Home

Agilent 1200 Series Diode Array and Multiple Wavelength Detector

1. A q D c p CD 2c REMOTE a j SI mS H O LI DA er QO N f L RS 232 oO Oo Co oy FR a VGC ii i LJ ere i E i A ANALOG ANALOG CHT CLUN fe 2 Oa 1 2 COMPACT FLASH C D c 3C as 5 5 alot D E C gt C c gt oma sz ce 3 gt C c 3 C 3 C i A A al gt gt jE ie Figure 8 Location of LAN interface and MAC label 48 1200 Series DAD and MWD Service Manual LAN Configuration 4 TCP IP parameter configuration To operate properly in a network environment the LAN interface must be configured with valid TCP IP network parameters These parameters are e IP address e Subnet Mask e Default Gateway The TCP IP parameters can be configured by the following methods e by automatically requesting the parameters from a network based BOOTP Server using the so called Bootstrap Protocol e by manually setting the parameters using Telnet e by manually setting the parameters using the Handheld Controller G1323B see page 68 or Instant Pilot G4208A see page 67 The LAN interface differentiates between several initialization modes The initialization mode short form init mode defines how to determine the active TCP IP parameters after power on The parameters may be derived from a Bootp cycle no
2. o a SS A EEEE Li gt 7 c SELD 1 ol Oa ee o FA FA conrie CAN _GAN f as 232 USB o _LAN i r h y fe O LA Le Bs A fo ANALOG ANALOG E gt Li i 2 COMPACT FLASH i SS _ iE pa gt gt C ae C C C Bi Q Q 2 a C DAE Power N E C C DE A C 4 DC KO c C c gt C A Figure 5 Rear View of Detector The PCMICIA slot has been removed from all detectors in November 2006 with the introduction of the G1315D DAD and G1365D MWD 40 1200 Series DAD and MWD Service Manual Installing the Detector 3 Status indicator _ 2 green yellow red iss i 7 On j K Line power switch x l l with green light Figure 6 Front View of Detector 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 panel is turned off The detector was shipped with default configuration settings To change these settings see Configuration Switches on page 50 1200 Series DAD and MWD Service Manual 41 3 Installing the Detector Flow Connections to the Detector Preparations Detector is
3. X i A SD Ree Figure 125 Power and Status Light Pipe 338 1200 Series DAD and MWD Service Manual Sheet Metal Kit Table 50 Sheet Metal Kit Parts Item Description Parts for Repairs 15 Part Number 1 3a 3b 3c Sheet metal kit C includes case top cover and front for G1315C G1365C only Screws M3 for cover and flow cell door Thumb screw for union holder Zero dead volume fitting Union holder clamp G1315 68717 5022 2112 0515 2769 5022 2184 G1315 05205 Figure 126 Sheet Metal Kit Parts 1200 Series DAD and MWD Service Manual 339 15 Parts for Repairs 340 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 16 Identifying Cables Cable Overview 342 Analog Cables 344 Remote Cables 347 BCD Cables 352 Auxiliary Cable 354 CAN Cable 355 External Contact Cable 356 RS 232 Cable Kit 357 LAN Cables 358 This chapter provides information on cables used with the 1200 series of HPLC modules ee Agilent Technologies 341 16 Identifying Cables Cable Overview Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations 342 Table 51 Cables Overview Type Description Part Number Analog 3390 2 3 integrators 01040 60101 cables 3394 6 integrators 35900 60750 35900A A D converter 35900 60750 General
4. 1 Introduction Introduction to the Detector The detector is designed for highest optical performance GLP compliance and easy maintenance It includes the following features 80 Hz data acquisition rate for ultra fast LC applications requires internal hard disk SL version only data recovery DRC feature provides data never lost insurance requires internal hard disk SL version only RFID tags for all flow cells and UV lamps provides traceable information about these assemblies long life deuterium with RFID tag and tungsten lamps for highest intensity and lowest detection limit over a wavelength range of 190 950 nm no loss in sensitivity for up to eight wavelengths simultaneous programmable slit from 1 16 nm for complete optimization of sensitivity linearity and spectral resolution optional flow cell cartridges with RFID tag standard 10 mm 13 ul semi micro 6 mm 5 ul micro 3 mm 2 ul 80 nl 500 nl 10 mm high pressure 10 mm 1 7 ul and prep cells are available and can be used depending on the application needs easy front access to lamps and flow cell for fast replacement and built in holmium oxide filter for fast wavelength accuracy verification built in temperature control for improved baseline stability additional diagnostic signals for temperature and lamp voltage monitoring For specifications see Performance Specifications on page 30 16 1200 Series DAD and MWD Service Manual Introduc
5. During calibration of the detector the calibration values are stored in ROM If no data is available in the spectrometer ROM the error message is generated Probable Causes e The detector is new e The detector has been repaired Suggested Actions Y Recalibrate the detector Y Exchange the optical unit 146 1200 Series DAD and MWD Service Manual Error Information 8 Diode Current Leakage When the detector is switched on the processor checks the leakage current of each of the optical diodes If the leakage current exceeds the upper limit the error message is generated Probable Causes e Defective optical unit e Defective detector main board Suggested Actions V Exchange the optical unit V Defective detector main board 1200 Series DAD and MWD Service Manual 147 8 148 Error Information Holmium Oxide Test Failed The holmium oxide test in the detector has failed During the holmium test the detector moves the holmium filter through the light path while monitoring the detector signal response As the edge of the filter passes through the light path the signal is interrupted This is used to determine the position of the filter and whether the filter is moving correctly If the filter fails to move the error message is generated Probable Causes e Lamps switched off e Defective or dirty flow cell e Defective filter assembly e Defective achromat assembly e Defective optical unit Suggested Acti
