Agilent Technologies G1315B User manual

A
Agilent 1200 Series
Diode Array and
Multiple Wavelength
Detectors
G1315B / G1365B
User Manual

21200 Series DAD and MWD User Manual
Notices
© Agilent Technologies, Inc. 2006
No part of this manual may be reproduced in
any form or by any means (including elec-
tronic storage and retrieval or translation
into a foreign language) without prior agree-
ment and written consent from Agilent
Technologies, Inc. as governed by United
States and international copyright laws.
Manual Part Number
G1315-90006
Edition
Edition 02/2006
Printed in Germany
Agilent Technologies
Hewlett-Packard-Strasse 8
76337 Waldbronn
Manual Structure
The User Manual G1315-90006 (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.
The Service Manual G1315-90106 (English)
contains the complete information about
the Agilent 1200 Series Diode Array and
Multiple Wavelength Detectors. It is
available as Adobe Reader file (PDF) only.
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Safety Notices
CAUTION
A CAUTION notice denotes a haz-
ard. It calls attention to an operat-
ing procedure, practice, or the like
that, if not correctly performed or
adhered to, could result in damage
to the product or loss of important
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CAUTION notice until the indicated
conditions are fully understood and
met.
WARNING
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly per-
formed or adhered to, could result
in personal injury or death. Do not
proceed beyond a WARNING
notice until the indicated condi-
tions are fully understood and
met.

1200 Series DAD and MWD User Manual 3
In This Manual…
This manual contains information for using your Diode Array
and Multiple Wavelength Detectors.
1 Introduction to the Detector
This chapter gives an introduction to the detector, instrument
overview and internal connectors.
2 Site Requirements and Specifications
This chapter gives information on environmental requirements,
physical and performance specifications.
3 Installing the Detector
This chapter describes the installation of the detector.
4 Using the Detector
This chapter provides information on how to set up the detector
for an analysis and explains the basic settings.
5 How to optimize 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 and the different user interfaces.
7 Maintenance and Repair
This chapter provides general information on maintenance and
repair of the detector.
8 Maintenance
This chapter describes the maintenance of the detector and the
required tests.

41200 Series DAD and MWD User Manual
9 Parts and Materials for Maintenance
This chapter provides information on parts for maintenance.
A Appendix
This chapter provides safetey and other general information.

1200 Series DAD and MWD User Manual 5
Contents
1 Introduction to the Detector
Introduction to the Detector 12
Optical System Overview 13
Early Maintenance Feedback (EMF) 16
EMF Counters 16
Using the EMF Counters 16
Electrical Connections 18
Instrument Layout 20
2 Site Requirements and Specifications
Site Requirements 22
Physical Specifications 25
Performance Specifications 26
3 Installing the Detector
Unpacking the Detector 30
Damaged Packaging 30
Delivery Checklist 30
Optimizing the Stack Configuration 32
Installing the Detector 35
Flow Connections to the Detector 38
4 Using the Detector
Setting up an Analysis 44

61200 Series DAD and MWD User Manual
Before Using the System 44
Requirements and Conditions 46
Optimization of the System 48
Preparing the HPLC System 49
Running the Sample and Verifying the Results 58
Special Settings of the Detector 59
Control Settings 59
Online Spectra 60
Analog Output Settings 61
Spectrum Settings 62
Peakwidth Settings 64
Slit Settings 65
Margin for Negative Absorbance Settings 66
Optimizing the Detector 66
5 How to optimize 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 77
Optimizing Spectral Acquisition (DAD only) 80
Margin for Negative Absorbance 81
Optimizing Selectivity 82
Quantifying Coeluting Peaks by Peak Suppression 82
Ratio Qualifiers for Selective Detection of Compound
Classes 84

1200 Series DAD and MWD User Manual 7
6 Troubleshooting and Diagnostics
Overview of the Detector’s Indicators and Test Functions 88
Status Indicators 89
Power Supply Indicator 89
Detector Status Indicator 90
User Interfaces 91
Agilent LC Diagnostic Software 92
7 Maintenance and Repair
Introduction into Repairing the Detector 94
Simple Repairs 94
Exchanging Internal Parts 94
Warnings and Cautions 95
Cleaning the Detector 96
Using the ESD Strap 97
8 Maintenance
Overview of Maintenance 100
Exchanging a Lamp 101
Exchanging a Flow Cell 103
Maintenance of Standard, Semi-Micro or Micro Flow Cell 106
Maintenance of High Pressure Flow Cell 111
Replacing Capillaries on a Standard Flow Cell 114
Replacing Capillaries on a Semi-Micro, Micro and High Pressure
Flow Cell 119
Nano Flow Cell - Replacing or Cleaning 123
Cleaning or Exchanging the Holmium Oxide Filter 128

81200 Series DAD and MWD User Manual
Correcting Leaks 131
Replacing Leak Handling System Parts 132
Replacing the Interface Board 133
Replacing the Detector’s Firmware 134
Tests & Calibrations 135
Intensity Test 136
Wavelength Verification and Recalibration 138
Holmium Oxide Test 139
Cell Test (ChemStation only) 141
9 Parts and Materials for Maintenance
Overview of Maintenance Parts 144
Standard Flow Cell 146
Semi-Micro Flow Cell 148
Micro Flow Cell 150
High Pressure Flow Cell 152
Prep Flow Cell - SST 154
Prep Flow Cell - Quartz 156
Nano Flow Cells 158
Accessory Kit 162
A Appendix
General Safety Information 166
Lithium Batteries Information 169
The Waste Electrical and Electronic Equipment (WEEE) Directive
(2002/96/EC) 170
Radio Interference 171

1200 Series DAD and MWD User Manual 9
Sound Emission 172
UV-Radiation 173
Solvent Information 174
Declaration of Conformity for HOX2 Filter 176
Agilent Technologies on Internet 177
Index

10 1200 Series DAD and MWD User Manual

11
Agilent 1200 Series Diode Array and Multiple Wavelength Detectors
User Manual
Agilent Technologies
1
Introduction to the Detector
Introduction to the Detector 12
Optical System Overview 13
Early Maintenance Feedback (EMF) 16
Electrical Connections 18
Instrument Layout 20
This chapter gives an introduction to the detector, instrument overview and
internal connectors.

