Agilent Technologies 1100 Series User manual

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Agilent 1100 Series
Fluorescence Detector
Reference Manual
Agilent G1321A
Asset # 304025

2 1100 Series FD Reference Manual
Notices
© Agilent Technologies, Inc. 2002
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
G1321-90002
Edition
Edition 07/02
Printed in Germany
Agilent Technologies
Hewlett-Packard-Strasse 8
76337 Waldbronn, Germany
Software Revision
This guide is valid for A.01.xx revisions of
the Agilent 1100 Series Fluorescence
Detector software, where xx refers to minor
revisions of the software that do not affect
the technical accuracy of this guide.
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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
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CAUTION notice until the indicated
conditions are fully understood and
met.
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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
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notice until the indicated condi-
tions are fully understood and
met.

1100 Series FD Reference Manual 3
In This Guide…
1 Installing the Fluorescence Detector
How to install the fluorescence detector
2 First Steps with the Fluorescence Detector
How to start with the detector
3 Optimizing the Fluorescence Detector
Detection with the Agilent 1100 series fluorescence detector,
either fluorescence or phosphorescence, can give you very
sensitive and selective results if you understand what you are
doing and why. This chapter explains in detail how to optimize
detection.
4 Troubleshooting and Test Functions
This chapter describes the detector’s built in troubleshooting
and test functions.
5 Repairing the Fluorescence Detector
Instructions on how to repair the detector
6 Identifying Parts and Materials
Detailed illustrations and listings for parts and materials
identification for the detector
7 Introduction to the Fluorescence Detector
An introduction to the detector
8 Therory of Operation
Instrument overview, theory of operation, external
communication and internal connectors

4 1100 Series FD Reference Manual
9 Introduction to the Control Module
This chapter is intended to introduce an operator to the screens
available for operation of the Agilent 1100 diode array detector
with the Agilent 1100 control module.
Please use the manual of Control module for further detailed
reference.
10 Specifications
Performance specifications of the detector

1100 Series FD Reference Manual 5
Contents
1 Installing the Fluorescence Detector
Site Requirements 14
Physical Specifications 16
Unpacking the Detector 17
Detector Accessory Kit Contents 18
Optimizing the Stack Configuration 20
Installing the Detector 22
Flow Connections to the Detector 24
2 First Steps with the Fluorescence Detector
Before You Start 30
Optimization Overview 31
Getting Started and Checkout 33
Starting Your Detector 33
Setting the Chromatographic Conditions 34
Observe the maxima via the isoabsorbance plot 36
Method Development 37
Step 1: Check the LC system for impurities 38
Step 2: Optimize limits of detection and selectivity 39
Step 3: Set up routine methods 48
Example: Optimization for Multiple Compounds 52
3 Optimizing the Fluorescence Detector
Optimization Overview 62

6 1100 Series FD Reference Manual
Design Features Help Optimization 63
Check Performance Before You Start 63
Finding the Best Wavelengths 64
A Real Example 65
Finding the Best Signal Amplification 66
Changing the Xenon Flash Lamp Frequency 67
Lamp life savings 68
Selecting the Best Response Time 69
Reducing Stray Light 71
4 Troubleshooting and Test Functions
Overview of the Detector’s Indicators and Test Functions 74
Status Indicators 75
Power Supply Indicator 75
Detector Status Indicator 76
Error Messages 77
Time-out 78
Shutdown 79
Remote Time-out 80
Synchronization Lost 81
Leak 82
Leak Sensor Open 84
Leak Sensor Short 85
Compensation Sensor Open 86
Compensation Sensor Short 87
Fan Failed 88
Motor Errors 89
Lamp Cover Open 91
FLF Board not found 92
ADC Not Calibrated 93

1100 Series FD Reference Manual 7
A/D Overflow 94
Flash Lamp Current Overflow 95
Flash Trigger Lost 96
Wavelength Calibration Failed 97
Wavelength Calibration Lost 98
Flow Cell Removed 99
No Peaks 100
Wavelength Verification and Calibration 101
Check of Raman Band of Water 104
The Wavelength Calibration Procedure 110
Preparation of the Glycogen Calibration Sample 110
Preparation of the Flow Cell 111
Wavelength Calibration 112
Verification 113
Test Functions 114
Lamp Intensity Test 115
Lamp Intensity History 116
Dark-Current Test 117
Excitation and Emission Grating Resistance History 118
Raman ASTM Signal-to-Noise Test 119
Using the Built-in Test Chromatogram 124
Using the Built-in DAC Test 127
5 Repairing the Fluorescence Detector
Introduction into Repairing the Fluorescence Detector 130
Overview of the Repairing of the Fluorescence Detector 133
Simple Repairs 134
Exchanging a Flow Cell 135
How to use the Cuvette 138
Flow Cell Flushing 139
Correcting Leaks 140

