Agilent Technologies 1100 Series User manual

A
Agilent 1100 Series
Fluorescence Detector
Reference Manual

2 1100 Series FD Reference Manual
Notices
© Agilent Technologies, Inc. 1998, 1999-
2004
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Manual Part Number
G1321-90003
Edition
Edition 05/2004
Printed in Germany
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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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A CAUTION notice denotes a
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A WARNING notice denotes a
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WARNING
notice until the indicated
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and met.

1100 Series FD Reference Manual 3
I 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
3Optimizing 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.
4Troubleshooting and Test Functions
This chapter describes the detector’s built in troubleshooting and test
functions.
5Repairing the Fluorescence Detector
Instructions on how to repair the detector
6Identifying Parts and Materials
Detailed illustrations and listings for parts and materials identification
for the detector
7Introduction to the Fluorescence Detector
An introduction to the detector
8Therory of Operation

4 1100 Series FD Reference Manual
Instrument overview, theory of operation, external communication and
internal connectors
9Introduction 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
1Installing 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 23
Flow Connections to the Detector 26
2First Steps with the Fluorescence Detector
Before You Start 32
Optimization Overview 33
Getting Started and Checkout 35
Starting Your Detector 35
Setting the Chromatographic Conditions 36
Observe the maxima via the isoabsorbance plot 38
Method Development 39
Step 1: Check the LC system for impurities 40
Step 2: Optimize limits of detection and selectivity 41
Step 3: Set up routine methods 51
Example: Optimization for Multiple Compounds 55

6 1100 Series FD Reference Manual
3Optimizing the Fluorescence Detector
Optimization Overview 64
Design Features Help Optimization 65
Check Performance Before You Start 65
Finding the Best Wavelengths 66
A Real Example 67
Finding the Best Signal Amplification 68
Changing the Xenon Flash Lamp Frequency 70
Lamp life savings 71
Selecting the Best Response Time 72
Reducing Stray Light 74
4Troubleshooting and Test Functions
Oerie of the Detetor’s Idiators ad Test Futios
78
Status Indicators 79
Power Supply Indicator 79
Detector Status Indicator 80
Error Messages 81
Time-out 82
Shutdown 83
Remote Time-out 84
Synchronization Lost 85
Leak 86
Leak Sensor Open 88

1100 Series FD Reference Manual 7
Leak Sensor Short 89
Compensation Sensor
Open
90
Compensation Sensor
Short
91
Fan Failed 92
Motor Errors 93
Lamp Cover Open 95
FLF Board not found 96
ADC Not Calibrated97
A/D Overflow 98
Flash Lamp Current Overflow 99
Flash Trigger Lost 100
Wavelength Calibration Failed 101
Wavelength Calibration Lost 102
Flow Cell Removed 103 No
Peaks 104
Wavelength Verification and Calibration 105
Check of Raman Band of Water 108
The Wavelength Calibration Procedure 114
Preparation of the Glycogen Calibration Sample 114
Preparation of the Flow Cell 115
Wavelength Calibration 116
Verification 117
Test Functions118
Lamp Intensity Test 119
Lamp Intensity History 120

8 1100 Series FD Reference Manual
Dark-Current Test 121
Excitation and Emission Grating Resistance History 122
Raman ASTM Signal-to-Noise Test 123
Using the Built-in Test Chromatogram 126
Using the Built-in DAC Test 129
5Repairing the Fluorescence Detector
Introduction into Repairing the Fluorescence Detector 132
Overview of the Repairing of the Fluorescence Detector
135
Simple Repairs 136
Exchanging a Flow Cell 137
How to use the Cuvette 140
Flow Cell Flushing 141
Correcting Leaks 142
Replacing Leak Handling System Parts 143
Exchanging Internal Parts 144
Removing the Covers 146
Removing the Rear Foam 148
Exchanging the Lamp 149
Exchanging the EX-condenser 154
Replacing the Lamp Cover Window 157
Exchanging the Processor Board 160
Exchanging the Fan 164
Exchanging the Leak Sensor or Leak Panel 166

