Agilent Technologies InfinityLab LC Series User manual

Refractive Index Detector
Agilent InfinityLab LC Series
User Manual
Agilent InfinityLab LC Series RID User Manual

Agilent InfinityLab LC Series RID User Manual
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EDITION 12/2019
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Agilent InfinityLab LC Series RID User Manual 3
In This Guide...
This manual covers the
•Agilent 1290 Infinity II Refractive Index Detector (G7162B)
•Agilent 1260 Infinity II Refractive Index Detector (G7162A)
1 Introduction to the Refractive Index Detector
This chapter gives an introduction to the Refractive Index Detector.
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 Module
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.
6Troubleshootingand Diagnostics
This chapter gives an overview about the troubleshooting and diagnostic features
and the different user interfaces.
7ErrorInformation
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 RID User Manual 4
8 Test Functions
This chapter describes the detector’s built in test functions.
9 Maintenance and Repair
This chapter provides general information on maintenance and repair of the
detector.
10 Parts for Maintenance
This chapter provides information on parts for maintenance.
11 Identifying Cables
This chapter provides information on cables used with the Agilent 1200 Infinity
Series modules.
12 Hardware Information
This chapter describes the module 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 safetey and other general information.

Agilent InfinityLab LC Series RID User Manual 5
Contents
1 Introduction to the Refractive Index Detector 9
Introduction to the Refractive Index Detector 10
G7162A Refractive Index Detector 12
G7162B Refractive Index Detector 14
How the Detector Operates 16
Detection Principle 18
Flow Path 20
Leak and Waste Handling 27
2 Site Requirements and Specifications 33
Site Requirements 34
Physical Specifications 37
Performance Specifications 38
3 Using the Module 42
Magnets 43
Turn on/off 44
Status Indicators 46
Instrument Configuration 47
Set up the Detector with Agilent Open Lab ChemStation 49
The Detector User Interface 50
Detector Control Settings 53
Method Parameter Settings 55
Agilent Local Control Modules 59
4 Preparing the Module 61
Leak and Waste Handling 62
Setting up an Analysis 64
Solvent Information 72

Agilent InfinityLab LC Series RID User Manual 6
5 Optimizing the Detector 77
Refractive Index Detector Optimization 78
6 Troubleshooting and Diagnostics 82
Available Tests vs User Interfaces 83
Agilent Lab Advisor Software 84
7ErrorInformation85
What Are Error Messages 86
General Error Messages 87
Refractive Index Detector Specific Error Messages 94
Not-Ready Messages 101
8 Test Functions 103
Introduction 104
Refractive Index Calibration 108
Optical Balance 114
Using the Build-in Test Chromatogram 117
ASTM Drift and Noise Test 119
D/A Converter (DAC) Test 123
Other Lab Advisor Functions 125
9 Maintenance and Repair 126
Introduction to Maintenance 127
Warnings and Cautions 128
Overview of Maintenance 130
Cleaning the Module 131
Remove and Install Doors 132
Flow Cell Flushing 134
Correct Leaks 135
Replace Leak Handling System Parts 138
Replace the Module Firmware 140

Agilent InfinityLab LC Series RID User Manual 7
10 Parts for Maintenance 141
Overview of Maintenance Parts 142
Accessory Kit 144
Leak Handling Parts 147
11 Identifying Cables 148
Cable Overview 149
Analog Cables 151
Remote Cables 153
CAN/LAN Cables 157
Agilent Module to PC 158
USB Cables 159
12 Hardware Information 160
Data Flow for Chromatographic Output 161
Firmware Description 162
Electrical Connections 165
Interfaces 168
Setting the 6-bit Configuration Switch 176
Instrument Layout 180
Early Maintenance Feedback 181
13 LAN Configuration 182
What You Have to Do First 183
TCP/IP parameter configuration 184
Configuration Switches 185
Initialization Mode Selection 186
Dynamic Host Configuration Protocol (DHCP) 188
Manual Configuration 191
PC and Agilent ChemStation Setup 195

Agilent InfinityLab LC Series RID User Manual 8
In This Guide...
14 Appendix 204
General Safety Information 205
Waste Electrical and Electronic Equipment (WEEE) Directive 211
Radio Interference 212
Sound Emission 213
Solvent Information 214
Agilent Technologies on Internet 216

Agilent InfinityLab LC Series RID User Manual 9
1 Introduction to the Refractive Index
Detector
Introduction to the Refractive Index Detector 10
G7162A Refractive Index Detector 12
Product Description 12
Features 13
G7162B Refractive Index Detector 14
Product Description 14
Features 15
How the Detector Operates 16
Detection Principle 18
Flow Path 20
Leak and Waste Handling 27
Leak Sensor 31
Waste Guidance 31
Waste Concept 32
This chapter gives an introduction to the Refractive Index Detector.

