Agilent Technologies 1260 Infinity User manual

Agilent 1260 Infinity
Evaporative Light
Scattering Detector
User Manual

Agilent 1260 Infinity ELSD User Manual
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G4218-90002
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06/2010
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Agilent 1260 Infinity ELSD User Manual 3
In This Guide...
This manual is designed to describe the installation; operation,
maintenance and basic troubleshooting of the G4218A Agilent
Evaporative Light Scattering Detector. It includes:
1 Introduction
2 Site Requirements and Specifications
Site requirements and specifications of the Agilent 1260 Infinity
Evaporative Light Scattering Detector
3 Installing the Detector
Installation of the detector.
4 Using the System
This chapter describes how to operate the Low Temperature
Evaporative Light Scattering Detector. It includes information
about starting the unit on a routine basis, collecting data and
shutting down the unit.
5 Optimizing Performance
This chapter shows how to optimize the detector to achieve best
results.
6 Troubleshooting and Diagnostics
This chapter describes a series of activities that should be
performed on a periodic basis to ensure maximum
performance. In addition, this chapter includes a protocol that
can be used to determine the cause of problems that are
observed with the instrument.
7 Maintenance
Introduction to maintenance and repair, instructions on simple,
routine repair procedures

4 Agilent 1260 Infinity ELSD User Manual
8PartsforRepair
Detailed illustrations and lists for identification of parts and
materials for repair
9 The Control Panel
This chapter describes the role of the various controls and
displays on the detector.
10 Appendix
This chapter contains safety information.

Agilent 1260 Infinity ELSD User Manual 5
Contents
1 Introduction 9
The Low Temperature Evaporative Light Scattering Detector 10
Principle of Operation 12
Nebulization 14
Evaporation of the Solvent 17
Detection 17
2 Site Requirements and Specifications 19
Site Requirements 20
Power Considerations 20
Gas Considerations 21
Power Cords 21
Exhaust venting and drain requirements 22
Location of the Detector in the Laboratory 23
Environment 23
Specifications 24
3 Installing the Detector 27
Lifting and Carrying the Module 28
Unpacking the System 30
Installing the Detector 32
Gas Supply 33
Vent the Exhaust Line to a Fume Hood 37
Electrical Connections 38
Additional Options 40

6 Agilent 1260 Infinity ELSD User Manual
Contents
Installing the Nebulizer and Nebulization Chamber Assembly 43
Connecting the Siphon Overflow 46
Connecting the Nebulization Gas to the Nebulizer 47
Connecting the Column 47
Powering Up the Unit 47
4UsingtheSystem49
Preparing the System for Operation 50
Auto-zeroing the Detector 51
Manual Auto-zeroing of the Detector 51
External Auto-zeroing of the Detector 51
Routine Operation of the System 52
Installation Test Procedure 54
Powering Down and Shutting Down the System 56
5 Optimizing Performance 59
Selecting the Optimum Temperature 60
Optimizing the Mobile Phase 62
Sample Pre-Treatment 62
Column Treatment 63
Optimizing the Filter 64
6 Troubleshooting and Diagnostics 65
Basics of Troubleshooting 66
Initial Troubleshooting Activities 67
If there is no response from the system 68
Perform the Noise Tests 69
Specific Detector Troubleshooting 70
Noise test procedures 71
Preliminary Activities 72

Contents
Agilent 1260 Infinity ELSD User Manual 7
Electronic Noise Test 73
Background Noise (Stray Light) Test 74
Solvent Noise Test 75
Column Noise Test 77
Troubleshooting based on diagnostic tests 78
Electronic noise test 78
Stray light test 78
Failed run of standard sample 78
Troubleshooting based on instrument signals 79
No signal is observed 79
Decrease in sensitivity 80
A noisy signal is observed 80
7 Maintenance 81
General inspection 82
Cleaning and Decontamination 83
Cleaning the Detector 83
Decontaminating the detector 83
Removing the nebulization chamber and nebulizer 84
Cleaning the Nebulizer 86
Adjusting stray light settings 89
8PartsforRepair91
Evaporative Light Scattering Detector Parts 92
9 The Control Panel 95
The Control Panel 96
The Digital Display 97
The User Interface 98