6. Figure 115 Parts at rear of the detector The PCMICIA slot has been removed from all detectors in November 2006 with the introduction of the G1315D DAD and G1365D MWD See also Removing the PCMCIA Interface on page 272 326 1200 Series DAD and MWD Service Manual Table 39 Parts At The Rear Of The Detector Rear Parts Parts for Repairs 15 Item Description Part Number Main board DADM for G1315 DAD SL minimum firmware B 01 01 G1315 66560 Main board DADM for G1315C DAD SL exchange assembly G1315 69560 Main board MWDM for G1365 MWD SL minimum firmware B 01 01 G1365 66560 Main board MWDM for G1365 MWD SL exchange assembly G1365 69560 Main board DADM for G1315D DAD minimum firmware B 01 04 G1315 66565 Main board DADM for G1315D DAD exchange assembly G1315 69565 Main board MWDM for G1365D MWD minimum firmware B 01 04 G1365 66565 Main board MWDM for G1365D MWD exchange assembly G1365 69565 Power supply for power and status light parts see page 338 0950 2528 1 Screws M4 8 mm lg 0515 0910 2 Hexagonal nut for remote connector 1251 7788 3 Nut for analog connector 2940 0256 3 Washer for analog connector 2190 0699 4 CompactFlash Card Kit for use with G1315C DAD SL and G1365C MWD SL 01100 68700 Cable CAN to Agilent 1200 Series modules 0 5 m Cable CAN to Agilent 1200 Series modules 1 m Cross over network cable shielded 3 m long for point to point connection Twisted pair network cable shielded 7 m long
7. Item Description Part Number 1 Front cover 5065 9982 2 Plastics includes base sides and top 5065 9985 3 Name plate Agilent 1200 Series 5042 8901 For correct assembling of the top and sides see Assembling the Main Cover on page 302 Figure 122 Plastic Parts 1200 Series DAD and MWD Service Manual 335 15 Parts for Repairs Leak Parts Table 47 Leak Parts Item Description Part Number 1 Leak sensor assembly 5061 3356 2 Leak pan G1315 45511 3 Leak funnel 5041 8388 4 Leak funnel holder 5041 8389 5 Clip 5041 8387 6 7 Corrugated tubing 120 mm lg re order 5m 5062 2463 A Hip il I Figure 123 Leak Parts 336 1200 Series DAD and MWD Service Manual Parts for Repairs 15 Foam Parts Table 48 Foam Parts Item Description Part Number 1 2 EPP foam kit C includes base and top G1315 68732 for G1315C G1365C only 3 Damper kit includes 7 bumpers G1315 68706 Do not order the individual part numbers mentioned on the foam Figure 124 Foam Parts 1200 Series DAD and MWD Service Manual 337 15 Parts for Repairs Power and Status Light Pipes Table 49 Power and Status Light 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 4
8. Test Failed Probable Causes e Defective slit assembly stray light e Defective detector main board e Defective optical unit Suggested Actions Y Run the Slit Test on page 164 part of the Self test on page 160 V Exchange the detector main board Exchange the optical unit 1200 Series DAD and MWD Service Manual 165 9 Test Functions Instrument G1315c Serial Number 2200000024 Operator Wolfgang Date 25 02 2005 Time 14 50 12 File C CHEM32 2 DIAGNOSE DAD_DARK2 DGR Dark Current Plot Dark Current Test Results Specification Measured Result Dark current maximum value lt 12000 cts 6056 cts Passed Dark current minimum value gt 0 ets 7994 cts Passed Figure 70 Dark Current Test Results report 166 1200 Series DAD and MWD Service Manual Test Functions 9 Intensity Test The test is for the standard flow cells 10 mm and 6 mm pathlength only The nano flow cells 80 nl and 500 nl cannot be run with this test due to its low volume The intensity test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm Four spectral ranges are used to evaluate the intensity spectrum The test is used to determine the performance of the lamps and optics see also Cell Test on page 174 When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents t
9. WARNING Do not let liquid drip into the detector It could cause shock hazard and it could damage the detector 204 1200 Series DAD and MWD Service Manual Maintenance and Repair 11 Using the ESD Strap Electronic boards are sensitive to electrostatic discharge ESD In order to prevent damage always use an ESD strap 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 89 Using the ESD Strap 1200 Series DAD and MWD Service Manual 205 11 Maintenance and Repair 206 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 12 Maintenance Overview of Maintenance 208 Exchanging a Lamp 209 Exchanging a Flow Cell 211 Maintenance of Standard Semi Micro or Micro Flow Cell 214 Maintenance of High Pressure Flow Cell 219 Replacing Capillaries on a Standard Flow Cell 222 Replacing Capillaries on a Semi Micro Micro and High Pressure Flow Cell 227 Nano Flow Cell Replacing or Cleaning 231 Cleaning or Exchanging the Holmium Oxide Filter 236 Correcting Leaks 239 Replacing Leak Handling System Parts 240 Replacing the CompactFlash Card G1315C G1365C only 241 Replacing the Detector s
