204
High Pressure Flow Cell 206
Prep Flow Cell - SST 208
Prep Flow Cell - Quartz 210
Nano Flow Cells 212
Accessory Kits 215
Holmium Oxide Filter 216
Leak Handling Parts 217

This chapter provides information on parts for maintenance and repair.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 195


10 Parts for Maintenance
Overview of Maintenance Parts

Overview of Maintenance Parts

Item p/n Description


1 5067-5737 Door left

2 5067-5736 Door right

3 G1103-60001 Tungsten lamp

4 2140-0820 Longlife Deuterium lamp “C“ (with black cover and RFID tag)

5 5043-1013 Tubing Clip

6 5043-0856 Leak Adapter

7 5063-6527 Tubing, Silicon Rubber, 1.2 m, ID/OD 6/9 mm


for Waste and Leak Adapter (ca. 85 mm required)

8 Flow cell with RFID tag


for details refer to specific flow cell

G1315-60022 Standard flow cell, 10 mm, 13 µL, 120 bar (12 MPa)

G5615-60022 Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar (12 MPa) for
MWD/DAD, includes 0890-1763 – 0.18 x 1500 mm PEEK capillary and
5063-6591 – PEEK fittings

G1315-60025 Semi-micro flow cell, 6 mm, 5 µL, 120 bar (12 MPa)

G1315-60024 Micro flow cell, 3 mm, 2 µL, 120 bar (12 MPa)

G1315-60015 High pressure flow cell, 6 mm, 1.7 µL, 400 bar (40 MPa)

G1315-60016 Prep flow cell SST - 3 mm, 120 bar (12 MPa)

G1315-60017 Prep flow cell quartz, 0.3 mm, 20 bar (2 MPa)

G1315-60018 Prep flow cell quartz, 0.06 mm (2 MPa)

G1315-68724 Semi-nano flow cell kit, 10 mm, 500 nL, 5 MPa

G1315-68716 Nano flow cell kit, 6 mm, 80 nL, 5 MPa

9 5022-6515 Union ZDV

10 Tube PTFE 0.8 mm x 2 m, re-order 5 m

11 G1315-87311 Capillary ST 0.17 mm x 380 mm S/S

79880-22711 Holmium oxide filter


(not shown)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 196


10 Parts for Maintenance
Overview of Maintenance Parts

3 6

1
8
7
4

2 9

11

10
Figure 47 Overview of maintenance parts

Agilent InfinityLab LC Series DAD WR and MWD User Manual 197


10 Parts for Maintenance
Standard Flow Cell

Standard Flow Cell

Item p/n Description


G1315-60022 Standard flow cell, 10 mm, 13 µL, 120 bar (12 MPa)

1 79883-22402 Window screw

2 5062-8553 Washer kit (10/pk)

3 79883-28801 Compression washer

4 79883-22301 Window holder

5 1000-0488 Quartz window

6 G1315-68711 Gasket BACK (PTFE), 2.3 mm hole, outlet side (12/pk)

7 G1315-68710 Gasket FRONT (PTFE), 1.3 mm hole, inlet side (12/pk)

8 Window assembly (comprises window screw, spring washers,


compression washer, window holder and quartz window)

9 G1315-87321 Capillary IN (0.17 mm, 590 mm lg) including heat exchanger

10 G1315-87302 Capillary OUT (0.17 mm, 200 mm lg)

11 G1315-84910 Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

5022-2184 Union ZDV

G1315-68712 Cell repair kit STD


includes window screw kit, 4 mm hexagonal wrench and seal kit

79883-68703 Window screw kit, includes 2 quartz windows, 2 compression


washers, 2 window holders, 2 window screws and 10 washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 198


10 Parts for Maintenance
Standard Flow Cell

8
7

6
5
4
3
11 2

1
9

10

Figure 48 Standard Flow Cell Parts

Gaskets # 6 and #7 have different hole diameters.


NOTE

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Quartz window
6 - Gasket

1 2 3 4 5 6

Figure 49 Orientation of Spring Washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 199


10 Parts for Maintenance
Standard Flow Cell Bio-inert

Standard Flow Cell Bio-inert

Item p/n Description


G5615-60022 Standard flow cell bio-inert, 10 mm, 13 µL, 120 bar (12 MPa) for
MWD/DAD, includes 0890-1763 – 0.18 x 1500 mm PEEK capillary and
5063-6591 – PEEK fittings

1 79883-22402 Window screw

2 5062-8553 Washer kit (10/pk)

3 79883-28801 Compression washer

4 79883-22301 Window holder

5 5190-0921 Sapphire window

6 G1315-68711 Gasket BACK (PTFE), 2.3 mm hole, outlet side (12/pk)

7 G1315-68710 Gasket FRONT (PTFE), 1.3 mm hole, inlet side (12/pk)

8 Window assembly (comprises window screw, spring washers,


compression washer, window holder and sapphire window)

9 G5615-87331 Capillary In (0.17 mm, 590 mm lg), including heat exchanger)

10 G5615-87302 Capillary Out (0.17 mm, 200 mm lg)

11 G1315-84910 Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

5022-2184 Union ZDV

G1315-68712 Cell repair kit STD


includes window screw kit, 4 mm hexagonal wrench and seal kit

G5615-68712 Cell repair kit for bio-inert cell


Contains: 1 x HEX KEY 4MM, 1 x Front seals 12/PK 1 x Back seals-std
cell 12/PK, 1 x Air cushion envelope A5, 1 x ST Cell Screw Kit bio-inert

79883-68704 Cell Screw Kit bio-inert


Contains: 2 x Sapphire Window, 2 x Cell screw assembly, 1 x Container

5067-5695 UHP-FF Fitting

Agilent InfinityLab LC Series DAD WR and MWD User Manual 200


10 Parts for Maintenance
Standard Flow Cell Bio-inert

8
7

6
5
4
3
11 2

1
9

10

Figure 50 Standard Flow Cell Bio-inert

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Sapphire window
6 - Gasket

1 2 3 4 5 6

Figure 51 Orientation of Spring Washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 201


10 Parts for Maintenance
Semi-Micro Flow Cell

Semi-Micro Flow Cell

Item p/n Description


G1315-60025 Semi-micro flow cell, 6 mm, 5 µL, 120 bar (12 MPa)

1 79883-22402 Window screw

2 5062-8553 Washer kit (10/pk)

3 79883-28801 Compression washer

4 79883-22301 Window holder

5 1000-0488 Quartz window

6 79883-68702 Gasket BACK (PTFE), 1.8 mm hole, outlet side (12/pk)

7 G1315-68710 Gasket FRONT (PTFE), 1.3 mm hole, inlet side (12/pk)

8 Window assembly (comprises window screw, spring washers,


compression washer, window holder and quartz window)

9 G1315-87319 Capillary IN (0.17 mm, 310 mm lg) including heat exchanger

10 G1315-87306 Capillary OUT (0.12 mm, 200 mm lg)

10 G1315-87302 Capillary OUT (0.17 mm, 200 mm lg)

11 G1315-84910 Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

5022-2184 Union ZDV

G1315-68713 Cell repair kit semi-micro, includes window screw kit, Gasket Kit BACK,
Gasket Kit FRONT and 4 mm hexagonal wrench

79883-68703 Window screw kit, includes 2 quartz windows, 2 compression


washers, 2 window holders, 2 window screws and 10 washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 202


10 Parts for Maintenance
Semi-Micro Flow Cell

8
7

6
5
4
3
11 2

1
9

10

Figure 52 Semi-Micro Flow Cell Parts

Gaskets # 6 and #7 have different hole diameters.


NOTE

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Quartz window
6 - Gasket

1 2 3 4 5 6

Figure 53 Orientation of Spring Washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 203


10 Parts for Maintenance
Micro Flow Cell

Micro Flow Cell

Item p/n Description


G1315-60024 Micro flow cell, 3 mm, 2 µL, 120 bar (12 MPa)

1 79883-22402 Window screw

2 5062-8553 Washer kit (10/pk)

3 79883-28801 Compression washer

4 79883-22301 Window holder

5 1000-0488 Quartz window

6 79883-68702 Gasket BACK (PTFE), 1.8 mm hole, outlet side (12/pk)

7 G1315-68710 Gasket FRONT (PTFE), 1.3 mm hole, inlet side (12/pk)

8 Window assembly (comprises window screw, spring washers,


compression washer, window holder and quartz window)

9 G1315-87339 DAD Heat Exchanger Capillary 310 mm, 0.12 mm i.d.

10 G1315-87306 Capillary OUT (0.12 mm, 200 mm lg)

10 G1315-87302 Capillary OUT (0.17 mm, 200 mm lg)

11 G1315-84910 Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

5022-2184 Union ZDV

G1315-68713 Cell repair kit semi-micro, includes window screw kit, Gasket Kit BACK,
Gasket Kit FRONT and 4 mm hexagonal wrench

79883-68703 Window screw kit, includes 2 quartz windows, 2 compression


washers, 2 window holders, 2 window screws and 10 washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 204


10 Parts for Maintenance
Micro Flow Cell

8
7

6
5
4
3
11 2

1
9

10

Figure 54 Micro Flow Cell Parts

Gaskets # 6 and #7 have different hole diameters.


