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252

1100 Series FD Reference Manual

7

Introduction to the Fluorescence Detector

Phosphorescence Detection

An appropriate parameter set will be specified as soon as you chose the 
phosphorescence detection mode (special setpoints under FLD parameter 
settings).

Figure 84

Measurement of Phosphorescence

Time [µsec]

Intensity

100%

Measurement

Flash

Phosphorescence

Summary of Contents for 1100 Series

Page 1: ...s1 Agilent 1100 Series Fluorescence Detector Reference Manual Agilent G1321A Asset 304025 ...

Page 2: ...s document that conflict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend Software and technical data rights granted to federal government customers include only th...

Page 3: ...erstand what you are doing and why This chapter explains in detail how to optimize detection 4 Troubleshooting and Test Functions This chapter describes the detector s built in troubleshooting and test functions 5 Repairing the Fluorescence Detector Instructions on how to repair the detector 6 Identifying Parts and Materials Detailed illustrations and listings for parts and materials identificatio...

Page 4: ...is intended to introduce an operator to the screens available for operation of the Agilent 1100 diode array detector with the Agilent 1100 control module Please use the manual of Control module for further detailed reference 10 Specifications Performance specifications of the detector ...

Page 5: ...st Steps with the Fluorescence Detector Before You Start 30 Optimization Overview 31 Getting Started and Checkout 33 Starting Your Detector 33 Setting the Chromatographic Conditions 34 Observe the maxima via the isoabsorbance plot 36 Method Development 37 Step 1 Check the LC system for impurities 38 Step 2 Optimize limits of detection and selectivity 39 Step 3 Set up routine methods 48 Example Opt...

Page 6: ...e Time 69 Reducing Stray Light 71 4 Troubleshooting and Test Functions Overview of the Detector s Indicators and Test Functions 74 Status Indicators 75 Power Supply Indicator 75 Detector Status Indicator 76 Error Messages 77 Time out 78 Shutdown 79 Remote Time out 80 Synchronization Lost 81 Leak 82 Leak Sensor Open 84 Leak Sensor Short 85 Compensation Sensor Open 86 Compensation Sensor Short 87 Fa...

Page 7: ...he Flow Cell 111 Wavelength Calibration 112 Verification 113 Test Functions 114 Lamp Intensity Test 115 Lamp Intensity History 116 Dark Current Test 117 Excitation and Emission Grating Resistance History 118 Raman ASTM Signal to Noise Test 119 Using the Built in Test Chromatogram 124 Using the Built in DAC Test 127 5 Repairing the Fluorescence Detector Introduction into Repairing the Fluorescence ...

Page 8: ...ter 168 Replacing the Mirror Assembly 172 Replacing the Slits 176 Removing the Optical Unit 178 Replacing PMT and or FLF board 180 Replacing FLL board and Trigger Pack 183 Replacing the EM and EX Grating 187 Exchanging the Power Supply 190 Replacing Status Light Pipe 193 Installing the Optical Unit 194 Replacing the Foams and Covers 196 Assembling the Main Cover 198 Replacing the Interface Board 1...

Page 9: ...Cables 229 Auxiliary Cable 232 CAN Cable 233 External Contact Cable 234 RS 232 Cable Kit 235 LAN Cables 236 7 Introduction to the Fluorescence Detector Introduction to the Detector 238 How the Detector Operates 239 Raman Effect 242 Optical Unit 243 Reference System 250 Analytical Information From Primary Data 251 Fluorescence Detection 251 Phosphorescence Detection 252 Processing of Raw Data 253 E...

Page 10: ...Firmware Updates 275 Raw Data Conversion to Fluorescence LU Units 276 Data flow for chromatographic output 277 Data flow for spectral output 278 Spectra Acquisition Modes 281 Optional Interface Boards 282 BCD Board 283 LAN Board 284 Interfaces 285 Analog Signal Output 286 GPIB Interface 286 CAN Interface 286 Remote Interface 287 RS 232C 288 Setting the 8 bit Configuration Switch 290 GPIB Default A...

Page 11: ... 299 Screens available from the System screen 315 Screens available from the Records screen 318 Diagnostics and Tests 323 10 Specifications Performance Specifications 328 A Safety Information General Safety Information 332 Lithium Batteries Information 335 Radio Interference 336 Sound Emission 337 UV Radiation 338 Solvent Information 339 Declaration of Conformity for HOX2 Filter 340 Agilent Techno...

Page 12: ...12 1100 Series FD Reference Manual ...

Page 13: ...ference Manual Agilent Technologies 1 Installing the Fluorescence Detector Site Requirements 14 Physical Specifications 16 Unpacking the Detector 17 Optimizing the Stack Configuration 20 Installing the Detector 22 Flow Connections to the Detector 24 ...

Page 14: ...tical It plugs into the power input socket at the rear of the detector The male end of each power cord is different and designed to match the wall socket of a particular country or region WARNING To disconnect the detector from line unplug the power cord The power supply still uses some power even if the power switch on the front panel is turned off WARNING Shock hazard or damage of your instrumen...

Page 15: ...le 1 on page 16 ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification refer also to Performance Specifications on page 328 is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest perfor...

Page 16: ...ge 100 120 or 220 240 VAC 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 180 VA 70 W 239 BTU Maximum Ambient operating temperature 0 40 C 32 104 F Ambient non operating temperature 40 70 C 4 158 F Humidity 95 at 25 40 C 77 104 F Non condensing Operating altitude Up to 2000 m 6500 ft Non operating altitude Up to 4600 m 14950 ft For storing the detector Safety standards IE...

Page 17: ...ent Delivery Checklist Ensure all parts and materials have been delivered with the detector The delivery checklist is shown below Please report missing or damaged parts to your local Agilent Technologies sales and service office CAUTION If there are signs of damage please do not attempt to install the detector Table 2 Detector Checklist Description Quantity Detector 1 Power cable 1 CAN cable Part ...

Page 18: ...100 1516 2 Capillary column detector one side preinstalled 380 mm lg 0 17 mm i d includes G1315 87311 1 Ferrule front SST 0100 0043 1 Ferrule back SST 0100 0044 1 Fitting SST 79814 22406 1 Hex key set 1 5 mm 8710 0641 1 Screwdriver hexagonal 4 mm 100 mm long 5965 0027 1 Screwdriver hexagonal 2 5 mm 100 mm long 5965 0028 1 Needle Syringe 9301 0407 Glass Syringe 9301 1446 Calibration Sample Glycogen...

Page 19: ...e Detector 1 1100 Series FD Reference Manual 19 Figure 1 Waste Tubing Parts Figure 2 Inlet Capillary Column Detector Parts Fitting male PEEK Tubing Ferrule front This side is preinstalled Ferrule back Fitting male SST Capillary ...

Page 20: ...a complete Agilent 1100 Series system you can ensure optimum performance by installing the following configuration This configuration optimizes the system flow path ensuring minimum delay volume Figure 3 Recommended Stack Configuration Front View Solvent cabinet Vacuum degasser Pump Column compartment Autosampler Detector Control module ...

Page 21: ... Fluorescence Detector 1 1100 Series FD Reference Manual 21 Figure 4 Recommended Stack Configuration Rear View GPIB or LAN to LC ChemStation Analog signal to recorder AC power Remote cable CAN Bus cable CAN Bus cable ...

Page 22: ... 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 7 Connect the analog cable s optional Preparations Locate bench space Provide power connections Unpack the detector Parts required Detector Power cord for...

Page 23: ...ch Interface board LAN or BCD EXT Security lever 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 WARNING To disconnect the detector from line unplug the power cord The power supply still uses some power even if the power switch at the front...

Page 24: ... observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used NOTE The flow cell is shipped with a filling of isopropanol also recommended when the instrument and or flow cell is shipped to another location This is to avo...

Page 25: ...ed before the fluorescence detector to prevent any overpressure to the quartz cell maximum 20 bar When working with detector behind the FLD on own risk determine the backpressure of this detector first by removing the column and the last detect and measuring system pressure at the application flow rate connecting the last detector without column and FLD and measuring the system pressure with flow ...

Page 26: ...r 5 Insert the flow cell and install the capillaries to the flow cell top is outlet bottom is inlet 6 Connect the waste tubing to the bottom waste fitting 7 Establish flow and observe if leaks occur 8 Replace the front cover The installation of the detector is now complete ...

Page 27: ...Detector Reference Manual Agilent Technologies 2 First Steps with the Fluorescence Detector Before You Start 30 Optimization Overview 31 Getting Started and Checkout 33 Method Development 37 Example Optimization for Multiple Compounds 52 ...

Page 28: ...usually give good results most of the time But experience shows that baseline noise can be higher lower signal to noise ratio when impurities are in the solvents Flush your solvent delivery system for at least 15 minutes before checking sensitivity If your pump has multiple channels you should also flush the channels not in use ...

Page 29: ...tion 2 Using an appropriate response time For most applications a setting of 4 seconds is adequate Only for high speed analyses short columns at high flow rates a lower setting is recommended Bear in mind that even if the response time is too high fast peaks will appear a little smaller and broader but retention time and peak areas are still correct and reproducible 3 Finding the optimum wavelengt...

Page 30: ...n contrast to other LC detectors the G1321A fluorescence detector equilibrates within seconds after the lamp is switched on 6 Do not overpressurize the detector quartz flow cell Be aware to not exceed a 20 bar pressure drop after the flow cell when hooking up additional devices like other detectors or a fraction collector It s better to place a UV detector before the G1321A fluorescence detector N...

Page 31: ...strument performs some internal checks and a calibration check which takes about 5 minutes 3 You are now ready to change the settings of your detector When required If you want to checkout the detector Hardware required LC system with G1321A FLD Parts required Start up Kit 5063 6528 includes Column Hypersil ODS 125 mm x 4 mm i d with 5 µm particles Part number 7982618 564 Cartridge Holder for colu...

Page 32: ...onditions Mobile phases A water 35 B Acetonitrile 65 Column OSD Hypersil column 125 mm x 4 mm i d with 5 µm particles Sample Isocratic standard sample 1 10 diluted in methanol Flow rate 1 5 ml min Compressibility A water 46 Compressibility B Acetonitrile 115 Stroke A and B auto Stop time 4 minutes Injection volume 5 µl Oven temperature 1100 30 C FLD Excitations Emission Wavelength EX 246 nm EM 317...

Page 33: ...parate screens 3 Start the run 4 The resulting chromatograms are shown in Figure 8 5 The excitation maxima is around 250 nm Figure 7 FLD Parameters Figure 8 Biphenyl peak with different excitation wavelengths In this example additional excitation wavelengths B C D are used This will increase the scan time and may lower the performance Ex 230 nm Ex 246 nm Ex 250 nm Ex 290 nm Biphenyl peak ...

Page 34: ... First Steps with the Fluorescence Detector Observe the maxima via the isoabsorbance plot 1 Load the data file λEX 246 nm λEM 317 nm and open the isoabsorbance plot 2 The maximum λEX will be found around 250 nm Figure 9 Isoabsorbance Plot ...

Page 35: ... from the operation modes during these steps Table 5 Steps for thorough method development Step 1 Check system Step 2 Optimize limits of detection and selectivity Step 3 Set up routine methods Fluorescence scan Find impurities for example in solvents and reagents Determine simultaneously the excitation and emission spectra of a pure compound Signal mode Perform wavelength switching Use for lowest ...

Page 36: ...t colors reflect different intensities Figure 10 shows a sample of slightly impure water which was planned for use as mobile phase The area where fluorescence of the contaminated water sample can be seen is between the stray light areas the first and second order Raleigh stray light and Raman stray light Since excitation and emission wavelength are the same for Raleigh stray light the area of firs...

Page 37: ...f interest Excitation and emission wavelengths can be selected for optimum limits of detection and best selectivity In general fluorescence spectra obtained with different instruments may show significant differences depending on the hardware and software used The traditional approach is to extract an appropriate excitation wavelength from the UV spectrum that is similar to the fluorescence excita...

Page 38: ...D and emission spectra with the FLD both in a single run Procedure I Take a fluorescence scan Because fluorescence spectra traditionally have not been easily available with previous LC fluorescence detectors standard fluorescence spectrophotometers have been used in the past to acquire spectral information for unknown compounds Unfortunately this approach limits optimization as there are differenc...

Page 39: ...noise that may be different upon excitation at 250 nm 315 nm or 350 nm The maximum of emission is observed at 440 nm Details for Figure 12 on page 42 All excitation and emission spectra of Quinidine 1 µg ml are shown in graphic Fluorescence intensity is plotted vs excitation and emission wavelengths Detector settings step size 5 nm PMT 12 Response time 4 s ...

Page 40: ... Series FD Reference Manual 2 First Steps with the Fluorescence Detector Figure 12 Characterization of a pure compound from a fluorescence scan 350 nm Ex 315 nm Ex 250 nm Ex Ex axis Em axis straylight 1 order ...