10. After calibration the holmium oxide test see Figure Holmium Oxide Test on page 169 provides verification of wavelength accuracy at three additional wavelengths 1200 Series DAD and MWD Service Manual 177 9 Test Functions Test Chromatogram 178 A pre defined test chromatogram on the detector main board is processed through ADC like normal signals from the diodes and can be used to check the Analog to Digital Converter and the data handling system The signal is available at the analog output and on the LAN The run time of the chromatogram is depending on the setting for response time peak width If no stop time is set the chromatogram will repeat continuously Table 21 Test Chromatogram Settings examples Response time Set Run Time 0 1 sec 0 28 min 0 2 sec 0 6 min 0 5 sec 1 2 min 1 sec 2 3 min 2 sec default 4 5 min 4 sec 9 min 8 sec 18 min 16 sec 36 min Table 22 Test Chromatogram Peak Heights Peak Absorbance approx 1 38 mAU 2 100 mAU 3 290 mAU 4 20 mAU 1200 Series DAD and MWD Service Manual Test Functions 9 Agilent ChemStation 1 Select the response time and stop time according to Table 21 on page 178 2 If required connect a recording device to the analog output 3 Activate the test chromatogram by typing into the command line or as pre run command PRINT SENDMODULE NDAD SIMU DFLT for G1315C D DAD or PRINT SENDMODULE NMWD SIMU DFLT for G1365C D MW
11. CAUTION Make sure to have easy access to the power cable of the instrument in order to disconnect the instrument from line 26 Power Cords Different power cords are offered as options with the detector The female end of all power cords is identical It plugs into the power input socket at the rear of the detector The male end of each power cord is different and designed to match the wall socket of a particular country or region 1200 Series DAD and MWD Service Manual Site Requirements and Specifications 2 Never operate your instrumentation from a power outlet that has no ground connection Never use a power cord other than the Agilent Technologies power cord designed for your region Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations CAUTION Bench Space The detector dimensions and weight see Table 1 allows you to place the detector on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 3 1 inches in the rear for air circulation and electric connections If the bench should carry a Agilent 1200 Series system make sure that the bench is designed to bear the weight of all modules The detector should be operated in a horizontal position Environment Your detector will work within the specifications at ambient temperatures and relativ
12. If an Agilent ChemStation is also connected restart the Agilent ChemStation now as well To change the product number go to the System screen 1 2 3 Press Tests F3 and select the detector being changed and press Enter While in the Tests screen press m m m dot m From the box now displayed select the Command and press Enter Into the box labeled Instr instruction enter the command TYPE XXXXX Letters and numbers are created using the up and down arrows XXXXX is the 5 character product number of the detector being changed There must be a space between the word TYPE and the product number Examples TYPE G1315C to configure as a DAD SL TYPE G1365C to configure as a MWD SL To configure the detector as G1315C DAD SL and G1315D DAD requires the correct main board version 1200 Series DAD and MWD Service Manual Repairs 13 WARNING If you enter the wrong type your module might not be accessible anymore with the Agilent ChemStation In such a case re enter the TYPE command correctly 5 Now press the Execute key Below the box a reply line should then say Reply RA 0000 TYPE XXXXX XXXXX is what you just entered 6 Turn the detector off then on again Turn on should be normal In the Records screen the product column should indicate the module you just entered If an Agilent ChemStation is also connected re boot it now 1200 Series DAD and MWD Service Manual 271 13 Repairs Removing the PCMCIA I
13. OE bd CE aura K safety standards LASINI ICIS NMD 00 m r 2 afe s e 7 s configuration switch o settings refer to Setting the 8 bit Configuration voltage range power consumption frequency 100 240 V DEO WA 59 60 He Rear View of Detector Electrical Connections and Label 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 2 Site Requirements and Specifications Site Requirements 26 Physical Specifications 29 Performance Specifications 30 This chapter provides information on environmental requirements physical and performance specifications ott Agilent Technologies 25 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the detector Power Consideration The detector power supply has wide ranging capabilities and accepts any line voltage in the range mentioned in Table 1 Consequently there is no voltage selector in the rear of the detector There are also no externally accessible fuses because automatic electronic fuses are implemented in the power supply To disconnect the detector from line unplug the power cord The power supply still uses some power even if the power switch on the front panel is turned off Shock hazard or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified
