Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual A
Notices © Agilent Technologies, Inc. 1995, 1996-2004 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.
In This Guide… This manual contains information for using your Diode Array and Multiple Wavelength Detectors.
1100 Series DAD and MWD Reference Manual
Contents 1 Installing the Detector Site Requirements 14 Physical Specifications 16 Unpacking the Detector 17 Damaged Packaging 17 Delivery Checklist 17 Optimizing the Stack Configuration Installing the Detector 22 Flow Connections to the Detector 2 20 25 How to optmize the Detector Optimizing the Detector Performance Optimization Overview 30 31 Optimizing for Sensitivity, Selectivity, Linearity and Dispersion Flow Cell Path Length 33 Peak width (response time) 35 Sample and Reference Wavelength
3 Troubleshooting and Test Functions Overview of the Detector’s Indicators and Test Functions 50 Status Indicators 51 Power Supply Indicator 51 Detector Status Indicator 51 Error Messages 53 Timeout 54 Shutdown 55 Remote Timeout 56 Synchronization Lost 57 Leak 58 Leak Sensor Open 60 Leak Sensor Short 61 Compensation Sensor Open 62 Compensation Sensor Short 63 Fan Failed 64 Open Cover 65 Cover Violation 66 Visible Lamp Current 67 Visible Lamp Voltage 68 Communication Error 69 Calibration Values Invalid 70
Illegal Value From „Air Inlet" Temperature Sensor Heater Failed 82 Heater Power At Limit 83 Wavelength Recalibration 81 84 Test Functions 85 Holmium Oxide Test 86 Intensity Test 88 Cell Test 90 Dark-Current Test 91 Filter Test 93 4 Repairing the Detector Introduction into Repairing the Detector Using the ESD Strap 98 Overview of the Repairing of the Detector 96 99 Simple Repairs 101 Exchanging a Lamp 102 Exchanging a Flow Cell 105 Repairing the Standard or Semi-Micro Flow Cell 108 Repairing the High P
Exchanging the Detector Main Board 143 Entering the Serial Number using the Control Module 146 Entering the Serial Number using the Agilent ChemStation 147 Exchanging the Fan (G1315A/G1365A) 148 Replacing Fan Parts (G1315B/G1365B) 150 Removing the Optical Unit (G1315A/G1365A) 154 Removing the Optical Unit (G1315B/G1365B) 156 Exchanging the Source Lens (Achromat) Assembly 158 Replacing the Holmium Oxide Filter Motor 162 Exchanging the Power Supply 164 Exchanging the Leak Sensor 167 Replacing Status Light Pip
Source Lens (Achromat) Assembly Cell Support Assembly Control Module 200 201 Sheet Metal Kit (G1315A/G1365A) 202 Sheet Metal Kit (G1315B/G1365B) 203 Plastic Parts Foam Parts 204 205 Power and Status Light Pipes Leak Parts 208 Cable Overview 210 Analog Cables 212 Remote Cables 215 BCD Cables 220 Auxiliary Cable 222 CAN Cable 223 External Contact Cable RS-232 Cable Kit LAN Cables 206 207 Accessory Kit 6 199 224 225 226 Introduction to the Detector Introduction to the Detector Optical Syste
Using the EMF Counters Electronics 235 237 Detector Main Board (DAM/MWM) Firmware Description Firmware Updates 238 246 247 Raw Data Conversion to Absorbance 248 Rawdata File 251 Peak Detector 251 Spectra Acquisition Modes (DAD only) 252 Optional Interface Boards 253 BCD Board 253 LAN Communication Interface Board 255 Interfaces 256 Analog Signal Output 257 GPIB Interface 257 CAN Interface 257 Remote Interface 257 RS-232C 259 Setting the 8-bit Configuration Switch 261 GPIB Default Addresses 262 Commu
Screens available from the System screen 282 Screens available from the Records screen 284 Diagnostics and Tests 8 290 Specifications Performance Specifications A 296 Safety Information General Safety Information 300 Lithium Batteries Information 303 Disposal of Mercury from Deuterium Lamp Radio Interference Sound Emission UV-Radiation 304 305 306 307 Solvent Information 308 Declaration of Conformity for HOX2 Filter Agilent Technologies on Internet 310 311 Index 1100 Series DAD and MW
1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 1 Installing the 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 25 Agilent Technologies 13
1 Installing the 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. 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.
Installing the Detector 1 WA R N I N G 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. WA R N I N G Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
1 Installing the Detector Physical Specifications Table 1 Physical Specifications Type Specification 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, Line frequency 50 or 60 Hz ± 5 % Power consumption (G1315/65B) 300 VA / 125 W / 427 BTU Maximum Ambient operating temperature 0 – 55 °C (32 – 131 °F) .
Installing the Detector 1 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. CAUTION 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.
1 Installing the Detector Detector Accessory Kit Contents Table 3 Accessory Kit Contents (Part Number G1315-68705) Description Part Number Quantity Teflon Tubing flexible i.d. 0.8 mm (flow cell to waste), re-order 5 m 5062-2462 2m Corrugated tubing (to waste), re-order 5 m 5062-2463 1.2 m Fitting male PEEK 0100-1516 2 Capillary column-detector 380 mm lg, 0.17 mm i.d.
Installing the Detector 1 Ferrule front This side is preinstalled Ferrule back Fitting male SST Capillary Figure 2 Inlet Capillary (Column-Detector) Parts 1100 Series DAD and MWD Reference Manual 19
1 Installing the 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.
Installing the Detector 1 Remote cable CAN Bus cable CAN Bus cable AC power Analog signal to recorder GPIB or LAN to LC ChemStation Figure 4 Recommended Stack Configuration (Rear View) 1100 Series DAD and MWD Reference Manual 21
1 Installing the Detector Installing the Detector Preparations Locate bench space Provide power connections Unpack the detector Parts required Detector Power cord, for other cables see below and “Cable Overview” on page 210 ChemStation and/or Control Module G1323A/B 1 Install the LAN interface board in the detector (if required), see “Replacing the Interface Board” on page 179. 2 Place the detector in the stack or on the bench in a horizontal position.
Installing the Detector 1 Status indicator green/yellow/red Line power switch with green light Figure 5 Front View of Detector 4 Connect the power cable to the power connector at the rear of the detector. 5 Connect the CAN cable to other Agilent 1100 Series modules. 6 If a Agilent ChemStation is the controller, connect either • the GPIB cable to the detector or • the LAN connection to the LAN interface board in the detector.
1 Installing the Detector Security lever Interface board Analog signal APG remote RS-232C CAN GPIB Power Configuration switch Figure 6 24 Rear View of Detector NOTE The detector is turned on when the line power switch is pressed and the green indicator lamp is illuminated. The detector is turned off when the line power switch is protruding and the green light is off. WA R N I N G To disconnect the detector from line, unplug the power cord.
Installing the Detector 1 Flow Connections to the Detector WA R N I N G NOTE Preparations Detector is installed in the LC system. Parts required Other modules Parts from accessory kit, see“Detector Accessory Kit Contents” on page 18.
1 Installing the Detector 1 Press the release buttons and remove the front cover to gain access to the flow cell area. 2 Press the release button and open the flow cell door. 3 Insert the flow cell and install the capillaries to the capillary holder (top is inlet, bottom is outlet). 4 If another Agilent 1100 Series module is positioned on top of the detector, route the tubing assembly waste from the accessory kit behind the capillary holder and connect the top end to the other module’s waste outlet.
Installing the Detector 5 Assemble the column-detector capillary from the accessory kit. One side is already factory-assembled 1 6 Connect the newly assembled fitting of the capillary to the top fitting holder and the other end to the column. Pre-assembled 7 Assemble the waste tubing from the accessory kit. 1100 Series DAD and MWD Reference Manual 8 Connect the waste tubing to the bottom fitting holder and a waste tubing to the leak outlet.
1 Installing the Detector 9 Remove the flow cell and establish a flow and observe for leaks. 10 Insert the flow cell, close the cover and replace the front cover. The installation of the detector is now complete. NOTE The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the ouside and to cover the deuterium lamp. Some types of the Agilent deuterium lamps show a light ring during operation.
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 2 How to optmize the Detector Optimizing the Detector Performance 30 Optimization Overview 31 Optimizing for Sensitivity, Selectivity, Linearity and Dispersion 33 Optimizing Selectivity 44 Agilent Technologies 29
2 How to optmize the Detector Optimizing the Detector Performance The detector has a variety of parameters that can be used to optimize performance. Depending on whether signal or spectral data need to be optimized, different settings are recommended. The following sections describe optimization for: • signal sensitivity, selectivity and linearity, • spectral sensitivity and resolution (DAD only), and • disk space required for storing data.
How to optmize the Detector 2 Optimization Overview Table 4 Optimization Overview Parameter Impact 1 Selection of flow cell • Choose flow cell according to used column, see Figure 7. • peak resolution versus sensitivity 2 Connection of flow cell • For flow rates from 0.5 ml/min connect column using the zero-dead-volume fittings of the detector. • For small column i.d. (e.g 1 mm) the inlet capillary of the micro flow cell can be connected directly to the column.
2 How to optmize the Detector Table 4 Optimization Overview, continued Parameter Impact 5 Setting the slit width • Use 4 nm slit for normal applications. • Use narrow slit (e.g 1 nm) if your analytes have narrow absorbance bands and for high concentrations. • Use a wide slit (e.g. 16 nm) to detect very low concentrations. • spectral resolution, sensitivity and linearity.
How to optmize the Detector 2 Optimizing for Sensitivity, Selectivity, Linearity and Dispersion Flow Cell Path Length Lambert-Beer’s law shows a linear relationship between the flow cell path length and absorbance.
2 How to optmize the Detector Analysis of pesticide standard Absorbance 6-mm optical path length 10-mm optical path length Time (min) Figure 8 Influence of Cell Path Length on Signal Height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards. To check photometric accuracy of the Agilent 1100 DAD/MWD it is necessary to have more precise information on path lengths of the flow cells.
How to optmize the Detector 2 Peak width (response time) Response time describes how fast the detector signal follows a sudden change of absorbance in the flow cell. The detector uses digital filters to adapt response time to the width of the peaks in your chromatogram. These filters do not affect peak area nor peak symmetry. When set correctly, such filters reduce baseline noise significantly (see Figure 9), but reduce peak height only slightly.
2 How to optmize the Detector Table 6 Peak Width — Response Time — Data Rate Peak Width Response Time Data Rate 0.01 min 0.2 s 20 Hz 0.02 min 0.5 s 10 Hz 0.05 min 1.0 s 5 Hz 0.10 min 2.0 s 2.5 Hz 0.20 min 4.0 s 1.25 Hz 0.40 min 8.0 s 0.6 Hz 0.80 min 16.0 s 0.3 Hz Sample and Reference Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 to 950 nm. Two lamps provide good sensitivity over the whole wavelength range.
How to optmize the Detector 2 Signal A in the detector default method is set to sample 250,100, reference 360,100, that is, the average absorbance from 200 – 300 nm minus the average absorbance from 300 – 400 nm. As all analytes show higher absorbance at 200 – 300 nm than at 300 – 400 nm, this signal will show you virtually every compound which can be detected by UV absorbance. Many compounds show absorbance bands in the spectrum. Figure 10 shows the spectrum of anisic acid as an example.
2 How to optmize the Detector A wide bandwidth has the advantage of reducing noise by averaging over a wavelength range — compared to a 4 nm bandwidth, the baseline noise is reduced by a factor of approximately 2.5, whereas the signal is about 75 % of a 4-nm wide band. The signal-to-noise ratio for a 30 nm bandwidth is twice that for a 4-nm bandwidth in our example.
PTH-PHE PTH-PRO PTH-ARG PTH-ALA PTH-ASN How to optmize the Detector 2 1 pmol each Wavelength 267 nm Reference 380 nm Wavelength 267 nm No reference Time (min) Grad.: 0.02 m KH2PO4/ACN from 12% ACN to 45% ACN in 12 min Figure 12 Gradient Analysis of PTH-Amino Acids (1 pmol each), with and without Reference Slit Width The detector has a variable slit at the entrance of the spectrograph. This is an effective tool to adapt the detector to changing demand of different analytical problems.
2 How to optmize the Detector 16 nm 4 nm 1 nm Figure 13 Benzene at 1, 4 and 16 nm slit width A wide slit uses more of the light shining through the flow cell. This gives lower baseline noise as shown in Figure 14. Slit width 1 nm Slit width 4 nm Slit width 16 nm Figure 14 Influence of the Slit Width on Baseline Noise However, with a wider slit, the spectrograph’s optical resolution (its ability to distinguish between different wavelengths) diminishes.
How to optmize the Detector 2 Furthermore, the absorbance is no longer strictly linear with concentration for wavelengths at a steep slope of a compound’s spectrum. Substances with fine structures and steep slopes like benzene are very rare. In most cases the width of absorbance bands in the spectrum is more like 30 nm as with anisic acid (see Figure 10). In most situations, a slit width of 4 nm will give the best results.
2 How to optmize the Detector Optimizing Spectral Acquisition (DAD only) Storage of all spectra consumes a lot of disk space. It is very useful to have all spectra available during optimization of a method or when analyzing unique samples. However when running many samples of the same type, the large size of data files with all spectra may become a burden. The detector provides functions to reduce the amount of data, yet retaining the relevant spectral information.