NOTE

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Quartz window
6 - Gasket

1 2 3 4 5 6

Figure 55 Orientation of Spring Washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 205


10 Parts for Maintenance
High Pressure Flow Cell

High Pressure Flow Cell

Item p/n Description


G1315-60015 High pressure flow cell, 6 mm, 1.7 µL, 400 bar (40 MPa)

1 Window assembly, comprises items 2, 3, 4, 5 and 6

2 79883-27101 Seal ring

3 1000-0953 Quartz window

4 79883-28802 Compression washer

5 5062-8553 Washer kit (10/pk)

6 79883-22404 Window screw

7 G1315-87325 Capillary IN (0.12 mm, 290 mm lg) including heat exchanger

8 G1315-87306 Capillary OUT (0.12 mm, 200 mm lg)

9 G1315-84901 Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

G1315-87312 Capillary ST 0.12 mm x 150 mm S/S

G1315-87311 Capillary ST 0.17 mm x 380 mm S/S

79883-68700 High pressure cell repair kit (includes 1 quartz window, 1 compression
washer, 5 spring washers, 2 seal rings)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 206


10 Parts for Maintenance
High Pressure Flow Cell

6
5
4
2
3 2

9
8

Figure 56 High pressure flow cell - parts

Agilent InfinityLab LC Series DAD WR and MWD User Manual 207


10 Parts for Maintenance
Prep Flow Cell - SST

Prep Flow Cell - SST

For more details on the Preparative Flow Cells refer to the technical note that
NOTE comes with the flow cells.

Item p/n Description


G1315-60016 Prep flow cell SST - 3 mm, 120 bar (12 MPa)
recommended flow rate: 50 mL/min

1 G1315-60021 Cell screw assembly (comprises window screw, spring washers,


compression washer, window holder and quartz window)

G1315-68712 Cell repair kit STD


includes window screw kit, 4 mm hexagonal wrench and seal kit

2 G1315-68711 Gasket BACK (PTFE), 2.3 mm hole, outlet side (12/pk)

3 G1315-68710 Gasket FRONT (PTFE), 1.3 mm hole, inlet side (12/pk)

4 G1315-87305 Capillary SST, 250 mm length, 0.5 mm i.d., o.D. 0.9 mm


with fittings for flow cell assembled

4a 5062-2418 1/16” fittings and ferrules


10/pk

5 G1315-27706 Cell body

6 G1315-84901 Clamp unit

7 G1315-84902 Handle for Clamp unit

0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

Agilent InfinityLab LC Series DAD WR and MWD User Manual 208


10 Parts for Maintenance
Prep Flow Cell - SST

1
3
5

2 1

6
4 - inlet
4 - outlet

4a

Figure 57 Prep Flow Cell - SST Parts

Gaskets #2 and #3 have different hole diameters.


NOTE

1 - Window screw
2 - Spring washers
3 - Compression washer
4 - Window holder
5 - Quartz window
6 - Gasket

1 2 3 4 5 6

Figure 58 Orientation of Spring Washers

Agilent InfinityLab LC Series DAD WR and MWD User Manual 209


10 Parts for Maintenance
Prep Flow Cell - Quartz

Prep Flow Cell - Quartz

For more details on the Preparative Flow Cells refer to the technical note that
NOTE comes with the flow cells.

Item p/n Description


G1315-60017 Prep flow cell quartz, 0.3 mm, 20 bar (2 MPa)

G1315-60018 Prep flow cell quartz, 0.06 mm (2 MPa)

1 0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

2 G1315-84902 Handle for Clamp unit

3 G1315-84901 Clamp unit

4 G1315-80004 Quartz body - Prep Cell 0.3 mm

4 G1315-80003 Quartz body - Prep Cell 0.06 mm

5 G1315-67302 PTFE tubing 80 cm length, 0.5 mm i.d., o.D. 1.6 mm

6 G1315-27705 Cell housing

7 G1315-67301 PTFE tubing 2 m length, 0.8 mm i.d., o.D. 1.6 mm

0100-1516 Finger-tight fitting PEEK, 2/pk

The flow cell comes with two tubings 0.8 mm i.d. and one 0.5 mm i.d. so that the
NOTE combination at the flow cell could be either 0.8/0.8 or 0.5/0.8 (inlet/outlet).
Standard is 0.8/0.8. Depending on the system pressure (<30 mL/min) or
bandbroadening, the inlet tubing might be changed to 0.5 mm.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 210


10 Parts for Maintenance
Prep Flow Cell - Quartz

2
3

Figure 59 Prep Flow Cell - Quartz Parts

Agilent InfinityLab LC Series DAD WR and MWD User Manual 211


10 Parts for Maintenance
Nano Flow Cells

Nano Flow Cells

The following kits are available:


Table 18 Nano-flow cell kits

Part number Comments

Semi-nano flow cell kit, 10 mm, 500 nL, 5 completely assembled (includes items 1, 2, 3, 4, 10,
MPa (G1315-68724) 11, 12, 13, 14, 15, and 16)

Nano flow cell kit, 6 mm, 80 nL, 5 MPa ( completely assembled (includes items 1, 2, 3, 4, 10,
G1315-68716) 11, 12, 13, 14, 15, and 16)

Figure 60 on page 213 shows all parts delivered with the nano-flow cell kits.
Generic parts for both nano-flow cells:

Item p/n Description


3 5063-6593 Fitting Screw
(for 4 mm wrench)

4 Cell ferrules are factory installed

5 5065-4422 PEEK fitting 1/32"

7 5063-6592 Litetouch ferrules LT-100, (1/32" Ferrule and SS lock ring)

8 5022-2146 Union Adjustment Tool

9 5022-2184 Union ZDV

10 G1315-45003 Torque adapter

14 G1315-84902 Handle for Clamp unit

15 G1315-84910 Clamp unit

16 0515-1056 Screw M 2.5, 4 mm lg


for cell body/clamp

17 8710-1534 Wrench, 4 mm both ends, open end

Agilent InfinityLab LC Series DAD WR and MWD User Manual 212


10 Parts for Maintenance
Nano Flow Cells

2
11
12 3, 4 3, 4 1

13
5

10 7
16
15
8 9
14

17

Figure 60 Content of kits

Specific parts for the semi-nano flow cell

Item p/n Description


G1315-68724 Semi-nano flow cell kit, 10 mm, 500 nL, 5 MPa

1 G1315-87333 PEEK coated fused silica capillary Inlet (100 µm) pre-mounted to cell,
includes Inlet capillary, 300 mm long, 100 µm i.d. with pre-fixed
ferrules (#4) and fittings (#3), plus one PEEK Fitting FT (#5)

2 G1315-87338 PEEK coated fused silica capillary Outlet (100 µm) pre-mounted to
cell, includes Outlet capillary, 120 mm long, 100 µm i.d. with pre-fixed
ferrules (#4) and fitting (#3), plus one PEEK Fitting FT (#5)

1 G1315-87323 PEEK coated fused silica capillary Inlet (50 µm) alternative, includes
Inlet capillary, 400 mm long, 50 µm i.d. with pre-fixed ferrules (#4) and
fittings (#3), plus one PEEK Fitting FT (#5)

2 G1315-87328 PEEK coated fused silica capillary Outlet (50 µm), alternative, includes
Outlet capillary, 120 mm long, 50 µm i.d. with pre-fixed ferrules (#4)
and fitting (#3), plus one PEEK Fitting FT (#5)

11 G1315-27703 Cell Housing (500 nL)

12 G1315-87101 Cell Seal Assembly (500 nL)

13 G1315-80001 Quartz Body (500 nL)

G1315-68715 Sealing Kit

Agilent InfinityLab LC Series DAD WR and MWD User Manual 213


10 Parts for Maintenance
Nano Flow Cells

Specific parts for the nano flow cell

Item p/n Description


G1315-68716 Nano flow cell kit, 6 mm, 80 nL, 5 MPa

1 G1315-87323 PEEK coated fused silica capillary Inlet (50 µm) alternative, includes
Inlet capillary, 400 mm long, 50 µm i.d. with pre-fixed ferrules (#4) and
fittings (#3), plus one PEEK Fitting FT (#5)

2 G1315-87328 PEEK coated fused silica capillary Outlet (50 µm), alternative, includes
Outlet capillary, 120 mm long, 50 µm i.d. with pre-fixed ferrules (#4)
and fitting (#3), plus one PEEK Fitting FT (#5)

1 G1315-87313 PEEK coated fused silica capillary Inlet (25 µm) alternative, includes
Inlet capillary, 200 mm long, 25 µm i.d. with pre-fixed ferrules (#4) and
fittings (#3), plus one PEEK Fitting FT (#5)

2 G1315-87318 PEEK coated fused silica capillary Outlet (25 µm) alternative, includes
Outlet capillary, 600 mm long, 25 µm i.d. with pre-fixed ferrules (#4)
and fitting (#3), plus one PEEK Fitting FT (#5)

G1315-27704 Cell Housing (80 nL)

G1315-87102 Cell Seal Assembly (80 nL)

G1315-80002 Quartz Body (80 nL)

G1315-68725 Sealing Kit 80 nL cell

Agilent InfinityLab LC Series DAD WR and MWD User Manual 214


10 Parts for Maintenance
Accessory Kits

Accessory Kits

Detector Accessory Kit (G7115-68755) contains the following items:

p/n Description
5062-8535 Waste accessory kit

5500-1155 Tube Connector, 90 degree, ID 6.4

0100-1516 Finger-tight fitting PEEK, 2/pk

5181-1516 CAN cable, Agilent module to module, 0.5 m

5500-1191 InfinityLab Quick Turn Capillary ST 0.12 mm x 280 mm, long socket

Agilent InfinityLab LC Series DAD WR and MWD User Manual 215


10 Parts for Maintenance
Holmium Oxide Filter

Holmium Oxide Filter

Item p/n Description


1 G7115-68700 Filter motor assembly (includes filter lever G1315-45001 and spring
1460-1510)

2 1460-1510 Spring

3 G1315-45001 Filter lever

4 79880-22711 Holmium oxide filter

When the filter motor has been removed, the filter lever should not be reused.
NOTE Use always a new filter lever to assure correct fit on the filter motor shaft.