8 Agilent 1260 Infinity ELSD User Manual
Contents
10 Appendix 107
Safety Information 108
Solvent Information 112
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC) 113
Lithium Batteries Information 114
Agilent Technologies on Internet 115
Index 117

9
Agilent 1260 Infinity Evaporative Light Scattering Detector
User Manual
Agilent Technologies
1
Introduction
The Low Temperature Evaporative Light Scattering Detector 10
Principle of Operation 12

10 Agilent 1260 Infinity ELSD User Manual
1 Introduction
The Low Temperature Evaporative Light Scattering Detector
The Low Temperature Evaporative Light Scattering Detector
The Agilent 1260 Infinity Evaporative Light Scattering Detector (Figure 1) is
designed to detect compounds in the eluent from high performance liquid
chromatography (HPLC), micro-HPLC, gel permeation chromatography (GPC)
or counter current chromatography (CCC). It is capable of monitoring eluent
flow rates from 5 µl/min to 5 ml/min. Evaporative light scattering detection is
a universal technique which can detect any non-volatile analyte. Detection
does not depend on the absorbtion of radiation and is not affected by the
absorbtion characteristics of the solvent; thus solvents which absorb UV
radiation can be used.
Figure 1 The Agilent 1260 Infinity
Evaporative Light Scattering Detector

Agilent 1260 Infinity ELSD User Manual 11
Introduction 1
The Low Temperature Evaporative Light Scattering Detector
The detector is controlled via the keypad and digital display on the front
panel. Alternatively, the system can be controlled by an external computer
using the RS-232 port. The output can be sent to a recorder or data station.
The detector includes a nebulizer, evaporation tube and detector head. The
evaporation tube is located in an oven to assist in the evaporation of the
solvent.

12 Agilent 1260 Infinity ELSD User Manual
1 Introduction
Principle of Operation
Principle of Operation
There are three steps in the operation of the detector:
1nebulization of the eluent,
2evaporation of the solvent and
3detection of the compound(s) of interest (Figure 2).
Nebulization involves the conversion of the eluent into a fine mist. The mist is
passed through an evaporator to vaporize solvent. In the detector unit, the
mist is irradiated by a light source and scattered light is measured by a
photomultiplier (PM). The degree of light scattering is related to the
concentration of the compound of interest in the sample. A cross sectional
view of the system is presented in Figure 3.
NEBULIZATION ÆEVAPORATION ÆDETECTION
Figure 2 Schematic Diagram of an Evaporative Light Scattering Detector

Agilent 1260 Infinity ELSD User Manual 13
Introduction 1
Principle of Operation
Figure 3 Schematic display of principle measurement steps in the ELSD of the Detector

14 Agilent 1260 Infinity ELSD User Manual
1 Introduction
Principle of Operation
Nebulization
The eluent from the chromatograph is nebulized by the inlet gas (typically
nitrogen). At the outlet of the nebulizer, the aerosol travels through a chamber.
Large droplets in the aerosol go to a siphon while the fine mist moves to the
evaporation tube. The overall design of the nebulizer is shown in Figure 1 and
the nebulization chamber is shown in Figure 5.
Five different nebulizers are available for optimizing the performance of the
detector at different HPLC flow rates (see Table 9). The user should select the
nebulizer to best match the flow rate that will be used with the separation
when the detector is ordered (the optimal range for each nebulizer is indicated
in Table 9). Additional nebulizers are available from Agilent Technologies and
can be easily installed, see “Installing the Nebulizer and Nebulization Chamber
Assembly” on page 43.