How to optmize the Detector 2 Threshold Sets the peak detector. Only spectra from peaks higher than threshold will be stored when a peak-controlled storage mode is selected. Margin for Negative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative (about -100 mAU). In some special case, for example, when gradient with absorbing solvents are used, the baseline may drift to more negative values.
2 How to optmize the Detector Optimizing Selectivity Quantifying Coeluting Peaks by Peak Suppression In chromatography, two compounds may often elute together. A conventional dual-signal detector can only detect and quantify both compounds independently from each other if their spectra do not overlap. However, in most cases this is highly unlikely.
How to optmize the Detector 2 WL1 (204 nm, caffeine) WL2 (222 nm, hydrochlorothiazide WL3 (260 nm, reference to suppress hydrochlorothiazide WL4 (282 nm, reference to suppress caffeine WL3 WL1 WL4 WL2 Wavelength (nm) Figure 15 Wavelength Selection for Peak Suppression With a UV-visible detector based on a diode array and the correct choice of a reference wavelength setting, quantitative detection is possible. To suppress caffeine, the reference wavelength must be set to 282 nm.
2 How to optmize the Detector Figure 16 Hydrochlorothiazide and caffeine Wavelength 204 nm No reference Hydrochlorothiazide and caffeine Wavelength 222 nm No reference Hydrochlorothiazide suppressed Wavelength 204 nm Reference 260 nm Caffeine suppressed Time (min) Time (min) Wavelength 222 nm Reference 282 nm Peak Suppression Using Reference Wavelength Ratio Qualifiers for Selective Detection of Compound Classes Ratio qualifiers can be used where, in a complex sample, only one particular class ne
How to optmize the Detector 2 Select 2 characteristic wavelengths Signal = WL1/WL2 20% Scaled o-Terphenyl Biphenyl WL2 WL1 Wavelength (nm) Figure 17 Wavelength Selection for Ratio Qualifiers Signals at 250 nm Biphenyl o-Terphenyl No selectivity With ratio qualifier 250/222 nm = 3.5 20% Time (min) Figure 18 Selectivity by Ratio Qualifiers In a four-component mixture, only biphenyl was recorded.
2 How to optmize the Detector The ratio range was set at 2 – 2.4 (2.2 ±10%). Only when the ratio between 249 and 224 nm was within this range, is the signal plotted. Of all four peaks, only the third fulfilled the criterion (Figure 18). The others were not plotted.
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 3 Troubleshooting and Test Functions Overview of the Detector’s Indicators and Test Functions 50 Status Indicators 51 Error Messages 53 Wavelength Recalibration 84 Test Functions 85 This chapter describes the detector’s built in troubleshooting and test functions.
3 Troubleshooting and Test Functions Overview of the Detector’s Indicators and Test Functions Status Indicators The detector is provided with two status indicators which indicate the operational state (prerun, run, and error states) of the detector. The status indicators provide a quick visual check of the operation of the detector (see page 51). Error Messages In the event of an electronic, mechanical or hydraulic failure, the detector generates an error message in the user interface.
Troubleshooting and Test Functions 3 Status Indicators Two status indicators are located on the front of the detector. The lower left indicates the power supply status, the upper right indicates the detector status. Status indicator green/yellow/red Line power switch with green light Figure 19 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch. When the indicator is illuminated (green) the power is ON.
3 Troubleshooting and Test Functions • When the status indicator is OFF (and power switch light is on), the detector is in a prerun condition, and is ready to begin an analysis. • A green status indicator, indicates the detector is performing an analysis (run mode). • A yellow indicator indicates a not-ready condition.
Troubleshooting and Test Functions 3 Error Messages Error messages are displayed in the user interface when an electronic, mechanical, or hydraulic (flow path) failure occurs which requires attention before the analysis can be continued (for example, repair, or exchange of consumables is necessary). In the event of such a failure, the red status indicator at the front of the detector is switched on, and an entry is written into the detector logbook.
3 Troubleshooting and Test Functions Timeout The timeout threshold was exceeded. Probable Causes • The analysis was completed successfully, and the timeout function switched off the pump as requested. • A not-ready state was present during a sequence or multiple-injection run for a period longer than the timeout threshold. Suggested Actions ✔ Check the logbook for the occurrence and source of a not-ready condition. Restart the analysis where required.
Troubleshooting and Test Functions 3 Shutdown An external instrument has generated a shut-down signal (through CAN or REMOTE lines). The detector continually monitors the remote input connectors for status signals. A LOW signal input on pin 4 of the remote connector generates the error message. Probable Causes • Leak detected in an external instrument with a remote connection to the system. • Shut-down in an external instrument with a remote connection to the system.
3 Troubleshooting and Test Functions Remote Timeout A not-ready condition is still present on the remote input. When an analysis is started, the system expects all not-ready conditions (e.g. a not-ready condition during detector balance) to switch to run conditions within one minute of starting the analysis. If a not-ready condition is still present on the remote line after one minute the error message is generated.
Troubleshooting and Test Functions 3 Synchronization Lost During an analysis, the internal synchronization or communication between one or more of the modules in the system has failed. The system processors continually monitor the system configuration. If one or more of the modules is no longer recognized as being connected to the system, the error message is generated. Probable Causes • CAN cable disconnected. • Defective CAN cable. • Defective main board in another module.
3 Troubleshooting and Test Functions Leak A leak was detected in the detector. The signals from the two temperature sensors (leak sensor and board-mounted temperature-compensation sensor) are used by the leak algorithm to determine whether a leak is present. When a leak occurs, the leak sensor is cooled by the solvent. This changes the resistance of the leak sensor which is sensed by the leak-sensor circuit on the detector main board. Probable Causes • Loose fittings. • Broken capillary.
Troubleshooting and Test Functions 3 to port# 4 of the sampler switching valve. This tube can then be taken to waste separately. The tube which normally serves as the detector cell outlet tube can be used for this purpose.
3 Troubleshooting and Test Functions Leak Sensor Open The leak sensor in the detector has failed (open circuit). The current through the leak sensor is dependent on temperature. A leak is detected when solvent cools the leak sensor, causing the leak sensor current to change within defined limits. If the current falls outside the lower limit, the error message is generated. Probable Causes • Leak sensor not connected to the detector main board. • Defective leak sensor.
Troubleshooting and Test Functions 3 Leak Sensor Short The leak sensor in the detector has failed (short circuit). The current through the leak sensor is dependent on temperature. A leak is detected when solvent cools the leak sensor, causing the leak sensor current to change within defined limits. If the current increases above the upper limit, the error message is generated. Probable Causes • Defective leak sensor. Suggested Actions ✔ Exchange the leak sensor.
3 Troubleshooting and Test Functions Compensation Sensor Open The ambient-compensation sensor (NTC) on the detector main board in the detector has failed (open circuit). The resistance across the temperature compensation sensor (NTC) on the detector main board is dependent on ambient temperature. The change in resistance is used by the leak circuit to compensate for ambient temperature changes. If the resistance across the sensor increases above the upper limit, the error message is generated.
Troubleshooting and Test Functions 3 Compensation Sensor Short The ambient-compensation sensor (NTC) on the detector main board in the detector has failed (short circuit). The resistance across the temperature compensation sensor (NTC) on the detector main board is dependent on ambient temperature. The change in resistance is used by the leak circuit to compensate for ambient temperature changes. If the resistance across the sensor falls below the lower limit, the error message is generated.
3 Troubleshooting and Test Functions Fan Failed The cooling fan in the detector has failed. The hall sensor on the fan shaft is used by the detector main board to monitor the fan speed. If the fan speed falls below two revolutions/second for more than five seconds, the error message is generated. Probable Causes • Fan cable disconnected. • Defective fan. • Defective detector main board. Suggested Actions ✔ Ensure the fan is connected correctly. ✔ Exchange fan. ✔ Exchange the detector main board.
Troubleshooting and Test Functions 3 Open Cover The top foam has been removed. The sensor on the detector main board detects when the top foam is in place. If the foam is removed, the fan is switched off, and the error message is generated. Probable Causes • The top foam was removed during operation. • Foam not activating the sensor. Suggested Actions ✔ Replace the top foam. ✔ Exchange the foam.
3 Troubleshooting and Test Functions Cover Violation The top foam has been removed. The sensor on the detector main board detects when the top foam is in place. If the foam is removed while the lamps are on (or if an attempt is made to switch on the lamps with the foam removed), the lamps are switched off, and the error message is generated. Probable Causes • The top foam was removed during operation. • Foam not activating the sensor. Suggested Actions ✔ Replace the top foam. ✔ Exchange the foam.
Troubleshooting and Test Functions 3 Visible Lamp Current The visible lamp current is missing. The processor continually monitors the lamp current during operation. If the current falls below the lower current limit, the error message is generated. Probable Causes • Visible lamp disconnected. • Defective visible lamp. • Defective detector main board. • Defective power supply. Suggested Actions ✔ Ensure the visible lamp connector is seated firmly. ✔ Exchange the visible lamp.
3 Troubleshooting and Test Functions Visible Lamp Voltage The visible lamp voltage is missing. The processor continually monitors the voltage across the lamp during operation. If the lamp voltage falls below the lower limit, the error message is generated. Probable Causes • Defective detector main board. • Defective power supply. Suggested Actions ✔ Exchange the detector main board. ✔ Exchange the power supply.
Troubleshooting and Test Functions 3 Communication Error An internal communication error between the main processor and the digital-signal processor has occurred. Probable Causes • Random communication error. • Defective detector main board. Suggested Actions ✔ Switch the detector off and on again at the power switch. If the error reoccurs, exchange the detector main board.
3 Troubleshooting and Test Functions Calibration Values Invalid The calibration values read from the spectrometer ROM are invalid. After recalibration, the calibration values are stored in ROM. The processor periodically checks if the calibration data are valid. If the data are invalid or cannot be read from the spectrometer ROM, the error message is generated. Probable Causes • Defective detector main board. • Defective optical unit. Suggested Actions ✔ Exchange the detector main board.
Troubleshooting and Test Functions 3 Diode Current Leakage When the detector is switched on, the processor checks the leakage current of each of the optical diodes. If the leakage current exceeds the upper limit, the error message is generated. Probable Causes • Defective optical unit. • Defective detector main board. Suggested Actions ✔ Exchange the optical unit. ✔ Defective detector main board.
3 Troubleshooting and Test Functions Holmium Oxide Test Failed The holmium oxide test in the detector has failed. During the holmium test, the detector moves the holmium filter through the light path while monitoring the detector signal response. As the edge of the filter passes through the light path, the signal is interrupted. This is used to determine the position of the filter, and whether the filter is moving correctly. If the filter fails to move, the error message is generated.
Troubleshooting and Test Functions 3 UV Lamp Current The UV lamp current is missing. The processor continually monitors the anode current drawn by the lamp during operation. If the anode current falls below the lower current limit, the error message is generated. Probable Causes • UV lamp disconnected. • Defective UV lamp or non-Agilent lamp. • Defective detector main board. • Defective power supply. Suggested Actions ✔ Ensure the UV lamp connector is seated firmly. ✔ Exchange the UV lamp.
3 Troubleshooting and Test Functions UV Lamp Voltage The UV lamp anode voltage is missing. The processor continually monitors the anode voltage across the lamp during operation. If the anode voltage falls below the lower limit, the error message is generated. Probable Causes • Defective UV lamp or non-Agilent lamp. • Defective detector main board. • Defective power supply. Suggested Actions ✔ Exchange the UV lamp. ✔ Exchange the detector main board. ✔ Exchange the power supply.
Troubleshooting and Test Functions 3 UV Ignition Failed The UV lamp failed to ignite. The processor monitors the UV lamp current during the ignition cycle. If the lamp current does not rise above the lower limit within 2 – 5 seconds, the error message is generated. Probable Causes • Lamp not connected. • Defective UV lamp or non-Agilent lamp. • Defective detector main board. • Defective power supply. Suggested Actions ✔ Ensure the lamp is connected. ✔ Exchange the UV lamp.
3 Troubleshooting and Test Functions UV Heater Current The UV lamp heater current is missing. During UV lamp ignition, the processor monitors the heater current. If the current does not rise above the lower limit within one second, the error message is generated. Probable Causes • UV Lamp not connected. • Ignition started without the top foam in place. • Defective UV lamp or non-Agilent lamp. • Defective detector main board. • Defective power supply. Suggested Actions ✔ Ensure the UV lamp is connected.
Troubleshooting and Test Functions 3 New Messages with the G1315B and G1365B detectors With the introduction of the G1315B DAD and the G1365B MWD a few new messages have been added to address the additional heating control for stabilization of the baseline in unstable environment.
3 Troubleshooting and Test Functions Module Type Changed At switch-on, the detector has recognized a new configuration. Only G1315B and G1365B detectors have built-in hardware for temperature control. The type of the module changed from A to B or vice versa because the hardware for the temperature control was either detected or not detected.
Troubleshooting and Test Functions 3 Type B, Parameter 1 or 3 Probable Causes • Detector has recognized the hardware for temperature control. This is because the detector didn't find the temperature hardware at last switch-on. Suggested Actions ✔ Power cycle the detector.
3 Troubleshooting and Test Functions Illegal Value From Temperature Sensor Mounted On The Fan Assembly This temperature sensor delivered a value outside the allowed range. The parameter of this event equals the measured temperature in 1/100 centigrade. As a result the temperature control is switched off. Probable Causes • The sensor is defect • Detector is exposed to illegal ambient conditions. Suggested Actions ✔ Ensure the connector to the detector main board is seated firmly.