Page 41: ...st fluorophores show strong absorption at these wavelengths and the quantum yield is high Excitation is sufficient for collecting emission spectra Figure 13 on page 44 contains all emission spectra obtained in a single run from a mix of 15 PNAs This set of spectra is used to set up a timetable for optimum emission wavelengths for all compounds The individual compound spectra in the isofluorescence...

Page 42: ... water B acetonitrile 50 50 Gradient 3 minutes 60 14 minutes 90 22 minutes 100 Flow rate 0 4 ml min Column temperature 18 C Injection volume 5 µl FLD settings PMT 12 response time 4 s step size 5 nm Figure 13 Optimization of the time program for the emission wavelength This shows the isofluorescence plot of emission spectra for 15 PNAs 5 µg ml with a fixed excitation wavelengths 260 nm ...

Page 43: ...optimized switching events for this example are summarized in Table 8 This timetable gives the conditions for optimum detection based on the results of two chromatographic runs Figure 14 Optimization of the time program for the excitation wavelength Table 8 Timetable for the analysis of 15 polynuclear aromatic hydrocarbons Time min Exitation Wavelength nm Emission Wavelength nm 0 260 350 8 2 260 4...

Page 44: ... available from the diode array detector the fluorescence detector is set to acquire emission spectra with a fixed excitation wavelength in the low UV range The example is taken from the quality control of carbamates Samples are analyzed for the impurities 2 3 diamino phenazine DAP and 2 amino 3 hydroxyphenazine AHP Reference samples of DAP and AHP were analyzed with diode array and fluorescence d...

Page 45: ...ities This is an impurity of carbamates The excitation spectrum in a second run shows the equivalence of UV spectra and fluorescence excitation spectra An excitation wavelength at 265 nm was used for taking the emission spectrum and an emission wavelength at 540 nm was used for taking the excitation spectrum The two upper traces are obtained using two different excitation wavelengths The lower tra...

Page 46: ...y than timetable controlled wavelength switching The Agilent 1100 Series FLD can in addition acquire fluorescence spectra while it records the detector signals for quantitative analysis Therefore qualitative data are available for peak confirmation and purity checks in routine analysis Table 9 Conditions for Figure 15 and Figure 16 on page 47 Column Zorbax SB 2 x 50 mm PNA 5 µm Mobile phase A wate...

Page 47: ...ative analysis Apart from complex matrices this is advantageous when watching for impurities at additional wavelengths It is also advantageous for reaching low limits of detection or increasing selectivity through optimum wavelength settings at any time The number of data points acquired per signal is reduced and thus limits of detection may be higher depending on the detector settings compared to...

Page 48: ...evelopment fluorescence excitation and emission spectra are collected from reference standards and entered into a library at the choice of the method developer All spectral data from unknown samples can then be compared automatically with library data Table 3 illustrates this principle using a PNA analysis The match factor given in the report for each peak indicates the degree of similarity betwee...

Page 49: ...ak confirmation using a fluorescence spectral library Meas Library CalTbl RetTime Signal Amount Purity Match Libary Name min min min ng Factor 4 859 4 800 5 178 1 1 47986e 1 1 993 Naphthalene em 6 764 7 000 7 162 1 2 16156e 1 1 998 Acenaphthene em 7 137 7 100 7 544 1 1 14864e 1 1 995 Fluorene em 8 005 8 000 8 453 1 2 56635e 1 1 969 Phenanthrene em 8 841 8 800 9 328 1 1 76064e 1 1 993 Anthracene em...

Page 50: ...are shown in Figure 18 on page 53 Table 12 Chromatographic Conditions Mobile phases A water 50 B Acetonitrile 50 Column Vydac C18 PNA 250 mm x 2 1 mm i d with 5 µm particles Sample PAH 0 5 ng Flow rate 0 4 ml min Compressibility A water 46 Compressibility B Acetonitrile 115 Stroke A and B auto Time Table at 0 minutes B 50 at 3 minutes B 60 at 14 5 minutes B 90 at 22 5 minutes B 95 Stop time 26 min...

Page 51: ... signal In this example just the time range of 13 minutes is displayed Figure 18 Detector Settings for Emission Scan DO NOT select additional emission wavelengths B C D Doing so will increase the scan time and will lower the performance Select a Excitation wavelength in the low UV 230 260 nm This will cover nearly all fluorescenceinyour sample ...

Page 52: ... 2 First Steps with the Fluorescence Detector 4 Use the isoabsorbance plot and evaluate the optimal emission wavelengths shown in the table below Figure 19 Chromatogram from Emissions Scan Figure 20 Isoabsorbance Plot from Emission Scan ...

Page 53: ...tion of the optimal excitation wavelength See Figure 21 Table 13 Peak Time Emission Wavelength 1 5 3 min 330 nm 2 7 2 min 330 nm 3 7 6 min 310 nm 4 8 6 min 360 nm 5 10 6 min 445 nm 6 11 23 min 385 nm Figure 21 Detector Settings for Excitation Scan DO NOT select additional excitation wavelengths B C D Doing so will increase the scan time and will lower the performance ...

Page 54: ...e baseline stabilizes Start the run 7 Load the signal 8 Use the isoabsorbance plot and evaluate the optimal excitation wavelengths in this example just in the time range of 13 minutes Figure 22 Chromatogram excitation scan at reference wavelength 260 330 nm Figure 23 Isoabsorbance Plot Excitation ...

Page 55: ...he complete information about emission from Figure 20 on page 54 and excitation maxima Table 14 Peak Time Emission Wavelength Excitation Wavelength 1 5 3 min 330 nm 220 280 nm 2 7 3 min 330 nm 225 285 nm 3 7 7 min 310 nm 265 nm 4 8 5 min 360 nm 245 nm 5 10 7 min 445 nm 280 nm 6 11 3 min 385 nm 270 330 nm ...

Page 56: ...o your needs 3 Set PMT gain to 16 4 Define a data file name and take a fluorescence scan After the scan is completed the isoabsorbance scan results appear see Figure 25 on page 59 NOTE The scan time will increase when the range is enlarged With the default values the scan takes about 2 minutes Figure 24 FLD special settings The wavelength range and step number defines the duration Using the maximu...

Page 57: ... Reference Manual 59 NOTE A low background will improve the signal to noise see also Reducing Stray Light on page 71 Figure 25 Fluorescence Scan of Water Note This white area is normally dark blue Raleigh scattering Raman scattering of water 2nd order of cutoff ...

Page 58: ...60 1100 Series FD Reference Manual 2 First Steps with the Fluorescence Detector ...

Page 59: ...ies 3 Optimizing the Fluorescence Detector Optimization Overview 62 Design Features Help Optimization 63 Finding the Best Wavelengths 64 Finding the Best Signal Amplification 66 Changing the Xenon Flash Lamp Frequency 67 Selecting the Best Response Time 69 Reducing Stray Light 71 ...

Page 60: ...62 1100 Series FD Reference Manual 3 Optimizing the Fluorescence Detector Optimization Overview Refer to Optimization Overview on page 31 for details ...

Page 61: ...ing to the specifications published by Agilent Technologies Your normal LC grade solvents may give good results most of the time but our experience shows that baseline noise can be higher with LC grade solvents than with fluorescence grade solvents Flush your solvent delivery system for at least 15 minutes before checking sensitivity If your pump has multiple channels you should also flush the cha...

Page 62: ...ngs As most organic molecules absorb best in the ultra violet range the Agilent 1100 fluorescence detector was designed to give an optimum signal to noise ratio in the 210 nm to 360 nm range of the spectrum To achieve greatest sensitivity the absorbance wavelength of your sample molecule should match the wavelength range for your instrument In other words an excitation wavelength in the ultra viol...

Page 63: ...n you are looking for the wavelength by scanning scan over the whole range As this example shows a maximum may be found in a completely different wavelength range Figure 26 Scan Orthophthalaldehyde Derivative of Alanine NOTE When comparing fluorescence excitation spectra directly with DAD spectra or literature based absorbance spectra you should consider large differences in the used optical bandw...

Page 64: ...s diluted 1000 times With increasing PMTGAIN there was an improvement in signal to noise up to 10 Above 10 the noise increased proportionately to the signal with no improvement in signal to noise The reason for this is the fact that quantification of baselines especially at low background levels is not sufficient for statistically working filter methods For the best gain check your solvent under f...

Page 65: ...nto the following modes Best sensitivity can be expected with no economy see Figure 28 Table 16 Flash Lamp Modes Positioning 296 Hz Standard 560 V 63 mJoule 18 8 W 74 Hz Economy 560 V 63 mJoule 4 7 W Rotation Multi Ex Em 74 Hz Standard 950 V 180 mJoule 13 3 W 74 Hz Economy 560 V 63 mJoule 4 7 W Figure 28 Xenon Flash Lamp Frequency Standard 296 Hz Economy 74 Hz ...

Page 66: ...3 Optimizing the Fluorescence Detector Lamp life savings There are three ways to save lamp life switch to lamp on during run without loss of sensitivity switch to economy mode with a certain loss of sensitivity a combination of the above ...

Page 67: ...3 1100 Series FD Reference Manual 69 Selecting the Best Response Time Data reduction using the RESPONSETIME function will increase your signal to noise ratio For example see Figure 29 Figure 29 Finding Best Response Time 1 sec 4 sec 8 sec ...

Page 68: ... the Agilent 1100 fluorescence detector is 4 seconds It is important to know that comparing sensitivity requires using the same response time A response time of 4 seconds default is equivalent to a time constant of 1 8 seconds and appropriate for standard chromatographic conditions Figure 30 Separation of Peaks using Responsetime Responsetime 2 sec Responsetime 8 sec ...

Page 69: ...n the emission wavelength is twice the excitation wavelength the 2nd order light is the limiting factor To explain the effect of such higher order light assume the detector is on but no sample is eluting through the flow cell The lamp sends 1 million photons into the flow cell at for example 280 nm Scattering on the surface of the flow cell and scattering from the molecules of solvent allow 0 1 of...

Page 70: ...of a known set of applications a 295 nm cut off filter is built in for undisturbed application up to 560 nm without compromises see Figure 31 on page 72 Figure 31 Reducing Stray Light Straylight Exitation300nm Secondorder light600nm nofilter filter280nm LU Wavelength nm Fluorescence ...

Page 71: ...l Agilent Technologies 4 Troubleshooting and Test Functions Overview of the Detector s Indicators and Test Functions 74 Status Indicators 75 Error Messages 77 Wavelength Verification and Calibration 101 The Wavelength Calibration Procedure 110 Test Functions 114 ...

Page 72: ...or message in the user interface For each message a short description of the failure a list of probable causes of the problem and a list of suggested actions to fix the problem are provided see Error Messages on page 77 Wavelength Recalibration Wavelength recalibration is recommended after repair of internal components to ensure correct operation of the detector The detector uses specific properti...

Page 73: ...r The lower left indicates the power supply status the upper right indicates the detector status Power Supply Indicator The power supply indicator is integrated into the main power switch When the indicator is illuminated green the power is ON Figure 32 Location of Status Indicators Line power switch with green light Status indicator green yellow red ...

Page 74: ...is run mode A yellow indicator indicates a not ready condition The detector is in a not ready state when it is waiting for a specific condition to be reached or completed for example immediately after changing a setpoint or while a self test procedure is running An error condition is indicated when the status indicator is red An error condition indicates the detector has detected an internal probl...

Page 75: ...res 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 This section describes the meaning of detector error messages and provides information on probable causes and suggested actions how to corre...

Page 76: ...gure LC system Probable Causes The analysis was completed successfully and the time out 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 time out threshold Suggested Actions Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required ...

Page 77: ...e 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 The degasser failed to generate sufficient vacuum for solvent degassing Suggested Actions Fix the leak in the external instrument before restarting the pump Check external instruments for a shut down condition Chec...

Page 78: ...sis If a not ready condition is still present on the remote line after one minute the error message is generated Probable Causes Not ready condition in one of the instruments connected to the remote line Defective remote cable Defective components in the instrument showing the not ready condition Suggested Actions Ensure the instrument showing the not ready condition is installed correctly and is ...

Page 79: ...e 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 Suggested Actions Ensure all the CAN cables are connected correctly Switch off the system Restart the system and determine which module or modules are not recogn...

Page 80: ...Exchange defective capillaries Exchange flow cell formation Detector leak error may be caused by the Agilent 1100 sampler In each sampler injection sequence step 2 ejects the mobile phase stored in the metering head during the previous injection This mobile phase is ejected through the short plastic tube connected to port 4 of the sampler switching valve The output of port 4 is integrated into the...

Page 81: ...ng the detector leak pan The leak drain for the detector can be connected to the detector s leak drain fitting and taken to waste separately 2 If it is desired that the system has only one leak drain tube then it s possible in increase the length of the small plastic tube which is connected to port 4 of the sampler switching valve This tube can then be taken to waste separately The tube which norm...

Page 82: ...ependent 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 FLM board Defective leak sensor Suggested Actions Ensure the leak sensor is connected correctly Exchange the leak sensor ...

Page 83: ...uit 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 ...