14. Refer also to General Safety Information on page 382 CAUTION A CAUTION notice denotes a haz ard It calls attention to an operat ing procedure practice or the like that if not correctly performed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated condi tions are fully understood and met 1200 Series DAD and MWD Service Manual In This Manual This manual contains information for using and servicing your Diode Array and Multiple Wavelength Detector G1315C D and G1365C D 1 Introduction This chapter gives an introduction to the detector instrument overview and internal connectors 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Installing the Detector This chapter provides information on unpacking checking on completeness stack considerations and installation of the detector 4 LAN Configuration This chapter provides information on connecting the detector to the Agilent ChemStation PC 5 Using the Detector This
15. Repairs on page 251 part of the Service Manual 202 1200 Series DAD and MWD Service Manual Maintenance and Repair 11 Warnings and Cautions 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 To prevent personal injury be careful when getting in contact with sharp metal areas 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 CAUTION Electronic boards and components are sensitive to electrostatic discharge ESD In order to prevent damage always use an ESD protection when handling electronic boards and components see Using the ESD Strap on page 205 Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product Always turn the deuterium lamp off before removing it 1200 Series DAD and MWD Service Manual 203 11 Maintenance and Repair Cleaning the Detector The detector case should be kept clean Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and mild detergent Do not use an excessively damp cloth allowing liquid to drip into the detector
16. for hub connections Analog cable BNC to general purpose spade lugs 5181 1516 5181 1519 5023 0203 5023 0202 01046 60105 1200 Series DAD and MWD Service Manual 327 15 Parts for Repairs Optical Unit Assembly 8 j aia ff A ULE G Figure 116 Optical Unit Parts 328 1200 Series DAD and MWD Service Manual Parts for Repairs 15 Table 40 Optical Unit Assembly Repair Parts Item Description Part Number Optical unit C for G1315C G1365C only G1315 60102 Optical unit C exchange assembly for G1315C G1365C only G1315 69102 1 Flow Cell for details see Standard Flow Cell on page 307 Semi Micro Flow Cell on page 309 High Pressure Flow Cell on page 313 or Nano Flow Cells on page 319 2 Capillary column detector 380 mm lg 0 17 i d see Accessory Kit on page 323 G1315 87311 Teflon tubing flexible i d 0 8 mm flow cell to waste see Accessory Kit on page 323 3 Zero dead volume fitting 5022 6515 4 Longlife Deuterium lamp C with ID tag with black cover 2140 0820 5 Tungsten lamp G1103 60001 6 Coupling lens assembly for other coupling lens assembly parts see page 330 G1103 68001 7 Source lens achromat assembly for other source lens assembly parts see page 331 G1315 65201 8 Cell support assembly for other cell support assembly parts see page 332 G1315 65202 9 10 11 12 Holmium oxide filter parts see page 333
17. 100 30 water 70 Acetonitrile Ambient sample 254 nm 4 nm bandwidth reference 360 nm 100 nm bandwidth Tul 1200 Series DAD and MWD Service Manual 79 5 80 Using the Detector Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 34 The exact profile of the chromatogram will depend on the chromatographic conditions Variations in solvent quality column packing standard concentration and column temperature will all have a potential effect on peak retention and response DADI A Sigmi 4 Reeet0 100 ONR O NON D mau 4 Figure 34 Typical Chromatogram with UV detector Optimization of the System The settings used for this analysis are specific for this purpose For other applications the system can be optimized in various ways Please refer to the section Optimizing the Detector on page 103 or Optimizing in the your module s Reference Manual 1200 Series DAD and MWD Service Manual Using the Detector 5 Preparing the HPLC System 1 Turn on the Agilent ChemStation PC and the monitor 2 Turn on the 1200 series HPLC modules 3 Start the Agilent ChemStation software If the pump autosampler thermostatted column compartment and detector are found the ChemStation screen should look like shown in Figure 35 The System status is red Not Ready System status E Smeets La gt eu Ahe Urea DEFAULT ro Dotai X esse
18. 1200 Series DAD and MWD Service Manual 137 8 138 Error Information to port 4 of the sampler switching valve This tube can then be taken to waste separately The tube which normally serves as the detector cell outlet tube can be used for this purpose Leak Sensor Open The leak sensor in the detector has failed open circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current falls outside the lower limit the error message is generated Probable Causes e Leak sensor not connected to the detector main board e Defective leak sensor Suggested Actions V Ensure the leak sensor is connected correctly V Exchange the leak sensor Leak Sensor Short The leak sensor in the detector has failed short circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current increases above the upper limit the error message is generated Probable Causes Defective leak sensor Suggested Actions V Exchange the leak sensor 1200 Series DAD and MWD Service Manual Error Information 8 Compensation Sensor Open The ambient compensation sensor NTC on the detector main board in the detector has failed open circuit The resistance
