Agilent Technologies InfinityLab 1290 Infinity II User manual

Agilent InfinityLab
Evaporative Light Scattering Detectors
User Manual
Agilent InfinityLab ELSD User Manual

Agilent InfinityLab ELSD User Manual
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Document No: D0013647 Rev. A
Edition: 08/2022
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Agilent InfinityLab ELSD User Manual 3
In This Book
This manual contains information on:
•Agilent 1260 Infinity II ELSD (G4260B)
•Agilent 1290 Infinity II ELSD (G7102A)
1 Introduction to the Detector
This chapter gives an introduction to the module, instrument overview, and internal
connectors.
2 Site Requirements and Specifications
This chapter provides information on environmental requirements, physical, and
performance specifications.
3 LAN Configuration
This chapter provides information on connecting the module to the control
software.
4UsingtheModule
This chapter explains the operational parameters of the ELSD.
5 Optimizing Performance
This chapter gives hints on how to optimize the performance or use additional
devices.
6Troubleshootingand 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 on how to recover from error
conditions.

Agilent InfinityLab ELSD User Manual 4
8 Maintenance
This chapter describes the maintenance of the ELSD.
9 Parts and Materials for Maintenance
This chapter provides information on parts for maintenance.
10 Appendix
This chapter provides addition information on safety, legal, and Web.

Agilent InfinityLab ELSD User Manual 5
Contents
1 Introduction to the Detector 7
Introduction to the ELSD 8
System Overview 9
2 Site Requirements and Specifications 16
Pre-installation Requirements 17
Site Requirements 18
Physical Specifications 21
Performance Specifications 23
3 LAN Configuration 27
What You Have to Do First 28
TCP/IP Parameter Configuration 29
PC and OpenLab CDS, OpenLab ChemStation or OpenLab EZChrom
Software Setup 36
4UsingtheModule41
Before Using the Detector 42
Instrument Controls 43
Operational Parameters 48
Controlling the ELSD During an Injection 52
Controlling the ELSD within OpenLab CDS, OpenLab ChemStation or
OpenLab EZChrom 54
General Considerations 55
5 Optimizing Performance 59
Do’s and Don’ts of ELS Detection 60
Location of the Detector Module 61
Pumping Systems 62
Mobile Phase Priming 63

Agilent InfinityLab ELSD User Manual 6
6 Troubleshooting and Diagnostics 64
Troubleshooting 65
Troubleshooting an HPLC System 66
General Problems 67
7 Error Information 74
What Are Error Messages 75
Module Specific Error Messages 76
8 Maintenance 83
Introduction to Maintenance 84
Cautions and Warnings 85
Cleaning the Module 87
Inspection of Cables 88
Drying the Diffuser 89
Cleaning the Nebulizer 90
Cleaning Evaporator Tube 91
Putting the Instrument into Storage 92
Updating Detector Firmware 93
9 Parts and Materials for Maintenance 98
Identifying Parts and Materials 99
10 Appendix 100
General Safety Information 101
Waste Electrical and Electronic Equipment (WEEE) Directive 105
Radio Interference 106
Agilent Technologies on Internet 107

Agilent InfinityLab ELSD User Manual 7
1 Introduction to the Detector
Introduction to the ELSD 8
System Overview 9
Basic Principles of Operation 9
Operational Parameters 12
Overview of ELS Detector 13
This chapter gives an introduction to the module, instrument overview, and
internal connectors.

1 Introduction to the Detector
Introduction to the ELSD
Agilent InfinityLab ELSD User Manual 8
Introduction to the ELSD
The Evaporative Light Scattering Detector is a unique and highly sensitive
detector for semi-volatile and non-volatile solutes in a liquid stream. It is mainly
used as a concentration detector for High Performance Liquid Chromatography
(HPLC). The solvent stream containing the solute material is nebulized and
carried by a gas flow through an evaporation chamber. The solvent is volatilized,
leaving a mist of solute particles that scatter light to a photosensitive device. The
signal is amplified and a voltage output provides the concentration of the solute
particles passing through the light.
The Agilent 1260 Infinity II ELSD or Agilent 1290 Infinity II ELSD may be used
alone, or as one of several detectors in a GPC or HPLC system. As the solvent or
eluent is evaporated during the analysis, the Agilent 1260 Infinity II ELSD or
Agilent 1290 Infinity II ELSD must be the last in series if used with other
detectors. If the Agilent 1260 Infinity II ELSD or Agilent 1290 Infinity II ELSD is
being used as the last detector in a series, care must be taken not to exceed the
recommended backpressure in detector cells in other units.
This manual instructs the user in the installation and operation of the Agilent
1260 Infinity II ELSD or Agilent 1290 Infinity II ELSD for standalone use and
control using Agilent OpenLab CDS, OpenLab ChemStation, or OpenLab
EZChrom.