3
4

Figure 61 Holmium Oxide Filter Parts

Agilent InfinityLab LC Series DAD WR and MWD User Manual 216


10 Parts for Maintenance
Leak Handling Parts

Leak Handling Parts

Item p/n Description


1 5043-0856 Leak Adapter

2 5063-6527 Tubing, Silicon Rubber, 1.2 m, ID/OD 6/9 mm

3 5061-3356 Leak Sensor Assembly

4 G7115-45000 Leak Plane 1260 DAD Infinity II

0515-2529 Screw Tapping PAN-HD-TORX T10 3x8 ST-ZN


(not shown)

5043-1013 Tubing Clip

Figure 62 Leak Parts

Agilent InfinityLab LC Series DAD WR and MWD User Manual 217


11 Identifying Cables

Cable Overview 219


Analog Cables 221
Remote Cables 223
BCD Cables 226
CAN/LAN Cables 228
Agilent 1200 module to PC 229

This chapter provides information on cables used with the Agilent 1200 Infinity
Series modules.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 218


11 Identifying Cables
Cable Overview

Cable Overview

Never use cables other than the ones supplied by Agilent Technologies to ensure
NOTE proper functionality and compliance with safety or EMC regulations.

Analog cables

p/n Description
35900-60750 Agilent module to 3394/6 integrators

35900-60750 Agilent 35900A A/D converter

01046-60105 Analog cable (BNC to general purpose, spade lugs)

Remote cables

p/n Description
03394-60600 Agilent module to 3396A Series I integrators

3396 Series II / 3395A integrator, see details in section “Remote


Cables” on page 223

03396-61010 Agilent module to 3396 Series III / 3395B integrators

5061-3378 Remote Cable

01046-60201 Agilent module to general purpose

BCD cables

p/n Description
03396-60560 Agilent module to 3396 integrators

G1351-81600 Agilent module to general purpose

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11 Identifying Cables
Cable Overview

CAN cables

p/n Description
5181-1516 CAN cable, Agilent module to module, 0.5 m

5181-1519 CAN cable, Agilent module to module, 1 m

LAN cables

p/n Description
5023-0203 Cross-over network cable, shielded, 3 m (for point to point connection)

5023-0202 Twisted pair network cable, shielded, 7 m (for point to point


connection)

RS-232 cables

p/n Description
RS232-61601 RS-232 cable, 2.5 m
Instrument to PC, 9-to-9 pin (female). This cable has special pin-out,
and is not compatible with connecting printers and plotters. It is also
called "Null Modem Cable" with full handshaking where the wiring is
made between pins 1-1, 2-3, 3-2, 4-6, 5-5, 6-4, 7-8, 8-7, 9-9.

5181-1561 RS-232 cable, 8 m

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11 Identifying Cables
Analog Cables

Analog Cables

One end of these cables provides a BNC connector to be connected to Agilent


modules. The other end depends on the instrument to which connection is being
made.

Agilent Module to 3394/6 Integrators

p/n 35900-60750 Pin 3394/6 Pin Agilent Signal Name


module

1 Not connected

2 Shield Analog -

3 Center Analog +

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11 Identifying Cables
Analog Cables

Agilent Module to BNC Connector

p/n 8120-1840 Pin BNC Pin Agilent Signal Name


module

Shield Shield Analog -

Center Center Analog +

Agilent Module to General Purpose

p/n 01046-60105 Pin Pin Agilent Signal Name


module

1 Not connected

2 Black Analog -

3 Red Analog +

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11 Identifying Cables
Remote Cables

Remote Cables

One end of these cables provides a Agilent Technologies APG (Analytical


Products Group) remote connector to be connected to Agilent modules. The
other end depends on the instrument to be connected to.

Agilent Module to 3396A Integrators

p/n 03394-60600 Pin 3396A Pin Agilent Signal Name Active


module (TTL)

9 1 - White Digital ground

NC 2 - Brown Prepare run Low

3 3 - Gray Start Low

NC 4 - Blue Shut down Low

NC 5 - Pink Not connected

NC 6 - Yellow Power on High

5,14 7 - Red Ready High

1 8 - Green Stop Low

NC 9 - Black Start request Low

13, 15 Not connected

Agilent Module to 3396 Series II / 3395A Integrators


Use the cable Agilent module to 3396A Series I integrators (03394-60600) and
cut pin #5 on the integrator side. Otherwise the integrator prints START; not
ready.

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11 Identifying Cables
Remote Cables

Agilent Module to 3396 Series III / 3395B Integrators

p/n 03396-61010 Pin 33XX Pin Agilent Signal Name Active


module (TTL)

9 1 - White Digital ground

NC 2 - Brown Prepare run Low

3 3 - Gray Start Low

NC 4 - Blue Shut down Low

NC 5 - Pink Not connected

NC 6 - Yellow Power on High

14 7 - Red Ready High

4 8 - Green Stop Low

NC 9 - Black Start request Low

13, 15 Not connected

Agilent Module to Agilent 35900 A/D Converters

p/n 5061-3378 Pin 35900 A/D Pin Agilent Signal Name Active
module (TTL)

1 - White 1 - White Digital ground

2 - Brown 2 - Brown Prepare run Low

3 - Gray 3 - Gray Start Low

4 - Blue 4 - Blue Shut down Low

5 - Pink 5 - Pink Not connected

6 - Yellow 6 - Yellow Power on High

7 - Red 7 - Red Ready High

8 - Green 8 - Green Stop Low

9 - Black 9 - Black Start request Low

Agilent InfinityLab LC Series DAD WR and MWD User Manual 224


11 Identifying Cables
Remote Cables

Agilent Module to General Purpose

p/n 01046-60201 Wire Color Pin Agilent Signal Name Active


module (TTL)

White 1 Digital ground

Brown 2 Prepare run Low

Gray 3 Start Low

Blue 4 Shut down Low

Pink 5 Not connected

Yellow 6 Power on High

Red 7 Ready High

Green 8 Stop Low

Black 9 Start request Low

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11 Identifying Cables
BCD Cables

BCD Cables

One end of these cables provides a 15-pin BCD connector to be connected to the
Agilent modules. The other end depends on the instrument to be connected to

Agilent Module to General Purpose

p/n G1351-81600 Wire Color Pin Agilent Signal Name BCD Digit
module

Green 1 BCD 5 20

Violet 2 BCD 7 80

Blue 3 BCD 6 40

Yellow 4 BCD 4 10

Black 5 BCD 0 1

Orange 6 BCD 3 8

Red 7 BCD 2 4

Brown 8 BCD 1 2

Gray 9 Digital ground Gray

Gray/pink 10 BCD 11 800

Red/blue 11 BCD 10 400

White/green 12 BCD 9 200

Brown/green 13 BCD 8 100

not connected 14

not connected 15 +5V Low

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11 Identifying Cables
BCD Cables

Agilent Module to 3396 Integrators

p/n 03396-60560 Pin 3396 Pin Agilent Signal Name BCD Digit
module

1 1 BCD 5 20

2 2 BCD 7 80

3 3 BCD 6 40

4 4 BCD 4 10

5 5 BCD0 1

6 6 BCD 3 8

7 7 BCD 2 4

8 8 BCD 1 2

9 9 Digital ground

NC 15 +5V Low

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11 Identifying Cables
CAN/LAN Cables

CAN/LAN Cables

Both ends of this cable provide a modular plug to be connected to


Agilent modules CAN or LAN connectors.
CAN Cables

p/n Description
5181-1516 CAN cable, Agilent module to module, 0.5 m

5181-1519 CAN cable, Agilent module to module, 1 m

LAN Cables

p/n Description
5023-0203 Cross-over network cable, shielded, 3 m (for point to point connection)

5023-0202 Twisted pair network cable, shielded, 7 m (for point to point


connection)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 228


11 Identifying Cables
Agilent 1200 module to PC

Agilent 1200 module to PC

p/n Description
RS232-61601 RS-232 cable, 2.5 m
Instrument to PC, 9-to-9 pin (female). This cable has special pin-out,
and is not compatible with connecting printers and plotters. It is also
called "Null Modem Cable" with full handshaking where the wiring is
made between pins 1-1, 2-3, 3-2, 4-6, 5-5, 6-4, 7-8, 8-7, 9-9.

5181-1561 RS-232 cable, 8 m

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12 Hardware Information

Firmware Description 231


Electrical Connections 234
Rear View of the Module 235
Serial Number Information (ALL) 235
Interfaces 236
Interfaces Overview 238
ERI (Enhanced Remote Interface) 240
USB (Universal Serial Bus) 242
Setting the 6-bit Configuration Switch 243
Special Settings 245
Instrument Layout 247
Early Maintenance Feedback (EMF) 248

This chapter describes the detector in more detail on hardware and electronics.