19. 132 compensation sensor open 139 compensation sensor short 139 cover violation 142 diode current leakage 147 DSP not running 158 fan failed 140 heater at limit 156 heater failed 155 holmium oxide test failed 148 ignition without cover 141 illegal value from air inlet sensor 154 illegal value from heater sensor 153 leak 137 leak sensor open 138 leak sensor short 138 no run data available in device 157 remote timeout 135 shutdown 134 synchronization lost 136 time out 133 uv heater current 152 uv ignition failed 151 393 uv lamp current 149 uv lamp voltage 150 visible lamp current 143 visible lamp voltage 144 wavelength calibration failed 145 ESD electrostatic discharge strap 205 exchanging see repairs F factory default settings 50 fan drive 361 parts 334 features safety and maintenance 31 filter test 162 firmware description 376 from internet 392 main system 376 resident system 376 updates 242 377 flow cell 18 choosing one 108 correction factors 110 installation 42 path length 110 rotation limiter 289 specifications 30 support windows 18 test 174 foam parts 337 fuses none in the instrument 379 G GLP features 31 grating 18 19 heater parts 334 high pressure flow cell dimensions 110 parts 313 holmium oxide declaration of conformity 391 filter 18 test 169 247 holmium oxide filter parts 333 humidity 29 information on uv rad
20. G1315 68710 No part number 79883 68703 G1315 68713 G1315 87305 5062 2418 G1315 27706 315 14 Parts and Materials for Maintenance 316 Table 32 Prep Flow Cell SST Parts continued Item Description Part Number 11 Handle for clamp unit G1315 84901 12 Clamp unit G1315 84902 13 Screw M 2 5 4 mm lg for cell body clamp 0515 1056 5 3 2 __ 0 0 0 5 A 1 6 NOTE Gaskets 6 and 7 have different hole diameters Figure 109 Prep Flow Cell SST Parts 1 window screw 2 spring washers i 3 compression washer 4 window holder 5 quartz window 6 Gasket Figure 110 Orientation of Spring Washers 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Prep Flow Cell Quartz For more details on the Preparative Flow Cells refer to the technical note that comes with the flow cells Table 33 Prep Flow Cell Quartz Parts Item Description Part Number Prep Flow Cell Quartz 0 3 mm 20 bar 2 MPa G1315 60017 completely assembled includes all items below Prep Flow Cell Quartz 0 06 mm 20 bar 2 MPa G1315 60018 completely assembled includes all items below 1 PTFE tubing 2 m length 0 8 mm i d 0 D 1 6 mm G1315 67301 with fittings for flow cell assembled see note below PTFE tubing 80 cm length 0 5 mm i d o D 1 6 mm G1315 67302 with fittings for flow cell assembled see note below 2 Fitting fingertight 2 pk 0100 1516 3 Cell housing G1315 27705 4
21. Turning the line power off and on again resets the power supply to normal operation if the cause of the overload condition has been removed An over temperature sensor in the main power supply is used to turn off output 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 61 Main Power Supply Specifications Maximum power 160 VA 130 W Continuous output Line Input 100 240 volts AC Wide ranging 10 line frequency of 50 60 Hz Output 1 24V 4 5 A maximum total power consumption of 24 V and 36 V must not exceed 107 W Output 2 36 V 2 5 A maximum Output 3 5V 3A Output 4 15V 03A Output 5 15V 03A 1200 Series DAD and MWD Service Manual 379 17 Hardware Information 380 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual A Appendix General Safety Information 382 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 385 Radio Interference 386 Sound Emission 387 UV Radiation 388 Solvent Information 389 Declaration of Conformity for HOX2 Filter 391 Agilent Technologies on Internet 392 This chap
22. caffeine the reference wavelength must be set to 282 nm At this wavelength caffeine shows exactly the same absorbance as at 222 nm When the absorbance values are subtracted from each another any indication of the presence of caffeine is eliminated In the same way hydrochlorothiazide can be suppressed if caffeine is to be quantified In this case the wavelength is set to 204 nm and the reference wavelength to 260 nm Figure 63 shows the chromatographic results of the peak suppression technique The trade off for this procedure is a loss in sensitivity The sample signal decreases by the absorbance at the reference wavelength relative to the signal wavelength Sensitivity may be decreased by as much as 10 30 1200 Series DAD and MWD Service Manual 121 6 How to optimize the Detector Hydrochlorothiazide Hydrochlorothiazide and caffeine and caffeine Wavelength 204 nm Wavelength 222 nm No reference No reference Hydrochlorothiazide Caffeine suppressed suppressed Wavelength 204 nm Wavelength 222 nm Reference 260 nm Reference 282 nm Time min Time min Figure 63 Peak Suppression Using Reference Wavelength Ratio Qualifiers for Selective Detection of Compound Classes Ratio qualifiers can be used where in a complex sample only one particular class needs to be analyzed a parent drug and its metabolites in a biological sample for example Another example is the selective analysis of derivatives after pre or postcolumn derivat
23. electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself 1200 Series DAD and MWD Service Manual Introduction 1 Electrical Connections e The CAN bus is a serial bus with high speed data transfer The two connectors for the CAN bus are used for internal Agilent 1200 Series module data transfer and synchronization e Two independent analog outputs provide signals for integrators or data handling systems e The REMOTE connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as start stop common shut down prepare and so on e With the appropriate software the LAN connector may be used to control the detector from a computer through a LAN connection This connector is activated and can be configured with the configuration switch next to the analog connectors see LAN Configuration on page 47 See your software documentation for further information e With the appropriate software the RS 232 connector may be used to control the detector from a computer through a RS 232 connection 3rd part software or for diagnosis firmware update See RS 232C on page 371 for further information e The power input socket accepts a line voltage of 100 240 V AC 10 with a line frequency of 50 or 60 Hz Maximum power consumption is 300 VA 125 W There is no voltage selector on your detector because
24. thr a hr unstable A C om baseline from unstable AJC 04 ad al baseline from stable A C stable AJC fa ee m 7 er eT a a a Sc a ns Temperature Plot Full scale 4 F 2 2 C Baseline Plot based on above temperature 120 minutes plots Full scale 0 7 mAU 120 minutes Figure 80 Wander effects based on instable lab conditions 190 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 Specifications and Conditions Short term noise ASTM 0 8 x 10 AU at 254 and 750 nm Drift 0 9 x 10 AU hr at 254 nm ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography ASTM information can be obtained via internet http www astm org Reference conditions cell path length 10 mm response time 2 s slit width 4 nm flow 1 ml min HPLC grade Methanol ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 C hour 1 8 F hour Turbulences around one minute or less can be ignored 1200 Series DAD and MWD Service Manual 191 10 192 Diagnostic Signals Principle of
25. 13 Flow cell door seal included G1315 68707 Screw Special for flow cell door 5022 2112 14 Ribbon Cable Optical Mainboard LNFE DADM MWDM G1315 81600 15 Cable grounding G1315 16 Sealing C for G1315C G1365C only G1315 47104 17 Damping kit includes 6 bumpers G1315 68706 18 Plug hole for lamp housing 6960 0002 19 Tag Reader Assembly Lamp C for G1315C G1365C only G1315 60006 Screw M2 2 4 5 mm Ig 0515 4780 20 Tag Reader Assembly Cell C for G1315C G1365C only G1315 60005 Hex screws M3 8 mm lg 0515 1050 21 Cell rotation limiter fixed with the screws of item 20 G1315 26100 1200 Series DAD and MWD Service Manual 329 15 Parts for Repairs Coupling Lens Assembly Table 41 Coupling Lens Assembly Item Description Part Number Coupling lens assembly G1103 68001 Retainer ring Washer spring wavy Lens support Siw rm Lens 5 Lens holder IZN Figure 117 Coupling Lens Assembly Parts 330 1200 Series DAD and MWD Service Manual Parts for Repairs 15 Source Lens Achromat Assembly Table 42 Source Lens Assembly Item Description Part Number Source lens achromat assembly includes a filter lever G1315 65201 G1315 45001 1 Lens achromatic 1000 0486 2 Spring compression 1460 2255 3 Spectro window 79880 28111 4 Holder When the filter motor has been removed the filter lever should not be reused Use always a new filter lever to assure correct fit on the filter motor
26. 345 x 435 x 140 mm 13 5 x 17 x 5 5 inches Comments Line voltage Line frequency Power consumption 100 240 VAC 10 50 or 60 Hz 5 160 VA 160 W 546 BTU Wide ranging capability Maximum Ambient operating temperature Ambient non operating temperature Humidity Operating altitude Non operating altitude Safety standards IEC CSA UL EN 0 55 C 32 131 F 40 70 C 4 158 F lt 95 at 25 40 C 77 104 F Up to 2000 m 6500 ft Up to 4600 m 14950 ft Installation category Il pollution degree 2 For indoor use only Research Use Only Not for use in Diagnostic Procedures Non condensing For storing the detector 1200 Series DAD and MWD Service Manual 29 2 Site Requirements and Specifications Performance Specifications Table 2 Performance Specifications G1315C D and G1365C D Type Specification Comments Detection type 1024 element photodiode array Light source Wavelength range Short term noise ASTM Single and Multi Wavelength Drift Linear absorbance range Wavelength accuracy Wavelength bunching Slit width Diode width Flow cells Deuterium and tungsten lamps 190 950 nm 0 8 x 10 AU at 254 and 750 nm 0 9 x 10 AU hr at 254 nm gt 2 AU upper limit 1nm 1 400 nm 1 2 4 8 16 nm lt 1nm Standard 13 pl volume 10 mm cell path length and 120 bar 1760 psi pressure maximum Semi Micro 5 pl volume 6 mm c
27. 358 Recommended Cables Table 52 Description Part number Cross over network cable shielded 3 m long 5023 0203 for point to point connection Twisted pair network cable shielded 7 m long 5023 0202 for hub connections 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 17 Hardware Information z Detector Main Board DADM MWDM 360 Setting the 8 bit Configuration Switch 372 Firmware Description 376 The Main Power Supply Assembly 378 This chapter describes the detector in more detail on hardware and electronics ee Agilent Technologies 359 17 Hardware Information Detector Main Board DADM MWDM This board controls all information and activities of all assemblies within the detector Through interfaces LAN CAN or RS 232C connected to the user interface the operator enters parameters changes modes and controls the detector Main features e lamp supply for UV and Vis lamp e CompactFlash card slot for standard for G1315C DAD SLand G1365C MWD SL e identification tag operation for flow cell and UV lamp e temperature control for optical unit for stable baseline e LAN on board e CAN for internal 1200 interfacing e RS 232 for third part control or service e 2 analog outputs 0 1 V or 0 100 mV full scale e leak sensing flow cell e safety switch turns off high voltages fan e USB for future use e no i