Page 84: ... The resistance across the temperature compensation sensor NTC on the FLM 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 Probable Causes Defective FLM board Suggested Actions Exchange the FLM board ...

Page 85: ...uit The resistance across the temperature compensation sensor NTC on the FLM 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 Probable Causes Defective FLF board Suggested Actions Exchange the FLF board ...

Page 86: ... on the fan shaft is used by the FLM 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 FLM board Suggested Actions Ensure the fan is connected correctly Exchange fan Exchange the FLM board ...

Page 87: ...ated encoder cables mixed on FLM board monochromator assembly not connected monochromator or encoder defective monochromator motor power driver defective check encoder connections to FLM check motor connections to FLF Ex and FLM Em and encoders to FLM replace monochromator assembly defective FLF board Ex or FLM board Em Encoder Index Not Found EX 6707 EM 6708 During initialization of the detector ...

Page 88: ... A mechanical shock to the instrument during operation may cause a movement of the monochromator The position is lost and the lamp will turn off short mechanical shock message appears intermittently without mechanical shock re ignite the lamp replace monochromator assembly Motor Speed Too Low EX 6715 EM 6716 For proper operation the monochromator gratings must run at a certain constant revolution ...

Page 89: ...es FD Reference Manual 91 Lamp Cover Open The lamp cover in the optical compartment has been removed The lamp cannot be turned on while this message is on Probable Causes lamp cover removed Suggested Actions close lamp cover and tighten the screws ...

Page 90: ... the main board FLM This message comes together with some other message generated on the FLF board e g Leak Probable Causes FLF board not connected to the FLM board defective FLF board defective FLM board Suggested Actions Check the connection between the FLF board and the FLM board Exchange the FLF board Exchange the FLM board ...

Page 91: ...tions 4 1100 Series FD Reference Manual 93 ADC Not Calibrated The analog to digital converter located on the FLF board cannot calibrate Probable Causes defective ADC or other FLF electronics Suggested Actions Exchange the FLF board ...

Page 92: ... an info event is written into the logbook If the message comes up during a run it includes the time of occurrence and when it disappears 1100 FLD 1 A D overflow RT is 0 32 min 16 33 24 02 11 99 1100 FLD 1 A D overflow finished RT is 0 67 min 16 33 46 02 11 99 Probable Causes PMT setting to high wavelength setting wrong Suggested Actions reduce PMT gain change wavelength setting NOTE If this condi...

Page 93: ...he xenon flash lamp is monitored constantly If the current gets too high an error is generated and the lamp is turned off Probable Causes shortage of flash lamp assembly shortage of trigger pack assembly defective FLL board Suggested Actions Exchange the flash lamp assembly Exchange the FLL board includes the trigger pack ...

Page 94: ...played when the flash trigger is no longer generated Probable Causes firmware problem defective encoder Suggested Actions Reboot the detector power cycle Multi Mode Off exchange the firmware or replace the main board Multi Mode Ex replace EX monochromator assembly Multi Mode Em replace EM monochromator assembly ...

Page 95: ...iled is displayed and the instrument stays in a Not Ready condition Probable Causes Flash lamp not ignited or position not correct Cell position not correct Solvent in the cell not clean or air bubble in the cell monochromator assembly position not correct after replacement Suggested Actions Check the flash lamp image and position See also No Peaks on page 100 Check the cell position Flush the flo...

Page 96: ...s the calibration factors should be reset to defaults values a new FLM board comes with default values In this case Wavelength Calibration Lost is displayed and the instrument stays in a Not Ready condition Probable Causes Reset of monochromator settings after exchange Replacement of FLM board Suggested Actions Perform a wavelength calibration ...

Page 97: ...an automatic cell recognition system When the flow cell is removed the lamp is turned off and a NOT READY condition exists If the flow cell is removed during an analysis a SHUT DOWN is generated Probable Causes Flow cell has been removed during analysis Suggested Actions Insert flow cell and turn on the lamp ...

Page 98: ...cks whether the lamp is on Probable Causes defective FLL board Trigger pack defective Xenon flash lamp wrong position of monochromator FLF board defective Suggested Actions Perform a Lamp Intensity Test on page 115 If no profile available very low counts replace FLL board Trigger pack replace Xenon flash lamp perform a Check of Raman Band of Water on page 104 to check the wavelength calibration re...

Page 99: ...ation and emission monochromator by applying the fundamental grating equation X only required if deviation is too large NOTE A complete wavelength calibration is not always required In most cases a quick wavelength accuracy verification is sufficient enough see the table below Table 18 Reasons for doing a Verification or Calibration Verification WL calibration interest X GLP compliance X cell chan...

Page 100: ...ted using Rayleigh stray light from the flow cell or cuvette measured with the photomultiplier tube NOTE The duration of the wavelength calibration is about 15 minutes plus setup time for the calibration sample and system Depending on the maximum intensity found during this scan the PMT gain will be changed automatically and requires an additional 1 minute per scan Figure 33 Wavelength Calibration...

Page 101: ... s variable 6 n Emission rotation scan full circle of scans depends on the required PMT gain 1 minute per scan 61 s variable 6 n Em rotation scan full circle instrument profile 9 s 6 n Em rotation scan full circle instrument profile 9 s 6 n Em rotation scan full circle instrument profile 9 s 6 n Em rotation scan full circle instrument profile 9 s 7 Emission rotation scan high resolution part I 44 ...

Page 102: ...97 nm 20 nm 3 Turn the pump on and flush with water for a few minutes to assure a clean flow cell Flow rate should be 0 5 to 1 ml min and the baseline stable 4 Define in Sample Information the file name and description 5 Start a run After the 1 minute run has completed enter the Data Analysis and evaluate the spectrum The maximum should be found at 397 nm 3 nm see Figure 34 on page 105 NOTE This t...

Page 103: ...nto the multi excitation mode and scan in the range of the expected maximum of 350 nm 20 nm 7 Define in Sample Information the file name and description 8 Start a run After the 1 minute run has completed enter the Data Analysis and evaluate the spectrum The maximum should be found at 350 nm 3 nm Figure 34 Emission Spectrum ...

Page 104: ...age 109 2 Copy the methods to your PC card and re boot the control module 3 On the Analysis screen press the Method button and copy the methods into the module 4 Load the method WLEXTEST The FLD will change into the multi emission mode and scan in the range of the expected maximum of 397 nm 20 nm Figure 35 Excitation Spectrum Figure 36 Copying Methods into the FLD ...

Page 105: ...he Analysis screen select Settings FL Detector Press then the Spectrum button will open the window below 7 Press the Store button a few times to store a few spectra in a temporary buffer 8 Press the Eval button to change to the following screen NOTE You may remove the flow cell and check for air bubbles After re inserting the cell turn the lamp on Figure 37 Online Emission Spectra Figure 38 Evalua...

Page 106: ... the multi excitation mode and scan in the range of the expected maximum of 350 nm 20 nm 11 Repeat steps step 6 to step 8 12 You can now select a stored spectra and evaluate print them The maximum should be found at 350 nm 3 nm Figure 39 Evaluating Online Excitation Spectra NOTE The spectra on the control module is a real raw data spectrum Therefore it looks not that smooth as on the Agilent ChemS...

Page 107: ...Value in WLEMTEST Peak Width 0 2 min 4 s standard 0 2 min 4 s standard Fit Spectral Range OFF OFF PMT Gain 12 12 Flash Lamp ON ON Spectrum Range EX 377 417 nm step 1 nm EM 330 370 nm step 1 nm Store Spectra All w o signal All w o signal EX Wavelength 350 nm ON 350 nm OFF EM Wavelength 397 nm OFF 397 nm ON Multi WL Settings Multi EX Multi EM ...

Page 108: ...ample 1 To prepare 10 ml of the calibration solution you have to use 10 mg of the Glycogen sample a tolerance of 20 is not critical 2 Fill the prepared amount into a suitable bottle vial 3 Fill 10 ml of distilled water into the vial and shake 4 Wait 5 minutes and shake again After 10 minutes the solution is ready When required If application requires or see Table 18 on page 101 Tools required Labo...

Page 109: ... position 6 Remove t he needle 7 Add the filter to the syringe and fit the needle to filter 8 Lift the needle tip and carefully eject approximately 0 5 ml to remove air out of the syringe and to flush the needle 9 Add the PEEK fitting to the needle tip and fix both at the flow cell inlet 10 Slowly inject about 0 2 ml and wait for about 10 seconds to inject another 0 1 ml This will assure that the ...

Page 110: ... and OK The history table will be updated NOTE If the wavelength calibration process fails refer to Wavelength Calibration Failed on page 97 NOTE To look at the history table ChemStation start a wavelength calibration and abort immediately No changes are made to the calibration at this time NOTE Rinse the flow cell with pure water at a minimum of 1 5 ml min to get rid of the Glycogen from the cell...

Page 111: ...nd Test Functions 4 1100 Series FD Reference Manual 113 Verification 1 Refit the capillary to the flow cell 2 Follow the procedure Check of Raman Band of Water on page 104 Figure 41 Wavelength Calibration User Interface ...

Page 112: ...ual 4 Troubleshooting and Test Functions Test Functions The light path is shown in Figure 42 Figure 42 Schematic of the Light Path PMT Reference Diode Excitation Grating Emission Grating Flow Cell or Cuvette Flash Tube Mirror Diffuser ...

Page 113: ...further evaluation of the test Results of this test are stored as lamp history date code intensity UV degradation especially below 250 nm is significantly higher compared to visible wavelength range Generally the LAMP ON during run setting or using economy mode will increase lamp life by a magnitude Figure 43 Lamp Intensity Test typical NOTE The profile can vary from instrument to instrument It is...

Page 114: ... lamp intensity test if the last one is older than one week are stored as lamp history date code intensity of four different wavelengths 250 nm 350 nm 450 and 600 nm in a buffer The data plot can be retrieved via the diagnostics and provides intensity data over a length of time Figure 44 Lamp Intensity History ...

Page 115: ...s off It also reads the signal of the reference diode The resulting values two via reference diode and two from PMT are shown in a table and checked against reasonable limits see below Dark Current Test Evaluation Test Failed Probable Causes Defective PMT Defective reference diode or A D converter Suggested Actions Exchange the PMT Exchange the FLF board Figure 45 Dark Current Test ...

Page 116: ...rating drives The number of revolutions after switching off the drives is a measure of friction The history may show an increasing friction of the drive s over a length of time The history data contains the data time information and the number of turns The data plot can be retrieved via the diagnostics Friction Evaluation Motor Error Probable Causes Friction too high 12 turns Defective monochromat...

Page 117: ...nal to Noise Test Conditions Duration approximately 23 minutes Report Style Agilent ChemStation Performance Noise Noise Determination 5 to 20 minutes Solvent LC grade water degassed Flow rate 0 5 1 ml min Figure 47 Raman ASTM Signal to Noise Test Dark current at 350 450 nm and PMT 12 ASTM Noise and drift at 350 397 nm PMT 12 and Responsetime 8 s taken from 5 to 20 minutes ...

Page 118: ... should be 200 with FLF board revision A The result should be 400 with FLF board revision B and above Figure 48 Raman ASTM signal noise calculation RamanASTM Height RamanCurrent Height DarkCurrent ñ ASTMNoise Height Raman Current average between 5 and 10 minutes Height Dark Current average between 21 and 22 minutes ASTMNoise time 5 to 20 minutes ...

Page 119: ...n 7 When the run is completed a report is displayed and the status line shows the Raman signal noise ratio value see Figure 49 which should be 200 with FLF board revision A or 400 with FLF board revision B and above 8 To re display the number type LEO_FLD_EVALUATE_NOISE_TEST and press Enter NOTE The method FLRAMTST M and the macro FLRAMTST MAC are part of the A 06 xx ChemStation software CD 1100FL...

Page 120: ...eeIfReportLoaded initNoiseDetermination This line loads the raman macro starts loading the noise evaluation generator and defines ASTM noise performance parameters based on ASTM interval definition of 0 5 minutes macro report mcx LEO_FLD_evaluate_Noise_Test This line starts the FLD ASTM calculation and restores original ASTM noise calculation based on 1 minute intervals ...

Page 121: ...ws low Raman values check for correctly positioned flow cell clean flow cell flush no air bubble s check via fluorescence scan or visual check of cell cuvette solvent inlet filter may create air bubbles in flow cell clean water Figure 51 Raman Test FLD Settings part of method Set the Stoptime 23 minutes see on page 121 ...

Page 122: ...ignal path from the detector to the ChemStation and the data analysis or via the analog output to the integrator or data system An example is shown in Figure 52 The chromatogram is continuously repeated until a stop is executed either by means of a stop time or manually Figure 52 Built in Test Chromatogram default settings NOTE The peak height is always the same but the area and the retention time...

Page 123: ...ormation no injection 3 Type into the command line or as pre run command PRINT SENDMODULE LFLD SIMU DFLT 4 The logbook shows Preparing for a simulation 5 Start the run The results are processed like a regular chromatogram Table 22 Peakwidth 0 05 min response time 1 s fast Stop time 1 2 minutes Peakwidth 0 20 min response time 4 s STD Stop time 4 8 minutes NOTE The test chromatogram is switched off...