Troubleshooting and Test Functions 3 Illegal Value From „Air Inlet" Temperature Sensor This temperature sensor (located on the detector main board) delivered a value outside the allowed range. The parameter of this event equals the measured temperature in 1/100 centigrade. As a result the temperature control is switched off. Probable Causes • The sensor is defect • Detector is exposed to illegal ambient conditions. Suggested Actions ✔ Verify that the ambient conditions are within the allowed range.
3 Troubleshooting and Test Functions Heater Failed Every time the deuterium lamp or the tungsten lamp is switched on or off a heater self-test is performed. If the test fails an error event is created. As a result the temperature control is switched off. Probable Causes • Defective connector or cable. • Defective heater. Suggested Actions ✔ Ensure the connector to the detector main board is seated firmly. ✔ Exchange heater assembly.
Troubleshooting and Test Functions 3 Heater Power At Limit The available power of the heater reached either the upper or lower limit. This event is sent only once per run. The parameter determines which limit has been hit: 0 means upper power limit hit (excessive ambient temperature drop). 1 means lower power limit hit (excessive ambient temperature increase). Probable Causes • Ambient conditions have changed too much during the run, so that optimum results may not be guaranteed.
3 Troubleshooting and Test Functions Wavelength Recalibration The detector uses the alpha (656.1 nm) and beta (486 nm) emission lines of the deuterium lamp for wavelength calibration. The sharp emission lines enable more accurate calibration than is possible with holmium oxide. When calibration is started, the 1-nm slit is moved into the light path automatically, and the gain is set to zero. To eliminate effects due to absorbing solvents, the test should be done with water in the flow cell.
Troubleshooting and Test Functions 3 Test Functions Holmium Oxide Test The built-in holmium oxide filter is used for verification of wavelength accuracy at three additional wavelengths. The test evaluates the results automatically, and provides a spectrum of the holmium oxide filter. Intensity Test The intensity test checks the lamp intensities (UV and visible lamps) over the complete spectral range. The test evaluates the results automatically, and provides an intensity spectrum.
3 Troubleshooting and Test Functions Holmium Oxide Test The holmium oxide test uses three characteristic absorbance maxima of the built-in holmium oxide filter to verify wavelength accuracy (see also “Wavelength Recalibration” on page 84). When the test is started, the 1-nm slit is moved into the light path automatically. To eliminate effects due to absorbing solvents, the test should be done with water in the flow cell.
Troubleshooting and Test Functions Figure 22 3 Holmium Oxide Test Results Test Failed Probable Causes • Absorbing solvent or air bubble in flow cell. • Incorrect calibration • Dirty or contaminated flow cell. • Dirty or contaminated optical components (achromat, windows). • Old or non-Agilent lamp. Suggested Actions ✔ Ensure the flow cell is filled with water. ✔ Recalibrate (see “Wavelength Recalibration” on page 84) and repeat the test. ✔ Run the cell test (see “Cell Test” on page 90).
3 Troubleshooting and Test Functions Intensity Test NOTE The test ist for the standard flow cells (10 mm and 6 mm pathlength) only. The nano-flow cells (80 nl and 500 nl) cannot be run with this test due to its low volume. The intensity test measures the intensity of the deuterium and tungsten lamps over the full wavelength range (190 – 950 nm). Four spectral ranges are used to evaluate the intensity spectrum.
Troubleshooting and Test Functions 3 Intensity Test Evaluation The Aligent ChemStation evaluates four spectral ranges automatically, and displays the limits for each range, the measured intensity counts, and passed or failed for each spectral range (see Figure 24). Figure 24 Intensity Test Results Test Failed Probable Causes • Absorbing solvent or air bubble in flow cell. • Dirty or contaminated flow cell. • Dirty or contaminated optical components (achromat, windows). • Old or non-Agilent lamp.
3 Troubleshooting and Test Functions Cell Test The cell test measures the intensity of the deuterium and tungsten lamps over the full wavelength range (190 – 950 nm), once with the flow cell installed, and once with the flow cell removed. The resulting intensity ratio is a measure of the amount of light absorbed by the flow cell. The test can be used to check for dirty or contaminated flow cell windows.
Troubleshooting and Test Functions 3 Dark-Current Test The dark-current test measures the leakage current from each diode. The test is used to check for leaking diodes which may cause non-linearity at specific wavelengths. During the test, the slit assembly moves to the dark position, cutting off all light falling onto the diode array. Next, the leakage current from each diode is measured, and displayed graphically (see Figure 26).
3 Troubleshooting and Test Functions Test Failed Probable Causes • Defective optical unit. Suggested Actions ✔ Exchange the optical unit.
Troubleshooting and Test Functions 3 Filter Test The filter test checks the correct operation of the filter assembly. When the test is started, the holmium oxide filter is moved into position. During filter movement, the absorbance signal is monitored. As the edge of the filter passes through the light path, an absorbance maximum is seen. Once the filter is in position, the absorbance maximum (of holmium oxide) is determined. Finally, the filter is moved out of the light path.
3 94 Troubleshooting and Test Functions 1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 4 Repairing the Detector Introduction into Repairing the Detector 96 Overview of the Repairing of the Detector 99 Simple Repairs 101 Exchanging Internal Parts 138 Agilent Technologies 95
4 Repairing the Detector Introduction into Repairing the Detector Simple Repairs The detector is designed for easy repair. The most frequent repairs such as lamp change and flow cell change can be done from the front of the detector with the detector in place in the system stack. These repairs are described in “Simple Repairs” on page 101. Exchanging Internal Parts Some repairs may require exchange of defective internal parts.
Repairing the Detector 4 CAUTION Electronic boards and components are sensitive to electronic discharge (ESD). In order to prevent damage always use an ESD protection (for example, the ESD wrist strap from the accessory kit) when handling electronic boards and components (see “Using the ESD Strap” on page 98). WA R N I N G Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product. Always turn the deuterium lamp off before removing it.
4 Repairing the Detector Using the ESD Strap Electronic boards are sensitive to electronic discharge (ESD). In order to prevent damage, always use an ESD strap supplied in the standard accessory kit (see “Accessory Kit” on page 208) when handling electronic boards and components. 1 Unwrap the first two folds of the band and wrap the exposed adhesive side firmly around your wrist. 2 Unroll the rest of the band and peel the liner from the copper foil at the opposite end.
Repairing the Detector 4 Overview of the Repairing of the Detector NOTE With the introduction of the G1315B/G1365B DAD/MWD some of the metal plates look different (no air openings) compared to the G1315A/G1365A DAD/MWD. The figures have changed for specific repairs only. Figure 29 shows the main assemblies and their locations.
4 Repairing the Detector Interface board, see page 179 Main Board, see page 143 Power supply, see page 164 Fan, see page 148 Lenses, see page 132 and page 158 Tungsten lamp, see page 102 Optical unit, see page 154 Leak handling system, see page 131 Deuterium lamp, see page 102 Holmium oxide filter and cell support window, see page 127 and page 135 Flow cell, see page 105 and page 108 Figure 29 100 Leak sensor, see page 167 Main Assemblies 1100 Series DAD and MWD Reference Manual
Repairing the Detector 4 Simple Repairs On the following pages repairs are described that can be carried out without opening the main cover. Table 7 Simple Repairs Procedure Typical Frequency Notes Deuterium lamp or tungsten lamp exchange If noise and/or drift exceeds your application limits or lamp does not ignite. An intensity test should be performed after replacement. Flow cell exchange If application requires a different flow cell type.
4 Repairing the Detector Exchanging a Lamp When required If noise or drift exceeds application limits or lamp does not ignite Tools required Screwdriver POZI 1 PT3 Parts required Longlife Deuterium lamp 2140-0813 (without black cover) Longlife Deuterium lamp 5181-1530 (with black cover) Deuterium lamp 2140-0590 (without black cover) Tungsten lamp G1103-60001 Preparations for this procedure: • Turn the lamp(s) off.
Repairing the Detector 2 Disconnect lamp from the connector and unscrew the lamp. 4 When replacing the vis-lamp, assure that the vis-lamp is inserted as shown (flat edge towards the deuterium lamp opposite as in the figure). 1100 Series DAD and MWD Reference Manual 4 3 Remove the lamp. Do not touch the glass bulb with your fingers. 5 Insert the lamp. Fix the screws and reconnect the lamp to connector.
4 Repairing the Detector 6 Replace the front cover. Next steps: • Reset the lamp counter as described in the user interface documentation. • Turn the lamp on. • Give the lamp 10 minutes to warm up. • Perform an intensity test, see “Intensity Test” on page 88.
Repairing the Detector 4 Exchanging a Flow Cell When required If an application needs a different type of flow cell or the flow cell needs repair. Tools required Two 1/4 inch wrenches for capillary connections Parts required Standard flow cell, 10 mm, 13 µl, 120 bar, G1315-60012 Semi-micro flow cell, 6 mm, 5 µl, 120 bar, G1315-60011 High pressure flow cell, 6 mm, 1.
4 Repairing the Detector 2 Press the release button and open the flow cell door. 3 Disconnect the cell inlet and the cell outlet capillary and the waste capillary from the capillary holder. 4 Remove the flow cell by pressing the flow cell holder. Note: The label attached to the flow cell provides information on part number, path length and maximum pressure.
Repairing the Detector 4 5 Insert the flow cell into the cell compartment and close the 6 Reconnect the waste capillary and the cell inlet and the cell door. cell outlet tubing to the capillary holder. Note: Next steps: To check for leaks, establish a flow and observe the flow cell (outside of the cell compartment) and all capillary connections.
4 Repairing the Detector Repairing the Standard or Semi-Micro Flow Cell NOTE When required If the flow cell needs repair due to leaks or contaminations (reduced light throughput) Tools required Two 1/4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks Parts required For parts, see “Standard Flow Cell” on page 186 and “Semi-Micro Flow Cell” on page 188 The gaskets used in the standard and semi-micro flow cell are different.
Repairing the Detector 4 2 Use a tooth pick to remove the quartz window from the Note: window assembly. If you want to replace the gasket only, continue with step 8. Do not mix the gasket #6 and # 7. They are different for standard and semi-mirco flow cell. 3 If the washers fall out of the window assembly, they must be inserted in the correct order with the Teflon® ring to prevent any leaks from the flow cell window.
4 Repairing the Detector 4 Assemble the washers and the window assembly in 5 Correct orientation of spring washers [2] is required. correct order. 6 Press the Teflon® ring into the window assembly. 7 Press the window assembly onto the new or cleaned quartz window.
Repairing the Detector 8 Insert a new gasket [6, 7] and the window assembly [1] into the cell body. Assure, that the gasket is on the bottom. 1 4 9 Using a 4-mm hex key, tighten the window screw hand tight plus a quarter turn. 7 6 1 Do not mix the gasket #6 and # 7 (different hole diameter) Next steps: • • • • • Reconnect the capillaries, see “Exchanging a Flow Cell” on page 105. Perform a leak test. Insert the flow cell.
4 Repairing the Detector Repairing the High Pressure Flow Cell When required If the flow cell needs repair due to leaks or contaminations (reduced light throughput) Tools required Two 1/4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks Parts required For parts see “High Pressure Flow Cell” on page 190 Preparations for this procedure: • Turn off the flow. • Remove the front cover. • Remove the flow cell, see “Exchanging a Flow Cell” on page 105.
Repairing the Detector If you want to replace the gasket only, continue with step 8. 4 2 Use a tooth pick to remove the quartz window from the window assembly. 3 If the washers fall out of the window assembly, they must be inserted in the correct order with the Teflon® ring to prevent any leaks from the flow cell window. Follow the procedure “Repairing the Standard or Semi-Micro Flow Cell” on page 108 for reassembling.
4 Repairing the Detector Replacing Capillaries on a Standard Flow Cell When required If the capillary is blocked Tools required Two 1/4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see “Standard Flow Cell” on page 186 Preparations for this procedure: • Turn off the flow. • Remove the front cover. • Remove the flow cell, see “Exchanging a Flow Cell” on page 105. 1 Identify the inlet and outlet capillaries.
Repairing the Detector Notes The fittings at the flow cell body are special types for low dead volumes and not compatible with other fittings. 4 2 After replacing the outlet capillary, fix it handtight first. Then do a 1/4 turn with a 4-mm wrench. When retightening the fittings, make sure that they are carefully tightened (handtight plus 1/4 turn with a wrench). Otherwise damage of the flow cell body or blockage may result.
4 Repairing the Detector 5 Unscrew the fixing screw and unwrap the inlet capillary from the grove in the flow cell body. 6 Take the new inlet capillary and bend it 90° about 35 mm from its end. Screw 35 mm 90° Inlet capillary with heat 7 Bend the caillary again by 90° as shown below. 8 Insert the capillary into the hole between fixing screw and the inlet fitting.
Repairing the Detector 9 The capillary lays in the grove and should be tied around the body (in the grove) 5 times. 4 10 Insert the fixing screw, so that the capillary cannot leave the grove. Screw Inlet capillary with heat 11 Fix the flow cell body to the heat exchanger. 12 Fix the inlet capillary to the flow cell body handtight first. Then do a 1/4 turn with a 4-mm wrench.
4 Repairing the Detector 13 Fix the new heat exchanger to the clamp unit. Next steps: • Reconnect the capillaries, see “Exchanging a Flow Cell” on page 105. • Perform a leak test. • Insert the flow cell. • Replace the front cover. • Perform a wavelength calibration, see “Wavelength Recalibration” on page 84 or holmium test, see “Holmium Oxide Test” on page 86 to check the correct positioning of the flow cell.