Agilent InfinityLab ELSD User Manual 9
1 Introduction to the Detector
System Overview
System Overview
Basic Principles of Operation
Nebulization
The eluent inlet is connected to the nebulizer via a short length of stainless steel
capillary tube. The incoming eluent stream passes through the heated nebulizer
and is mixed with the incoming nebulizer gas stream. The mixed gas and eluent
stream form an aerosol plume containing a uniform dispersion of droplets that
then passes as a continuous flow into the evaporator section. Any larger droplets
or the inefficiently nebulized droplets collect in the nebulizer chamber waste trap
and then drain off via the waste outlet into a collection bottle.
Evaporation
After nebulization, the atomized spray is propelled through the evaporation tube
assisted by the carrier gas. In the evaporator section, the solvent is removed
leaving a stream of dry particles of the analyte. A diffuser located in the
evaporator assists in the drying of the particles, acting as an efficient heat
exchanger, prevents ballistic particles reaching the scattering chamber and
randomizes the particle plume. The ELS Detector uses patented gas flow
technology in the evaporation zone to aid evaporation at low temperatures. By
adding a stream of dry nitrogen (evaporation gas) at the entrance of the
evaporator tube less volatile solvents (for example, water) are easily evaporated.
This evaporation gas is controlled by the user and facilitates subambient
operation.

1 Introduction to the Detector
System Overview
Agilent InfinityLab ELSD User Manual 10
Detection
Light in the optical chamber is passed through the instrument at right angles to
the direction of particle flow. A light trap is located opposite the source of light to
capture the transmitted incident beam eliminating internal reflections within the
instrument body. When pure solvent is being evaporated, only its vapor passes
through the light path and the amount of light scattered to the photomultiplier is
small and gives a constant baseline response. When a nonvolatile solute is
present a particle cloud passes through the light path, causing light to be
scattered. This scattered light enters the optical aperture of the detection system
and generates a signal response from the photodiode in real time. The quantity
of light detected depends on the solute concentration and solute particle size
distribution.
Figure 1 Principles of Operation
1. Nebulization 2. Evaporation 3. Detection

Agilent InfinityLab ELSD User Manual 11
1 Introduction to the Detector
System Overview
Theory
There are four main processes, by which the path of electromagnetic radiation or
light can change direction, when passing through a medium containing a
suspended particulate phase, see Figure 2 on page 11.
Figure 2 ELSD Scattering Mechanisms
The importance of each of these processes depends on the radius of the particle
(r) compared to the wavelength (λ) of the incident light. Rayleigh scattering is
predominant when r/λis < 5·10-2. When particle dimensions are greater than λ/20
they no longer behave as point sources, and Mie scattering becomes
predominant. Once particle size approaches the wavelength of incident light then
reflection and refraction begin to prevail.
The relative importance of refraction and reflection can be understood by
examining the effects of the incident light on a single spherical particle whose
equilateral axis lies in the same plane as the photodetector and light source. With
this configuration, refraction is of greater significance than reflection. Most
organic compounds have refractive indices between 1.3 and 1.5. Changes in the
refractive index within this range will not greatly affect the quantity of light
reaching the detector. This accounts for similarities in the sensitivity of the
instrument to various compounds.
Reflection Refraction
Mie Rayleigh

1 Introduction to the Detector
System Overview
Agilent InfinityLab ELSD User Manual 12
Operational Parameters
The ELS Detector responds to all compounds that are less volatile than the
mobile phase and is independent of a compound’s optical properties. It therefore
provides advantages over other spectroscopic detectors for detecting
compounds that are deficient in a UV chromophore or fluorophore.
The removal of aqueous mobile phase within an ELSD is typically achieved by
setting the evaporator temperature to the eluent’s boiling point (for example
100 °C) to remove the solvent. For nonvolatile compounds, operating at these
high temperatures maximizes the signal response.
However, at these temperatures volatile and semivolatile compounds are
destroyed and are therefore not detected. This is problematic for small
molecules, such as pharmaceuticals and drug candidates.
The ELS detector is designed to evaporate difficult solvents at ambient and
subtemperatures to maximize detection of semivolatile compounds.
The ELSD has patented technology that reduces the evaporation time of highly
aqueous solvents at low temperature, and also prevents the evaporation tube
becoming saturated, which would otherwise prevent further evaporation
occurring.
Using this patented evaporation gas technology, a 20 µm droplet of water at
30 °C can be dried ca. 3x faster than just temperature alone. Using the Agilent
1290 Infinity II ELSD (G7102A), water can be evaporated as low as 20 °C,
providing maximum sensitivity to thermally sensitive compounds. For maximum
sensitivity of nonvolatile compounds, the evaporation gas can be turned off at
higher evaporation temperatures.
Therefore, unlike other ELS detectors, where the evaporator temperature is set
according to the type of mobile phase, the ELS detector evaporator temperature
is independent of the mobile phase. So, the ELS detector can be set at 30 °C for
all types of mobile phase provided the evaporator gas flow is adjusted
accordingly. This method of operation ensures that the ELSD sensitivity is
maximized even for low molecular weight compounds.
To prevent against unnecessary gas usage, a controlled gas shutoff valve is
integrated into the detector gas manifold. This shutoff valve will only allow gas to
pass into the instrument when in RUN mode. Should the instrument default to
STANDBY mode, the gas will reduce to a default value of 1.2 SLM for 15 min
before closing.