12 1200 Series DAD and MWD User Manual
1 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:
•long-life deuterium 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 five wavelengths simultaneous,
•programmable slit from 1–16 nm for complete optimization of sensitivity,
linearity and spectral resolution,
•optional flow-cell cartridges with I.D. tag (standard 10 mm 13 µl,
semi-micro 6 mm 5 µl, micro 3 mm 2 µl, 80 nl/500 nl 10 mm, high pressure
10 mm 1.7 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 (G1315B DAD
and G1365B MWD).
For specifications, see “Performance Specifications” on page 26.

1200 Series DAD and MWD User Manual 13
Introduction to the Detector 1
Optical System Overview
Optical System
The optical system of the detector is shown in Figure 1. 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
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
Figure 1 Optical System of the Detector
Tungsten lamp
Deuterium lamp
Holmium oxide filter
Achromat (source lens)
Flow cell
Slit
Diode arra
y
Grating
Cell suppo
r
window
Spectro le
n
Coupling lens

14 1200 Series DAD and MWD User Manual
1 Introduction to the Detector
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.
Achromat
(Source Lens)
The achromat receives the light from both lamps and focuses it so that the
beam passes through the flow cell.
Holmium Oxide
Filter
The holmium oxide filter is electromechanically actuated. During the holmium
filter test it moves into the light path.
Cell Support
Window
The cell support window assembly separates the holmium filter area from the
flow cell area.
Flow Cell
Compartment
The optical unit has a flow cell compartment for easy access to flow cells. A
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 spectograph 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 Entrance
Slit System
The micro-slit system makes use of the mechanical properties of silicon
combined with the precise structuring capabilities of bulk micro-machining. It
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.

1200 Series DAD and MWD User Manual 15
Introduction to the Detector 1
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.

16 1200 Series DAD and MWD User Manual
1 Introduction to the Detector
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 detector 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
The detector provides two EMF counters for the lamps. The counters
increment increments with lamp use, and can be assigned a maximum limit
which provides visual feedback in the user interface when the limit is
exceeded. The counters can be reset to zero after the lamp is exchanged. The
detector provides the following EMF counters:
•Deuterium Lamp On-Time
•Tungsten Lamp On-Time
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
lamp burn time is dependent on the requirements for the analysis (high or low
sensitivity analysis, wavelength etc.), therefore, the definition of the maximum
limits need to be determined based on the specific operating conditions of the
instrument.

1200 Series DAD and MWD User Manual 17
Introduction to the Detector 1
Setting the EMF Limits
The setting of the EMF limits must be optimized over one or two maintenance
cycles. Initially, no EMF limit should be set. When instrument performance
indicates maintenance is necessary, take note of the values displayed by lamp
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.

18 1200 Series DAD and MWD User Manual
1 Introduction to the Detector
Electrical Connections
•The GPIB connector is used to connect the detector with a computer. The
address and control switch module next to the GPIB connector determines
the GPIB address of your detector. The switches are preset to a default
address which is recognized once after power is switched on.
•The CAN bus is a serial bus with high speed data transfer. The two
connectors for the CAN bus are used for internal Agilent 1200 Series
module data transfer and synchronization.
•Two independent analog outputs provide signals for integrators or data
handling systems.
•The interface board slot is used for external contacts and BCD bottle
number output or LAN connections.
•The REMOTE connector may be used in combination with other analytical
instruments from Aligent Technologies if you want to use features such as
start, stop, common shut down, prepare, and so on.
•With the appropriate software, the RS-232C connector may be used to
control the detector from a computer through a RS-232C connection. This
connector is activated and can be configured with the configuration switch
next to the GPIB connector. See your software documentation for further
information.
•The power input socket accepts a line voltage of 100 – 240 V AC ± 10 % with
a line frequency of 50 or 60 Hz. Maximum power consumption is
300 VA/125 W. There is no voltage selector on your detector because the
power supply has a wide-ranging capability. There are no externally
accessible fuses, because automatic electronic fuses are implemented in the
power supply. The security lever at the power input socket prevents that the
detector cover is taken off when line power is still connected.
WARNING Never use cables other than the ones supplied by Aligent Technologies to ensure
proper functionality and compliance with safety or EMC regulations.

1200 Series DAD and MWD User Manual 19
Introduction to the Detector 1
Figure 2 Rear View of Detector - Electrical Connections and Label
Analog signals
APG remote
RS-232C
CAN GPIB Power
Configuration switch
Interface board Security lever
voltage range
power consumption /
frequency
safety standards
product number
serial number
configuration switch
settings
serial number:
DE manufactured in Germany
62006
01 week of last major change
00130 number of unit

20 1200 Series DAD and MWD User Manual
1 Introduction to the Detector
Instrument Layout
The industrial design of the detector 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 detector 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.