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12 Hardware Information
Firmware Description

Firmware Description

The firmware of the instrument consists of two independent sections:


• a non-instrument specific section, called resident system
• an instrument specific section, called main system

Resident System
This resident section of the firmware is identical for all Agilent
1100/1200/1220/1260/1290 series modules. Its properties are:
• the complete communication capabilities (CAN, LAN, USB and RS- 232)
• memory management
• ability to update the firmware of the 'main system'

Main System
Its properties are:
• the complete communication capabilities (CAN, LAN, USB and RS- 232)
• memory management
• ability to update the firmware of the 'resident system'
In addition the main system comprises the instrument functions that are divided
into common functions like
• run synchronization through APG/ERI remote,
• error handling,
• diagnostic functions,
• or module specific functions like
• internal events such as lamp control, filter movements,
• raw data collection and conversion to absorbance.

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12 Hardware Information
Firmware Description

Firmware Updates
Firmware updates can be done with the Agilent Lab Advisor software with files
on the hard disk (latest version should be used).
Required tools, firmware and documentation are available from the Agilent web:
http://www.agilent.com/en-us/firmwareDownload?whid=69761
The file naming conventions are:
PPPP_RVVV_XXX.dlb, where
• PPPP is the product number, for example, 1315B for the G1315B DAD,
• R the firmware revision, for example, A for G1315B or B for the G1315C DAD,
• VVV is the revision number, for example 650 is revision 6.50,
• XXX is the build number of the firmware.
For instructions on firmware updates refer to section Replacing Firmware in
chapter "Maintenance" or use the documentation provided with the Firmware
Update Tools.

Update of main system can be done in the resident system only. Update of the
NOTE resident system can be done in the main system only.
Main and resident firmware must be from the same set.

Main FW update
Resident System Main System

Resident FW Update

Figure 63 Firmware Update Mechanism

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12 Hardware Information
Firmware Description

Some modules are limited in downgrading due to their mainboard version or


NOTE their initial firmware revision. For example, a G1315C DAD SL cannot be
downgraded below firmware revision B.01.02 or to a A.xx.xx.
Some modules can be re-branded (e.g. G1314C to G1314B) to allow operation in
specific control software environments. In this case, the feature set of the target
type is used and the feature set of the original one is lost. After re-branding (e.g.
from G1314B to G1314C), the original feature set is available again.
All this specific information is described in the documentation provided with the
firmware update tools.

The firmware update tools, firmware and documentation are available from the
Agilent web.
• http://www.agilent.com/en-us/firmwareDownload?whid=69761

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12 Hardware Information
Electrical Connections

Electrical Connections

• The CAN bus is a serial bus with high-speed data transfer. The two
connectors for the CAN bus are used for internal module data transfer and
synchronization.
• One analog output provides signals for integrators or data handling systems.
• The ERI/REMOTE connector may be used in combination with other analytical
instruments from Agilent Technologies if you want to use features such as
start, stop, common shutdown, prepare, and so on.
• With the appropriate software, the LAN connector may be used to control the
module from a computer through a LAN connection. This connector is
activated and can be configured with the configuration switch.
• With the appropriate software, the USB connector may be used to control the
module from a computer through a USB connection.
• The power input socket accepts a line voltage of 100 – 240 VAC ± 10 % with a
line frequency of 50 or 60 Hz. Maximum power consumption varies by
module. There is no voltage selector on your module because the power
supply has wide-ranging capability. There are no externally accessible fuses
because automatic electronic fuses are implemented in the power supply.

Never use cables other than the ones supplied by Agilent Technologies to ensure
NOTE proper functionality and compliance with safety or EMC regulations.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 234


12 Hardware Information
Electrical Connections

Rear View of the Module

Figure 64 Rear view of the detector

Serial Number Information (ALL)


The serial number information on the instrument labels provide the following
information:

CCXZZ00000 Format

CC Country of manufacturing
• DE = Germany
• JP = Japan
• CN = China

X Alphabetic character A-Z (used by manufacturing)

ZZ Alpha-numeric code 0-9, A-Z, where each combination


unambiguously denotes a module (there can be more than one
code for the same module)

00000 Serial number

Agilent InfinityLab LC Series DAD WR and MWD User Manual 235


12 Hardware Information
Interfaces

Interfaces

The Agilent InfinityLab LC Series modules provide the following interfaces:


Table 19 Agilent InfinityLab LC Series Interfaces

Module CAN USB LAN RS-232 Analog APG (A) Special


(on-board) / ERI (E)

Pumps

G7104A/C 2 No Yes Yes 1 A

G7110B 2 Yes Yes No No E

G7111A/B, G5654A 2 Yes Yes No No E

G7112B 2 Yes Yes No No E

G7120A, G7132A 2 No Yes Yes 1 A

G7161A/B 2 Yes Yes No No E

Samplers

G7129A/B/C 2 Yes Yes No No E

G7167A/B, G7137A, G5668A 2 Yes Yes No No E

G7157A 2 Yes Yes No No E

Detectors

G7114A/B 2 Yes Yes No 1 E

G7115A 2 Yes Yes No 1 E

G7117A/B/C 2 Yes Yes No 1 E

G7121A/B 2 Yes Yes No 1 E

G7162A/B 2 Yes Yes No 1 E

G7165A 2 Yes Yes No 1 E

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12 Hardware Information
Interfaces

Table 19 Agilent InfinityLab LC Series Interfaces

Module CAN USB LAN RS-232 Analog APG (A) Special


(on-board) / ERI (E)

Fraction Collectors

G7158B 2 Yes Yes No No E

G7159B 2 Yes Yes No No E

G7166A 2 No No No No No Requires a host module


with on-board LAN with
minimum FW B.06.40 or
C.06.40, or with
additional G1369C LAN
Card

G1364E/F, G5664B 2 Yes Yes No No E THERMOSTAT for


G1330B

Others

G7116A/B 2 No No No No No Requires a host module


with on-board LAN or
with additional G1369C
LAN Card.

G7122A No No No Yes No A

G7170B 2 No No No No No Requires a host module


with on-board LAN with
minimum FW B.06.40 or
C.06.40, or with
additional G1369C LAN
Card

The detector (DAD/MWD/FLD/VWD/RID) is the preferred access point for


NOTE control via LAN. The inter-module communication is done via CAN.

• CAN connectors as interface to other modules


• LAN connector as interface to the control software
• RS-232C as interface to a computer
• USB (Universal Series Bus) as interface to a computer
• REMOTE connector as interface to other Agilent products
• Analog output connector(s) for signal output

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12 Hardware Information
Interfaces

Interfaces Overview
CAN
The CAN is inter-module communication interface. It is a 2-wire serial bus
system supporting high speed data communication and real-time requirement.

LAN
The modules have either an interface slot for a LAN card (e.g. Agilent G1369B/C
LAN Interface) or they have an on-board LAN interface (e.g. detectors G1315C/D
DAD and G1365C/D MWD). This interface allows the control of the
module/system via a PC with the appropriate control software. Some modules
have neither on-board LAN nor an interface slot for a LAN card (e.g. G1170A
Valve Drive or G4227A Flexible Cube). These are hosted modules and require a
Host module with firmware B.06.40 or later or with additional G1369C LAN Card.

If an Agilent detector (DAD/MWD/FLD/VWD/RID) is in the system, the LAN


NOTE should be connected to the DAD/MWD/FLD/VWD/RID (due to higher data load).
If no Agilent detector is part of the system, the LAN interface should be installed
in the pump or autosampler.

USB
The USB interface replaces the RS-232 Serial interface in new FUSION generation
modules. For details on USB refer to “USB (Universal Serial Bus)” on page 242.

Analog Signal Output


The analog signal output can be distributed to a recording device. For details
refer to the description of the module’s mainboard.

Remote (ERI)
The ERI (Enhanced Remote Interface) connector may be used in combination
with other analytical instruments from Agilent Technologies if you want to use
features as common shut down, prepare, and so on.
It allows easy connection between single instruments or systems to ensure
coordinated analysis with simple coupling requirements.
The subminiature D connector is used. The module provides one remote
connector which is inputs/outputs (wired- or technique).

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12 Hardware Information
Interfaces

To provide maximum safety within a distributed analysis system, one line is


dedicated to SHUT DOWN the system’s critical parts in case any module detects
a serious problem. To detect whether all participating modules are switched on
or properly powered, one line is defined to summarize the POWER ON state of all
connected modules. Control of analysis is maintained by signal readiness READY
for next analysis, followed by START of run and optional STOP of run triggered on
the respective lines. In addition PREPARE and START REQUEST may be issued.
The signal levels are defined as:
• standard TTL levels (0 V is logic true, + 5.0 V is false),
• fan-out is 10,
• input load is 2.2 kOhm against + 5.0 V, and
• output are open collector type, inputs/outputs (wired- or technique).

All common TTL circuits operate with a 5 V power supply. A TTL signal is defined
NOTE as "low" or L when between 0 V and 0.8 V and "high" or H when between 2.0 V
and 5.0 V (with respect to the ground terminal).

Table 20 ERI signal distribution

Pin Signal Description

1 START REQUEST (L) Request to start injection cycle (for example, by start key on any
module). Receiver is the autosampler.

2 STOP (L) Request to reach system ready state as soon as possible (for
example, stop run, abort or finish and stop injection). Receiver is any
module performing run-time controlled activities.