1100 Series FD Reference Manual 9
Replacing the EM-Condenser or Cutoff-Filter 169
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
Replaig the Detetor’s Firare 200
6Identifying Parts and Materials
Overview of Main Assemblies 202
Optical Unit Assembly 204
Lamp Cover Parts 207
Control Module 208
Sheet Metal Kit 209
Plastic Parts 210
Foam Parts 211

10 1100 Series FD Reference Manual
Power and Status Light
Pipes
Leak Parts 213
Cuvette Kit 214
Spare Parts 215
Accessory Kit 216
Cable Overview 218
Analog Cables 220
Remote Cables
223
BCD Cables 230
Auxiliary Cable
232
CAN Cable 233
212
External Contact Cable
RS-232 Cable Kit 235
LAN Cables 236
234
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

1100 Series FD Reference Manual 11
Phosphorescence Detection 252 Processing
of Raw Data 253
Electrical Connections 256
Instrument Layout 258
Early Maintenance Feedback (EMF) 259
EMF Counters 259
Using the EMF Counters261
8Theory of Operation
Electronics 264
Detector Main Board (FLM) 265
Detector Frontend Board (FLF) 269
FLF Board revisions 273
How to retrieve the FLF board revision 274
Detector Lamp Supply Board (FLL) 275
Firmware Description 276
Firmware Updates 277
Raw Data Conversion to Fluorescence (LU) Units 278
Data flow for chromatographic output 279
Data flow for spectral output 280
Spectra Acquisition Modes 283
Optional Interface Boards 284
BCD Board 284
LAN Communication Interface Board 286
Interfaces 287

12 1100 Series FD Reference Manual
Analog Signal Output 288
GPIB Interface 288
CAN Interface 288
Remote Interface 289 RS-
232C 290
Setting the 8-bit Configuration Switch 292
GPIB Default Addresses 293
Communication Settings for RS-232C Communication 294
Forced Cold Start Settings 295 Stay-
Resident Settings 296
The Main Power Supply Assembly 297
9Introduction to the Control Module
Major keys on the Agilent 1100 Control Module 300
Screens available from the Analysis screen 301
Screens available from the System screen 317
Screens available from the Records screen 320
Diagnostics and Tests 325
10 Specifications
Performance Specifications 330
A Safety Information
General Safety Information 334
Lithium Batteries Information 337

1100 Series FD Reference Manual 13
Radio Interference 338
Sound Emission 339
UV-Radiation (UV-lamps only) 340
Solvent Information 341
Agilent Technologies on Internet 343
Index

12 1100 Series FD Reference Manual Agilent 1100 Series
Fluorescence Detector Reference Manual
1
Installing the Fluorescence Detector
Site Requirements 14
Physical Specifications 16
Unpacking the Detector 17
Optimizing the Stack Configuration 20
Installing the Detector 23
Flow Connections to the Detector
26

15
Agilent Technologies
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.
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.
Shock hazard or damage of your instrumentation can result, if the devices are connected to a line
voltage higher than specified.
Make sure to have easy access to the power cable of the instrument, in order to disconnect the
instrument from line.
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
WARNING
CAUTION

1 Installing the Fluorescence Detector
16 1100 Series FD Reference Manual
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.
Never use cables other than the ones supplied by Agilent Technologies to ensure proper
functionality and compliance with safety or EMC regulations.
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 330) 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.
Do not store, ship or use your detector under conditions where temperature
fluctuations could cause condensation within the detector. Condensation will damage the system
WARNING
WARNING
CAUTION

Installing the Fluorescence Detector 1
1100 Series FD Reference Manual 17
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.
Physical Specifications
Table 1 Physical Specifications
Type
Specification
Comments
Weight
11.5 kg (26 lbs)
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

1 Installing the Fluorescence Detector
18 1100 Series FD Reference Manual
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.
If there are signs of damage, please do not attempt to install the detector.
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.
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
CAUTION

Installing the Fluorescence Detector 1
1100 Series FD Reference Manual 19
Accessory kit (see Table 3 on page 18)
1
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

1 Installing the Fluorescence Detector
20 1100 Series FD Reference Manual
ESD wrist strap
9300-1408
1
Figure 1 Waste Tubing Parts
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.
Fitting male PEEK
Tubing
Figure 2
Inlet Capillary (Col
umn-Detector) Parts
Ferrule front
This side is
preinstalled
Ferrule back
Fitting male SST
Capillary