Page 124: ...d chromatogram enabled 4 Enter the Plot function and select Signal A and or Analog x set a time range of 10 minutes and the FLD signal from 1 to 50 LU 5 Start the run After the run has finished the plot can be printed to a connected printer by pressing the m key and selecting Print Plot NOTE If an Agilent ChemStation is connected the next step will start the Agilent ChemStation simultaneously and ...

Page 125: ...constant value corresponding to the ZERO OFFSET value In addition to the constant voltage is a switched voltage with a duration of 12 seconds and a height of 10 µV see Figure 53 1 Enable the function System Tests FLD Enable DAC Test Pattern 2 Start the plot mode e g Agilent 3396 with ATTN 4 ZERO 50 CS 5 3 Stop the plot and disable the TAC Test System Tests FLD Disable DAC Test Pattern 4 Evaluate t...

Page 126: ...128 1100 Series FD Reference Manual 4 Troubleshooting and Test Functions ...

Page 127: ...or Reference Manual Agilent Technologies 5 Repairing the Fluorescence Detector Introduction into Repairing the Fluorescence Detector 130 Overview of the Repairing of the Fluorescence Detector 133 Simple Repairs 134 Exchanging Internal Parts 142 ...

Page 128: ...nnected These repairs are described in Exchanging Internal Parts on page 142 WARNING To prevent personal injury the power cable must be removed from the instrument before opening the detector cover Do not connect the power cable to the detector while the covers are removed When working with solvents please observe appropriate safety procedures for example goggles safety gloves and protective cloth...

Page 129: ...er or a solution of water and mild detergent Do not use an excessively damp cloth allowing liquid to drip into the detector WARNING Eye damage may result from directly viewing the light produced by the Xenon flash lamp used in this product Always turn the xenon flash lamp off before removing it WARNING Do not let liquid drip into the detector It could cause shock hazard and it could damage the det...

Page 130: ...supplied in the standard accessory kit see Accessory Kit on page 216 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 3 Attach the copper foil to a convenient and exposed electrical ground Figure 54 Using the ES...

Page 131: ...ee page 135 Leak handling system see page 141 Leak sensor see page 165 Interface board see page 199 Excitation Monochromator see page 147 FLM Board see page 159 Photomultiplier Tube see page 180 Fan see page 163 Power supply see page 190 Emission Monochromator see page 147 Flash lamp see page 147 Flash lamp supply see page 183 Optical unit see page 178 condenser 1 see page 180 Mirror see page 172 ...

Page 132: ...ifferent flow cell type or if defective Complete Assembly A wavelength calibration check should be performed after replacement If the flow cell is removed and inserted then a quick calibration check is performed If this fails you must do a wavelength recalibration see Wavelength Verification and Calibration on page 101 Flow cell flushing If flow cell is contaminated Leak sensor drying If leak has ...

Page 133: ...onnections Parts required Standard flow cell 8 µl 20 bar G1321 60005 Cuvette for off line measurements 8 µl 20 bar G1321 60007 refer to How to use the Cuvette on page 138 for more information on usage NOTE DO NOT install the inlet capillary to the outlet connection of the flow cell This will result in poor performance Preparations for this procedure Turn off the flow 1 Press the release buttons an...

Page 134: ...s information on part number cell volume and maximum pressure The cell type will be automatically detected There are no parts that can be replaced on the flow cell If defective leaky the flow cell has to be replaced completely 4 Insert the flow cell and tighten the thumb screws Reconnect the capillaries to the flow cell DO NOT install the inlet capillary to the outlet connection of the flow cell T...

Page 135: ...detector may overload the quartz flow cell and will lead to a defective cell maximum pressure is 20 bar 2 MPa Always use the outlet capillary set supplied with the accessory kit Note To check for leaks establish a flow and observe the flow cell outside of the cell compartment and all capillary connections 5 Replace the front cover Note Perform a wavelength verification to check the correct positio...

Page 136: ... connections for easier injections with a syringe identification lever for cell auto recognition system 1 Install the cuvette instead of the standard flow cell 2 Connect the waste tubing to the outlet of the cuvette 3 Use the syringe see Cuvette Kit on page 214 to inject the compound 4 Setup the parameters for the Fluorescence Scan under Special Setpoints 5 Select Take Fluorescence Scan on the use...

Page 137: ...distilled water nitric acid 65 tubings to waste NOTE Aqueous solvents in the flow cell can built up algae Algae do fluoresce Therefore do not leave aqueous solvents in the flow cell for longer periods Add a small percentage of organic solvents e g Acetonitrile or Methanol 5 CAUTION This concentration of nitric acid is dangerous and proper attention to safety should be given Also the nitric acid fl...

Page 138: ...nd the leak pan 3 Observe the capillary connections and the flow cell area for leaks and correct if required 4 Replace the front cover When required If a leakage has occurred in the flow cell area or at the capillary connections Tools required Tissue Two 1 4 inch wrenches for capillary connections Parts required None Figure 56 Observing for Leaks Leak sensor ...

Page 139: ...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 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 Figure 57 Replacing Leak Handling System Parts Leak tubing Leak funnel Leak funnel ...

Page 140: ...el is turned off When working with solvents please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used NOTE Always operate the detector with the top covers in place CAUTION There will be a risk of damaging hardwa...

Page 141: ...Repairing the Fluorescence Detector 5 1100 Series FD Reference Manual 143 WARNING Eye damage may result from directly viewing the light produced by the xenon flash lamp used in this product ...

Page 142: ... work inside and the following procedures CAUTION There will be a risk of damaging hardware due to overheating when operating the instrument without covers Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench 1 Press the release buttons and remove the front cover Unclip and remove the waste fu...

Page 143: ...e clips on the rear of the cover 3 If installed unscrew and remove the interface board Place the board on the ESD kit 4 Lift the cover up and slide it towards the rear 5 Unscrew the screws at the rear of the top plate Slide the plate towards the front and remove it Warning Do not connect a power plug to the detector module after removing the top covers ...

Page 144: ... When required For all repairs inside the detector Parts required Depends on the work inside and the following procedures Preparations for this procedure Start with Removing the Covers on page 144 1 Using a pliers disconnect the cables from the main board 2 Carefully remove the rear foam A B A B A ...

Page 145: ...nstrument should not be operated without Xenon flash lamp Otherwise the Triggerpack electronics will be damaged NOTE When loosening or removing screws take care that they do not fall into the instrument This may result in a complete removal of other assemblies Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell or disconnect the tubings from the fl...

Page 146: ...Using the 4 mm hexagonal key unscrew the five screws remove the cover and place it on the bench without turning it around Note DO NOT unscrew the grounding screw marked with X 4 Using the 2 5 mm hexagonal key unscrew the two screws and remove the brass pad together with its holder A B A B A Rear foam A B A B A ...

Page 147: ...a few turns 6 Tip the holder to release the lamp and trigger pack Slide the cables of the trigger pack through the holder WARNING While pulling off the lamp be careful that you do not scrape your skin on the metal plates Do not remove the bottom pad Otherwise the lamp will loose its correct position during reinstallation ...

Page 148: ...from the trigger pack 8 Carfully insert the new lamp completely into the trigger pack and slide the cables through the holder 9 Place the lamp on the bottom pad 10 Refit the trigger pack holder by moving the lamp towards the condenser Leave a distance of about 0 5 mm between each other Refit the screws ...

Page 149: ...e brass holder 13 Replace the lamp housing cover and fix the screws Carefully insert the rear foam Reconnect the monochromator cables to the main board Left is excitation right is emission Next Steps Replace the covers as described in Replacing the Foam and the Top Cover on page 149 Re install the detector in the stack Enter the replacement of the lamp in the maintenance logbook this will reset th...

Page 150: ...should not be operated without Xenon flash lamp Otherwise the Triggerpack electronics will be damaged NOTE When loosening or removing screws take care that they do not fall into the instrument This may result in a complete removal of other assemblies Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell or disconnect the tubings from the flow cell Re...

Page 151: ...the 4 mm hexagonal key unscrew the five screws remove the cover and place it on the bench without turning it around Note DO NOT unscrew the grounding screw marked with X 4 Using a 2 5 mm hexagonal key loosen the screw and remove the condenser There is a mechanical stop for the condenser A B A B A Rear foam A B A B A ...

Page 152: ...to the main board Left is excitation right is emission Next Steps Replace the covers as described in Replacing the Foam and the Top Cover on page 149 Re install the detector in the stack Enter the replacement of the lamp in the maintenance logbook this will reset the lamp counter Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as descr...

Page 153: ...w 1000 0999 NOTE When loosening or removing screws take care that they do not fall into the instrument This may result in a complete removal of other assemblies Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell or disconnect the tubings from the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in R...

Page 154: ... 4 mm hexagonal key unscrew the five screws remove the cover and place it on the bench without turning it around Note DO NOT unscrew the grounding screw marked with X 4 Using the 2 5 mm hexagonal key unscrew one screws and loosen the other one Slide the window holder out of the window area A B A B A Rear foam A B A B A ...

Page 155: ...5 1100 Series FD Reference Manual 157 5 Use a toothpick to remove the window Note The quartz window may be cleaned with alcohol e g ethanol 6 Insert the cleaned or new window 7 Slide the window holder across the window and fix the screws ...

Page 156: ...d fix the screws Carefully insert the rear foam Reconnect the monochromator cables to the main board Left is excitation right is emission Next Steps Replace the covers as described in Replacing the Foam and the Top Cover on page149 Re install the detector in the stack Turn the lamp on A B A B A Rear foam EM EX ...

Page 157: ...nch to unscrew the REMOTE and the GPIB connector and a 15 mm wrench to unscrew the nuts of the ANALOG connectors 6 Disconnect all connectors from the processor board When required If detector main board is defective or for repair on other assemblies Tools required Screwdriver POZI 1 PT3 Flat screw driver Hexagonal wrenches 5 mm 7 mm and 15 mm Parts required Detector main board FLM G1321 69500 exch...

Page 158: ...rews at the REMOTE and GPIB connectors and the nuts of the ANALOG connectors NOTE When removing connectors counter hold with one hand on connector J12 Figure 59 Location of Connectors on FLM Board J1 GPIB J2 RS 232C J3 REMOTE J4 5 Analog output J6 7 CAN J11 Power supply J12 EM Monochromator J14 EX Monochromator J17 NOT USED J18 FLF board J2 J1 J2 J3 J4 J5 J1 B S1 J1 J1 J1 J1 J2 J2 J6 J7 NOTE An in...

Page 159: ...sing 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 5 Alphabetic characters and numbers are created using the up and down arrows In the box labeled Serial enter the 10 character serial number for the detector When the 10 character ser...

Page 160: ...y the module serial number you just entered 2 Turn off the detector then on again and restart the Agilent ChemStation If the serial number you have just entered is different than the original module serial number you will be given the opportunity to edit the configure 1100 access screen during the restart of the Agilent ChemStation 3 After start up the serial number you have just entered can be se...

Page 161: ...fan must be installed in the correct orientation to ensure optimum cooling and operation of the detector Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in Removing the Covers on page 144 1 Disconnect the emission and the excitation cables and from the detec...

Page 162: ...from the rear towards the front of the detector Insert the fan Lift the main board slightly Reconnect the fan cable and route it underneath the board 5 Carefully insert the rear foam Reconnect the monochromator cables to the main board Left is excitation right is emission Next Steps Replace the covers as described in Replacing the Foam and the Top Cover on page149 Re install the detector in the st...

Page 163: ...POZI 1 PT3 Flat screwdriver Parts required Leak sensor assembly 5061 3356 Leak Pan G1321 45501 Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in Removing the Covers on page 144 Remove the flow cell 1 Locate the leak sensor cable ...

Page 164: ...iring the Fluorescence Detector 2 Disconnect the leak sensor cable using your left hand 3 Pull out the leak sensor Note If you want to replace just the leak sensor continue with step 8 4 Using flat screw driver release the leak base two clasps ...

Page 165: ...completely 7 Replace the leak pan into the cabinet bottom Press the leak pan completely down into its recess 8 Replace the leak sensor using your left hand and reconnect the connector Next Steps Replace the covers as described in Replacing the Foams and Covers on page 196 Re install the flow cell and the front panel Re install the detector in the stack B B B ...

Page 166: ...Parts required Condenser assembly EM 1000 1124 Cutoff filter 295 nm 5062 8530 Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in Removing the Covers on page 144 Remove the flow cell 1 Disconnect the emission and the excitation cables and from the detector ma...

Page 167: ...eference Manual 169 2 Carefully remove the front foam holding the foam as shown Note Locate the condenser assembly and the cutoff filter 3 The cutoff filter can be replaced just by sliding it out and back in 4 Use a 2 5 mm hexagonal key to loosen the screw ...

Page 168: ... 5 Slide out the condenser assembly and place it in a safe location 6 Slide in the condenser assembly completely with the larger lens diameter towards the cutoff filter 7 Use a 2 5 mm hexagonal key to fix the screw Replace the cutoff filter 8 Carefully replace the front foam ...