8 1100 Series FD Reference Manual
Replacing Leak Handling System Parts 141
Exchanging Internal Parts 142
Removing the Covers 144
Removing the Rear Foam 146
Exchanging the Lamp 147
Exchanging the EX-condenser 152
Replacing the Lamp Cover Window 155
Exchanging the Processor Board 159
Exchanging the Fan 163
Exchanging the Leak Sensor or Leak Panel 165
Replacing the EM-Condenser or Cutoff-Filter 168
Replacing the Mirror Assembly 172
Replacing the Slits 176
Removing the Optical Unit 178
Replacing PMT and/or FLF board 180
Replacing FLL board and Trigger Pack 183
Replacing the EM and EX Grating 187
Exchanging the Power Supply 190
Replacing Status Light Pipe 193
Installing the Optical Unit 194
Replacing the Foams and Covers 196
Assembling the Main Cover 198
Replacing the Interface Board 199
Replacing the Detector’s Firmware 200
6 Identifying Parts and Materials
Overview of Main Assemblies 202
Optical Unit Assembly 204
Lamp Cover Parts 207
Control Module 208
Sheet Metal Kit 209

1100 Series FD Reference Manual 9
Plastic Parts 210
Foam Parts 211
Power and Status Light Pipes 212
Leak Parts 213
Cuvette Kit 214
Spare Parts 215
Accessory Kit 216
Cable Overview 218
Analog Cables 220
Remote Cables 223
BCD Cables 229
Auxiliary Cable 232
CAN Cable 233
External Contact Cable 234
RS-232 Cable Kit 235
LAN Cables 236
7 Introduction to the Fluorescence Detector
Introduction to the Detector 238
How the Detector Operates 239
Raman Effect 242
Optical Unit 243
Reference System 250
Analytical Information From Primary Data 251
Fluorescence Detection 251
Phosphorescence Detection 252
Processing of Raw Data 253
Electrical Connections 256

10 1100 Series FD Reference Manual
Instrument Layout 258
Early Maintenance Feedback (EMF) 259
EMF Counters 259
Using the EMF Counters 261
8 Theory of Operation
Electronics 264
Detector Main Board (FLM) 265
Detector Frontend Board (FLF) 269
Detector Lamp Supply Board (FLL) 273
Firmware Description 274
Firmware Updates 275
Raw Data Conversion to Fluorescence (LU) Units 276
Data flow for chromatographic output 277
Data flow for spectral output 278
Spectra Acquisition Modes 281
Optional Interface Boards 282
BCD Board 283
LAN Board 284
Interfaces 285
Analog Signal Output 286
GPIB Interface 286
CAN Interface 286
Remote Interface 287
RS-232C 288
Setting the 8-bit Configuration Switch 290
GPIB Default Addresses 291
Communication Settings for RS-232C Communication 292
Forced Cold Start Settings 293

1100 Series FD Reference Manual 11
Stay-Resident Settings 294
The Main Power Supply Assembly 295
9 Introduction to the Control Module
Major keys on the Agilent 1100 Control Module 298
Screens available from the Analysis screen 299
Screens available from the System screen 315
Screens available from the Records screen 318
Diagnostics and Tests 323
10 Specifications
Performance Specifications 328
ASafetyInformation
General Safety Information 332
Lithium Batteries Information 335
Radio Interference 336
Sound Emission 337
UV-Radiation 338
Solvent Information 339
Declaration of Conformity for HOX2 Filter 340
Agilent Technologies on Internet 341
Index

12 1100 Series FD Reference Manual

13
Agilent 1100 Series Fluorescence Detector
Reference Manual
Agilent Technologies
1
Installing the Fluorescence Detector
Site Requirements 14
Physical Specifications 16
Unpacking the Detector 17
Optimizing the Stack Configuration 20
Installing the Detector 22
Flow Connections to the Detector 24

14 1100 Series FD Reference Manual
1Installing the Fluorescence Detector
Site Requirements
A suitable environment is important to ensure optimal performance of the
detector.
Power Consideration
The detector power supply has wide ranging capabilities and accepts any line
voltage in the range mentioned in Table 1 on page 16. Consequently, there is
no voltage selector in the rear of the detector. There are also no externally
accessible fuses, because automatic electronic fuses are implemented in the
power supply.
Power Cords
Different power cords are offered as options with the detector. The female end
of all power cords is identical. It plugs into the power-input socket at the rear
of the detector. The male end of each power cord is different and designed to
match the wall socket of a particular country or region.
WARNING To disconnect the detector from line, unplug the power cord. The power supply still
uses some power, even if the power switch on the front panel is turned off.
WARNING Shock hazard or damage of your instrumentation can result, if the devices are
connected to a line voltage higher than specified.
WARNING 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 Never use cables other than the ones supplied by Agilent Technologies to ensure
proper functionality and compliance with safety or EMC regulations.