Agilent InfinityLab LC Series RID User Manual 10
1 Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
The Standard Optical (G7162A) and Micro Optical (G7162B) detectors are
designed for highest optical performance, GLP compliance, and easy
maintenance. They include the following features:
•advanced temperature controlled detector optics ready to use within two
hours of installation,
•automatic zero and automatic purge combined with a recycle valve for
automatic solvent recycling allow uninterrupted operation,
•durable tungsten lamp with a life expectancy of 40000 hours,
•automatic light intensity control circuit to ensure the optimum performance of
the optics,
•integrated diagnostics for efficient troubleshooting,
•built-in refractive index calibration,
•front access to valves and capillaries for easy maintenance.
For specifications, see “Performance Specifications” on page 38.
Figure 1 The Agilent 1200 Infinity Series Refractive Index Detector

Agilent InfinityLab LC Series RID User Manual 11
1 Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
G7162A Refractive Index Detector
This detector is equipped with the standard optical unit and is used for all
standard applications.
It comprises the following features:
•inlet port to sample cell 62 µL,
•inlet port to outlet port 590 µL,
•maximum data rate up to 74 Hz.
G7162B Refractive Index Detector Micro
This detector is equipped with the micro optical unit and is used for all low
volume applications.
It comprises the following features:
•inlet port to sample cell 10 µL,
•inlet port to outlet port 265 µL,
•maximum data rate up to 148 Hz,
•LED illumination.

Agilent InfinityLab LC Series RID User Manual 12
1 Introduction to the Refractive Index Detector
G7162A Refractive Index Detector
G7162A Refractive Index Detector
Product Description
The Agilent 1260 Infinity II Refractive Index Detector (RID) is the ideal detector for
fast and reliable LC results when routinely analyzing non-UV absorbing
substances, such as carbohydrates, lipids, and polymers. The 1260 Infinity II RID
is also the detector of choice for gel permeation chromatography (GPC) or size
exclusion chromatography (SEC).
Figure 2 Overview of the detector
Status indicator
Interface port area
Service door
Power switch
Leak drain

Agilent InfinityLab LC Series RID User Manual 13
1 Introduction to the Refractive Index Detector
G7162A Refractive Index Detector
Features
•High sensitivity and robust detection with an excellent reproducibility of only
0.1 % RSD
•Precise temperature control from ambient +5 °C to 55 °C to minimize
baseline drift and optimize compound response
•Automatic light level adjustment compensates for lamp degradation and flow
cell staining, ensuring optimum performance and lowest maintenance
•Integrated solvent recycle valve for solvent recycling between runs
•Programmable reference cell purging (autopurge) and auto-zeroing of the
detector baseline before each run for unattended operation
•Convenient front access to the flow connections and valves next to the optical
unit
•Early Maintenance Feedback (EMF) for prior notification of detector
maintenance and continuous tracking of reference flow cell purging with user
settable limits
•Fast and simple troubleshooting via diagnostic signal data collection
•Automatic offset adjustment for easy detection and quantification of negative
peaks, and a time-programmable polarity switch for simple inversion of peaks
for ease of integration
•Excellent linear response for compounds with little or no UV chromaphore in a
wide concentration range

Agilent InfinityLab LC Series RID User Manual 14
1 Introduction to the Refractive Index Detector
G7162B Refractive Index Detector
G7162B Refractive Index Detector
Product Description
The 1290 Infinity II Refractive Index Detector is equipped with an ultralow
dispersion microflow cell, which significantly reduces run times for higher
sample throughput and improved resolution. Lower solvent consumption means
much lower cost of analysis. A high-performance detector of choice for accurate,
reproducible, routine analysis of polymers and other compounds that aren’t
detectable by UV.
Figure 3 Overview of the detector
Status indicator
Interface port area
Service door
Power switch
Leak drain

Agilent InfinityLab LC Series RID User Manual 15
1 Introduction to the Refractive Index Detector
G7162B Refractive Index Detector
Features
•Shorter run times – for considerably higher sample throughput.
•Ultralow dispersion – for improved sample definition and resolution.
•Reduced solvent consumption – for significant savings in analysis cost.
•Ideal tool for polymer analysis – consistent molecular weights, micro or
analytical scale.
•Excellent sensitivity – achieve low limits of detection.
•148 Hz data rate – even the narrowest distribution peaks can be detected and
accurately quantified.
•Minimized band broadening – high-definition sample profiling.
•Fast startup – advanced low thermal mass design means that initial setup is
typically less than two hours.
•Further time and solvent saving – a recycle valve enables sample to be
recirculated when the sample is not passing through the flow cell.
•Automatic purging of reference flow cell – using programmable purge and
wait times.
•Easy maintenance – convenient front access for maintaining instrument
uptime.
•Early maintenance feedback (EMF) – indicates that preventative maintenance
is due.
•Extensive diagnostics – includes error detection and display with Instant Pilot
controller and Lab Advisor software.
•RoHS compliant – aligned with European Union directives regarding specific
hazardous materials.