Page 169: ...d in Replacing the Foams and Covers on page 196 Re install the flow cell and the front panel Re install the detector in the stack Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as described in chapter Wavelength Verification and Calibration on page 101 ...

Page 170: ...e of any optical component during this procedure This will reduce the reflection efficiency NOTE One side of the mirror is marked R representing the rear side Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in Removing the Covers on page 144 1 Disconnect the...

Page 171: ... Detector 5 1100 Series FD Reference Manual 173 2 Carefully remove the front foam holding the foam as shown 3 Remove the UV protector 4 Locate the mirror assembly 5 Use a pair of tweezers to lift off the top of the mirror holder ...

Page 172: ... mirror into the holder The mirror surface faces towards the light The back side is marked as shown Note If the mirror is inserted in the opposite direction the detector cannot be aligned correctly 8 Replace the mirror assembly and lock the top over the pin 9 Replace the UV protector Mirror surface faces to this side R ...

Page 173: ...s as described in Replacing the Foams and Covers on page 196 Re install the flow cell and the front panel Re install the detector in the stack Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as described in chapter Wavelength Verification and Calibration on page 101 ...

Page 174: ...8102 also used for PMT NOTE DO NOT touch the surface of any optical component during this procedure This will deteriorate the reflection process Preparations for this procedure Turn off the detector Disconnect the power cable Remove the flow cell Remove detector from stack and place it on the workbench Remove the covers as described in Removing the Covers on page 144 1 Carefully remove the front f...

Page 175: ...e spring part of the slit Next Steps Replace the UV protector Replace the front foam Replace the covers as described in Replacing the Foams and Covers on page 196 Re install the flow cell and the front panel Re install the detector in the stack Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as described in chapter Wavelength Verificat...

Page 176: ...tical unit a clean workbench with ESD protection mat must be available Otherwise optical components or electronic boards may be damaged NOTE DO NOT remove the foam from the optical unit unless it is required during a procedure Otherwise parts can fall out Preparations for this procedure Turn off the detector Disconnect the power cable Disconnect capillaries Remove detector from stack and place it ...

Page 177: ...bly 3 Disconnect the leak sensor cable J3 and unscrew the grounding screw 4 Disconnect the optical unit cable J18 and the EM motor cable J20 5 Remove the optical unit and place it on the bench ESD protection required Next Steps Depending on the replacement you want to perform proceed to the following procedures A B A B A Rear foam J3 Screw B ...

Page 178: ...re either R928HA 185 to 900 nm or R3788HA 185 to 750 nm No other PMTs are recommended FLF Board G1321 69531 requires firmware revision A 04 06 or above FLR Reference Diode board G1321 66533 CAUTION When working on the optical unit a clean workbench with ESD protection mat must be available Otherwise optical components or electronic boards may be damaged Preparations for this procedure Optical unit...

Page 179: ... a flat screw driver to release the wires 4 Remove the FLF board carefully in an upwards motion and place it on an ESD protected mat 5 If you need to replace either the board or the PMT assembly remove the PMT assembly from its socket 6 Replace the PMT assembly or the FLF board 7 Re install the PMT assembly in the socket A B C D PMT assembly Safety actuator FLR board REF diode ...

Page 180: ...t the wires to the connector Use a flat screw driver to release the wire socket 11 Put the wires into the released contacts using the tweezers Order of wires left to right Next Steps Reinstall the optical unit as described in Installing the Optical Unit on page 194 If you replaced a G1321 66501 FLF board by a G1321 66511 FLF board update the FLD firmware to revision A 03 7x or above to make it com...

Page 181: ... unit a clean workbench with ESD protection mat must be available Otherwise optical components or electronic boards may be damaged WARNING The instrument should not be operated without Xenon flash lamp Otherwise the Triggerpack electronics will be damaged Preparations for this procedure Optical unit has been removed as described in Removing the Optical Unit on page 178 The foam must be in place Ot...

Page 182: ...key unscrew the five screws and lift the cover 3 Using the 2 5 mm hexagonal key unscrew the two screws and remove the pad A 4 Remove the lamp as described in Exchanging the Lamp on page 147 5 Disconnect the wires from the connector Use a flat screw driver to release the wires A B A B A A A B FLL Board ...

Page 183: ...afe place Then pull out the FLL board 7 Insert the new FLL board Fit the wires through the holes and the Ferret 8 Put the wires into the released contacts using the tweezers Order of wires left to right 9 Reinstall the lamp as described in Exchanging the Lamp on page 147 FLL Board Ferret FLL Board Ferret green empty brown yellow white A B ...

Page 184: ...Next Steps Replace the covers as described in Replacing the Foam and the Top Cover on page149 Re install the detector in the stack Reset the lamp counter as described in the user interface documentation Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as described in chapter Wavelength Verification and Calibration on page 101 A B A B A ...

Page 185: ...tical components or electronic boards may be damaged NOTE The grating assembly is shipped with a special transport packaging and includes a protection ring DO NOT touch the grating surface and DO NOT bend the protection ring Preparations for this procedure Optical unit has been removed as described in Removing the Optical Unit on page 178 The cables from the position encoders at the rear of the EM...

Page 186: ...g assembly and the protection ring from its location 4 Insert the new protection ring into its position Do not bend the protection ring 5 For reinstallation route the cable first through the hole Carefully insert the grating into its position while pulling the cable slightly from below The couple spring has to be clipped into the protection ring TOP mark Protection ring Couple Spring ...

Page 187: ...einstall the optical unit as described in Installing the Optical Unit on page 194 Enter the replacement in the maintenance logbook Reset the monochromator settings to default using the diagnose functions In this case Wavelength Calibration Lost is displayed and the instrument stays in Not Ready condition until you perform a wavelength calibration Perform a wavelength verification to check the corr...

Page 188: ...exchanging the complete assembly No serviceable parts are inside Preparations for this procedure Turn off the lamp Switch off the detector and disconnect the cables Remove the detector from the stack and place it on the workbench Remove the front cover and top cover see Removing the Covers on page 144 Remove the processor board see Exchanging the Processor Board on page 159 Remove the fan assembly...

Page 189: ...Unscrew the power supply at the rear of the module 3 Press down the power switch light pipe to remove it from the coupler 4 Remove the power supply completely Re use the coupler on the new power supply The repair of the power supply assembly is comprised of exchanging the complete assembly No serviceable parts are inside Power switch light pipe Coupler ...

Page 190: ...m piece Slide it in underneath the leak drain 8 Reinstall the processor board see Exchanging the Processor Board on page 159 9 Reinstall the fan assembly see Exchanging the Fan on page 163 10 Reinstall the optical unit see Installing the Optical Unit on page 194 11 Reinstall the front cover top cover see Replacing the Foams and Covers on page 196 12 Replace detector into the stack 13 Reconnect the...

Page 191: ...1 PT3 Parts required Status light pipe 5041 8384 Preparations for this procedure Remove the front cover and top cover see Removing the Covers on page 144 1 The status light pipe is clipped into the top cover 2 Replace the top cover see Replacing the Foams and Covers on page 196 3 Replace the detector into the stack and reconnect the cables and capillaries 4 Turn on the detector ...

Page 192: ...ls required Screwdriver POZI 1 PT3 Hexagonal key 4 mm WARNING For safe operation make sure that the ground cable is reconnected Preparations for this procedure All previous work has been completed Power supply has been installed Fan has been installed The optical unit has its foam cover attached 1 Place the optical unit in the instrument Reconnect the grounding screw J3 Screw ...

Page 193: ...hromator and EX monochromator to the detector main board FLM Next Steps Replace the covers as described in Replacing the Foams and Covers on page 196 Re install the flow cell and the front panel Re install the detector in the stack Turn the lamp on Perform a wavelength verification to check the correct positioning of the replaced assemblies as described in chapter Wavelength Verification and Calib...

Page 194: ... 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 NOTE The front cover across the optical unit should only be removed when required during a procedure This will keep dust away from optical components 1 Carefully insert the rear foam 2 Route the cables towards the main board and reconnec...

Page 195: ...top plate screws 4 Replace the cover 5 If required insert the interface board and fix the screws 6 Replace the waste funnel assmbly and the front panel Next Steps Replace the detector into the stack and Reinstall the flow cell Reconnect the power cable and turn on the detector Turn the lamp on Ensure correct fit with Z plane ...

Page 196: ...ght NOTE The plastics kit contains all parts but it is not assembled WARNING If you mistakenly insert the left or right side in the opposite position you may not be able to remove that side from the top part 1 Place the top part on the bench and insert the left and right sides into the top part 2 Replace the cover Next steps Replace the detector in the stack and reconnect the cables and capillarie...

Page 197: ...he board slide in the new interface board and fix it with the board s screws 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 Interface board LAN see LAN Board on page 284 Tools required None Figure 60 Location of the Interface Board Interface board ...

Page 198: ...the version on board is older than the previously installed one To upgrade the detector s firmware the following steps have to be taken 1 Load the firmware into the detector see help system of your user interface 2 If FLM board was replaced reenter the serial number information of the module through the user interface see Entering the Serial Number using the Control Module on page 161 or Entering ...

Page 199: ...terials Overview of Main Assemblies 202 Optical Unit Assembly 204 Lamp Cover Parts 207 Control Module 208 Sheet Metal Kit 209 Plastic Parts 210 Foam Parts 211 Power and Status Light Pipes 212 Leak Parts 213 Cuvette Kit 214 Spare Parts 215 Accessory Kit 216 Cable Overview 218 RS 232 Cable Kit 235 LAN Cables 236 ...

Page 200: ...ies and their locations Figure 61 Main Assemblies 12 Flow cell 3 Interface board not shown 8 Excitation Monochromator 1 FLM Board 10 Photomuliplier 4 Fan 2 Power Supply 9 Emission Monochromator 5 Optical unit 6 Flash lamp For other parts within the optical unit see page 204 7 Mirror 11 condenser EM 13 Leak Sensor 14 Cable FLM FLF ...

Page 201: ...ee page 284 Fuse for BCD board 250 mA total of 4 are on the board 2110 0004 4 Fan assembly 3160 1017 5 Optical unit exchange assembly for additional optical unit parts see page 204 G1321 69002 6 Xenon flash lamp 2140 0600 7 Mirror 1000 1000 8 Excitation Monochromator assembly complete G1321 60003 9 Emission Monochromator assembly complete G1321 60004 10 Photomuliplier tube assembly PMT see also pa...

Page 202: ...inlet i d length 0 17 mm 80 mm outlet i d length 0 25 mm 80 mm G1321 60005 Cuvette 8 µl 20 bar inlet i d length 0 5 mm 80 mm outlet i d length 0 5 mm 80 mm G1321 60007 Screw for flow cell cuvette G1321 22400 9 Slit EM 2x8 G1321 08102 10 Photomuliplier tube assembly PMT see also page 180 for additional information 1970 0201 11 Condenser Emission 1000 1124 12 Front end Board FLF underneath the optic...

Page 203: ...e chassis G1321 61602 17 Screw M5 x 25 mm for chassis cable 0515 2574 Screw 2 5 mm hex for monochromator lamp pad condenser 1 slits etc 0515 1052 Screw M4 x 25 mm hex for lamp housing 0515 2548 Screw M4 x 8 mm for FLF board 0515 2549 Table 25 Optical Unit Assembly continued Item Description Part Number ...

Page 204: ...omuliplier 7 Emission Monochromator 11 Condenser EM 2 Xenon Flash Lamp below pad 3 Condenser EX 1 FLL Board Trigger Pack 5 Mirror 8 Flow Cell 9 Slit EM PMT 4 Slit EX 12 FLF Board underneath 12a Reference diode FLR 9 Slit EM PMT 16 Cable chassis 17 Screw chassis 13 Cutoff Filter 14 Carbon filter mat 15 Cable FLM FLF 12b Diffuser plate ...

Page 205: ...terials 6 1100 Series FD Reference Manual 207 Lamp Cover Parts Table 26 Lamp Cover Parts Item Description Part Number 1 Plate G1321 08100 2 Screw 2 5 mm hex 0515 1052 3 Quartz Window 1000 0999 Figure 63 Lamp Cover Parts 1 2 3 ...

Page 206: ...rol Module Table 27 Control Module Parts Item 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 64 Control Module ...

Page 207: ... FD Reference Manual 209 Sheet Metal Kit Table 28 Sheet Metal Kit Parts Item Description Part Number 1 Sheet metal kit includes case and top cover G1321 68701 2 Screws M3 for cover and flow cell door 5022 2112 Figure 65 Sheet Metal Kit Parts 1 1 2 ...

Page 208: ...escription 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 NOTE For correct assembling of the top and sides see Assembling the Main Cover on page 198 Figure 66 Plastic Parts 2 3 1 4 ...

Page 209: ... Parts Item Description Part Number 1 2 EPP foam kit includes bottom and top rear G1321 68702 3 Foam Pads located underneath the optical set of two G1321 68700 4 Guides for interface board 5041 8395 NOTE Do not order the individual part numbers imprinted on the foam Figure 67 Foam Parts 1 2 4 3 ...