Repairing the Detector 4 Replacing Capillaries on a Semi-Micro and High Pressure Flow Cell When required If the capillary is blocked Tools required Two 1/4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see “Semi-Micro Flow Cell” on page 188 Preparations for this procedure: • Turn off the flow. • Remove the front cover. • Remove the flow cell, see “Exchanging a Flow Cell” on page 105.
4 Repairing the Detector Notes The fittings at the flow cell body are special types for low dead volumes and not compatible with other fittings. 2 After replacing the outlet capillary, fix it handtight first. Then do a 1/4 turn with a 4-mm wrench. When retightening the fittings, make sure that they are carefully tightened (handtight plus 1/4 turn with a wrench). Otherwise damage of the flow cell body or blockage may result.
Repairing the Detector 5 Fix the new heat exchanger to the clamp unit and the heat exchanger to the cell body. 4 6 Fix the inlet capillary to the flow cell body handtight first. Then do a 1/4 turn with a 4-mm wrench. Inlet capillary Next steps: • • • • • Reconnect the capillaries, see “Exchanging a Flow Cell” on page 105. Perform a leak test. Insert the flow cell. Replace the front cover.
4 Repairing the Detector Nano Flow Cell - Replacing or Cleaning When required If parts are contaminated or leaky. Tools required Screwdriver POZI 1 PT3 Two 1/4 inch wrenches for capillary connections Parts required For parts identification refer to “Nano Flow Cells” on page 192 (80 nl and 500 nl). NOTE For details refer to the technical that comes with the nano-flow cell kit. NOTE The quartz block can be cleaned with alcohol. DO NOT touch the inlet and outlet windows at the quartz block.
Repairing the Detector 4 3 Unscrew the capillaries from the flow cell. DO NOT use the adapter at this time! 4 Using for example a toothpick, press on the plastic part and slide the quartz body out of the cell housing. 5 The quartz body and the cell seal assembly can be separated for cleaning purpose. 6 This figure shows the correct holding of the quartz body and the cell seal assembly.
4 Repairing the Detector 7 Replace the cell seal assembly onto the quartz body. Always use a new seal assembly to exclude damage during disassembling. 9 Insert the flow cell capillaries and tighten them fingertight. Use the wrench and torque adapter as described on page 126 and tighten the fittings alternately. 124 8 Slide the quartz body completely into the cell body to the front stop (use for example a toothpick). 10 Reassemble the flow cell body to the holder.
Repairing the Detector 11 Re-install the flow cell and connect the capillaries to the union holder. 4 12 Perform a leak test with the flow cell outside of the detector. 13 If no leak is observed, install the flow cell and you are ready to work. 14 Make sure that the flow cell assembly is inserted correctly and fits perfectly in the optical unit (especially when PEEK capillaries are used).
4 Repairing the Detector Adapter Wrench DO NOT press down more than shown here max 0.
Repairing the Detector 4 Cleaning or Exchanging the Holmium Oxide Filter NOTE When required If holmium oxide filter is contaminated Tools required Screwdriver POZI 1 PT3 Screwdriver flat blade Two 1/4 inch wrenches for capillary connections A pair of tweezers Parts required Holmium oxide filter 79880-22711 See also “Declaration of Conformity for HOX2 Filter” on page 310. Preparations for this procedure: 1 Unscrew the six screws and remove the flow cell cover. • Turn off the flow.
4 Repairing the Detector 2 If not already in this position, move the filter up. 3 While releasing the holder with a screwdriver, carefully remove the holmium oxide filter using a pair of tweezers covered with lint-free cloth or tape. Note: Do not scratch the holmium oxide filter. 4 While releasing the holder with a screw driver, carefully insert the holmium oxide filter. The holmium oxide filter can be cleaned with alcohol and a lint-free cloth.
Repairing the Detector 5 Replace the flow cell cover and fix the six screws. 4 Next steps: • Perform a holmium oxide test, see “Holmium Oxide • • • 1100 Series DAD and MWD Reference Manual Test” on page 86 to check the proper function of the holmium oxide filter. Insert the flow cell, see “Exchanging a Flow Cell” on page 105. Replace the front cover. Turn on the flow.
4 Repairing the Detector Correcting Leaks When required If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections Tools required Tissue Two 1/4 inch wrenches for capillary connections Parts required None 1 Remove the front cover. 2 Use tissue to dry the leak sensor area and the leak pan. 3 Observe the capillary connections and the flow cell area for leaks and correct, if required. 4 Replace the front cover.
Repairing the Detector 4 Replacing Leak Handling System Parts When required If the parts are corroded or broken Tools required None Parts required Leak funnel 5061-3356 Leak funnel holder 5041-8389 Leak tubing (120 mm) 0890-1711 1 Remove the front cover. 2 Pull the leak funnel out of the leak funnel holder. 3 Pull out the leak funnel with the tubing. 4 Insert the leak funnel with the tubing in its position. 5 Insert the leak funnel into the leak funnel holder. 6 Replace the front cover.
4 Repairing the Detector Cleaning or Replacing Coupling Lens Assembly When required The coupling lens assembly is located between the tungsten and the deuterium lamp. It may be replaced when light transmission is reduced and a lamp exchange or window cleaning does not improve the light throughput. Tools required Screwdriver POZI 1 PT3 hexagonal key 1.5 mm A pointed pair of pliers Parts required Coupling lens assembly G1103-68001 Preparations for this procedure: • Turn off the lamp(s). 1 Use the 1.
Repairing the Detector 2 Carefully slide the lens assembly to the right into the 4 3 Remove the lens assembly completely. deuterium lamp area by pushing it from the tungsten lamp side with the hex key. 4 The assembly may be disassembled using a pair of pliers to remove the retainer ring. 5 The lens may be cleaned or the complete assembly must be exchanged.
4 Repairing the Detector 6 Insert the rebuilt or new lens assembly and slide it into its 7 Align the lens assembly with the wall of the deuterium holder. area. Fix the setscrew that secures the lens assembly. Next steps: • Replace both lamps. • Perform an intensity test to check the proper function. • Replace the front cover.
Repairing the Detector 4 Cleaning or Replacing Cell Support Window When required This window is located between the holmium oxide filter and the flow cell. It may be replaced when the transmission of light is reduced and a lamp exchange or a window cleaning does not improve the light throughput. Tools required Screwdriver POZI 1 PT3 hexagonal key 1.5 mm Pointed pair of pliers Parts required Cell support window 79880-28111 Cell support window assembly G1315-65202 For others.
4 Repairing the Detector 2 If not already in this position, move the holmium oxide filter down. 4 Carefully slide the assembly to the right into the flow cell 3 Use the 1.5-mm hex key to loosen the setscrew that secures the cell support assembly. 5 Remove the cell support assembly completely. compartment by pushing it from the holmium oxide filter side.
Repairing the Detector 6 The assembly may be disassembled using a pair of pliers to remove the retainer ring. The window may be cleaned or the complete assembly must be exchanged. 4 7 Insert the rebuilt or new assembly and slide it in until it is stopped by the filter lever. Retainer ring Washer Spectro window Cell support 8 Leave slight clearance for movement of the filter lever between both, the lens assembly and the filter lever, and fix the setscrew.
4 Repairing the Detector Exchanging Internal Parts WA R N I N G The following procedures require opening the main cover of the detector. Always ensure the detector is disconnected from the line power when the main cover is removed. The security lever at the power input socket prevents that the detector cover is taken off when line power is still connected. WA R N I N G To disconnect the detector from line, unplug the power cord.
Repairing the Detector 4 WA R N I N G Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product. Always turn off the deuterium lamp before removing the deuterium lamp. NOTE With the introduction of the G1315B/G1365B DAD/MWD some of the metal plates look different (no air openings) compared to the G1315A/G1365A DAD/MWD. The figures have changed for specific repairs only.
4 Repairing the Detector Removing the Top Cover and Foam When required For all repairs inside the detector Tools required Screwdriver POZI 1 PT3 Screwdriver Parts required Depends on the work inside and the following procedures Preparations for this procedure: • • • • 140 Turn off the detector. Disconnect the power cable. Disconnect capillaries. Remove detector from stack and place it on the working bench. 1 Press the release buttons and remove the front cover. Unclip the waste funnel assembly.
Repairing the Detector 4 2 Install the ESD strap. If installed, unscrew and remove the 3 Move the power lock across the power inlet and lift the interface board. Place the board on the ESD kit. 4 Lift the cover up and slide it towards the rear. clips of the cover. 5 Unscrew the screws at the rear of the top plate, slide the plate towards the front and remove it.
4 Repairing the Detector 6 Disconnect the lamps from their connectors. 7 Remove the two lamp connectors towards the back by depressing their connector tabs with a screwdriver. 8 While removing the top foam section completely, route the lamp cables through the hole in the foam. Note: Do not connect a power plug to the detector module after removing the top covers.
Repairing the Detector 4 Exchanging the Detector Main Board When required If detector main board is defective or for repair on other assemblies Tools required Screwdriver POZI 1 PT3 Hexagonal wrenches 5 mm, 7 mm and 15 mm Parts required Detector main board (DAM) G1315-69540 (exchange assembly) for G1315A/B DAD Detector main board (MWM) G1365-69540 (exchange assembly) for G1365A/B MWD 1 Turn off the lamp. 2 Switch off the module, and disconnect the cables.
4 Repairing the Detector NOTE When removing connectors, counter-hold with one hand on connector J13.
Repairing the Detector 4 7 Remove the detector main board. Place the board on the ESD kit. 8 In most cases the RFI spring plate remains on the interface connectors of the board. Carefully remove the spring plate and place it back into its position in the instrument before installing a new board. 9 On the new board check the switch setting of address switch S1, see “Setting the 8-bit Configuration Switch” on page 261.
4 Repairing the Detector Entering the Serial Number using the Control Module 1 Connect the control module to the detector. Turn on the detector. 2 In the control module, press System (F5), then Records (F4). Using the up/down arrows, make sure that the detector is highlighted. 3 Press FW Update (F5). Now, press the m key. This will display a box which says Update Enter Serial#. 4 Press Enter. This will display the box labeled Serial#.
Repairing the Detector 4 Entering the Serial Number using the Agilent ChemStation Module serial numbers are entered by typing specific commands in the command line at the bottom of the main user interface screen. 1 To enter a module serial number, type the following command in the command line (depends on the detector type, either DAD or MWD): print sendmodule$(ldad, "ser YYYYYYYYYY") print sendmodule$(lmwd, "ser YYYYYYYYYY") Where: YYYYYYYYYY is the 10-character serial number of the module in question.
4 Repairing the Detector Exchanging the Fan (G1315A/G1365A) NOTE Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer to “Replacing Fan Parts (G1315B/G1365B)” on page 150. When required If the fan is defective or noisy Tools required Screwdriver POZI 1 PT3 Parts required Fan assembly 3160-1016 Preparations for this procedure: • Turn off the lamp. • Switch off the detector, and disconnect the cables and acpillaries.
Repairing the Detector The fan must be installed in the correct orientation (see arrow on the fan) to ensure optimum cooling and operation of the detector. The direction of air flow is from the front towards the rear. 4 The figure below shows the required air flow direction. AIRFLOW G1315/65A G1315/65B 2 Insert the fan assembly into its location and Reconnect the connector to the main board (fan J16), see figure below for location.
4 Repairing the Detector Replacing Fan Parts (G1315B/G1365B) NOTE With the introduction of the G1315B/G1365B DAD/MWD a heater and a temperature sensor was added to the standard fan assembly. Also the air flow direction is reversed (now: rear to front). Use this procedure for the the G1315B/G1365B only. For G1315A/G1365A detectors refer to “Exchanging the Fan (G1315A/G1365A)” on page 148.
Repairing the Detector The heater and temperature sensor assemblies are clipped into the fan assembly. In case the temperature sensor or the heater assembly fails, they can be unclipped separately from the fan assembly. 4 2 To unclip the heater from the fan, use a pair of pliers, squeeze the clips and push them through the hole. Repeat this with the three remaining clips.
4 Repairing the Detector 5 To re-install the sensor holder (here shown with the sensor), bring the holder into its position and slide it carefully across the fan cable. 6 Clip the sensor carefully into its holder and route the cables as shown. Assure, that the fan rotates smoothly without any scraping noise. Otherwise correct the position of the sensor holder. 7 Position the heater assembly as shown and clip the heater onto the fan. The cables should be oriented towards the left corner.
Repairing the Detector The figure below shows the required air flow direction. 4 8 Insert the fan assembly into its location. AIRFLOW G1315/65A G1315/65B 9 Reconnect the connectors to the main board (fan J16), temperature sensor (J18) and heater (J17), see figure below for location. 1100 Series DAD and MWD Reference Manual Next Steps: • Reinstall the top foam section, top cover and front cover, see “Replacing the Foam and the Top Cover” on page 175.
4 Repairing the Detector Removing the Optical Unit (G1315A/G1365A) NOTE NOTE Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer to “Removing the Optical Unit (G1315B/G1365B)” on page 156. When required For all repairs inside the optical unit Tools required Screwdriver POZI 1 PT3 Parts required Optical unit G1315-69002 (exchange assembly) or Individual parts depending on the following procedures Use this procedure for the G1315A/G1365A only. 1 Turn off the lamp.