28. DAD 1 No Run data available in device 10 07 24 11 20 05 CP Macro Analyzing rawdata SHORT_02 D 10 07 25 11 20 05 Method Instrument Error Method Sequence stopped 10 07 25 11 20 05 Method Method aborted 10 09 52 11 20 05 Figure 67 Instrument Logbook The logbook does not indicate a communication loss power fail It just shows the recovering Power on Lamps on 1200 Series DAD and MWD Service Manual 157 8 Error Information DSP Not Running This error message comes up when the communiucation between the optical unit and the main board has a problem Probable Causes Random communication error e Defective detector main board e Defective optical unit Suggested Actions V Switch the detector off and on again at the power switch If the error reoccurs V Check cable between optical unit and detector main board V Exchange the detector main board Y Replace optical unit 158 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 9 Test Functions Self test 160 Filter Test 162 Slit Test 164 Dark Current Test 165 Intensity Test 167 Holmium Oxide Test 169 Spectral Flatness Test 172 ASTM Noise Test 173 Cell Test 174 Wavelength Verification and Recalibration 176 Test Chromatogram 178 Diagnosis Information on Agilent ChemStation 181 This chapter describes the detector s built in test functions ee Agilent Technologies 159 9 Test Func
29. DAD and MWD Service Manual Hardware Information 17 Table 58 8 bit Configuration Switch Function SW 6 Link Configuratio Mode Selection Auto negotiation xX 10 MBit half duplex xX 10 MBit full duplex 100 MBit half duplex 100 MBit full duplex Bootp Bootp amp Store Using Stored Using Default Watchdog Boot Resident System X Stop Early To Debug Disable Watchdog Revert to Default Data Coldstart Legend 0 switch down 1 switch up x any position N A not assigned When selecting the mode TEST the LAN settings are Auto Negotiation amp Using Stored 1200 Series DAD and MWD Service Manual 373 17 Hardware Information LAN Settings For details on the LAN settings configuration refer to LAN Configuration on page 47 RS 232C Communication Settings The communication protocol used in this instrument supports only hardware handshake CTS RTS The RS 232 communication is always active parallel to the CAN and LAN communication For details see also RS 232C on page 371 Per default the module will use e 19200 baud e 8 data bit with no parity and e one start bit and one stop bit are always used not selectable Boot Resident Settings Firmware update procedures may require this mode in case of firmware loading errors main firmware part If you use the following switch settings a
30. Group remote connector to be connected to Agilent 1200 Series modules The other end depends on the instrument to be connected to Agilent 1200 to 3390 Integrators Connector Pin Pin Signal Name Active 01046 60203 3390 Agilent 1200 TTL 2 1 White Digital ground NC 2 Brown Prepare run Low 7 3 Gray Start Low D NC 4 Blue Shut down Low 2 NC 5 Pink Not connected 6 NC 6 Yellow Power on High NC 7 Red Ready High NC 8 Green Stop Low NC 9 Black Start request Low 1200 Series DAD and MWD Service Manual 347 16 348 Identifying Cables Agilent 1200 to 3392 3 Integrators Connector Pin Pin Signal Name Active 01046 60206 3392 3 Agilent 1200 TTL 3 1 White Digital ground aa NC 2 Brown Prepare run Low a NN Gray tart ow M S OY 11 3 G s L 0090 00 NC 4 Blue Shut down Low B j NC 5 Pink Not connected Ae ey ee NC 6 Yellow Power on High 9 7 Red Ready High 4 Key 1 8 Green Stop Low NC 9 Black Start request Low Agilent 1200 to 3394 Integrators Connector Pin Pin Signal Name Active 01046 60210 3394 Agilent 1200 TTL 9 1 White Digital ground G NC 2 Brown Prepare run Low 80 3 3 Gray Start Low ie e i NC 4 Blue Shut down Low o a NC 5 Pink Not connected Os ie NC 6 Yellow Power on High O 5 14 7 Red Ready High 6 8 Green Stop Low 1 9 Black Start request Low 13 15 Not connec
31. Item Description Part Number 3 Fitting Screw for 4 mm wrench QTY 2 reorder 10 pk 5063 6593 4 Cell ferrules are factory installed 5 PEEK fitting 1 32 not attached to capillaries reorder 10 pk 5065 4422 7 Litetouch ferrules LT 100 1 32 Ferrule and SS lock ring QTY 2 reorder 10 pk 5063 6592 8 Union Adjustment Tool used for item 7 5022 2146 9 ZDV SS Union no fitting OTY 2 5022 2184 10 Torque Adapter G1315 45003 14 Handle for clamp unit G1315 84902 15 Clamp unit G1315 84910 16 Screw M 2 5 4 mm long for cell body clamp 0515 1056 17 Wrench open end 4 mm supplied with standard accessory kit 8710 1534 G1315 68705 of your detector 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Table 36 lists the specific parts for the 500 nl flow cell Table 36 Specific 500 nl Flow Cell Parts Item Description Part Number 500 nl Flow Cell Kit G1315 68724 1 PEEK coated fused silica capillary Inlet 100 pm 61315 87333 pre mounted to cell includes Inlet capillary 300 mm long 100 um i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 PEEK coated fused silica capillary Outlet 100 um G1315 87338 pre mounted to cell includes Outlet capillary 120 mm long 100 um i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 1 PEEK coated fused silica capillary Inlet 50 um G1315 87323 alternative includes Inlet capillary 400 mm lo