3 READY (H) System is ready for next analysis. Receiver is any sequence
controller.

4 POWER ON (H) All modules connected to system are switched on. Receiver is
any module relying on operation of others.

5 Not used

6 SHUT DOWN (L) System has serious problem (for example, leak: stops pump).
Receiver is any module capable to reduce safety risk.

7 START (L) Request to start run / timetable. Receiver is any module


performing run-time controlled activities.

8 PREPARE (L) Request to prepare for analysis (for example, calibration,


detector lamp on). Receiver is any module performing pre-analysis
activities.

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12 Hardware Information
Interfaces

Special Interfaces
There is no special interface for this module.

ERI (Enhanced Remote Interface)


ERI replaces the AGP Remote Interface that is used in the HP
1090/1040/1050/1100 HPLC systems and Agilent 1100/1200/1200 Infinity
HPLC modules. All new InfinityLab LC Series products using the FUSION core
electronics use ERI. This interface is already used in the Agilent Universal
Interface Box 2 (UIB2)

ERI Description
The ERI interface contains eight individual programmable input/output pins. In
addition, it provides 24 V power and 5 V power and a serial data line to detect and
recognize further add-ons that could be connected to this interface. This way the
interface can support various additional devices like sensors, triggers (in and out)
and small controllers, etc.

ERI

Figure 65 Location of the ERI interface (example shows a G7114A/B VWD)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 240


12 Hardware Information
Interfaces

Pin Enhanced Remote

1 IO 1 (START
REQUEST)

2 IO 2 (STOP)

3 IO 3 (READY)

4 IO 4 (POWER ON)

5 IO 5 (NOT USED)

6 IO 6 (SHUT DOWN)

7 IO 7 (START)

8 IO 8 (PREPARE)

9 1 wire DATA

10 DGND

11 +5 V ERI out

12 PGND

13 PGND

14 +24 V ERI out

15 +24 V ERI out

IO (Input/Output) Lines
• Eight generic bi-directional channels (input or output).
• Same as the APG Remote.
• Devices like valves, relays, ADCs, DACs, controllers can be
supported/controlled.

1-Wire Data (Future Use)


This serial line can be used to read out an EPROM or write into an EPROM of a
connected ERI-device. The firmware can detect the connected type of device
automatically and update information in the device (if required).

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12 Hardware Information
Interfaces

5V Distribution (Future Use)


• Available directly after turning on the hosting module (assures that the
firmware can detect certain basic functionality of the device).
• For digital circuits or similar.
• Provides 500 mA maximum.
• Short-circuit proof with automatic switch off (by firmware).

24V Distribution (Future Use)


• Available by firmware command (defined turn on/off).
• For devices that need higher power
• Class 0: 0.5 A maximum (12 W)
• Class 1: 1.0 A maximum (24 W)
• Class 2: 2.0 A maximum (48 W)
• Class depends on hosting module’s internal power overhead.
• If a connected device requires more power the firmware detects this
(overcurrent detection) and provides the information to the user interface.
• Fuse used for safety protection (on board).
• Short circuit will be detected through hardware.

USB (Universal Serial Bus)


USB (Universal Serial Bus) - replaces RS232, supports:
• a PC with control software (for example Agilent Lab Advisor)
• USB Flash Disk

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12 Hardware Information
Setting the 6-bit Configuration Switch

Setting the 6-bit Configuration Switch

The 6-bit configuration switch is located at the rear of the module with FUSION
electronics. Switch settings provide configuration parameters for LAN and
instrument specific initialization procedures.
All modules with FUSION electronics:
• Default is ALL switches DOWN (best settings).
• Default IP address for LAN 192.168.254.11
• For specific LAN modes switches 4-5 must be set as required.
• For boot resident/cold start modes switches 1+2 or 6 must be UP.

Configuration switch

Figure 66 Location of Configuration switch (example shows a G7114A/B VWD)

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12 Hardware Information
Setting the 6-bit Configuration Switch

Table 21 6-bit Configuration Switch

Mode Function/Setting

Switch 1 Switch 2 Switch 3 Switch 4 Switch 5 Switch 6

COM1 0 n.a.2 n.a. LAN Init Mode n.a.

Use Default IP Address3 0 0 0 0 0

Use Stored IP Address 0 0 0 1 0

Use DHCP to request IP Address4 0 0 1 0 0

Test 1 System n.a. n.a. n.a. ColdStart

Boot Main System / Keep Data 0 0 0 0 0

Boot Resident System / Keep Data 1 0 0 0 0

Boot Main System / Revert to


0 0 0 0 1
Default Data

Boot Resident System / Revert to


1 0 0 0 1
Default Data

1 When selecting mode COM, settings are stored to non-volatile memory. When selecting mode TEST, COM settings are taken from
non-volatile memory.

2 not assigned - Always keep these switches on position ‘0’ (off)

3 Default IP Address is 192.168.254.11

4 Host Name will be the MAC address.

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12 Hardware Information
Setting the 6-bit Configuration Switch

Special Settings
Boot-Resident/Main
Firmware update procedures may require this mode in case of firmware loading
errors (main/resident firmware part).
If you use the following switch settings and power the instrument up again, the
instrument firmware stays in the resident/main mode. In resident mode, it is not
operable as a module. It only uses basic functions of the operating system for
example, for communication. In this mode the main firmware can be loaded
(using update utilities).

Forced Cold Start


A forced cold start can be used to bring the module into a defined mode with
default parameter settings.
• Boot Main System / Revert to Default Data
The instrument will boot to main mode and changes to the module’s default
parameter. May be also required to load resident firmware into the module.
• Boot Resident System / Revert to Default Data
The instrument will boot to resident mode and changes to the module’s
default parameter. May be also required to load main firmware into the
module.

Loss of data
C AU T I O N
Forced cold start erases all methods and data stored in the non-volatile
memory. Exceptions are calibration settings, diagnosis and repair log books
which will not be erased.
 Save your methods and data before executing a forced cold start.

If you use the following switch settings and power the instrument up again, it will
start as described above.

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12 Hardware Information
Setting the 6-bit Configuration Switch

Table 22 Boot Resident / Forced Coldstart

SW1 SW2 SW3 SW4 SW5 SW6 Init Mode

1 0 0 0 0 0 Boot Main System / Keep Data

1 1 0 0 0 0 Boot Resident System / Keep Data

1 0 0 0 0 1 Boot Main System / Revert to Default Data

1 1 0 0 0 1 Boot Resident System / Revert to Default Data

Note: The setting '0' (down) is essential.

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12 Hardware Information
Instrument Layout

Instrument Layout

The industrial design of the module incorporates several innovative features. It


uses Agilent’s E-PAC concept for the packaging of electronics and mechanical
assemblies. This concept is based upon the use of expanded polypropylene
(EPP) layers of foam plastic spacers in which the mechanical and electronic
boards components of the module are placed. This pack is then housed in a
metal inner cabinet which is enclosed by a plastic external cabinet. The
advantages of this packaging technology are:
• virtual elimination of fixing screws, bolts or ties, reducing the number of
components and increasing the speed of assembly/disassembly,
• the plastic layers have air channels molded into them so that cooling air can
be guided exactly to the required locations,
• the plastic layers help cushion the electronic and mechanical parts from
physical shock, and
• the metal inner cabinet shields the internal electronics from electromagnetic
interference and also helps to reduce or eliminate radio frequency emissions
from the instrument itself.

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12 Hardware Information
Early Maintenance Feedback (EMF)

Early Maintenance Feedback (EMF)

Maintenance requires the exchange of components which are subject to wear or


stress. Ideally, the frequency at which components are exchanged should be
based on the intensity of usage of the module and the analytical conditions, and
not on a predefined time interval. The early maintenance feedback (EMF) feature
monitors the usage of specific components in the instrument, and provides
feedback when the user-selectable limits have been exceeded. The visual
feedback in the user interface provides an indication that maintenance
procedures should be scheduled.

EMF Counters
EMF counters increment with use and can be assigned a maximum limit which
provides visual feedback in the user interface when the limit is exceeded. Some
counters can be reset to zero after the required maintenance procedure.

Lamp Type Counter Reset Comment

lamp with RFID tag NO

lamp without RFID tag YES via Lab Advisor or Instant Pilot

The detector provides the following EMF counters:


• Deuterium Lamp On-Time
• Number of UV lamp ignitions

Using the EMF Counters


The user-settable EMF limits for the EMF Counters enable the early maintenance
feedback to be adapted to specific user requirements. The useful maintenance
cycle is dependent on the requirements for use. Therefore, the definition of the
maximum limits need to be determined based on the specific operating
conditions of the instrument.

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12 Hardware Information
Early Maintenance Feedback (EMF)

Setting the EMF Limits


The setting of the EMF limits must be optimized over one or two maintenance
cycles. Initially the default EMF limits should be set. When instrument
performance indicates maintenance is necessary, take note of the values
displayed by the EMF counters. Enter these values (or values slightly less than the
displayed values) as EMF limits, and then reset the EMF counters to zero. The
next time the EMF counters exceed the new EMF limits, the EMF flag will be
displayed, providing a reminder that maintenance needs to be scheduled.