Installing the Fluorescence Detector 1
1100 Series FD Reference Manual 15
Bench Space
The detector dimensions and weight (see Table 1 on page 16) allows you to
place the detector on almost any desk or laboratory bench. It needs an
additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm
(3.1 inches) in the rear for air circulation and electric connections.
If the bench should carry a Agilent 1100 Series system, make sure that the
bench is designed to bear the weight of all modules.
The detector should be operated in a horizontal position.
Environment
Your detector will work within the specifications at ambient temperatures and
relative humidity described in Table 1 on page 16.
ASTM drift tests require a temperature change below 2 ∞C/hour (3.6 ∞F/hour)
over one hour period. Our published drift specification (refer also to
“Performance Specifications" on page 328) is based on these conditions.
Larger ambient temperature changes will result in larger drift.
Better drift performance depends on better control of the temperature
fluctuations. To realize the highest performance, minimize the frequency and
the amplitude of the temperature changes to below 1 ∞C/hour (1.8 ∞F/hour).
Turbulences around one minute or less can be ignored.
CAUTION Do not store, ship or use your detector under conditions where temperature
fluctuations could cause condensation within the detector. Condensation will damage
the system electronics. If your detector was shipped in cold weather, leave it in its box
and allow it to warm up slowly to room temperature to avoid condensation.

16 1100 Series FD Reference Manual
1Installing the Fluorescence Detector
Physical Specifications
Table 1 Physical Specifications
Type Specification Comments
Weight 11.5kg(26lbs)
Dimensions
(width×depth×height)
345 × 435 × 140 mm
(13.5 × 17 × 5.5 inches)
Line voltage 100 – 120 or 220 – 240 VAC, ± 10 % Wide-ranging capability
Line frequency 50 or 60 Hz ±5%
Power consumption 180 VA / 70 W / 239 BTU Maximum
Ambient operating temperature 0 – 40 ∞C (32 – 104 ∞F)
Ambient non-operating temperature -40 – 70 ∞C (-4 – 158 ∞F)
Humidity < 95%, at 25 – 40 ∞C (77 – 104 ∞F) Non-condensing
Operating altitude Up to 2000 m (6500 ft)
Non-operating altitude Up to 4600 m (14950 ft) For storing the detector
Safety standards: IEC, CSA, UL, EN Installation category II, pollution degree 2

Installing the Fluorescence Detector 1
1100 Series FD Reference Manual 17
Unpacking the Detector
Damaged Packaging
If the delivery packaging shows signs of external damage, please call your
Agilent Technologies sales and service office immediately. Inform your service
representative that the detector may have been damaged during shipment.
Delivery Checklist
Ensure all parts and materials have been delivered with the detector. The
delivery checklist is shown below. Please report missing or damaged parts to
your local Agilent Technologies sales and service office.
CAUTION If there are signs of damage, please do not attempt to install the detector.
Table 2 Detector Checklist
Description Quantity
Detector 1
Power cable 1
CAN cable (Part number 5181-1519) 1
Flow cell 1 (built-in)
Optional flow cell/cuvette as ordered
Reference Manual 1
Accessory kit (see Ta b l e 3 on page 18) 1

18 1100 Series FD Reference Manual
1Installing the Fluorescence Detector
Detector Accessory Kit Contents
Table 3 Accessory Kit Contents (Part Number G1321-68705)
Description Part Number Quantity
Teflon Tubing flexible i.d. 0.8 mm (flow cell to waste),
re-order 5 m
5062-2462 2 m
Corrugated tubing (to waste), re-order 5 m 5062-2463 1.2 m
Fitting male PEEK 0100-1516 2
Capillary column-detector, one side preinstalled
380 mm lg, 0.17 mm i.d. includes:
G1315-87311 1
Ferrule front SST 0100-0043 1
Ferrule back SST 0100-0044 1
Fitting SST 79814-22406 1
Hex key set 1 – 5 mm 8710-0641 1
Screwdriver hexagonal 4 mm, 100 mm long 5965-0027 1
Screwdriver hexagonal 2.5 mm, 100 mm long 5965-0028 1
Needle-Syringe 9301-0407
Glass-Syringe 9301-1446
Calibration Sample, Glycogen 5063-6597
Sample filter, diameter=3 mm, pore size 0.45 µm 5061-3367
(pack of 100)
5
Wrench open end 1/4 – 5/16 inch 8710-0510 1
ESD wrist strap 9300-1408 1

Installing the Fluorescence Detector 1
1100 Series FD Reference Manual 19
Figure 1 Waste Tubing Parts
Figure 2 Inlet Capillary (Column-Detector) Parts
Fitting male PEEK
Tub ing
Ferrule front
This side is
preinstalled
Ferrule back
Fitting male SST
Capillary

20 1100 Series FD Reference Manual
1Installing the Fluorescence Detector
Optimizing the Stack Configuration
If your detector is part of a complete Agilent 1100 Series system, you can
ensure optimum performance by installing the following configuration. This
configuration optimizes the system flow path, ensuring minimum delay
volume.
Figure 3 Recommended Stack Configuration (Front View)
Solvent cabinet
Vacuum degasser
Pump
Column compartment
Autosampler
Detector
Control module