Page 210: ...Pipes Item Description Part Number Power supply assembly 0950 2528 Screw M4 x 0 7 8 mm lg to fix power supply at rear panel 0515 0910 Washer 2190 0409 1 Power light pipe 5041 8382 2 Status light pipe 5041 8384 3 Power switch button 5041 8381 4 Coupler for power supply actuator 5041 8383 Figure 68 Power and Status Light Pipe 1 2 4 3 ...

Page 211: ... Leak Parts Item Description Part Number 1 Leak sensor assembly 5061 3356 2 Leak pan G1321 45501 3 Leak funnel 5041 8388 4 Leak funnel holder 5041 8389 5 Corrugated tubing 120 mm lg re order 5 m 5062 2463 6 Corrugated tubing 1200 mm lg re order 5 m 5062 2463 Figure 69 Leak Parts 1 6 5 3 2 4 ...

Page 212: ...3 Cuvette Kit Item Description Part Number FLD Cuvette Kit 8 µl 20 bar G1321 60007 includes Tubing flexible 1 meter SST Fitting QTY 1 79814 22406 SST front ferrule QTY 1 0100 0043 SST back ferrule QTY 1 0100 0044 PEEK fitting QTY 1 0100 1516 Needle Syringe 9301 0407 Glass Syringe 9301 1446 ...

Page 213: ...ese parts may affect the performance of the detector and may not fulfill the instruments specifications Table 34 Spare Parts Description Part Number Cutoff filter kit 389 nm 408 nm 450 nm 500 nm 550 nm 5061 3327 Cutoff filter kit 380 nm 399 nm 418 nm 470 nm 520 nm 5061 3328 Cutoff filter kit 280 nm 295 nm 305 nm 335 nm 345 nm 5061 3329 Cutoff filter 370 nm 1000 0822 Photo multiplier Tube PMT R928H...

Page 214: ...5 m 5062 2462 2 Fitting male PEEK Qty 2 0100 1516 3 Capillary column detector 380 mm lg 0 17 i d includes items 4 5 and 6 not assembled G1315 87311 4 Ferrule front SST qty 1 0100 0043 5 Ferrule back SST qty 1 0100 0044 6 Fitting SST qty 1 79814 22406 Screwdriver hexagonal 4 mm 100 mm long 5965 0027 Screwdriver hexagonal 2 5 mm 100 mm long 5965 0028 Needle Syringe 9301 0407 Glass Syringe 9301 1446 ...

Page 215: ...Identifying Parts and Materials 6 1100 Series FD Reference Manual 217 Figure 70 Waste Tubing Parts Figure 71 Inlet Capillary Column Detector Parts 1 2 3 6 4 5 This end is pre installed ...

Page 216: ...Agilent 35900A A D converter 35900 60750 General purpose spade lugs 01046 60105 3390 2 3 integrators 01040 60101 Remote cables 3390 integrator 01046 60203 3392 3 integrators 01046 60206 3394 integrator 01046 60210 3396A Series I integrator 03394 60600 3396 Series II 3395A integrator see page 225 3396 Series III 3395B integrator 03396 61010 Agilent 1100 1050 modules HP 1046A FLD 5061 3378 HP 1046A ...

Page 217: ...323 81600 External contacts Agilent 1100 Series interface board to general purpose G1103 61611 GPIB cable Agilent 1100 module to Agilent ChemStation 1 m 10833A Agilent 1100 module to Agilent ChemStation 2 m 10833B RS 232 cable Agilent 1100 module to a computer This kit contains a 9 pin female to 9 pin female Null Modem printer cable and one adapter 34398A LAN cable Twisted pair cross over LAN cabl...

Page 218: ...ted to Agilent 1100 Series modules The other end depends on the instrument to which connection is being made Agilent 1100 to 3390 2 3 Integrators Table 37 Connector 01040 60101 Pin 3390 2 3 Pin Agilent 1100 Signal Name 1 Shield Ground 2 Not connected 3 Center Signal 4 Connected to pin 6 5 Shield Analog 6 Connected to pin 4 7 Key 8 Not connected ...

Page 219: ...00 to 3394 6 Integrators Agilent 1100 to BNC Connector Table 38 Connector 35900 60750 Pin 3394 6 Pin Agilent 1100 Signal Name 1 Not connected 2 Shield Analog 3 Center Analog Table 39 Connector 8120 1840 Pin BNC Pin Agilent 1100 Signal Name Shield Shield Analog Center Center Analog ...

Page 220: ...0 Series FD Reference Manual 6 Identifying Parts and Materials Agilent 1100 to General Purpose Table 40 Connector 01046 60105 Pin 3394 6 Pin Agilent 1100 Signal Name 1 Not connected 2 Black Analog 3 Red Analog ...

Page 221: ...t 1100 Series modules The other end depends on the instrument it is to be connected to Agilent 1100 to 3390 Integrators Table 41 Connector 01046 60203 Pin 3390 Pin Agilent 1100 Signal Name Active TTL 2 1 White Digital ground NC 2 Brown Prepare run Low 7 3 Gray Start Low NC 4 Blue Shut down Low NC 5 Pink Not connected NC 6 Yellow Power on High NC 7 Red Ready High NC 8 Green Stop Low NC 9 Black Star...

Page 222: ...un 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 Table 43 Connector 01046 60210 Pin 3394 Pin Agilent 1100 Signal Name Active TTL 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 5 14 7 ...

Page 223: ...nnected Table 43 Connector 01046 60210 Pin 3394 Pin Agilent 1100 Signal Name Active TTL NOTE START and STOP are connected via diodes to pin 3 of the 3394 connector Table 44 Connector 03394 60600 Pin 3394 Pin Agilent 1100 Signal Name Active TTL 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 5 14 7 Red ...

Page 224: ...tors Table 45 Connector 03396 61010 Pin 33XX Pin Agilent 1100 Signal Name Active TTL 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 Not connected ...

Page 225: ...rown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink Not connected 6 Yellow 6 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low Table 47 Connector 01046 60202 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 ...

Page 226: ...eneral Purpose Table 48 Connector 01046 60201 Pin Universal Pin Agilent 1100 Signal Name Active TTL 1 White Digital ground 2 Brown Prepare run Low 3 Gray Start Low 4 Blue Shut down Low 5 Pink Not connected 6 Yellow Power on High 7 Red Ready High 8 Green Stop Low 9 Black Start request Low ...

Page 227: ...to the Agilent 1100 Series modules The other end depends on the instrument it is to be connected to Agilent 1100 to 3392 3 Integrators Table 49 Connector 18584 60510 Pin 3392 3 Pin Agilent 1100 Signal Name BCD Digit 10 1 BCD 5 20 11 2 BCD 7 80 3 3 BCD 6 40 9 4 BCD 4 10 7 5 BCD0 1 5 6 BCD 3 8 12 7 BCD 2 4 4 8 BCD 1 2 1 9 Digital ground 2 15 5 V Low 6 Key ...

Page 228: ...nd Materials Agilent 1100 to 3396 Integrators Table 50 Connector 03396 60560 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 5 V Low ...

Page 229: ...t 1100 to General Purpose Table 51 Connector 18594 60520 Wire Color Pin Agilent 1100 Signal Name BCD Digit Green 1 BCD 5 20 Violet 2 BCD 7 80 Blue 3 BCD 6 40 Yellow 4 BCD 4 10 Black 5 BCD0 1 Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground White 15 5 Vt Low ...

Page 230: ...ides a modular plug to be connected to the Agilent 1100 Series vacuum degasser The other end is for general purpose Agilent 1100 Series Degasser to general purpose Table 52 Connector G1322 61600 Color Pin Agilent 1100 Signal Name White 1 Ground Brown 2 Pressure signal Green 3 Yellow 4 Grey 5 DC 5 V IN Pink 6 Vent ...

Page 231: ...CAN Cable Both ends of this cable provide a modular plug to be connected to Agilent 1100 Series module s CAN bus connectors Table 53 Agilent 1100 module to module 0 5 m 5181 1516 Agilent 1100 module to module 1 m 5181 1519 Agilent 1100 module to control module G1323 81600 ...

Page 232: ...pose Agilent 1100 Series Interface Board to general purpose Table 54 Connector G1103 61611 Color Pin Agilent 1100 Signal Name White 1 EXT 1 Brown 2 EXT 1 Green 3 EXT 2 Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yel...

Page 233: ...e and one adapter Use the cable and adapter to connect Agilent Technologies instruments with 9 pin male RS 232 connectors to most PCs or printers Agilent 1100 module to PC RS 232 Cable Kit 34398As Table 55 Instrument DCD RX TX DTR GND DSR RTS CTS RI DCD RX TX DTR GND DSR RTS CTS RI PC 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 DB9 Male DB9 Female DB9 Female DB9 Male ...

Page 234: ...nd Materials LAN Cables Recommended Cables For point to point connection not using a network hub use a twisted pair cross over LAN cable P N 5183 4649 10 feet long For standard network connections using a hub use category 5 UTP cables P N G1530 61480 8 m long ...

Page 235: ...ologies 7 Introduction to the Fluorescence Detector Introduction to the Detector 238 How the Detector Operates 239 Raman Effect 242 Optical Unit 243 Analytical Information From Primary Data 251 Electrical Connections 256 Instrument Layout 258 Early Maintenance Feedback EMF 259 ...

Page 236: ... lamp for highest intensity and lowest detection limit multi wavelength mode for on line spectra spectra acquisition and simultaneous multi signal detection optional cuvette is available and can be used for off line measurements easy front access to flow cell for fast replacement and built in wavelength accuracy verification For specifications see Performance Specifications on page 328 Figure 72 T...

Page 237: ...ms of energy each with its own excitation process For example when the excitation energy is light the process is called photoluminescence In basic cases the emission of light is the reverse of absorption see Figure 73 With sodium vapor for example the absorption and emission spectra are a single line at the same wavelength The absorption and emission spectra of organic molecules in solution produc...

Page 238: ...o one of the vibrational and rotational sub levels of its ground state emitting light see Figure 74 The characteristic maxima of absorption for a substance is its λEX and for emission its λEM Photoluminescence is the collective name for two phenomena fluorescence and phosphorescence which differ from each other in one characteristic way the delay of emission after excitation If a molecule emits li...

Page 239: ... back again before it can return to its ground state Since the chance of colliding with another molecule with the necessary spin for change is slight the molecule remains in its triplet state for some time During the second spin change the molecule loses more energy by relaxing without radiation The light which is emitted during phosphorescence therefore has less energy and is at a longer waveleng...

Page 240: ...the incident light Ei and the Raman scattered light Es is equal to the energy involved in changing the molecule s vibrational state i e getting the molecule to vibrate Ev This energy difference is called the Raman shift Ev Ei Es Several different Raman shifted signals will often be observed each being associated with different vibrational or rotational motions of molecules in the sample The partic...

Page 241: ...enser excitation slit mirror excitation grating flow cell emission condenser cut off filter emission slit emission grating and photo multiplier tube are housed in the metal casting inside the detector compartment The fluorescence detector has grating grating optics enabling the selection of both excitation and emission wavelengths The flow cell can be accessed from the front of the fluorescence de...

Page 242: ...to the Fluorescence Detector Figure 77 Optical Unit Xenon Flash lamp Flash lamp board EM Grating assembly Photo Multiplier Tube Slit EM EX Grating assembly Flow Cell Condenser EM Mirror Condenser EX Slit EX Trigger Pack Cutoff filter REF Diode Diffuser ...

Page 243: ...on the sensitivity requirements You can economize during automatic operation using keyboard setpoints so the lamp flashes during your analysis only The lamp can be used until it no longer ignites but the noise level may increase with usage UV degradation especially below 250 nm is significantly higher compared to Visible wavelength range Generally the LAMP ON during run setting or using economy mo...

Page 244: ...nochromator grating onto the cell entrance slit The holographic concave grating is the main part of the monochromator dispersing and reflecting the incident light The surface contains many minute grooves 1200 of them per millimeter The grating carries a blaze to show improved performance in the visible range Y Figure 79 Mirror Assembly Mirror Grating EX inside ...

Page 245: ...phase brushless DC motor the position of the grating determining the wavelength or wavelength range of the light falling onto the flow cell The grating can be programmed to change its position and therefore the wavelength during a run For spectra acquisition and multi wavelength detection the grating rotates at 4000 rpm The excitation and emission gratings are similar in design but have different ...

Page 246: ...e from the sample in the flow cell is collected at right angles to the incident light by a second lens and passes through a second slit Before the luminescence reaches the emission monochromator a cut off filter removes light below a certain wavelength to reduce noise from 1st order scatter and 2nd order stray light see Figure 80 on page 247 The selected wavelength of light is reflected onto the s...

Page 247: ... that a current can be measured The amplification is a function of the voltage at the dynodes and is microprocessor controlled You can set the amplification using the PMTGAIN function This type of so called side on photo multiplier is compact ensuring fast response conserving the advantages of the short optical path shown in Figure 77 on page 244 PMTs are designed for specific wavelength ranges Th...