Repairing the Detector 10 Remove the two rubber shock absorbers. 4 11 Disconnect the SCI cable (J23) and the holmium oxide filter motor (J19) from the detector main board. 12 Remove the optical unit from the instrument holding the one hand at back of the heat sink.
4 Repairing the Detector Removing the Optical Unit (G1315B/G1365B) NOTE When required For all repairs inside the optical unit Tools required Screwdriver POZI 1 PT3 Parts required Optical unit G1315-69002 (exchange assembly) or Individual parts depending on the following procedures With the introduction of the G1315B/G1365B DAD/MWD the appearance of the z-plane (front metal plane) has been changed (no holes any more) and an isolation seal between the optical unit and the z-plane.
Repairing the Detector 4 2 Remove the two rubber shock absorbers. 3 Slide the z-plane to the front and remove it from the module. 4 Disconnect the SCI cable (J23) and the holmium oxide filter motor (J19) from the detector main board. 5 Remove the optical unit from the instrument holding the one hand at back of the heat sink.
4 Repairing the Detector Exchanging the Source Lens (Achromat) Assembly NOTE When required The source lens (achromat) assembly might be cleaned or replaced when the transmission of light is reduced and a lamp exchange or new spectro windows do not improve the light throughput Tools required Screwdriver POZI 1 PT3 hexagonal key 1.
Repairing the Detector 4 2 Pull the filter motor off the shaft. Keep the spring and the lever fixture in a safe place. Remove the filter lever on the other side. 3 Use the 1.5-mm hexagonal key to loosen the setscrew that secures the source lens assembly. 4 Use the 1.5-mm hexagonal key to loosen the setscrew that secures the cell support assembly. 5 Carefully slide the assembly to the right by pushing it from the deuterium lamp side with a hexagonal wrench.
4 Repairing the Detector 6 Remove the achromat assembly. 8 Remove the spring and the spectro window from the holder. 7 Use a metal blade (12-mm width, 1-mm thick) to unscrew the lens achromatic. 11 Replace the achromat assembly, move it completely into the optical and fix the setscrew. 9 Clean (with alcohol and lint-free cloth) or replace the spectro window. Do not clean the achromatic lens with any liquid. To clean use dry air only.
Repairing the Detector 12 Before installing the filter motor, press the filter lever in from the other side. 13 While counter-holding the filter lever, insert the filter motor onto the filter shaft until it clicks into the final position. 14 Slide in the cell support assembly until it is stopped by the holmium filter. Leave about 0.2-mm clearance for movement of the filter lever between both the lens assembly and the filter lever, and fix the setscrew.
4 Repairing the Detector Replacing the Holmium Oxide Filter Motor NOTE When required If defective Tools required Screwdriver POZI 1 PT3 hexagonal key 3 mm Parts required Filter motor assembly G1315-68700 (includes filter lever G1315-45001 and spring 1460-1510) For others see “Holmium Oxide Filter” on page 197 If the filter motor was removed, the filter lever should not be reused. Always use a new filter lever to assure correct fit on the filter motor shaft.
Repairing the Detector 4 2 Pull the filter motor off the shaft. Keep the spring in a safe place. 3 Before installing the filter motor, press the filter lever in from the other side. 4 While counter-holding the filter lever, press the filter motor onto the filter shaft until it clicks into the final position. Next steps: 1100 Series DAD and MWD Reference Manual • Check that the filter lever is moveable.
4 Repairing the Detector Exchanging the Power Supply NOTE When required If defective Tools required Screwdriver POZI 1 PT3 Wrench 1/4 inch Wrench 5 mm Wrench 7 mm Parts required Power supply 0950-2528 The repair level of the power supply assembly is exchanging the complete assembly. No serviceable parts are inside. 1 Turn off the lamp. 2 Switch off the detector, and disconnect the cables. 3 Remove the detector from the stack and place it on the working bench.
Repairing the Detector 5 Carefully remove the bottom foam part by sliding it out towards the rear. 6 Unscrew the power supply at the rear of the module. 7 Press down the power switch light pipe to remove it from the coupler. 8 Remove the power supply completely. Re-use the coupler on the new power supply. 4 Power switch light pipe Coupler The repair level of the power supply assembly is exchange of the complete assembly. No serviceable parts inside.
4 Repairing the Detector 9 Insert the power supply into its location and fix it with the screws at the rear panel. 10 Press down and clip in the power switch light pipe into the power supply. Power switch light pipe 11 Reinstall bottom foam part. Slide it in underneath the leak drain. 166 Next steps: • Reinstall the processor board, see “Exchanging the Detector Main Board” on page 143.
Repairing the Detector 4 Exchanging the Leak Sensor When required If defective Tools required Screwdriver POZI 1 PT3 Parts required Leak sensor assembly 5061-3356 WA R N I N G Do not switch on the detector when the cover is removed. CAUTION Electronic boards and components are sensitive to electronic discharge (ESD).
4 Repairing the Detector 12 Remove the leak pan from the cabinet bottom. 13 Remove the leak sensor assembly from the leak pan. 14 Replace the leak sensor assembly into the leak pan. 15 Route the leak sensor cable through the z-plane.
Repairing the Detector 16 Replace the leak pan into the cabinet bottom. 4 Next steps: • Reconnect the leak sensor cable to the processor board (J21). • Replace the optical unit, see “Installing the Optical Unit (G1315A/G1365A)” on page 171 or “Installing the Optical Unit (G1315B/G1365B)” on page 173. • Replace the front cover, top cover and top foam section, see “Replacing the Foam and the Top Cover” on page 175. • Replace the detector into the stack. • Reconnect the cables. • Turn on the detector.
4 Repairing the Detector Replacing Status Light Pipe When required If part was broken or removed Tools required Screwdriver POZI 1 PT3 Parts required Status light pipe 5041-8384 Preparations for this procedure: 1 The status light pipe is clipped into the top cover. • Remove the front cover and top cover, see “Removing the Top Cover and Foam” on page 140. Next steps: • Replace the top cover, see “Replacing the Foam and the Top Cover” on page 175.
Repairing the Detector 4 Installing the Optical Unit (G1315A/G1365A) When required When repairs have been completed Tools required Screwdriver POZI 1 PT3 NOTE Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer to “Installing the Optical Unit (G1315B/G1365B)” on page 173 CAUTION The fan must be installed in the correct orientation to ensure correct cooling and operation of the detector, see “Exchanging the Fan (G1315A/G1365A)” on page 148.
4 Repairing the Detector 2 Carefully insert the optical unit into the instrument holding the one hand at back of the heat sink. 3 Reconnect the SCI cable (J23) and the holmium oxide filter motor (J19) to the detector main board. 4 Replace the two rubber shock absorbers and reconnect the ground connector. Next steps: NOTE 172 • Reinstall the fan assembly (J16). Ensure the correct direction of air flow. • Reinstall the flow cell cover, see “Cleaning or Exchanging the Holmium Oxide Filter” on page 127.
Repairing the Detector 4 Installing the Optical Unit (G1315B/G1365B) When required When repairs have been completed Tools required Screwdriver POZI 1 PT3 NOTE Use this procedure for the the G1315B/G1365B only. For G1315A/G1365A detectors refer to “Installing the Optical Unit (G1315A/G1365A)” on page 171. CAUTION The fan must be installed in the correct orientation to ensure correct cooling and operation of the detector, see “Replacing Fan Parts (G1315B/G1365B)” on page 150.
4 Repairing the Detector 2 Carefully insert the optical unit into the instrument holding the one hand at back of the heat sink. 3 Reconnect the SCI cable (J23) and the holmium oxide filter motor (J19) to the detector main board. 4 Replace the two rubber shock absorbers and reconnect the ground connector. Next steps: NOTE 174 • Reinstall the fan assembly (J16). Ensure the correct direction of air flow. • Reinstall the flow cell cover, see “Cleaning or Exchanging the Holmium Oxide Filter” on page 127.
Repairing the Detector 4 Replacing the Foam and the Top Cover When required When all repairs have been completed Tools required Screwdriver POZI 1 PT3 Prerequisites The detector is open and other procedures have been carried out Preparations for this procedure: • All the work within the module should be completed. 1100 Series DAD and MWD Reference Manual 1 Route the lamp connector cables through the hole in the foam.
4 Repairing the Detector 2 Insert the foam and make sure that the foam is installed correctly. 4 Reconnect the lamps. 3 Press the lamp cables into the foam channel and reconnect the lamp connectors to the front panel. 5 Slide the top plate towards the rear and fix the top plate screws.
Repairing the Detector 6 Replace the cover. 8 Replace waste funnel assembly and the front panel. 4 7 If required, insert the interface board and fix the screws. Next steps: • Replace the detector into the stack. • Reconnect the hydraulic connections • Reconnect the power cable and turn on the detector.
4 Repairing the Detector Assembling the Main Cover NOTE WA R N I N G When required If cover is broken Tools required None Parts required Plastics kit 5062-8582 (includes base, top, left and right) The plastics kit contains all parts, but it is not assembled. In case you insert the left or right side in the opposite position, you may not be able to remove the side from the top part. 1 Place the top part on the bench and insert the left and right side into the top part. 2 Replace the cover.
Repairing the Detector 4 Replacing the Interface Board When required For all repairs inside the detector or for installation of the board Part required Interface board (BCD) G1351-68701 with external contacts and BCD outputs, see “BCD Board” on page 253 Interface board (LAN) see “LAN Communication Interface Board” on page 255. Tools required None 1 Install the ESD strap. Move the power lock across the power inlet. 2 If required, unscrew and remove the interface board.
4 Repairing the Detector Replacing the Detector’s Firmware The installation of new firmware is required: • if new version solves problems of currently installed version, or • if after exchange of the detector main board (DAM or MWM) the version on board is older than previous installed one. To upgrade the detector’s firmware the following steps have to be performed: 1 Load the firmware into the detector, see help system of your user interface.
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 5 Identifying Parts and Materials Overview of Main Assemblies 182 Optical Unit Assembly 184 Standard Flow Cell 186 Semi-Micro Flow Cell 188 High Pressure Flow Cell 190 Nano Flow Cells 192 Fan Assembly Parts 196 Holmium Oxide Filter 197 Coupling Lens Assembly 198 Source Lens (Achromat) Assembly 199 Cell Support Assembly 200 Control Module 201 Sheet Metal Kit (G1315A/G1365A) 202 Sheet Metal Kit (G1315B/G1365B) 203 Plastic Part
5 Identifying Parts and Materials Overview of Main Assemblies 3 1 2 4 6 7 2 10 Figure 35 182 8 9 10 11 5 13 12 Overview of Main Assemblies 1100 Series DAD and MWD Reference Manual
Identifying Parts and Materials Table 8 5 Main Assemblies Item Description Part Number 1 Main board DAM for G1315A/B DAD (exchange assembly) G1315-69540 Main board DAM for G1365A/B MWD (exchange assembly) G1365-69540 Hexagonal nut for GPIB connector 0380-0643 Hexagonal nut for RS-232C connector 1251-7788 Nut for analog connector 2940-0256 Washer for analog connector 2190-0699 Cable CAN to Agilent 1100 Series modules 5181-1516 2 Power supply, for power and status light parts see page 2
5 Identifying Parts and Materials Optical Unit Assembly Table 9 Optical Unit Assembly Item Description Part Number 1 Optical unit (exchange assembly) G1315-69002 2 Semi-flow cell, 6 mm, 5 µl, maximum pressure 120 bar, see page 186 G1315-60011 2 Standard flow cell, 10 mm, 13 µl, maximum pressure 120 bar, see page 186 G1315-60012 2 High Pressure flow cell, 6 mm 1.
Identifying Parts and Materials 5 13 9 12 7 14 1 15 16 4 3 8 2 7 6 11 10 5 17 Figure 36 Optical Unit Parts 1100 Series DAD and MWD Reference Manual 185
5 Identifying Parts and Materials Standard Flow Cell Table 10 Item 186 Standard Flow Cell Parts Description Part Number Standard flow cell assembly, 10 mm, 13 µl, maximum pressure 120 bar G1315-60012 1 Window screw 79883-22402 2 Spring washers, pack of 10 5062-8553 3 Compression washer 79883-28801 4 Window holder 79883-22301 5 Quartz window 1000-0488 6 Gasket BACK (Teflon), 2.3 mm hole, outlet side See kits below 7 Gasket FRONT (Teflon), 1.
Identifying Parts and Materials 5 NOTE Gaskets # 6 and #7 have different hole diameters. 8 7 6 5 4 3 2 1 9 11 10 Figure 37 Standard Flow Cell Parts 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - Gasket Figure 38 Orientation of Spring Washers.
5 Identifying Parts and Materials Semi-Micro Flow Cell Table 11 Item 188 Semi-Micro Flow Cell Parts Description Part Number Semi-micro flow cell assembly, 6 mm, 5 µl, maximum pressure 120 bar G1315-60011 1 Window screw 79883-22402 2 Spring washers, pack of 10 5062-8553 3 Compression washer 79883-28801 4 Window holder 79883-22301 5 Quartz window 1000-0488 6 Gasket BACK (Teflon), 1.8 mm hole, outlet side See kits below 7 Gasket FRONT (Teflon), 1.
Identifying Parts and Materials 5 NOTE Gaskets # 6 and #7 have different hole diameters. 8 7 6 5 4 3 2 1 9 11 10 Figure 39 Semi-Micro Flow Cell Parts 1 - window screw 2 - spring washers 3 - compression washer 4 - window holder 5 - quartz window 6 - Gasket Figure 40 Orientation of Spring Washers.