This function is only available via Agilent Lab Advisor or Instant Pilot.
NOTE

Agilent InfinityLab LC Series DAD WR and MWD User Manual 249


13 LAN Configuration

What You Have to Do First 251


TCP/IP parameter configuration 252
Configuration Switches 253
Initialization Mode Selection 254
Dynamic Host Configuration Protocol (DHCP) 256
General Information (DHCP) 256
Setup (DHCP) 257
Manual Configuration 259
With Telnet 260
With the Instant Pilot (G4208A) 263

This chapter provides information on connecting the module to the Agilent


ChemStation PC.

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13 LAN Configuration
What You Have to Do First

What You Have to Do First

The module has an on- board LAN communication interface.

This chapter is generic and may show figures that differ from your module. The
NOTE functionality is the same.

1 Note the MAC (Media Access Control) address for further reference. The MAC
or hardware address of the LAN interfaces is a world wide unique identifier.
No other network device will have the same hardware address. The MAC
address can be found on a label at the rear of the module underneath the
configuration switch (see Figure 68 on page 251).

Part number of the detector main board


Revision Code, Vendor, Year and Week of assembly
MAC address
Country of Origin

Figure 67 MAC-Label

2 Connect the instrument's LAN interface (see Figure 68 on page 251) to


• the PC network card using a crossover network cable (point-to-point) or
• a hub or switch using a standard LAN cable.

LAN interface

MAC label

Figure 68 Location of LAN interfaces and MAC label

Agilent InfinityLab LC Series DAD WR and MWD User Manual 251


13 LAN Configuration
TCP/IP parameter configuration

TCP/IP parameter configuration

To operate properly in a network environment, the LAN interface must be


configured with valid TCP/IP network parameters. These parameters are:
• IP address
• Subnet Mask
• Default Gateway
The TCP/IP parameters can be configured by the following methods:
• by automatically requesting the parameters from a network-based DHCP
Server (using the so-called Dynamic Host Configuration Protocol). This mode
requires a LAN-onboard Module or a G1369C LAN Interface card, see “Setup
(DHCP)” on page 257
• by manually setting the parameters using Telnet
• by manually setting the parameters using the Local Controller
The LAN interface differentiates between several initialization modes. The
initialization mode (short form ‘init mode’) defines how to determine the active
TCP/IP parameters after power-on. The parameters may be derived non-volatile
memory or initialized with known default values. The initialization mode is
selected by the configuration switch, see Table 23 on page 254.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 252


13 LAN Configuration
Configuration Switches

Configuration Switches

The configuration switch can be accessed at the rear of the module.

Configuration switch

Figure 69 Location of Configuration switch (example shows a G7114A/B VWD)

The module is shipped with all switches set to OFF, as shown above.

To perform any LAN configuration, SW1 and SW2 must be set to OFF.
NOTE

Agilent InfinityLab LC Series DAD WR and MWD User Manual 253


13 LAN Configuration
Initialization Mode Selection

Initialization Mode Selection

The following initialization (init) modes are selectable:


Table 23 Initialization Mode Switches

SW1 SW2 SW3 SW4 SW5 SW6 Init Mode

0 0 0 0 0 0 Use Default IP Address

0 0 0 0 1 0 Use Stored IP Address

0 0 0 1 0 0 Use DHCP

Note: The setting ‘0’ (down) is essential.

Default IP address for LAN is 192.168.254.11.


DHCP address is the module’s LAN MAC address.

Using Stored
When initialization mode Using Stored is selected, the parameters are taken from
the non-volatile memory of the module. The TCP/IP connection will be
established using these parameters. The parameters were configured previously
by one of the described methods.

Non-Volatile
RAM
Active
Parameter
Stored
Parameter

Figure 70 Using Stored (Principle)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 254


13 LAN Configuration
Initialization Mode Selection

Using Default
When Using Default is selected, the factory default parameters are taken instead.
These parameters enable a TCP/IP connection to the LAN interface without
further configuration, see Table 24 on page 255.

Default Active
Parameter Parameter

Figure 71 Using Default (Principle)

Using the default address in your local area network may result in network
NOTE problems. Take care and change it to a valid address immediately.

Table 24 Using Default Parameters

IP address: 192.168.254.11

Subnet Mask: 255.255.255.0

Default Gateway not specified

Since the default IP address is a so-called local address, it will not be routed by
any network device. Thus, the PC and the module must reside in the same
subnet.
The user may open a Telnet session using the default IP address and change the
parameters stored in the non-volatile memory of the module. He may then close
the session, select the initialization mode Using Stored, power-on again and
establish the TCP/IP connection using the new parameters.
When the module is wired to the PC directly (e.g. using a cross-over cable or a
local hub), separated from the local area network, the user may simply keep the
default parameters to establish the TCP/IP connection.

In the Using Default mode, the parameters stored in the memory of the module
NOTE are not cleared automatically. If not changed by the user, they are still available,
when switching back to the mode Using Stored.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 255


13 LAN Configuration
Dynamic Host Configuration Protocol (DHCP)

Dynamic Host Configuration Protocol (DHCP)

General Information (DHCP)


The Dynamic Host Configuration Protocol (DHCP) is an auto configuration
protocol used on IP networks. The DHCP functionality is available on all Agilent
HPLC modules with on-board LAN Interface or LAN Interface Card G1369C, and
“B”-firmware (B.06.40 or above) or modules with "D"-firmware. All modules
should use latest firmware from the same set.
When the initialization mode “DHCP” is selected, the card tries to download the
parameters from a DHCP Server. The parameters obtained become the active
parameters immediately. They are not stored to the non-volatile memory of the
card.
Besides requesting the network parameters, the card also submits its hostname
to the DHCP Server. The hostname equals the MAC address of the card, e.g.
0030d3177321. It is the DHCP server's responsibility to forward the
hostname/address information to the Domain Name Server. The card does not
offer any services for hostname resolution (e.g. NetBIOS).

DHCP Active
Server Parameter

Figure 72 DHCP (Principle)

1 It may take some time until the DHCP server has updated the DNS server with
NOTE the hostname information.
2 It may be necessary to fully qualify the hostname with the DNS suffix, e.g.
0030d3177321.country.company.com.
3 The DHCP server may reject the hostname proposed by the card and assign a
name following local naming conventions.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 256


13 LAN Configuration
Dynamic Host Configuration Protocol (DHCP)

Setup (DHCP)

The DHCP functionality is available on all Agilent HPLC modules with on-board LAN Interface or LAN
Interface Card G1369C, and “B”-firmware (B.06.40 or above) or modules with "D"-firmware. All
modules should use latest firmware from the same set.

1 Note the MAC address of the LAN interface (provided with G1369C LAN
Interface Card or mainboard). This MAC address is on a label on the card or at
the rear of the mainboard, for example, 0030d3177321.
On the Local Controller the MAC address can be found under Details in the
LAN section.

Figure 73 LAN Setting on Instant Pilot

Agilent InfinityLab LC Series DAD WR and MWD User Manual 257


13 LAN Configuration
Dynamic Host Configuration Protocol (DHCP)

2 Set the configuration switch to DHCP either on the G1369C LAN Interface
Card or the mainboard of above mentioned modules.
Table 25 G1369C LAN Interface Card (configuration switch on the card)

SW 4 SW 5 SW 6 SW 7 SW 8 Initialization Mode

ON OFF OFF OFF OFF DHCP

Table 26 LC Modules with 8-bit configuration switch (B-firmware) (configuration switch at rear
of the instrument)

SW 6 SW 7 SW 8 Initialization Mode

ON OFF OFF DHCP

3 Turn on the module that hosts the LAN interface.


4 Configure your Control Software (e.g. OpenLAB CDS ChemStation Edition, Lab
Advisor, Firmware Update Tool) and use MAC address as host name, e.g.
0030d3177321.
The LC system should become visible in the control software (see Note in
section “General Information (DHCP)” on page 256).

Agilent InfinityLab LC Series DAD WR and MWD User Manual 258


13 LAN Configuration
Manual Configuration

Manual Configuration

Manual configuration only alters the set of parameters stored in the non-volatile
memory of the module. It never affects the currently active parameters.
Therefore, manual configuration can be done at any time. A power cycle is
mandatory to make the stored parameters become the active parameters, given
that the initialization mode selection switches are allowing it.

TELNET
Session
Non-Volatile
RAM

Stored
Parameter

Control
Module

Figure 74 Manual Configuration (Principle)

Agilent InfinityLab LC Series DAD WR and MWD User Manual 259


13 LAN Configuration
Manual Configuration

With Telnet
Whenever a TCP/IP connection to the module is possible (TCP/IP parameters set
by any method), the parameters may be altered by opening a Telnet session.
1 Open the system (DOS) prompt window by clicking on Windows START
button and select “Run...”. Type “cmd” and press OK.
2 Type the following at the system (DOS) prompt:
• c:\>telnet <IP address> or
• c:\>telnet <host name>

Figure 75 Telnet - Starting a session

where <IP address> may be the assigned address from a Bootp cycle, a
configuration session with the Handheld Controller, or the default IP address
(see “Configuration Switches” on page 253).
When the connection was established successfully, the module responds
with the following:

Figure 76 A connection to the module is made

Agilent InfinityLab LC Series DAD WR and MWD User Manual 260


13 LAN Configuration
Manual Configuration

3 Type
? and press enter to see the available commands.

Figure 77 Telnet Commands

Table 27 Telnet Commands

Value Description

? displays syntax and descriptions of commands

/ displays current LAN settings

ip <x.x.x.x> sets new ip address

sm <x.x.x.x> sets new subnet mask

gw <x.x.x.x> sets new default gateway

exit exits shell and saves all changes

4 To change a parameter follows the style:


• parameter value, for example:
ip 134.40.28.56
Then press [Enter], where parameter refers to the configuration parameter
you are defining, and value refers to the definitions you are assigning to that
parameter. Each parameter entry is followed by a carriage return.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 261


13 LAN Configuration
Manual Configuration

5 Use the “/” and press Enter to list the current settings.

information about the LAN interface


MAC address, initialization mode
Initialization mode is Using Stored
active TCP/IP settings

TCP/IP status - here ready


Figure 78 Telnet - Current settings in "Using Stored" mode connected to PC with controller software (e.g. Agilent
ChemStation), here not connected

6 Change the IP address (in this example 192.168.254.12) and type “/” to list
current settings.

change of IP setting to
Initialization mode is Using Stored

active TCP/IP settings

stored TCP/IP settings in non-volatile memory

connected to PC with controller software (e.g. Agilent


ChemStation), here not connected

Figure 79 Telnet - Change IP settings

7 When you have finished typing the configuration parameters, type


exit and press Enter to exit with storing parameters.