Page 248: ...t transmitted by the flow cell and corrects flash lamp fluctuations and long term intensity drift Because of a non linear output of the diode depending on the EX wavelength the measured data are normalized A diffuser is located in front of the reference diode see Figure 77 on page 244 This diffuser is made of quartz reduces light and allows integral measurement of the light ...

Page 249: ...ence measured by the fluorescence detector will have different characteristics You must decide using your knowledge of the sample what mode of detection you will use Fluorescence Detection When the lamp flashes the fluorescing compounds in your sample will luminesce almost simultaneously see Figure 83 The luminescence is short lived therefore the fluorescence detector need only measure over a shor...

Page 250: ...tor Phosphorescence Detection An appropriate parameter set will be specified as soon as you chose the phosphorescence detection mode special setpoints under FLD parameter settings Figure 84 Measurement of Phosphorescence Time µsec Intensity 100 Measurement Flash Phosphorescence ...

Page 251: ... multi wavelength mode is set then the flash frequency is 74 Hz You can improve the signal to noise characteristics by disabling the economy mode The data resolution is 20 bit at a response time of 4 seconds default which is equivalent to a time constant of 1 8 seconds and appropriate for standard chromatographical conditions Weak signals may cause errors in Figure 85 LAMP Frequency of Flash Fluor...

Page 252: ... your amplification for the peak with the highest emission raise the PMTGAIN setting until the best signal to noise is achieved After the photons are converted and multiplied into an electronic signal the signal at present analog is tracked and held beyond the photo multiplier After being held the signal is converted by an A to D converter to give one raw data point digital Eleven of these data po...

Page 253: ...5 length of the boxcar element using the RESPONSETIME function the longer the RESPONSETIME the greater the number of data points averaged A four fold increase in RESPONSETIME for example 1 sec to 4 sec doubles the signal to noise ratio Figure 87 RESPONSETIME Signal to Noise Ratio ...

Page 254: ...ruments from Agilent Technologies if you want to use features such as start stop common shut down prepare and so forth With the appropriate software the RS 232C connector may be used to control the detector from a computer through a RS 232C connection This connector is activated and can be configured with the configuration switch next to the GPIB connector see Communication Settings for RS 232C Co...

Page 255: ...NING Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Figure 88 Electrical Connections Analog signal APG remote RS 232C CAN GPIB Power Configuration switch Interface board Security lever ...

Page 256: ...then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations the plastic...

Page 257: ... counters for the lamp The counters increment with lamp use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded The counters can be reset to zero after the lamp is exchanged The detector provides the following EMF counters number of flashes low power mode multiples of 1000 flashes number of flashes high power mode multiples of 1000 fl...

Page 258: ...Reference Manual 7 Introduction to the Fluorescence Detector Figure 89 Lamp life 0 1 0 2 0 3 0 4 0 5 10 10 10 10 8 9 10 11 Numberofflashesto75 ofintitialradiometriclight output Inputenergyperflash J Numberof flashes 0 05 ...

Page 259: ...need to be determined based on the specific operating conditions of the instrument 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 displaye...

Page 260: ...262 1100 Series FD Reference Manual 7 Introduction to the Fluorescence Detector ...

Page 261: ...Electronics 264 Detector Main Board FLM 265 Detector Frontend Board FLF 269 Detector Lamp Supply Board FLL 273 Firmware Description 274 Raw Data Conversion to Fluorescence LU Units 276 Optional Interface Boards 282 Interfaces 285 Setting the 8 bit Configuration Switch 290 The Main Power Supply Assembly 295 ...

Page 262: ...tronics are comprised of four main components detector main board FLM see page 265 detector frontend board FLF see page 269 detector lamp board FLL see page 273 power supply see page 295 Optional interface board BCD external contacts see page 283 interface board LAN see page 284 ...

Page 263: ...connected to the user interface the operator enters parameters changes modes and controls the detector Figure 90 Detector Electronic Overview Main Power Supply Interfaces CAN GPIB RS232 Analog Outputs Agilent 1100 Core Processor ASIC Flash Lamp Supply Flash Trigger Timing Control Xenon Flash Lamp EX Motor EM Motor Motor Power Control PMT Voltage Photomultiplier Reference Diode Analog Frontend FLM ...

Page 264: ...core bus as well as with the SRAM static random access memory of 4 512 kilobyte the flash EEPROM electrically erasable programmable read only memory of 1 MB and the 1 128 KB battery backed NV RAM non volatile Battery life is designed to last for more than 25 years under normal operating conditions Control lines provide communication to the frontend board which provides high voltage power supplies ...

Page 265: ...driver REMOTE driver RS 232C driver FPGA Field Programmable Gate Array PWM driver EM Motor driver Fan EM Mono chromator Memory Real time clock Control lines MPS main power supply J4 J5 J22 J20 J11 J2 J3 J6 J7 J1 Interface board J21 PWM drivers Low pass filters and signal conditioning Analog out 1 Analog out 2 J18 Main Control Functional Block Diagram FLM sense Detector Frontend Board FLF J18 Detec...

Page 266: ...he electronic memory when the module is turned off For safety information on lithium batteries see Lithium Batteries Information on page 335 Analog Outputs There are two independent analog outputs 0 1 V full scale Digital data from the ASIC is converted into a pulse width modulated signal PWM The PWM signal is then fed to an amplitude modulator which precisely turns the reference signal on and off...

Page 267: ...gnals monochromator positions board temperature leak sensor status Then the digital data are polled by the FPGA on the FLM main board to be available for calculations Flash Lamp Power Supply The flash lamp is operated with discharge voltages of 500 V or 1250 V The electronics design provides the voltages using a regulating pulse width modulator to switch a 24 V rail with a chopping frequency of 40...

Page 268: ... ionized channel from the ignition electrode to the cathode If this ionization is existent the voltage difference between anode and cathode leads to a flash discharge within a very short time 1 µs After the flash the system pauses the regulator to force the ionized path to break down rapidly before charging the capacitors for the next cycle Flash Lamp Overcurrent Protection A special firmware cont...

Page 269: ... transformer The feedback loop has a D A converter controlled base voltage to set the desired output voltage The PMT output delivers a current signal which is proportional to the detected light and to the actual working voltage Figure 92 Block diagram FLF Flash Lamp Supply PMT voltage Supply EX Motor Driver Cell Detection Read Write Port Leak Sensor circuit A D Converter 16 bit Lamp Cover Safety S...

Page 270: ... chassis to detect leakage of the cell assy In case of a leakage the complete Agilent 1100 System is shut down to prevent system damage This block consists of a PTC for the leak detection and a NTC for the ambient temperature compensation A leak would cool down the PTC and this change in resistance would generate a leak signal Digital Interface The control and data lines from and to the Fluorescen...

Page 271: ...backflowing current from generating negative lamp discharge currents which may damage the flash lamp Lamp Ignition Control An ignition voltage is switched by a thyristor to the TriggerPac ignition transformer to built a small ionized channel refer Igniting the Flash Lamp on page 270 A freewheeling diode forces the thyristor to switch off again to prevent lamp damage Figure 93 Block Diagram FLL Boa...

Page 272: ...N and RS 232C memory management ability to update the firmware of the main system Main System Its properties are the complete communication capabilities GPIB CAN LAN and RS 232C memory management ability to update the firmware of the resident system In addition the main system comprises the instrument functions that are divided into common functions like run synchronization through APG remote erro...

Page 273: ...aming conventions are xxxx vvv DLB where xxxxis the product number for example 1315 for the G13151A DAD and vvvis the revision number for example 104 is revision 1 04 For instructions refer to your user interface NOTE Update of main system can be done in the resident system only Update of the resident system can be done in the main system only Figure 94 Firmware Update Mechanism Resident System Ma...

Page 274: ...t or luminescence units is used as new unit and will indicate the light intensity not comparable with the physical unit Lumen These units are calculated from the PMT photomuliplier tube in the emission path and a reference diode located behind the flow cell see figure below Figure 95 Optical Diagram of the FLD ...

Page 275: ...nt filter Figure 96 Data flow for chromatographic output PMT Raw Signal acquisition position Reference Diode Raw Signal acquisition position Dark subtraction Dark subtraction Normalization of reference signal Divide PMT Reference Diode Filtering Channel A B C D Output LU PMT gain Peakwidth Responsetime EX wavelength Influences Influences Peak Detector will be executed at each flash assigned for ch...

Page 276: ...MT raw signal acquisition position reference diode raw signal acquisition position dark subtraction dark subtraction normalization of reference signal divide PMT reference collect data for complete spectra spectra output LU Influences normalization to spectra LU concentration correction ChemStation Spline algorithm Data Analysis Control Module Online Monitor ...

Page 277: ...eference diode located behind the flow cell measures the excitation EX light within the flow cell and corrects flash lamp fluctuations Because of a non linear output of the diode depending on the EX wavelength the measured data are now normalized to get better real light level values within the flow cell Divide PMT Reference Diode With this calculation the output of the detector will suppress lamp...

Page 278: ... scan If all spectra without signal is used as spectra acquisition mode Peak Detector The peak detector PD always uses signal A as the pilot signal The PD is adjusted by means of two setpoints peakwidth and threshold Both setpoints are time programmable While the PD threshold is a method parameter of its own the PD peakwidth parameter is derived from the general peakwidth PKWD parameter At the sta...

Page 279: ...ctra is measured and stored In addition the next baseline spectra is stored all in peak The peak detectors will start and stop spectrum acquisition at begin and end of a detected peak In addition the next baseline spectra is stored all periodically all spectra are stored The period depends on the spectra range and step and the number of selected chromatographical outputs signals all without signal...

Page 280: ...ds The Agilent 1100 Series modules have one optional board slot that allows addition of an interface board to the modules Table 58 Optional Interface Boards Description Part Number BCD Board G1351 68701 Fuse 250 mA four are on the board 2110 0004 LAN Board see next page for details ...

Page 281: ...elay contacts The maximum settings are 30 V AC DC 250 mA fused There are general purpose cables available to connect the BCD output see BCD Cables on page 229 and the external outputs see External Contact Cable on page 234 to external devices Figure 98 Block Diagram BCD Board Processor interface Board identification BCD register External contacts Line driver 12 4 x 250 mA BCD connector External co...

Page 282: ...les P N G1530 61480 8 m long 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 DAD MWD VWD Pump ALS or G13XX 66500 FLD RID and above a DOS ChemStation software revision A 06 01 or above Table 59 LAN Boards Agilent Order Number Supported ne...

Page 283: ...ion of the connectors Figure 6 on page 23 Table 60 Agilent 1100 Series Interfaces Interface Type Pumps Autosampler DA Detector MW Detector FL Detector VW Detector RI Detector Thermostatted Column Compartment Vacuum Degasser 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 Yes No...

Page 284: ...PIB connector determine the GPIB address of your module The switches are preset to a default address and recognized by the operating software from Agilent Technologies CAN Interface The CAN is an intermodule communication interface It is a 2 wire serial bus system supporting high speed data communication and real time requirement Table 61 Default Addresses Autosampler 28 Autosampler 28 Pump 22 RID...

Page 285: ... powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREPARE and START REQUEST may be issued The signal level is defined as standard TTL levels 0 V is logic true 5 V is false fan out is 10 inpu...

Page 286: ...pins are defined as follows 6 POWER ON H All modules connected to system are switched on Receiver is any module relying on operation of others 7 READY H System is ready for next analysis Receiver is any sequence controller 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 ac...

Page 287: ...able Pin Direction Function 1 In DCD 2 In RxD 3 Out TxD 4 Out DTR 5 Ground 6 In DSR 7 Out RTS 8 In CTS 9 In RI Figure 99 RS 232 Cable Instrument DCD RX TX DTR GND DSR RTS CTS RI DCD RX TX DTR GND DSR RTS CTS RI PC 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 DB9 Male DB9 Female DB9 Female DB9 Male ...

Page 288: ...s Switches 1 and 2 define which set of parameters for example for GPIB RS 232C and so on 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 Figure 100 8 bit Configuration Switch Table 64 8 bit Configuration Switch Mode Select 1 2 3 4 5 6 7 8 GPIB 0 0 GPIB Address RS 232C 0 1 Baud rate Data Bits Parity R...

Page 289: ...witch twice for example for both GPIB and RS 232C GPIB Default Addresses If you just want to change the GPIB address and need a detailed procedure refer to the Installing Your Agilent ChemStation System handbook Default GPIB address is set to the following addresses where 0 means that the switch is down and 1 means that the switch is up Table 65 Default Addresses for Agilent Series 1100 Modules Mo...

Page 290: ...s in the non volatile memory Use the following tables for selecting the setting which you want to use for RS 232C communication The number 0 means that the switch is down and 1 means that the switch is up Table 66 Communication Settings for RS 232C Communication Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baud rate Data Bits Parity Table 67 Baud Rate Settings Switches Baud Rate Switches Baud Rate 3 4 ...