5 Identifying Parts and Materials High Pressure Flow Cell Table 12 Item 190 Repair Parts: Micro Flow Cell Assembly Description Part Number High pressure flow cell assembly, 6 mm, 1.7 µl, maximum pressure 400 bar G1315-60015 1 Window assembly, comprises items 2, 3, 4, 5 and 6 2 Seal ring 79883-27101 3 Quartz window 1000-0953 4 Compression washer 79883-28802 5 Spring washers (pack of 10) 5062-8553 6 Window screw 79883-22404 7 Capillary IN (0.
Identifying Parts and Materials 5 6 5 4 2 3 2 1 7 9 8 Figure 41 High Pressure Flow Cell Assembly Parts 1100 Series DAD and MWD Reference Manual 191
5 Identifying Parts and Materials Nano Flow Cells The following kits are available: Table 13 Nano-flow cell kits Description Part number 500 nl Flow Cell Kit includes Flow cell assembly (10 mm, 500 nl, 5 MPa) completely assembled (includes items 1, 2, 3, 4, 10, 11, 12, 13, 14, 15, and 16) G1315-68724 80 nl Flow Cell Kit includes Flow cell assembly (10 mm, 500 nl, 5 MPa) completely assembled (includes items 1, 2, 3, 4, 10, 11, 12, 13, 14, 15, and 16) G1315-68716 Figure 42 shows all parts delivered
Identifying Parts and Materials 5 Table 14 lists the generic parts for both nano-flow cells: Table 14 Generic Parts Item Description Part Number 3 Fitting Screw (for 4 mm wrench), QTY=2 (reorder 10/pk) 5063-6593 4 Cell ferrules are factory installed 5 PEEK fitting 1/32" (not attached to capillaries), (reorder 10/pk) 5065-4422 Litetouch ferrules LT-100, (1/32" Ferrule and SS lock ring), QTY=2 (reorder 10/pk) 5063-6592 8 Union Adjustment Tool, used for item #7 5022-2146 9 ZDV SS Union, no
5 Identifying Parts and Materials Table 15 lists the specific parts for the 500 nl flow cell. Table 15 Item 194 Specific 500 nl Flow Cell Parts Description Part Number 500 nl Flow Cell Kit G1315-68724 1 PEEK coated fused silica capillary Inlet (100 µm) pre-mounted to cell, includes Inlet capillary, 300 mm long, 100 µm i.d.
Identifying Parts and Materials 5 Table 16 lists the specific parts for the 80 nl flow cell. Table 16 Item Specific 80 nl Flow Cell Parts Description Part Number 80 nl Flow Cell Kit G1315-68716 1 PEEK coated fused silica capillary Inlet (50 µm) pre-mounted to cell, includes Inlet capillary, 400 mm long, 50 µm i.d.
5 Identifying Parts and Materials Fan Assembly Parts Table 17 Fan Assembly Parts Item Description Part Number 1 Fan (for all DAD/MWDs) 3160-1016 2 Heater assembly (G1315/65B only) G1315-60000 3 Temperature sensor assembly (G1315/65B only) G1315-60003 4 Sensor holder (G1315/65B only) G1315-22300 2 1 4 3 Figure 43 196 Fan Assembly Parts 1100 Series DAD and MWD Reference Manual
Identifying Parts and Materials 5 Holmium Oxide Filter Table 18 NOTE Holmium Oxide Filter Assembly Parts Item Description Part Number 1 Holmium oxide filter motor assembly, includes items 2 and 4 G1315-68700 2 Holmium oxide filter lever G1315-45001 3 Holmium oxide filter 79880-22711 4 Spring 1460-1510 When the filter motor has been removed, the filter lever should not be reused. Use always a new filter lever to assure correct fit on the filter motor shaft.
5 Identifying Parts and Materials Coupling Lens Assembly Table 19 Item Coupling Lens Assembly Description Part Number Coupling lens assembly G1103-68001 1 Retainer ring 2 Washer-spring wavy 3 Lens support 4 Lens 5 Lens holder 1 2 3 4 5 Figure 45 198 Coupling Lens Assembly Parts 1100 Series DAD and MWD Reference Manual
Identifying Parts and Materials 5 Source Lens (Achromat) Assembly Table 20 Item NOTE Source Lens Assembly Description Part Number Source lens (achromat) assembly includes a filter lever G1315-45001 G1315-65201 1 Lens achromatic 1000-0486 2 Spring compression 1460-2255 3 Spectro window 79880-28111 4 Holder When the filter motor has been removed, the filter lever should not be reused. Use always a new filter lever to assure correct fit on the filter motor shaft.
5 Identifying Parts and Materials Cell Support Assembly Table 21 Item Cell Support Assembly Description Part Number Cell support assembly G1315-65202 1 Retainer ring 0510-1638 2 Washer-spring wavy 3050-1591 3 Spectro window 79880-28111 4 Cell support G1315-24701 1 2 3 4 Figure 47 200 Cell Support Assembly Parts 1100 Series DAD and MWD Reference Manual
Identifying Parts and Materials 5 Control Module Table 22 Item Cotrol Module Parts Description Part Number Control Module, replacement part including cable G1323-67001 Plastic Housing Kit, includes front, back and a clamp 5062-8583 CAN cable Agilent 1100 module to control module G1323-81600 Figure 48 Control Module 1100 Series DAD and MWD Reference Manual 201
5 Identifying Parts and Materials Sheet Metal Kit (G1315A/G1365A) NOTE For the information on the sheet metal kit for the G1315B and G1365B refer to “Sheet Metal Kit (G1315B/G1365B)” on page 203.
Identifying Parts and Materials 5 Sheet Metal Kit (G1315B/G1365B) NOTE For the information on the sheet metal kit for the G1315A and G1365A refer to “Sheet Metal Kit (G1315A/G1365A)” on page 202.
5 Identifying Parts and Materials Plastic Parts NOTE Table 25 Plastics Parts Item Description Part Number 1 Front cover 5062-8582 2 Plastics, includes base, sides and top 5062-8565 3 Name plate Agilent 1100 Series 5042-1381 4 Name plate Serial Number (w/o serial number) 5042-1314 For correct assembling of the top and sides, see “Assembling the Main Cover” on page 178.
Identifying Parts and Materials 5 Foam Parts Table 26 NOTE Foam Parts Item Description Part Number 1, 2 EPP foam kit, includes base and top G1315-68722 3 Damper kit (includes 7 bumpers) G1315-68706 4 Guides for interface board 5041-8395 Do not order the individual part numbers mentioned on the foam.
5 Identifying Parts and Materials Power and Status Light Pipes Table 27 Item Power and Status Light Pipes Description Part Number Power supply assembly 0950-2528 Screw M4 x 0.
Identifying Parts and Materials 5 Leak Parts Table 28 Leak Parts Item Description Part Number 1 Leak sensor assembly 5061-3356 2 Leak pan G1315-45501 3 Leak funnel 5041-8388 4 Leak funnel holder 5041-8389 5 Clip 5041-8387 6 Corrugated tubing, 120 mm lg, re-order 5 m 5062-2463 7 Corrugated tubing, 120 mm lg, re-order 5 m 5062-2463 5 2 4 3 1 6 7 Figure 54 Leak Parts 1100 Series DAD and MWD Reference Manual 207
5 Identifying Parts and Materials Accessory Kit This kit contains some accessories and tools needed for the installation and repair of the detector. Table 29 Item Accessory Kit Parts Description Part Number Accessory kit G1315-68705 Corrugated tubing (to waste), re-order 5 m 5062-2463 1 Teflon Tubing flexible i.d. 0.8 mm (flow cell to waste), re-order 5 m 5062-2462 2 Fitting male PEEK, Qty=1 0100-1516 3 Capillary column – detector 380 mm lg, 0.17 i.d.
Identifying Parts and Materials 5 2 1 Figure 55 4 Waste Tubing Parts 5 6 3 Figure 56 This end is pre-installed Inlet Capillary (Column-Detector) Parts 1100 Series DAD and MWD Reference Manual 209
5 Identifying Parts and Materials Cable Overview WA R N I N G Never use cables other than the ones supplied by Aligent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
Identifying Parts and Materials Table 30 5 Cables Overview, continued Type Description Part Number BCD cables 3396 integrator 03396-60560 General purpose (spade Lugs) G1351-81600 Auxiliary Agilent 1100 Series vacuum degasser G1322-61600 CAN cables Agilent 1100 module to module, 0.
5 Identifying Parts and Materials Analog Cables One end of these cables provides a BNC connector to be connected to Agilent 1100 Series modules. The other end depends on the instrument to which connection is being made.
Identifying Parts and Materials 5 Agilent 1100 to 3394/6 Integrators Connector 35900-60750 Pin 3394/6 Pin Agilent 1100 1 Signal Name Not connected 2 Shield Analog - 3 Center Analog + Pin BNC Pin Agilent 1100 Signal Name Shield Shield Analog - Center Center Analog + Agilent 1100 to BNC Connector Connector 8120-1840 1100 Series DAD and MWD Reference Manual 213
5 Identifying Parts and Materials Agilent 1100 to General Purpose Connector 01046-60105 Pin 3394/6 Pin Agilent 1100 1 214 Signal Name Not connected 2 Black Analog - 3 Red Analog + 1100 Series DAD and MWD Reference Manual
Identifying Parts and Materials 5 Remote Cables One end of these cables provides a Aligent Technologies APG (Analytical Products Group) remote connector to be connected to Agilent 1100 Series modules. The other end depends on the instrument to be connected to.
5 Identifying Parts and Materials Agilent 1100 to 3392/3 Integrators Connector 01046-60206 4 - Key Pin 3392/3 Pin Agilent 1100 Signal Name Active (TTL) 3 1 - White Digital ground NC 2 - Brown Prepare run Low 11 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 9 7 - Red Ready High 1 8 - Green Stop Low NC 9 - Black Start request Low Pin 3394 Pin Agilent 1100 Signal Name Active (TTL) 9 1 - White Digital ground NC
Identifying Parts and Materials NOTE 5 START and STOP are connected via diodes to pin 3 of the 3394 connector.
5 Identifying Parts and Materials Agilent 1100 to 3396 Series III / 3395B Integrators Connector 03396-61010 Pin 33XX Pin Agilent 1100 Signal Name 9 1 - White Digital ground NC 2 - Brown Prepare run Low 3 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 14 7 - Red Ready High 4 8 - Green Stop Low NC 9 - Black Start request Low 13, 15 Active (TTL) Not connected Agilent 1100 to HP 1050, HP 1046A or Agilent 35900 A/D Con
Identifying Parts and Materials 5 Agilent 1100 to HP 1090 LC or Signal Distribution Module Connector 01046-60202 5 - Key Pin HP 1090 Pin Agilent 1100 Signal Name Active (TTL) 1 1 - White Digital ground NC 2 - Brown Prepare run Low 4 3 - Gray Start Low 7 4 - Blue Shut down Low 8 5 - Pink Not connected NC 6 - Yellow Power on High 3 7 - Red Ready High 6 8 - Green Stop Low NC 9 - Black Start request Low Pin Agilent 1100 Signal Name Active (TTL) 1 - White Digital gro
5 Identifying Parts and Materials BCD Cables One end of these cables provides a 15-pin BCD connector to be connected to the Agilent 1100 Series modules.
Identifying Parts and Materials 5 Agilent 1100 to 3396 Integrators Connector 03396-60560 1100 Series DAD and MWD Reference Manual Pin 3392/3 Pin Agilent 1100 Signal Name BCD Digit 1 1 BCD 5 20 2 2 BCD 7 80 3 3 BCD 6 40 4 4 BCD 4 10 5 5 BCD0 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 +5V Low 221
5 Identifying Parts and Materials Auxiliary Cable One end of this cable provides a modular plug to be connected to the Agilent 1100 Series vacuum degasser. The other end is for general purpose.
Identifying Parts and Materials 5 CAN Cable Both ends of this cable provide a modular plug to be connected to Agilent 1100 Series module’s CAN-bus connectors. Agilent 1100 module to module, 0.
5 Identifying Parts and Materials External Contact Cable 5 10 15 1 6 11 One end of this cable provides a 15-pin plug to be connected to Agilent 1100 Series module’s interface board. The other end is for general purpose.
Identifying Parts and Materials 5 RS-232 Cable Kit This kit contains a 9-pin female to 9-pin female Null Modem (printer) cable and one adapter. Use the cable and adapter to connect Aligent Technologies instruments with 9-pin male RS-232 connectors to most PCs or printers.
5 Identifying Parts and Materials LAN Cables Recommended Cables Table 31 226 Description Part number Cross-over network cable (shielded, 3 m long), (for point to point connection) 5023-0203 Twisted pair network cable (shielded, 7 m long) (for hub connections) 5023-0202 1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 6 Introduction to the Detector Introduction to the Detector 228 Optical System Overview 229 Electrical Connections 232 Instrument Layout 234 Early Maintenance Feedback (EMF) 235 Electronics 237 Detector Main Board (DAM/MWM) 238 Firmware Description 246 Raw Data Conversion to Absorbance 248 Optional Interface Boards 253 Interfaces 256 Setting the 8-bit Configuration Switch 261 The Main Power Supply Assembly 266 Agilent Techn
6 Introduction to the Detector Introduction to the Detector The detector is designed for highest optical performance, GLP compliance and easy maintenance.