Figure 80 Closing the Telnet Session

If the Initialization Mode Switch is changed now to “Using Stored” mode, the
NOTE instrument will take the stored settings when the module is re-booted. In the
example above it would be 192.168.254.12.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 262


13 LAN Configuration
Manual Configuration

With the Instant Pilot (G4208A)


To configure the TCP/IP parameters before connecting the module to the
network, the Instant Pilot (G4208A) can be used.
1 From the Welcome screen press the More button.
2 Select Configure.
3 Press the module button of the module that hosts the LAN interface (usually
the detector).
4 Scroll down to the LAN settings.

Figure 81 Instant Pilot - LAN Configuration (Edit mode)

5 Press the Edit button (only visible if not in Edit mode), perform the required
changes and press the Done button.
6 Leave the screen by clicking Exit.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 263


14 Appendix

General Safety Information 265


General Safety Information 265
Safety Standards 265
General 265
Before Applying Power 266
Ground the Instrument 266
Do Not Operate in an Explosive Atmosphere 267
Do Not Remove the Instrument Cover 267
Do Not Modify the Instrument 267
In Case of Damage 267
Solvents 268
Safety Symbols 269
Waste Electrical and Electronic Equipment (WEEE) Directive 271
Radio Interference 272
Sound Emission 273
UV-Radiation 274
Solvent Information 275
Declaration of Conformity for HOX2 Filter 276
Installation of Stainless Steel Cladded PEEK Capillaries 277
First Step: Finger-tight Fitting 277
Second Step: Installation to Connector 278
Removing Capillaries 282
Agilent Technologies on Internet 283

This chapter provides addition information on safety, legal and web.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 264


14 Appendix
General Safety Information

General Safety Information

General Safety Information


The following general safety precautions must be observed during all phases of
operation, service, and repair of this instrument. Failure to comply with these
precautions or with specific warnings elsewhere in this manual violates safety
standards of design, manufacture, and intended use of the instrument. Agilent
Technologies assumes no liability for the customer’s failure to comply with these
requirements.

Ensure the proper usage of the equipment.


WAR N IN G
The protection provided by the equipment may be impaired.
 The operator of this instrument is advised to use the equipment in a
manner as specified in this manual.

Safety Standards
This is a Safety Class I instrument (provided with terminal for protective earthing)
and has been manufactured and tested according to international safety
standards.

General
Do not use this product in any manner not specified by the manufacturer. The
protective features of this product may be impaired if it is used in a manner not
specified in the operation instructions.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 265


14 Appendix
General Safety Information

Before Applying Power


Wrong voltage range, frequency or cabling
WAR N IN G
Personal injury or damage to the instrument
 Verify that the voltage range and frequency of your power distribution
matches to the power specification of the individual instrument.
 Never use cables other than the ones supplied by Agilent Technologies
to ensure proper functionality and compliance with safety or EMC
regulations.
 Make all connections to the unit before applying power.

Note the instrument's external markings described under “Safety Symbols” on


NOTE page 269.

Ground the Instrument


Missing electrical ground
WAR N IN G
Electrical shock
 If your product is provided with a grounding type power plug, the
instrument chassis and cover must be connected to an electrical ground
to minimize shock hazard.
 The ground pin must be firmly connected to an electrical ground (safety
ground) terminal at the power outlet. Any interruption of the protective
(grounding) conductor or disconnection of the protective earth terminal
will cause a potential shock hazard that could result in personal injury.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 266


14 Appendix
General Safety Information

Do Not Operate in an Explosive Atmosphere


Presence of flammable gases or fumes
WAR N IN G
Explosion hazard
 Do not operate the instrument in the presence of flammable gases or
fumes.

Do Not Remove the Instrument Cover


Instrument covers removed
WAR N IN G
Electrical shock
 Do Not Remove the Instrument Cover
 Only Agilent authorized personnel are allowed to remove instrument
covers. Always disconnect the power cables and any external circuits
before removing the instrument cover.

Do Not Modify the Instrument


Do not install substitute parts or perform any unauthorized modification to the
product. Return the product to an Agilent Sales and Service Office for service and
repair to ensure that safety features are maintained.

In Case of Damage
Damage to the module
WAR N IN G
Personal injury (for example electrical shock, intoxication)
 Instruments that appear damaged or defective should be made
inoperative and secured against unintended operation until they can be
repaired by qualified service personnel.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 267


14 Appendix
General Safety Information

Solvents
Toxic, flammable and hazardous solvents, samples and reagents
WAR N IN G
The handling of solvents, samples and reagents can hold health and safety
risks.
 When working with these substances observe appropriate safety
procedures (for example by wearing goggles, safety gloves and
protective clothing) as described in the material handling and safety
data sheet supplied by the vendor, and follow good laboratory practice.
 Do not use solvents with an auto-ignition temperature below 200 °C
(392 °F). Do not use solvents with a boiling point below 56 °C (133 °F).
 Avoid high vapor concentrations. Keep the solvent temperature at least
40 °C (72 °F) below the boiling point of the solvent used. This includes
the solvent temperature in the sample compartment. For the solvents
methanol and ethanol keep the solvent temperature at least 25 °C
(45 °F) below the boiling point.
 Do not operate the instrument in an explosive atmosphere.
 Do not use solvents of ignition Class IIC according IEC 60079-20-1 (for
example, carbon disulfide).
 Reduce the volume of substances to the minimum required for the
analysis.
 Never exceed the maximum permissible volume of solvents (8 L) in the
solvent cabinet. Do not use bottles that exceed the maximum
permissible volume as specified in the usage guideline for solvent
cabinet.
 Ground the waste container.
 Regularly check the filling level of the waste container. The residual free
volume in the waste container must be large enough to collect the waste
liquid.
 To achieve maximal safety, regularly check the tubing for correct
installation.

For details, see the usage guideline for the solvent cabinet. A printed copy of the
NOTE guideline has been shipped with the solvent cabinet, electronic copies are
available in the Agilent Information Center or via the Internet.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 268


14 Appendix
General Safety Information

Safety Symbols
Table 28 Symbols

The apparatus is marked with this symbol when the user shall refer to the
instruction manual in order to protect risk of harm to the operator and to
protect the apparatus against damage.

Indicates dangerous voltages.

Indicates a protected ground terminal.

The apparatus is marked with this symbol when hot surfaces are available
and the user should not touch it when heated up.

Sample Cooler unit is designed as vapor-compression refrigeration system.


Contains fluorinated greenhouse gas (refrigerant) according to the Kyoto
protocol.
For specifications of refrigerant, charge capacity, carbon dioxide equivalent
(CDE), and global warming potential (GWP) see instrument label.

Flammable Material
For Sample Thermostat which uses flammable refrigerant consult Agilent
Information Center / User Manual before attempting to install or service this
equipment. All safety precautions must be followed.

Confirms that a manufactured product complies with all applicable


European Community directives. The European Declaration of Conformity is
available at:
http://regulations.corporate.agilent.com/DoC/search.htm

Manufacturing date.

Power symbol indicates On/Off.


The apparatus is not completely disconnected from the mains supply when
the power switch is in the Off position

Pacemaker
Magnets could affect the functioning of pacemakers and implanted heart
defibrillators.
A pacemaker could switch into test mode and cause illness. A heart
defibrillator may stop working. If you wear these devices keep at least
55 mm distance to magnets. Warn others who wear these devices from
getting too close to magnets.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 269


14 Appendix
General Safety Information

Table 28 Symbols

Magnetic field
Magnets produce a far-reaching, strong magnetic field. They could damage
TVs and laptops, computer hard drives, credit and ATM cards, data storage
media, mechanical watches, hearing aids and speakers. Keep magnets at
least 25 mm away from devices and objects that could be damaged by
strong magnetic fields.

Indicates a pinching or crushing hazard

Indicates a piercing or cutting hazard.

A WARNING
WAR N IN G
alerts you to situations that could cause physical injury or death.
 Do not proceed beyond a warning until you have fully understood and
met the indicated conditions.

A CAUTION
C AU T I O N
alerts you to situations that could cause loss of data, or damage of equipment.
 Do not proceed beyond a caution until you have fully understood and met
the indicated conditions.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 270


14 Appendix
Waste Electrical and Electronic Equipment (WEEE) Directive

Waste Electrical and Electronic Equipment


(WEEE) Directive

This product complies with the European WEEE Directive marking requirements.
The affixed label indicates that you must not discard this electrical/electronic
product in domestic household waste.

