Agilent Technologies 1200 series User manual

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Agilent 1200 Series
Refractive Index
Detector
User Manual

1200 Series RID User Manual
Notices
© Agilent Technologies, Inc. 2006
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Manual Part Number
G1362-90010
Edition
02/06
Printed in Germany
Agilent Technologies
Hewlett-Packard-Strasse 8
76337 Waldbronn, Germany
Manual Structure
The Service Manual G1362-90110 (English)
contains the complete information about
the Agilent 1200 Series Refractive Index
Detector. It is available as Adobe Reader file
(PDF) only.
The User Manual G1362-90010 (English)
and its localized versions contain a subset
of the Service Manual and is shipped with
the detector in printed matter.
Latest versions of the manuals can be
obtained from the Agilent web.
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This guide is valid for B.01.xx revisions of
the Agilent 1200 Series ChemStation Soft-
ware, where xx refers to minor revisions of
the software that do not affect the technical
accuracy of this guide.
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met.

1200 Series RID User Manual 3
In This Guide…
This manual contains user information about the Agilent 1200 Series
Refractive Index Detector. The manual describes the following:
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 Installing the Refractive Index Detector
This chapter provides information on unpacking, checking on completeness,
stack considerations and installation of the detector.
4 Using the Refractive Index Detector
This chapter provides information on how to set up the detector for an
analysis and explains the basic settings.
5 Optimizing the Refractive Index Detector
This chapter provides information on how to optimize the detector.
6 Troubleshooting Overview
This chapter gives an overview about the troubleshooting and diagnostic
features.
7 Repairing the Refractive Index Detector
This chapter provides general information on repairing the detector.
8 Maintaining the Refractive Index Detector
This chapter describes the maintenance of the detector.
A Safety Information
This chapter provides additional information on safety, legal and web.

4 1200 Series RID User Manual

Contents
1200 Series RID User Manual 1
Contents
1 Introduction to the Refractive Index Detector 5
Introduction to the Refractive Index Detector 6
How the Detector Operates 8
Refractive Index Detection 8
Detection Principle 11
Flow Path 14
Electrical Connections 19
Instrument Layout 21
Early Maintenance Feedback (EMF) 22
EMF Counters 22
Using the EMF Counters 22
2 Site Requirements and Specifications 25
Site Requirements 26
Physical Specifications 28
Performance Specifications 29
3 Installing the Refractive Index Detector 33
Unpacking the Detector 34
Optimizing the Stack Configuration 37
Installing the Detector 39
Flow Connections to the Detector 42
4 Using the Refractive Index Detector 45
Operation of the Refractive Index Detector 46
Before Using the System 46

2 1200 Series RID User Manual
Contents
Refractive Index Detector Control 47
Refractive Index Detector Settings 49
Refractive Index Detector More Settings 51
Running a Checkout Sample 54
Checking Baseline Noise and Drift 59
5 Optimizing the Refractive Index Detector 67
Refractive Index Detector Optimization 68
Potential Causes for Baseline Problems 70
Detector Equilibration 71
6 Troubleshooting Overview 73
Overview of the Detector’s Indicators and Test Functions 74
Status Indicators 75
Power Supply Indicator 75
Detector Status Indicator 75
7 Repairing the Refractive Index Detector 77
Introduction to the Repairing the Refractive Index Detector 78
Using the ESD Strap 80
8 Maintaining the Refractive Index Detector 81
Detector Maintenance Procedures 82
Flow Cell Flushing 83
Correcting Leaks 84
Replacing Leak Handling System Parts 85
Replacing the Detector’s Firmware 86
A Safety Information 87
General Safety Information 88

Contents
1200 Series RID User Manual 3
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC) 91
Radio Interference 92
Sound Emission 93
Solvent Information 94
Agilent Technologies on Internet 96

4 1200 Series RID User Manual
Contents

5
Agilent 1200 Series Refractive Index Detector
User Manual
Agilent Technologies
1
Introduction to the Refractive Index
Detector
Introduction to the Refractive Index Detector 6
How the Detector Operates 8
Detection Principle 11
Flow Path 14
Electrical Connections 19
Instrument Layout 21
Early Maintenance Feedback (EMF) 22
This chapter gives an introduction to the Refractive Index Detector.

6 1200 Series RID User Manual
1 Introduction to the Refractive Index Detector
Introduction to the Refractive Index Detector
The detector is designed for highest optical performance, GLP compliance and
easy maintenance. It includes 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 40,000 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 29.

1200 Series RID User Manual 7
Introduction to the Refractive Index Detector 1
Figure 1 The Agilent 1200 Series Refractive Index Detector

8 1200 Series RID User Manual
1 Introduction to the Refractive Index Detector
How the Detector Operates
Refractive Index Detection
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.
Snells’s Law
n
n2
n1
----- α1
sin
α2
sin
-------------==
Where:
n = Refractive index of medium 1 relative to
medium 2
n2= Refractive index of medium 2
n1= Refractive index of medium 1
α1= angle of incident light in medium 1
α2=angle of refraction in medium 2

1200 Series RID User Manual 9
Introduction to the Refractive Index Detector 1
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.
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
Figure 2 Light Refraction
Medium 1
Medium 2
α1α2 g
γtan
n1n–2
n1
-----------------=
Where:
γ= angle of external deflection

10 1200 Series RID User Manual
1 Introduction to the Refractive Index Detector
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

1200 Series RID User Manual 11
Introduction to the Refractive Index Detector 1
Detection Principle
Detector Design
The Agilent 1200 Series 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 3).

12 1200 Series RID User Manual
1 Introduction to the Refractive Index Detector
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 3 Detection Principle
Diode 1 Diode 2
Zero glass
Light receiver Reference cell
Sample cell Mirror
Slit

1200 Series RID User Manual 13
Introduction to the Refractive Index Detector 1
Figure 4 Optical Path
diodes
zero glass
Deflected light
collimator lens
reference cell
mirror
lamp
condenser lens
incident light
sample cell

14 1200 Series RID User Manual
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 °C
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 (see Figure 5). 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.

1200 Series RID User Manual 15
Introduction to the Refractive Index Detector 1
1Flow in
2Heater
3Heat exchanger
4Sample cell
5Purge valve
6Recycle valve
7Waste container
8Reference cell
9Solvent bottle
Figure 5 Flow Path
2
1
34
3
5
6
7
8
9
Flow path with purge valve off
Flow path with purge valve on

16 1200 Series RID User Manual
1 Introduction to the Refractive Index Detector
Figure 6 G1362A Physical Plumbing Connections
from optical unit
sample cell (top right)
bottom left
(1)
COM
Purge valve
Recycle valve
WASTE
IN
top left
optical unit (from and to reference cell)
(3)
(2)
(4)
Capillaries (1) to (4) are part of the optical unit assembly. They are made of SST with an ID of 1.0 mm, except for (2),
which has an ID of 0.2 mm. All other tubings (to and from the purge and the reference valve) are made of Teflon and are
available as a kit (PN G1362-68709)
COM
to optical unit
sample cell (bottom right)
RECYCLE
NO
NC
NO NC
C ON N E C T I N G P O R T S
Metal union
block
COM = COMMON
NO = NORMALLY OPEN
NC = NORMALLY CLOSED