Introduction to the Detector 6 Optical System Overview Optical System The optical system of the detector is shown in Figure 57. 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.
6 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.
Introduction to the Detector Diode Array 6 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.
6 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 (see “GPIB Default Addresses” on page 262) which is recognized once after power is switched on. • The CAN bus is a serial bus with high speed data transfer.
Introduction to the Detector 6 Security lever Interface board Analog signals APG remote RS-232C CAN GPIB Power Configuration switch Figure 58 Electrical Connections 1100 Series DAD and MWD Reference Manual 233
6 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.
Introduction to the Detector 6 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.
6 Introduction to the Detector 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.
Introduction to the Detector 6 Electronics The electronics are comprised of four main components: • detector main board (DAM/MWM), see page 238. • power supply, see page 266. Optional: • interface board (BCD/external contacts), see page 253. • interface board (LAN), see page 255.
6 Introduction to the Detector Detector Main Board (DAM/MWM) This board controls all information and activities of all assemblies within the detector. Through interfaces (LAN, CAN, GPIB or RS-232C) connected to the user interface, the operator enters parameters, changes modes and controls the detector.
Introduction to the Detector 6 Conversion and subsequent calculation to achieve absorbance values include the following tasks: • dark current correction, • PDA (photo diode array) temperature compensation, • absorbance calculation, and • signal averaging. SIMM Memory Module The main board versions -66500, -66520 and -66530 provided 4 slots for extended memory (up to 4 × 1 MB or up to 4 × 4 MB to accommodate more run buffer (signal and spectral data).
6 Introduction to the Detector Main Control Functional Block Status Temp sensor 4 control LEDs 8-bit switch GPIB driver CAN driver DAM/MWM “B” Temp Sensor “B” Heater PWM drivers ASIC application specific integrated circuit Fan sense Holmium motor Motor driver REMOTE driver Interface board RS-232C driver Main processor Safety lock Real Control lines Diagnostic data PWM drivers Analog out 1 Low pass filters & signal conditioning SSP signal & spectra Serial bus processor Memory Lamp supply
Introduction to the Detector 6 SCI Board The SCI (spectrograph connector interface), located on the optical unit assembly is the interface between micro-slit, PDA and detector main board. In addition, wavelength calibration data and manufacturing data from the manufacturing process (for example, serial number, dates, and so on) are stored in the EEPROM.
6 Introduction to the Detector DAM/MWM PFP functional block diagram RAM PFP digital processor Serial interface PFP ASIC EPLD PDA address lines Data bus Control lines EEPROM data bus 16 bit / 160 kHz A/D converter SCI board DAM/MWM Control Function Block / SSP Processor PDA control lines PDA signal Test signals, GND, Vref ramp Figure 60 242 PDA signal conditioning electronics PDA temperature sensor Block Diagram PFP Functions 1100 Series DAD and MWD Reference Manual
Introduction to the Detector 6 Deuterium Lamp Filament Control Before ignition, the deuterium lamp filament control circuit provides a constant voltage of 2.5 VDC at approximately 6 A to the filament of the deuterium lamp. The deuterium lamp filament control circuit is enabled by the processor on the DAM board. Deuterium Lamp Current Control The deuterium lamp current control circuit comprises two parts. One part generates an ignition pulse of 600 VDC for the lamp, resulting in lamp ignition.
6 Introduction to the Detector Detector Main Board Lamp Supply Functional Block Diagram Filament Deuterium lamp filament control Shut down Anode Deuterium lamp current control Control bus DAM/MWM Control Function Block Deuterium lamp sense Tungsten lamp voltage control Diagnostic A/D converter Control bus Figure 61 244 Block Diagram Lamp Supply Functions 1100 Series DAD and MWD Reference Manual
Introduction to the Detector 6 Diagnostic A/D Converter The diagnostic A/D converter senses currents and voltages of the deuterium and tungsten lamps and converts the analog signals into digital values. The digital values are transferred via the control bus on the detector main board. When values are outside the normal range, an appropriate error message is generated and the lamps will be switched off.
6 Introduction to the Detector Firmware Description The firmware of the instrument consists of two independent sections: • a non-instrument specific section, called resident system, • an instrument specific section, called main system. Resident System This resident section of the firmware is identical for all Agilent 1100 series modules. Its properties are: • the complete communication capabilities (GPIB, CAN and RS-232C), • memory management, • ability to update the firmware of the ‘main system’.
Introduction to the Detector 6 Firmware Updates Firmware updates can be done using your user interface: • handheld control module with files from a PC-card or • Agilent ChemStation with files from floppy disk The file naming conventions are: xxxx-vvv.DLB, where xxxx vvv is the product number, for example, 1315 for the G1315A DAD, and is the revision number, for example 104 is revision 1.04 For instructions refer to your user interface.
6 Introduction to the Detector Raw Data Conversion to Absorbance The raw data flow (from the photodiode array) and conversion to absorbance spectra for each data point is a multiple step process. This process is outlined in this section. For exact mathematical equations for the transformation, see the Understanding Your Agilent ChemStation handbook. Figure 63 shows the firmware flow diagram.
Introduction to the Detector 6 Subtract dark signal Raw data Temperature Temperatur e filter Gain correction Temperatur ecorrection Absorbance calculation Filtering Spectra runbuffer DAD Deuterium line data Signal calculation Wavelength axis linearization Wavelength calibration table Absorbance spectra Figure 63 LC signals Firmware Flow Diagram 1100 Series DAD and MWD Reference Manual 249
6 Introduction to the Detector Temperature Correction The quantum efficiency of the photodiode array depends on the temperature and is different for each wavelength. The temperature dependency follows a monotone increasing function over the wavelength scale, which means it increases with longer wavelengths (above 600 nm). To correct the intensity spectrum for temperature effects, the temperature on the photodiode array is averaged.
Introduction to the Detector 6 continuous, linear scale, an interpolation algorithm is applied. This algorithm uses a wavelength calibration table and actual wavelength data, derived from the deuterium emission lines at 486 nm and 656 nm. Wavelength calibration is done for each individual spectrograph during the production process. The individual calibration coefficients are stored in the wavelength calibration table in an EEPROM (electrically erasable PROM), which is part of the spectrograph electronics.
6 Introduction to the Detector slope of this signal (upslope, apex, downslope and baseline) and stores spectra according to the operator’s instructions. During the run the PD-peakwidth parameter can be changed by time-programming. Spectra Acquisition Modes (DAD only) The spectra acquisition mode allows automatic storage of spectra during a run. The mode can be changed during the run by time-programming.
Introduction to the Detector 6 Optional Interface Boards The Agilent 1100 Series modules have one optional board slot that allows addition of an interface board to the modules. Table 33 Optional Interface Boards Description Part Number BCD Board G1351-68701 Fuse 250 mA (four are on the board) 2110-0004 LAN Communication Interface Board G1369A or G1369-60001 BCD Board The BCD board provides a BCD output for the bottle number of the Agilent 1100 Series autosampler and four external contacts.
6 Introduction to the Detector There are general purpose cables available to connect the BCD output, see “BCD Cables” on page 220 and the external outputs, see “External Contact Cable” on page 224 to external devices.
Introduction to the Detector 6 LAN Communication Interface Board NOTE One board is required per Agilent 1100 stack. It is recommended to add the LAN board to the detector with highest data rate. NOTE The LAN board can only be used together with: a main board version G13XX-66520 (for G1315A, G1365A, G1314A, G1310A, G1311A, G1312A and G1313A) or newer and on all other 1100 modules. a DOS-ChemStation software revision A.06.01 or above. The following cards can be used with the Agilent 1100 modules.
6 Introduction to the Detector Interfaces The Agilent 1100 Series modules provide the following interfaces: Table 36 Agilent 1100 Series Interfaces Interface Type Pumps Autosampler DA Detector MW Detector FL Detector VW Detector RI Detector Thermostatted Vacuum Column Degasser Compartment CAN Yes Yes Yes Yes Yes No GPIB Yes Yes Yes Yes Yes No RS-232C Yes Yes Yes Yes Yes No Remote Yes Yes Yes Yes Yes Yes Analog Yes No 2× 1× No Yes* Interface board Yes Yes Yes
Introduction to the Detector 6 Analog Signal Output The analog signal output can be distributed to a recording device. For details refer to the description of the module’s main board. GPIB Interface The GPIB connector is used to connect the module with a computer. The address and control switches next to the GPIB connector determine the GPIB address of your module. The switches are preset to a default address and recognized by the operating software from Aligent Technologies.
6 Introduction to the Detector Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements. The subminiature D connector is used. The module provides one remote connector which is inputs/outputs (wired-or technique). To provide maximum safety within a distributed analysis system, one line is dedicated to SHUT DOWN the system’s critical parts in case any module detects a serious problem.
Introduction to the Detector Table 38 6 Remote Signal Distribution, continued Pin Signal Description 8 STOP (L) Request to reach system ready state as soon as possible (for example, stop run, abort or finish and stop injection). Receiver is any module performing run-time controlled activities. 9 START REQUEST (L) Request to start injection cycle (for example, by start key on any module). Receiver is the autosampler.
6 Introduction to the Detector Instrument DCD RX TX DTR GND DSR RTS CTS RI DB9 Male Figure 65 260 PC 1 2 3 4 5 6 7 8 9 DB9 Female 1 2 3 4 5 6 7 8 9 DB9 Female DCD RX TX DTR GND DSR RTS CTS RI DB9 Male RS-232 Cable 1100 Series DAD and MWD Reference Manual
Introduction to the Detector 6 Setting the 8-bit Configuration Switch The 8-bit configuration switch is located next to the GPIB connector. Switch settings provide configuration parameters for GPIB address, serial communication protocol and instrument specific initialization procedures.
6 Introduction to the Detector In the non-volatile memory, the parameters are kept, regardless of whether you turn the instrument off and on again. They will be kept until the same set of parameters is changed and the power is reset. All other previously stored configuration settings will still remain in the non-volatile memory. In this way, you can store more than one set of parameters using the same 8-bit configuration switch twice, for example, for both GPIB and RS-232C.
Introduction to the Detector 6 Communication Settings for RS-232C Communication The communication protocol used in this instrument supports only hardware handshake (CTS/RTS). Switches 1 in down and 2 in up position define that the RS-232C parameters will be changed. Once the change has been completed, the instrument must be powered up again in order to store the values in the non-volatile memory.
6 Introduction to the Detector Table 45 Parity Settings Switches Parity 7 8 0 0 No Parity 1 0 Odd Parity 1 1 Even Parity One start bit and one stop bit are always used (not selectable). Per default, the module will turn into 19200 baud, 8 data bit with no parity. Forced Cold Start Settings Switches 1 and 2 do not force storage of this set of parameters in non-volatile memory. Returning switches 1 and 2 to other positions (other than being both up) will allow for normal operation.
Introduction to the Detector 6 Stay-Resident Settings Firmware update procedures may require this mode in case of firmware loading errors. Switches 1 and 2 do not force storage of this set of parameters in non-volatile memory. Returning switches 1 and 2 to other positions (other than being both up) will allow for normal operation. If you use the following switch settings and power the instrument up again, the instrument firmware stays in the resident part, that is, it is not operable as a detector.
6 Introduction to the Detector The Main Power Supply Assembly The main power supply comprises a closed assembly (no onsite repair possibility). The power supply provides all DC voltages used in the module except for the voltages supplied by the lamp power supply to the deuterium and tungsten lamps in the detectors. The line voltage can vary in a range from 100 – 120 or 220 – 240 volts AC ± 10 % and needs no manual setting.
Introduction to the Detector 6 No accessible hardware fuse is needed because the main power supply is safe against any short circuits or overload conditions on the output lines. When overload conditions occur, the power supply turns off all output voltages. Turning the line power off and on again resets the power supply to normal operation if the cause of the overload condition has been removed.
6 268 Introduction to the Detector 1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 7 Control Module Screens for Agilent 1100 DAD and MWD Major keys on the Agilent 1100 Control Module 270 Control Module - Unsupported Module 271 Screens available from the Analysis screen 272 Screens available from the System screen 282 Screens available from the Records screen 284 Diagnostics and Tests 290 Agilent Technologies 269
7 Control Module Screens for Agilent 1100 DAD and MWD Major keys on the Agilent 1100 Control Module Table 49 NOTE ESC Return to previous screen and scroll through top layer views (Analysis, Settings) m Open context sensitive menus i Information/help Enter Store changed parameters or execute the choice from a pull-down menu On/Off Switch on lamp(s) Start Start a run Plot View the chromatogram Views Change between view of analysis - status - system screens The screens shown on the next pa
Control Module Screens for Agilent 1100 DAD and MWD 7 Control Module - Unsupported Module In case the control module shows the following screen and the yellow LED on the detector is not flashing, the used firmware in the Control Module is not able to control the G1315B DAD or G1365B MWD. These detectors require firmware revision B.01.04 or above (G1323B).
7 Control Module Screens for Agilent 1100 DAD and MWD Screens available from the Analysis screen The Analysis screen This is the wake-up screen, if the Agilent 1100 detector is the only configured Agilent 1100 module. It is used to enter the most common detector method parameters. The m-key allows access to the context sensitive menu. Setup view leads you to add sections for additional Agilent 1100 modules. Restart re-boots the control module. Lamp ON/OFF Use the F8 key (On/Off) to turn on the lamp(s).