Agilent InfinityLab LC Series RID User Manual 16
1 Introduction to the Refractive Index Detector
How the Detector Operates
How the Detector Operates
Refractive
index
When a beam of light passes from one medium into another, the wave velocity
and direction changes. The change in direction is called refraction. The
relationship between the angle of incidence and the angle of refraction is
expressed in Snell's Law of refraction.
Where:
•n = Refractive index of medium 1 relative to medium 2
•n
2
= Refractive index of medium 2
•n
1
= Refractive index of medium 1
•α
1
= angle of incident light in medium 1
•α
2
= angle of refraction in medium 2
Figure 4 Light Refraction
Medium 1
Medium 2

Agilent InfinityLab LC Series RID User Manual 17
1 Introduction to the Refractive Index Detector
How the Detector Operates
According to the formula below small angles of external deflection are
proportional to the difference between the refractive indices of medium 1 and
medium 2.
Where:
•γ= angle of external deflection
•n
2
= Refractive index of medium 2
•n
1
= Refractive index of medium 1
Factors that Affect Refractive Index
The refractive index of a medium is affected by a number of factors;
1Wavelength
The refractive index varies with changes in the wavelength of the incident light
beam.
2Density
As the density of the medium changes the refractive index changes. At a fixed
wavelength of incident light the changes in refractive index are generally linear
in relation to the changes in medium density.
The density of a medium will be affected by the following factors:
•Composition (if not a pure substance)
•Temperature
•Pressure

Agilent InfinityLab LC Series RID User Manual 18
1 Introduction to the Refractive Index Detector
Detection Principle
Detection Principle
Detector Design
The Agilent 1200 Infinity II Refractive Index Detector is a differential
refractometer that measures the deflection of a light beam due to the difference
in refractive index between the liquids in the sample and reference cells of a
single flow cell.
A beam of light from the lamp passes through a flow cell which is separated
diagonally into sample and reference cells. At the rear of the flow cell a mirror
reflects the light back through the flow cell and via a zero glass, which affects the
path of the light beam, to the light receiver. The light receiver has two diodes
each of which produces an electrical current proportional to the amount of light
that falls upon it (see Figure 5 on page 18).
Figure 5 Light path

Agilent InfinityLab LC Series RID User Manual 19
1 Introduction to the Refractive Index Detector
Detection Principle
Measurements
Initially both sample and reference cell are flushed with mobile phase. The
reference cell is then closed and solvent flows only through the sample cell. The
refractive index of the mobile phase in both cells is the same and the position of
the zero glass can be adjusted so that the detector is in optical balance with an
equal amount of light falls on each diode.
When sample elutes from the column into the sample cell the refractive index of
the cell contents changes. The change in refractive index deflects the light beam
as it passes through the flow cell resulting in an unequal amount of light falling
on each diode. The change in current from the diodes that this causes is
amplified and used to produce the calibrated detector signal. This signal
expressed, as nano Refractive Index Units (nRIU), corresponds to the difference
between the refractive index of sample in the sample cell and the mobile phase in
the reference cell.
Figure 6 Optical Path
Zero glass
Deflected light
Collimator lens
Reference cell
Mirror
Condenser lens
Incident light
Sample cell
Lamp
Diodes

Agilent InfinityLab LC Series RID User Manual 20
1 Introduction to the Refractive Index Detector
Flow Path
Flow Path
The column eluent enters the optical unit through the in port and passes through
a heat exchanger. The combination of the heat exchanger and control of the
optical unit temperature in the range of 5 °C above ambient to 55 °CC minimizes
changes in refractive index due to temperature variations. The eluent flows
through the sample cell and via the same heat exchanger to the purge valve. With
the purge valve in the OFF position the eluent passes to the recycle valve. If the
recycle valve is also in the OFF/WASTE position the eluent will flow via the waste
port into the waste container.
If the recycle valve is in the ON/BOTTLE position the eluent will flow via the
recycle port back to the solvent bottle. The recycle valve can be manually set to
the ON or OFF position or the Automatic recycling after analysis mode can be
enabled. In this mode the recycle valve will automatically switch to the ON
position after each analysis has been completed and return to the OFF position
before the next analysis starts. Using this mode provides the benefits of
uninterrupted flow through the detector without the problems of excessive
solvent usage or the contamination of mobile phase with recycled sample
compounds.
If the purge valve is in the on position the eluent cannot pass immediately to the
recycle valve but will instead flow via a second heat exchanger through the
reference cell and then into the recycle valve. Periodically switching the purge
valve to the on position while only mobile phase is flowing will ensure that the
liquid in the reference cell is as similar as possible to the flowing solvent. The
purge valve can be manually set to the on position for a defined time or the
Automatic purge mode can be enabled. In this mode the purge valve will
automatically switch to the ON position for a defined purgetime prior to the start
of each analysis. If a purgetime is set then a waittime must also be set to allow
the detector baseline to stabilize after the switching of the purge valve position.
After both the purgetime and waittime have been completed the analysis will
start. If the Automatic zero before analysis mode is enabled the detector output
will be set to zero immediately before the analysis begins.
The different flow paths depend on the status of the Purge Valve and Recycle
Valve.