Do not dispose of in domestic household waste


NOTE
To return unwanted products, contact your local Agilent office, or see
http://www.agilent.com for more information.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 271


14 Appendix
Radio Interference

Radio Interference

Cables supplied by Agilent Technologies are screened to provide optimized


protection against radio interference. All cables are in compliance with safety or
EMC regulations.

Test and Measurement


If test and measurement equipment is operated with unscreened cables, or used
for measurements on open set-ups, the user has to assure that under operating
conditions the radio interference limits are still met within the premises.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 272


14 Appendix
Sound Emission

Sound Emission

Sound pressure
Sound pressure Lp <70 db(A) accroding to DIN-EN 27779

Schalldruckpegel
Schalldruckpegel Lp <70 db(A) nach DIN-EN 27779

Agilent InfinityLab LC Series DAD WR and MWD User Manual 273


14 Appendix
UV-Radiation

UV-Radiation

This information is only valid for UV-lamps without cover (e.g. 2140-0590 and
NOTE 2140-0813).

Emissions of ultraviolet radiation (200-315 nm) from this product is limited such
that radiant exposure incident upon the unprotected skin or eye of operator or
service personnel is limited to the following TLVs (Threshold Limit Values)
according to the American Conference of Governmental Industrial Hygienists:
Table 29 UV-Radiation Limits

Exposure/day Effective Irradiance

8 hours 0.1 µW/cm2

10 minutes 5.0 µW/cm2

Typically the radiation values are much smaller than these limits:
Table 30 UV-Radiation Typical Values

Position Effective Irradiance

Lamp installed, 50 cm distance Average 0.016 µW/cm2

Lamp installed, 50 cm distance Maximum 0.14 µW/cm2

Agilent InfinityLab LC Series DAD WR and MWD User Manual 274


14 Appendix
Solvent Information

Solvent Information

Flow Cell
To protect optimal functionality of your flow-cell:
• Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and
thus impair the optical properties of the flow cell.

Use of Solvents
Observe the following recommendations on the use of solvents.
• Brown glass ware can avoid growth of algae.
• Avoid the use of the following steel-corrosive solvents:
• solutions of alkali halides and their respective acids (for example, lithium
iodide, potassium chloride, and so on),
• high concentrations of inorganic acids like sulfuric acid and nitric acid,
especially at higher temperatures (if your chromatography method allows,
replace by phosphoric acid or phosphate buffer which are less corrosive
against stainless steel),
• halogenated solvents or mixtures which form radicals and/or acids, for
example:
2CHCl3 + O2→ 2COCl2 + 2HCl
This reaction, in which stainless steel probably acts as a catalyst, occurs
quickly with dried chloroform if the drying process removes the stabilizing
alcohol,
• chromatographic grade ethers, which can contain peroxides (for example,
THF, dioxane, diisopropyl ether) should be filtered through dry aluminium
oxide which adsorbs the peroxides,
• solvents containing strong complexing agents (e.g. EDTA),
• mixtures of carbon tetrachloride with 2-propanol or THF.
• Avoid the use of dimethyl formamide (DMF). Polyvinylidene fluoride (PVDF),
which is used in leak sensors, is not resistant to DMF.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 275


14 Appendix
Declaration of Conformity for HOX2 Filter

Declaration of Conformity for HOX2 Filter

Agilent InfinityLab LC Series DAD WR and MWD User Manual 276


14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

Installation of Stainless Steel Cladded PEEK


Capillaries

This installation procedure applies for capillaries and corresponding fittings used
NOTE in modules delivered before January 2013.

The 1260 Infinity Bio-inert LC system uses PEEK capillaries that are cladded with
stainless steel. These capillaries combine the high pressure stability of steel with
the inertness of PEEK. They are used in the high pressure flow path after sample
introduction (loop/needle seat capillary) through the thermostatted column
compartment/heat exchangers to the column. Such capillaries need to be
installed carefully in order to keep them tight without damaging them by
over-tightening.
The installation consists of two steps. In the first step, the fitting is installed
finger-tight without using tools. Finger-tight means that the fitting will grip and
hold the capillary. This brings the fitting to the appropriate start position (marked
as 0 ° below) for the second step.

First Step: Finger-tight Fitting


1 Tighten the fitting using your fingers.

Agilent InfinityLab LC Series DAD WR and MWD User Manual 277


14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

Second Step: Installation to Connector


In the second step (“Second Step: Installation to Hard Connectors” on page 278
or “Second Step: Installation to Soft Connectors” on page 279), a wrench is used
to rotate the fitting relative to the finger-tight position by a defined angle. For
each of the cases mentioned above, there is a recommended range in which the
fitting is tight.
Staying below this range could create a leak, either a visible one or a micro-leak,
potentially biasing measurement results. Exceeding the recommended range
could damage the capillary.
Alternatively, a torque wrench may be used. The target torque for all connections
is about 0.7 Nm. When using a torque wrench, read instructions for that tool
carefully, as wrong handling may easily miss the correct torque.

Second Step: Installation to Hard Connectors


Use this procedure for hard connectors made from metal (titanium) or ceramics.
In the system, these are connections to and from the analytical head of the
autosampler (connections to injection valve and needle), and to a metal column.

First installation of a capillary to a hard connector


1 When tightening a fitting for the first time, start from the finger-tight position
(which is not necessarily a vertical wrench position) and rotate the wrench by
135 – 180 °. Staying below 135 ° (grey arrow) will be insufficiently tight, more
than 180 ° (red arrow) could damage the capillary.

possibly
leaky

recommended
range

Agilent InfinityLab LC Series DAD WR and MWD User Manual 278


14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

Second and subsequent installations of a capillary to a hard connector


1 When tightening the fitting for the second and subsequent times, again start
from the finger-tight position (which is not necessarily a vertical wrench
position) and rotate the wrench by 90 – 135 °. Staying below 90 ° (grey arrow)
could be insufficiently tight, more than 135 ° (red arrow) could damage the
capillary.

possibly
leaky

recommended
range

Second Step: Installation to Soft Connectors


Use this procedure for soft connectors, which are typically made from PEEK.
These are the following connections:
• to and from all bio-inert valves (injection valve in the autosampler and valves
in the thermostatted column compartment and 1290 Infinity Valve Drive),
• bio-inert ZDV unions (detector flow cells, multi-draw upgrade kit, capillary to
capillary connections, for example, for heat exchangers),
• to the autosampler needle and
• to PEEK columns (like many bio-inert columns).
For the installation of bio-inert ZDV unions, refert to the Technical Note
"Installation of stainless steel cladded PEEK capillaries" (p/n G5611-90120).

Agilent InfinityLab LC Series DAD WR and MWD User Manual 279


14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

First installation of a capillary to a soft connector


1 When tightening a fitting for the first time, start from the finger-tight position
(which does not necessarily need to be a vertical wrench position) and rotate
the wrench by 180 – 210 °. Staying below 180 ° (grey arrow) will not be
sufficiently tight, more than 210 ° (red arrow) could damage the capillary.
possibly
leaky

recommended
range

Second and subsequent installations of a capillary to a soft connector


1 When tightening the fitting for the second and subsequent times, again start
from the finger-tight position (which is not necessarily a vertical wrench
position) and rotate the wrench by 135 – 180 °. Staying below 135 ° (grey
arrow) could be insufficiently tight enough, more than 180 ° (red arrow) could
damage the capillary.

possibly
leaky

recommended
range

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14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

Summary for Second Step


Table 31 Summary for second step

2ndStep First installation Subsequent installations

Hard connectors
possibly
possibly leaky
leaky

recommended
range
recommended
range

Soft connectors
possibly
leaky possibly
leaky

recommended recommended
range range

Agilent InfinityLab LC Series DAD WR and MWD User Manual 281


14 Appendix
Installation of Stainless Steel Cladded PEEK Capillaries

Removing Capillaries
Potential damage of capillaries
C AU T I O N
 Do not remove fittings from used capillaries.

To keep the flow path free of stainless steel, the front end of the capillary is made
of PEEK. Under high pressure, or when in contact with some solvents, PEEK can
expand to the shape of the connector where the capillary is installed. If the
capillary is removed, this may become visible as a small step. In such cases, do
not try to pull the fitting from the capillary, as this can destroy the front part of the
capillary. Instead, carefully pull it to the rear. During installation of the capillary,
the fitting will end up in the correct position.

Rear Front

Step

Figure 82 Capillary fitting

Agilent InfinityLab LC Series DAD WR and MWD User Manual 282


14 Appendix
Agilent Technologies on Internet

Agilent Technologies on Internet

For the latest information on products and services visit our worldwide web site
on the Internet at:
http://www.agilent.com

Agilent InfinityLab LC Series DAD WR and MWD User Manual 283


In This Book

This manual contains technical reference


information about the Agilent 1260 Infinity II
Diode Array and Multiple Wavelength
Detectors G7115A WR and G7165A.
The manual describes the following:
• introduction and specifications,
• installation,
• using and optimizing,
• troubleshooting and diagnose,
• maintenance,
• parts identification,
• hardware information,
• safety and related information.

www.agilent.com
Agilent Technologies Inc. 2016-2021
Edition: 03/2021
Document No: SD-29000218 Rev. E

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