Control Module Screens for Agilent 1100 DAD and MWD 7 The lamp(s) can be selected individually. Setup View In the Setup view, e.g. another module can be added to the view.
7 Control Module Screens for Agilent 1100 DAD and MWD Here, e.g. the column compartment parameters are shown on the display as well. The number of parameters on the display are restricted as additional modules are added. Maximum 4 modules are shown automatically. If more modules are in the system, you have to chose in Setup view. With the Settings key you open a pull-down menu where you can select the DAD modules.
Control Module Screens for Agilent 1100 DAD and MWD 7 Use the m-key for the context sensitive menu. The Status command pulls up a monitor screen displaying signals and spectra as programmed. Reset will load the DAD or MWD default parameters. Balance brings the baseline back to set offset. Use F1-key (More) opens a pull-down menu. Selecting More and Settings pull down menu you can enter special DAD or MWD setpoints.
7 Control Module Screens for Agilent 1100 DAD and MWD Selecting More and Signals C-E on the pull down menu you can enter additional DAD or MWD signal parameters. Settings - Timetable With the F2 key (Timetable) you can list the timetable for the DAD or MWD. Press F7 key (Insert) to add entries or F6 key (Delete) to remove entries.
Control Module Screens for Agilent 1100 DAD and MWD 7 Press the F7 key (Insert) to add a timetable events. Use the F6 key (Done) to view the entered lines of the timetable. Use the m-key for the context sensitive menu. It gives you additional tools for the timetable. Settings - Analog With the F3 key (Analog) you can change the settings for the analog outputs.
7 Control Module Screens for Agilent 1100 DAD and MWD Settings - Spectrum Range FOR G1315A/B DAD: With the F4 key (Spectrum) you can change the settings for the spectrum acquisition. FOR G1365A/B MWD: You can change the settings for the spectrum acquisition (STOP FLOW). The spectrum is started via “Sample, Holmium and Dark Current Spectrum” on page 291. Settings - Run times With the F5 key (Runtimes) you can change the stop time and the post-run time.
Control Module Screens for Agilent 1100 DAD and MWD 7 Press F5 key (Views) and select Status. Status This is an example if an Agilent 1100 DAD or MWD is configured standalone.
7 Control Module Screens for Agilent 1100 DAD and MWD Signal plot Press F6 key (Plot) to enter the plot screen (available also from the Analysis and System screen). Here you can observe the online signal(s). To add additional online signals (maximum 3), press F6 key (Select). If more than one signal is configured (see next), use the 1-2-3 number key to switch between the signals. Press F6 key (Select). Here you can add additional online signals (maximum are 3), press F6 key (Select).
Control Module Screens for Agilent 1100 DAD and MWD 7 Method screens Use ESC to return to the Analysis screen. Use the F3 key (Method) to view the parameters in a method and F8 key (Save As) to save the method in the module(s). The PC-Card key is only active when a PCMCIA card is inserted in the control module. Use F2 key (PC-Card) to save a method on a PCMCIA card. Use the Right/Left arrows to switch between PC-Card and Instrument window. Use the UP/Down arrows to select the method.
7 Control Module Screens for Agilent 1100 DAD and MWD Screens available from the System screen System screen Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. This screen shows the last activities in the system. System - Control Use the F1 key (Control) to select the FL-Detector. Here you receive information about the not-ready conditions if needed. F2 key (Reset) does a re-initialization of the DAD or MWD.
Control Module Screens for Agilent 1100 DAD and MWD 7 System - Configuration Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F2 key (Configure) to select the DAD or MWD. Here you define further special setpoints for the DAD or MWD operation. Use the F1 key (Interfaces) to access the interface settings (if required).
7 Control Module Screens for Agilent 1100 DAD and MWD Screens available from the Records screen Records screen Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F4 key (Records) to select the DAD or MWD. Errors are reported either into the System Log (F2) or Error Log (F3). System / Error Log Use the F2 key (System Log) or F3 key (Error Log) to look for errors.
Control Module Screens for Agilent 1100 DAD and MWD 7 Info Log Use the m-key to receive a pop-up menu, Select Info Log. A list of the last events are listed. For troubleshooting reasons they can be printed or saved to a file on the PCMCIA card. EMF (Early Maintenance Feedback) Use the F1 key (EMF) to set EMF parameters. Choose menu item 1 (Setup limits) to select lamp-on level for the UV and Vis lamp at which you want to receive a warning. If a set limit has been exceeded, a message box will pop up.
7 Control Module Screens for Agilent 1100 DAD and MWD Firmware Update Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F3 key (Records) to select the DAD or MWD. Use the F5 key (FW Update) to enter the Update section. If you want to update the resident firmware (together with specific main firmware revisions), select the a file from the PCMCIA card (RES_n_nn.DLB) and press execute.
Control Module Screens for Agilent 1100 DAD and MWD 7 Use the F5 key (FW Update) to enter the Update section. Select the file from the PCMCIA card (1315-nnn.DLB for DAD or 1365-nnn.DLB for MWD) and press execute. When the update has finished the update, press F7 key (Transfer) to return the module into the normal mode (LED on module should stay yellow). If you have not saved your methods, please do it before continuing. Otherwise they will be overwritten during the update process.
7 Control Module Screens for Agilent 1100 DAD and MWD Changing the serial number In case the serial number of the module has to be added, use the m-key to open the menu Enter Serial#. Choose System from the pull-down menu. Use the F3 key (Records) to select the DAD or MWD. Use the F4 key (Maint log) to view and edit the maintenance logbook.
Control Module Screens for Agilent 1100 DAD and MWD 7 Maintenance activities Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F3 key (Records) to select the DAD or MWD. Use the F4 key (Maint log) to view and edit the maintenance logbook. Use the F7 key (Add) to add new maintenance activities. If an activity is not listed, you can type the activity into the line “Add” using the control modules key pad.
7 Control Module Screens for Agilent 1100 DAD and MWD Diagnostics and Tests Tests screen Use the Esc key to receive Views on the F5 key. Choose System from the pull-down menu. Use the F3 key (Tests) to select the DAD or MWD. Several tests are available to test the Agilent 1100 DAD or MWD. Additional test are listed in the function box. Refer to “Troubleshooting and Test Functions” on page 49 for more information on the tests.
Control Module Screens for Agilent 1100 DAD and MWD 7 Wavelength Calibration Use the F1 key (Calibrate) and then F8 key (Execute) to start the DAD or MWD wavelength calibration (with water in the flow cell). If a deviation is found, press Adjust. Sample, Holmium and Dark Current Spectrum Use the F2 key (Spectrum) to take a spectrum (sample, dark current or holmium). Use the Left/Right arrow to move the curser within the spectrum to find the wavelength of interest.
7 Control Module Screens for Agilent 1100 DAD and MWD Built-in Test Chromatogram (Simulation) To start the built-in test chromatogram, use the F8 key (Execute) to enable the simulation. Then press the m-key to open the pop-up menu. Select Start to start a run (all modules in the Agilent 1100 system must be in ready state).
Control Module Screens for Agilent 1100 DAD and MWD 7 Use the F6 key (Plot) to view the signal. A simulated chromatogram (4 peaks) will repeat until the run is stopped. The signal is also available on the analog output. A change of the peak width will change the retention times. Slit Test Use the F3 key (Slit Test) to test the movement of the electromechanical slit assembly.
7 294 Control Module Screens for Agilent 1100 DAD and MWD 1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual 8 Specifications Performance Specifications 296 Agilent Technologies 295
8 Specifications Performance Specifications Table 50 296 Performance Specifications Agilent 1100 Series DAD and MWD Type Specification Comments Detection type 1024-element photodiode array Light source Deuterium and tungsten lamps Wavelength range 190 – 950 nm Short term noise (ASTM) Single and Multi-Wavelengt ± 1 × 10-5 AU at 254 and 750 nm See “” on page 297 Drift 2 × 10-3 AU/hr at 254 nm See “” on page 297 Linear absorbance range > 2 AU (upper limit) See “” on page 297 Wavelength a
Specifications Table 50 8 Performance Specifications Agilent 1100 Series DAD and MWD, continued Type Specification Control and data evaluation Agilent ChemStation for LC Analog outputs Recorder/integrator: 100 mV or 1 V, output range 0.
8 298 Specifications 1100 Series DAD and MWD Reference Manual
Agilent 1100 Series Diode Array and Multiple Wavelength Detectors Reference Manual A Safety Information General Safety Information 300 Lithium Batteries Information 303 Disposal of Mercury from Deuterium Lamp 304 Radio Interference 305 Sound Emission 306 UV-Radiation 307 Solvent Information 308 Declaration of Conformity for HOX2 Filter 310 Agilent Technologies on Internet 311 Agilent Technologies 299
A Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Aligent Technologies assumes no liability for the customer’s failure to comply with these requirements.
Safety Information CAUTION A The operator of this instrument is advised that if the equipment is used in a manner not specified in this manual, the protection provided by the equipment may be impaired. Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed. Energy available at many points may, if contacted, result in personal injury.
A Safety Information Safety Symbols Table 51 shows safety symbols used on the instrument and in the manuals. Table 51 Symbol ! Safety Symbols Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage. Indicates dangerous voltages. Indicates a protected ground terminal. Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product.
Safety Information A Lithium Batteries Information WA R N I N G Danger of explosion if battery is incorrectly replaced. Replace only with the same or equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed.
A Safety Information Disposal of Mercury from Deuterium Lamp The long-life deuterium lamp (part number 5181-1528) includes a timer, which contains mercury. The timer has to be disposed of locally according to national waste disposal regulations.
Safety Information A Radio Interference Never use cables other than the ones supplied by Aligent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and/or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.
A Safety Information Sound Emission Manufacturer’s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991. This product has a sound pressure emission (at the operator position) < 70 dB.
Safety Information A UV-Radiation Emissions of ultraviolet radiation (200-315 nm) from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs (Threshold Limit Values) according to the American Conference of Governmental Industrial Hygienists: Table 52 UV-Radiation Limits Exposure/day Effective Irradiance 8 hours 0.1 µW/cm2 10 minutes 5.
A Safety Information Solvent Information Observe the following recommendations on the use of solvents. Flow Cell Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and thus impair the optical properties of the flow cell. Prevent any crystallization of buffer solutions. This will lead into a blockage/damage of the flow cell. If the flow cell is transported while temperatures are below 5 degree C, it must be assured that the cell is filled with alcohol.
Safety Information A • Chromatographic grade ethers, which can contain peroxides (for example, THF, dioxane, di-isopropylether) such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides. • Solutions of organic acids (acetic acid, formic acid, and so on) in organic solvents. For example, a 1-% solution of acetic acid in methanol will attack steel. • Solutions containing strong complexing agents (for example, EDTA, ethylene diamine tetra-acetic acid).
A Safety Information Declaration of Conformity for HOX2 Filter We herewith inform you that the holmium oxide glass filter (type Hoya HY-1) (Part No. 79880-22711) meets the following specification of absorbance maxima positions: 361.0 nm - 418.9 nm - 453.7 nm - 536.7 nm (spectral bandwidth: 2 nm). Agilent Technologies guarantees the traceability of the specified absorbance maxima to a National Institute of Standards & Technology (NIST) holmium oxide solution standard with a lot-to-lot tolerance of ±0.3nm.
Safety Information A Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at: http://www.agilent.com Select “Products” - “Chemical Analysis” It will provide also the latest firmware of the Agilent 1100 series modules for download.
A 312 Safety Information 1100 Series DAD and MWD Reference Manual
Index A accessory kit, 18, 208 accuracy of wavelength, 296 achromat (source lens), 229 Agilent on internet, 311 algea information, 308 alpha and beta line, 84 analog signal output, 257 APG remote interface, 257 array, 230 ASTM environmental conditions, 15 ASTM - reference, 297 cell support windows, 229 choosing a flow cell, 32 configuration switch default settings, 261 description and factory settings, 261 control module diagnostics and tests, 290 EMF, 285 firmware update, 286 serial number change of MWD,
Index visible lamp current, 67 visible lamp voltage, 68 wavelength calibration failed, 70 ESD (electrostatic discharge) strap, 98 exchanging.
Index for sensitivity, selectivity, linearity, dispersion, 33 how to get the best performance, 30 margins for negative absorbance, 43 of selectivity, 44 overview, 31 peak width, 35 sample and reference wavelength, 36 slit width, 39 spectra acquisition, 42 theshold, 43 P parts identification, 181 accessory kit, 208 achromat (source lens), 199 cable overview, 210 cables - analog, 212 cables - APG remote, 215 cables - auxiliary, 222 cables - BCD, 220 cables - CAN, 223 cables - external contact, 224 cables -
Index spectrograph, 229, 230 diodes per nm, 230 stack configuration, 20, 21 front view, 20 rear view, 21 steps, 42 T temperature control, 245 test chromatogram on control module, 292 test functions, 50 tests dark current, 85, 91 filter, 85, 93 flow cell, 85, 90 holmium oxide, 85, 86 intensity, 85, 88 overview, 85 tests on control module, 290 threshold, 43 troubleshooting error messages, 50, 53 status indicators, 50, 51 U unpacking, 17 unsupported Module, 271 using EMF, 235 uv-radiation, 307 V variable e
www.agilent.com In This Book This manual contains technical reference information about the Agilent 1100 Series diode array detectors. The manual describes the following: • installing the detector, • introduction to the diode array detector and its optimization, • diagnostics and troubleshooting, • repairing the detector, • parts and materials, • theory of operation, and • screens of the local control module.