Agilent 1260 Infinity ELSD User Manual 15
Introduction 1
Principle of Operation
Figure 4 Design of the Nebulizer
Peek inlet
Colored Seal
Ring
Gas inlet

16 Agilent 1260 Infinity ELSD User Manual
1 Introduction
Principle of Operation
Figure 5 The Nebulizer
To HPLC system
Inlet for nitrogen
To waste
Siphon
To evaporator
and detection
Nebulization chamber
Nebulizer
Colored seal

Agilent 1260 Infinity ELSD User Manual 17
Introduction 1
Principle of Operation
Evaporation of the Solvent
A heated tube is used to evaporate the solvent. The exit of the heated tube
leads directly into the detector cell.
In liquid chromatography, water and organic solvents with low boiling points
are typically employed (e.g. methanol, acetonitrile). A typical mobile phase for
a reverse phase separation using evaporative light scattering detection might
be methanol/water (60/40) while a typical mobile phase for normal phase
separation might be hexane.
If acids, bases and salts are used to modify mobile phase to provide the
desired separation, they should able to be readily evaporated, sublimed or
decomposed into gases in the evaporation tube. Mobile phase modifiers that
are commonly used when an evaporative light scattering detector is employed
include NH4OH, (C2H5)3N, NH4OAc, HCOOH, CH3COOH, CF3COOH and HNO3.
Detection
The carrier gas transports the microparticles from the heating tube into the
detection chamber (Figure 6).
Figure 6 The Detection Chamber
Detection chamber
Photomultiplier
Light trap
Addtitional gas
Heating tube
LED

18 Agilent 1260 Infinity ELSD User Manual
1 Introduction
Principle of Operation
The detector chamber contains a light emitting diode (LED) and a
photomultiplier that is positioned at an angle of 120owith respect to the light
beam (Figure 6). When the carrier gas contains microparticles, the light is
scattered and is detected by the photomultiplier.
The intensity of the scattered light is a function of the mass of the scattering
particles and generally follows an exponential relationship, which is shown in
Equation 1.
I = k mb(1)
where:
Iis the intensity of light
mis the mass of the scattering particles
kand bare constants
A plot of log I versus log m provides a linear response. The values of the
constants (k and b) depend on a variety of experimental conditions (e.g. the
temperature and the nature of the mobile phase).
A gas inlet before the detector chamber provides a concentric shield for the
carrier gas. This serves to eliminate diffusion of the carrier gas and eliminates
contamination of the detector cell.

19
Agilent 1260 Infinity Evaporative Light Scattering Detector
User Manual
Agilent Technologies
2
Site Requirements and Specifications
Site Requirements 20
Specifications 24

20 Agilent 1260 Infinity ELSD User Manual
2 Site Requirements and Specifications
Site Requirements
Site Requirements
A suitable environment is important to ensure optimum performance of the
Agilent 1260 Infinity detector.
Power Considerations
The detector is configured for either 100 V AC / 50-60 Hz, 115 V AC / 60 Hz or
230 V AC / 50 Hz input power depending on the country to which it is shipped.
Ensure that the voltage value indicated on the power connector on the rear
panel corresponds to the line voltage in your facility.
The detector requires G4218-64000 230 V, 1.7 A, 400 W, 50 Hz, G4218-6410 115
V, 1.8 A, 210 W, 60 Hz, G4218-64020 100 V, 2.1 A, 210 W, 50/60 Hz. Check that
the power lines can provide sufficient current.
The detector must be connected to a properly grounded three prong plug to
ensure proper operation of the system. If a two prong outlet is used, make sure
that the ground wire is used to ground the instrument. It is recommended that
all components of the HPLC system are connected to a common ground.
The detector should not be connected to an electrical line which also serves
units with a large power drain or which may be subject to power surges. Such
units include refrigerators, ovens, centrifuges and fume hoods.
WARNING Incorrect line voltage at the instrument
Shock hazard 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.