Page 291: ...p will allow for normal operation If you use the following switch settings and power the instrument up again a forced cold start has been completed To return to normal operation set switches back to your GPIB or RS 232 configuration settings Table 69 Parity Settings Switches Parity 7 8 0 0 No Parity 1 0 Odd Parity 1 1 Even Parity CAUTION Forced cold start erases all methods and data stored in the ...

Page 292: ...tions 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 It only uses basic functions of the operating system for example for communication To return to normal operation set switches back to your GPIB or RS 232C configuration s...

Page 293: ...ne voltage can vary in a range from 100 120 or 220 240 volts AC 10 and needs no manual setting To disconnect the instrument from line unplug the power cord The power supply still uses some power even if the power switch on the front panel is turned off Figure 101 Main Power Supply MPS Blockdiagram 3 6 V s u p p l y 2 4 V s u p p l y 5 V s w i t c h i n g r e g u l a t o r l i n e a r v o l t a g e...

Page 294: ...tput voltages if the temperature exceeds the acceptable limit for example if the cooling fan of the instrument fails To reset the main power supply to normal operating conditions turn the instrument off wait until it is approximately at ambient temperature and turn the instrument on again The following table gives the specifications of the main power supply Table 72 Main Power Supply Specification...

Page 295: ...lent Technologies 9 Introduction to the Control Module Major keys on the Agilent 1100 Control Module 298 Screens available from the Analysis screen 299 Screens available from the System screen 315 Screens available from the Records screen 318 Diagnostics and Tests 323 ...

Page 296: ...arameters 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 NOTE The screens shown on the next pages are based on Control Module firmware revision B 01 01 LC Module firmware revision 3 8x NOTE In case the control module s display seems to be frozen hang up due to a communicati...

Page 297: ...en This is the wake up screen if the Agilent 1100 fluorescence detector is the only configured Agilent 1100 module It is used to enter the most common FLD 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 ...

Page 298: ... 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 The number of parameters on the display are restricted as additional modules are added The m key gives access to a context sensitive menu e g when the cursor is positioned in the excitatio...

Page 299: ...ettings key you open a pull down menu where you can select the FLD module Settings Within the Settings you can change the FLD parameters and with a different set of parameters available through the F1 5 keys F7 key resets the FLD to default values F8 opens a window to turn on the lamp ...

Page 300: ...Status command pulls up a monitor screen displaying signals and spectra as programmed Reset will load the FLD default parameters Use F1 key More opens a pull down menu The item Scan is available when Multi Ex or Multi Em mode has been selected The Phosphor mode is not available with FLD firmware revisions A 03 6X and below ...

Page 301: ...k for optimum signal noise and dynamic range under current conditions in the flow cell Selecting More and Lamp on the pull down menu you can enter different lamp operating modes Deselect Not Ready when lamp is off when you keep the FLD on during analysis with another detector Selecting More and Scan on the pull down menu you can enter setpoints for spectrum acquisition Multi Ex or Multi Em ...

Page 302: ...n menu you can enter setpoints for taking for the 3D fluorescence scans Data can only be displayed using the 3D Agilent ChemStation software Selecting More and Phosphor on the pull down menu you can enter setpoints for measuring phosphorescence This mode is not available with FLD firmware revisions A 03 6X and below ...

Page 303: ...ble you can list the timetable for the FLD Press F7 key Insert to add entries or F6 key Delete to remove entries Press the F7 key Insert to add 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 ...

Page 304: ...ts Settings Spectrum Monitor With the F4 key Spectrum you can watch the signals and spectra on line as programmed The F6 key Store will restart acquisition of spectra and loads the spectrum into memory in the control module Spectra are lost when a new analysis is started or when the Control Module is switched off The F8 key Eval leads to the next screen below ...

Page 305: ...to change setpoints for spectra acquisition From Menu item 1 Setup Multi WL you can switch between Excitation and Emission spectra and choose simultaneous multi wavelengths detection From Menu item 2 Setup Scan you can set spectra acquisition parameter Store spectra is only valid if an Agilent Chemstation is connected ...

Page 306: ...lot to enlarge the spectrum plot Use F6 key Print to print the plot to a printer The F8 key Scan will return to the acquisition screen During spectra review press the m key to open the context sensitive menu The menu item 1 Clear All Spectra empties the memory in the Control Module The menu item 4 Save Spectrum leads to the next screen ...

Page 307: ...s csv files and viewed with Microsoft Excel software Letters of the filename can be entered by pressing several times the numerical keys see Reference Manual of the Control Module With the F8 key Cursor you can cruise with the cursor through the spectrum The F6 key Print starts printing of the spectrum Press Esc key to return to previous screen ...

Page 308: ...10 1100 Series FD Reference Manual 9 Introduction to the Control Module Settings Run times With the F5 key Runtimes you can change the stop time and the post run time Press F5 key Views and select Status ...

Page 309: ...Introduction to the Control Module 9 1100 Series FD Reference Manual 311 Status This is an example if an Agilent 1100 FLD is configured stand alone Press the m key to open the context sensitive menu ...

Page 310: ...ot screen available also from the Analysis and System screen Here you can observe the on line signal s To add additional on line 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 the m key to open the context sensitive menu ...

Page 311: ...modules Use the Right Left arrows to switch between Available and Selected Signals Use the F8 key Move to enter available signals into the box for selected signals or vice versa 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 mdodule s The PC Card key is only active when a PCMCIA card is i...

Page 312: ...ave 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 Use the F7 F8 keys Copy to enter available signals into the box for selected signals or vice versa Press the m key to open the context sensitive menu ...

Page 313: ...ule 9 1100 Series FD Reference Manual 315 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 ...

Page 314: ...nformation about the not ready conditions if needed F2 key Reset does a re initialization of the FLD Use the F8 key On Off to turn on the lamp s 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 FLD Here you define further special setpoints for the FLD operation ...

Page 315: ...Introduction to the Control Module 9 1100 Series FD Reference Manual 317 Use the F1 key Interfaces to access the interface settings if required ...

Page 316: ...ntrol Module 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 FLD Errors are reported either into the System Log F2 or Error Log F3 ...

Page 317: ...Log to look for errors For troubleshooting reasons they can be printed or saved to a file on the PCMCIA card pressing the m key 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 pressing the m key ...

Page 318: ...hoose menu item 1 Setup limits to select lamp on level for the Xenon lamp at which you want to receive a warning If a set limit has been exceeded a message box will pop up This will not stop a sequence or run information only to plan maintenance activities If you press Reset the limits will be removed Ignore will continue to keep the EMF flag set ...

Page 319: ...e from the PCMCIA card RESnnnn DLB and press execute If you want to update the main firmware press F7 key Transfer to turn the module into the resident mode LED on module should blink yellow 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 FLD Use the F5 key FW Update to enter the Update section Select the a file from the PCM...

Page 320: ...ule 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 FLD Use the F4 key Maint log to view and edit the maintenance logbook Use the F7 key Add to add new maintenance activities ...

Page 321: ...sc key to receive Views on the F5 key Choose System from the pull down menu Use the F3 key Tests to select the FLD Several tests are available to test the Agilent 1100 FLD Additional test are listed in the function box Press the m key to open the context sensitive menu Menu item 3 Schematics will popup the FLD diagram ...

Page 322: ...teristic Use the F5 key Lamp Char to get the instrument profile Use F8 key Take to generate a new profile Wavelength Calibration Use the F1 key Calibrate and then F8 key Execute to start the FLD wavelength calibration with Glycogen in the flow cell If a deviation is found press Adjust ...

Page 323: ...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 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 peakwidth will change the retention times ...

Page 324: ...326 1100 Series FD Reference Manual 9 Introduction to the Control Module ...

Page 325: ...327 Agilent 1100 Series Fluorescence Detector Reference Manual Agilent Technologies 10 Specifications Performance Specifications 328 ...

Page 326: ...conds 8 seconds responsetime see note below this table see Raman ASTM Signal to Noise Test on page 119 Light source Xenon Flash Lamp normal mode20 W economy mode 5 W Pulse frequency 296 Hz for single signal mode 74 Hz for spectral mode Excitation Monochromator Range 200 nm 700 nm and zero order Bandwidth 20 nm fixed Monochromator concave holographic grating F 1 6 blaze 300 nm Emission Monochromato...

Page 327: ...data evaluation Agilent ChemStation for LC Agilent 1100 Control Module with limited spectral data analysis and printing of spectra Analog outputs Recorder integrator 100 mV or 1 V output range 102 luminescence units two outputs Communications Controller area network CAN GPIB RS 232C LAN APG Remote ready start stop and shut down signals Safety and maintenance Extensive diagnostics error detection a...

Page 328: ...length accuracy using the Raman band of water Housing All materials recyclable Environment 0 to 40 C constant temperature at 95 humidity non condensing Dimensions 140 mm x 345 mm x 435 mm 5 5 x 13 5 x 17 inches height x width x depth Weight 11 5 kg 25 5 lbs Table 74 Performance Specifications Agilent 1100 Series Fluorescence Detector Type Specification Comments NOTE Reference conditions standard c...

Page 329: ...ent Technologies A Safety Information General Safety Information 332 Lithium Batteries Information 335 Radio Interference 336 Sound Emission 337 UV Radiation 338 Solvent Information 339 Declaration of Conformity for HOX2 Filter 340 Agilent Technologies on Internet 341 ...

Page 330: ...protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured agai...

Page 331: ... the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting Safety Symbols Table 75 shows safety symbols used on the instrument and in the manuals Table 75 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user sh...

Page 332: ...hysical injury or damage to the equipment Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A caution alerts you to situations that could cause a possible loss of data Do not proceed beyond a caution until you have fully understood and met the indicated conditions ...

Page 333: ... RID IMDG is not allowed Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries WARNING Lithiumbatteri Eksplosionsfare ved fejlagtic handtering Udskiftning ma kun ske med batteri af samme fabrikat og type Lever det brugte batteri tilbage til leverandoren WARNING Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri so...

Page 334: ...ies 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 ...

Page 335: ...is 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 Sound Pressure Lp 70 dB A At Operator Position Normal Operation According to ISO 7779 1988 EN 27779 1991 Type Test ...

Page 336: ... to the following TLVs Threshold Limit Values according to the American Conference of Governmental Industrial Hygienists Typically the radiation values are much smaller than these limits Table 76 UV Radiation Limits Exposure day Effective Irradiance 8 hours 0 1 µW cm2 10 minutes 5 0 µW cm2 Table 77 UV Radiation Typical Values Position Effective Irradiance Lamp installed 50 cm distance average 0 01...

Page 337: ...aphy method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCl3 O2 2COCl2 2HCl This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Chromatographic grade ethers which ...

Page 338: ...ational Institute of Standards Technology NIST holmium oxide solution standard with a lot to lot tolerance of 0 3 nm The wavelength calibration filter built into the Agilent Technologies UV visible detectors is made of this material and meets these specifications It is therefore suitable for wavelength calibration of these detectors within the specified wavelength accuracy of the respective detect...

Page 339: ...echnologies 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 ...

Page 340: ...342 1100 Series FD Reference Manual A Safety Information ...

Page 341: ...em screen 315 Tests and Diagnostic screens 323 Timetable screens 305 cut off filter 243 cutoff filter other type 215 cuvette 238 how to use 138 D DAC test 127 dark current test 117 degradation UV 115 245 delivery checklist 17 dimensions and weight 16 dispersion of light 247 E early maintenance feedback EMF 259 electrical connections description of 256 EMF early maintenance feedback 259 emission co...

Page 342: ...N 286 GPIB 286 overview 285 RS 232C 288 internet 341 Introduction to the Detector 238 L lamp intensity history 116 lamp intensity test 115 LAN interface board 282 LAN cables 236 LAN interface board 284 leaks correcting 140 line voltage and frequency 16 luminescence 239 M message A D overflow 94 ADC not calibrated 93 compensation sensor open 86 compensation sensor short 87 encoder index not found 8...

Page 343: ...exchanging a flow cell 135 exchanging a lamp 147 exchanging EX condenser 152 exchanging internal parts 142 exchanging leak sensor 165 exchanging main board FLM 159 exchanging power supply 190 exchanging the fan 163 installing the optical unit 194 introduction 130 of the detector 3 129 removing covers 144 146 removing optical unit 178 removing rear foam 146 replacing cutoff filter 168 replacing EM ...

Page 344: ...peration and electronics 263 troubleshooting error messages 74 77 no peaks 100 status indicators 74 75 U unpacking 17 using EMF 259 UV degradation 115 245 W wavelength recalibration 74 101 wavelength calibration 101 wavelength calibration procedure 101 110 wavelength calibration steps 103 wavelength shift of spectra 32 weight and dimensions 16 X xenon flash lamp 243 245 ...

Page 345: ......

Page 346: ...rence information about the Agilent 1100 Series fluorescence detector The manual describes the following installing the detector optimization of the detector diagnostics and troubleshooting repairing the detector parts and materials and introduction to the detector and theory of operation ...

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