Agilent InfinityLab ELSD User Manual 13
1 Introduction to the Detector
System Overview
Overview of ELS Detector
Figure 3 ELSD overview (front)
1
2
3
4
1 Front screen display
2Keypad
3 Eluent inlet
4 Solvent waste outlet

1 Introduction to the Detector
System Overview
Agilent InfinityLab ELSD User Manual 14
Figure 4 ELSD overview (rear)
1
2
3
4
5
6
7
8
9
1 Vapor Sensor vent
2 Serial RS232 port
3 LAN connector (only active on G7102A)
4 Firmware button
5 I/O connector (Remote Start input)
6MainsSwitch
7MainsInput
8GasInletport
9Exhaustport

Agilent InfinityLab ELSD User Manual 15
1 Introduction to the Detector
System Overview
Table 1 ELS Detector I/O connections
I/O description Pin number
Inputs Timetable Start 14 & ground
Injection Sync 13 & ground
Remote A/Z 7 & ground
Output Pump stop contact closure – normally open 3 & 10
Ground (to case) 1, 5, 6, 11
NOTE
To make appropriate remote start and A/Z connections from a third-party LC, a
third-party remote start cable for Dimension software (Remote start cable
(PL0890-0350)) can be purchased from Agilent Technologies.

Agilent InfinityLab ELSD User Manual 16
2 Site Requirements and Specifications
Pre-installation Requirements 17
Site Requirements 18
Physical Specifications 21
Physical Specifications Agilent 1260 Infinity II ELSD (G4260B) 21
Physical Specifications Agilent 1290 Infinity II ELSD (G7102A) 22
Performance Specifications 23
Performance Specifications (G4260B) 23
Performance Specifications (G7102A) 25
This chapter provides information on environmental requirements, physical, and
performance specifications.

Agilent InfinityLab ELSD User Manual 17
2 Site Requirements and Specifications
Pre-installation Requirements
Pre-installation Requirements
For a detailed description of the environmental and operating requirements of
the ELSD, see the Site Preparation Checklist.
This manual will give you an overview of the ELS detector and describe its
operation in more detail.

2 Site Requirements and Specifications
Site Requirements
Agilent InfinityLab ELSD User Manual 18
Site Requirements
A suitable environment is important to ensure optimal performance of the
instrument, see the Site Preparation Checklist for more details.
Laser Safety
The Agilent 1290 Infinity II ELSD (G7102A) is classified as a "Laser Class 1"
product (IEC825-1, CFR1040.10 & 1040.11). During normal operation of the ELSD
no laser light is accessible to the user.
Power Considerations
Check the operating voltage of your instrument on the IEC inlet fuse holder on
rear of unit.
WARNING
Eye damage by laser light
Hazardous laser light can injure eyes.
Do not remove covers and interlocks.
Observe and note the laser warning signs carefully.
WARNING
Hazard of electrical shock or damage of your instrumentation
can result, if the devices are connected to a line voltage higher than
specified.
Connect your instrument to the specified line voltage only.
WARNING
Inaccessible power plug.
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 ELSD User Manual 19
2 Site Requirements and Specifications
Site Requirements
Power Cords
Your detector is delivered with a power cord which matches the wall socket of
your particular country or region. The plug on the power cord which connects to
the rear of the instrument is identical for all types of power cord.
WARNING
Absence of ground connection or use of unspecified power cord
The absence of ground connection or the use of unspecified power cord
can lead to electric shock or short circuit.
Never operate your instrumentation from a power outlet that has no
ground connection.
Never use a power cord other than the Agilent Technologies power cord
designed for your region.
WARNING
Use of unsupplied cables
Using cables not supplied by Agilent Technologies can lead to damage of
the electronic components or personal injury.
Never use cables other than the ones supplied by Agilent Technologies
to ensure proper functionality and compliance with safety or EMC
regulations.
WARNING
Unintended use of power cords
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.

2 Site Requirements and Specifications
Site Requirements
Agilent InfinityLab ELSD User Manual 20
Bench Space
The module dimensions and weight (see Table 2 on page 21) 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 15 cm (5.9 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.
NOTE
Agilent recommends that you install the HPLC instrument in the InfinityLab Flex
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.