32. Please find below the details of the Agilent 1200 DAD MWD flow cells Table 18 Correction factors for Agilent 1200 DAD MWD flow cells Flow cell type Cell volume Part number Path length Path length Correction nominal actual factor Standard flow cell 13 pl G1315 60022 10mm 9 80 0 07 mm 10 9 8 Semi micro flow cell 5 ul G1315 60025 6mm 5 80 0 07 mm 6 5 8 Micro flow cell 2 pl G1315 60024 3mm 3 00 0 05 mm 3 3 0 07 mm 500 Nanoliter flow cell kit 0 5 pl G1315 68724 10 mm 10 00 0 02 mm 10 10 80 Nanoliter flow cell kit 0 08 pl G1315 68716 6mm 6 00 0 02 mm 6 6 High Pressure flow cell 1 7 pl G1315 60015 6mm 5 75 0 07 mm 6 5 75 110 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 Peak width response time Response time describes how fast the detector signal follows a sudden change of absorbance in the flow cell The detector uses digital filters to adapt response time to the width of the peaks in your chromatogram These filters do not affect peak area nor peak symmetry When set correctly such filters reduce baseline noise significantly see Figure 56 but reduce peak height only slightly In addition these filters reduce the data rate to allow optimum integration and display of your peaks and to minimize disk space required to store chromatograms and spectra DAD1 A Sig 254 4 Ref off NOISE INM1NM D mAU F Unfiltered iu A EN AAE T T T T T T T T 05 4 15 2 25 3 36 mir DAD1 A Sig
33. Series DAD and MWD Service Manual 133 8 Error Information Shutdown An external instrument has generated a shut down signal through CAN or REMOTE lines The detector continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable Causes e Leak detected in an external instrument with a remote connection to the system e Shut down in an external instrument with a remote connection to the system e The degasser failed to generate sufficient vacuum for solvent degassing Suggested Actions V Fix the leak in the external instrument before restarting the pump V Check external instruments for a shut down condition V Check the degasser for an error condition Refer to the Reference Manual for the Aligent 1200 Series vacuum degasser 134 1200 Series DAD and MWD Service Manual Error Information 8 Remote Timeout A not ready condition is still present on the remote input When an analysis is started the system expects all not ready conditions e g a not ready condition during detector balance to switch to run conditions within one minute of starting the analysis If a not ready condition is still present on the remote line after one minute the error message is generated Probable Causes e Not ready condition in one of the instruments connected to the remote line e Defective remote cable e Defective components in the instrume
34. Store mode see Table 6 on page 51 Start the Agilent Bootp Service and open its window If required modify the parameters for the detector according to your needs using the existing configuration Press OK to exit the Bootp Manager Now turn on the detector and view the Bootp Server window After some time the Agilent Bootp Service will display the request from the LAN interface The parameters are now stored permanently in the non volatile memory of the detector 7 Close the Agilent Bootp Service and turn off the detector 8 Change the settings of the detector s Configuration Switch to Using Stored mode see Table 6 on page 51 Power cycle the detector The detector can be accessed now via LAN without the Agilent Bootp Service refer to PC and Agilent ChemStation Setup on page 71 1200 Series DAD and MWD Service Manual 61 4 LAN Configuration Manual Configuration 62 Manual configuration only alters the set of parameters stored in the non volatile memory of the detector It never affects the currently active parameters Therefore manual configuration can be done at any time A power cycle is mandatory to make the stored parameters become the active parameters given that the initialization mode selection switches are allowing it Non Volatile RAM Stored Parameter a Control Module Figure 19 Manual Configuration Principle 1200 Series DAD and MWD Service Manual L
35. Store SampleBw Reference Bw Store Sample Bw Reference Bw Pui a oa fe fico fio fom a ose fe oso 100 afm 8 Not Ready Information os s4 fie f aso froo nm B T Jass fie faso fioo nm ee er pop far fio jem cr foro fe for fro fom D feso fis feso fioo gem p feso fis feso fron nm E feso fie feso fioo em E feso fis feso fioo 2f mm FT feso fie feso foo em e feso fis feso fioo Sf mm ero fea fie o fiw fom Gr o fre o foo io Ha f2s0 fie faco fioo nm HET feeo fie Jaso fioo nm Spectrum Ore Every 2nd spectrum Store Every 2nd spectrum None Range pex Baselines Range fiso to 400 nm Apex Slopes B aselines Step Allin peak Step 2 0 nm Every 2nd spectrum Threshold Threshold 11 00 mA Figure 50 98 Spectra Settings 1200 Series DAD and MWD Service Manual Table 15 Spectrum Settings Using the Detector 5 Store None Apex Baselines Apex Slopes Baselines All in Peak Every 2nd spectrum All Range Step Threshold Defines at which points on signal A spectra will be taken and saved Signal A is used to control the peak controlled spectra acquisition the other signals have no influence on spectra acquisition No spectra are taken Spectra are taken at the apex and baselines of the peak Spectra are taken at the apex baselines upslope and downslope of the peak All spectra within the peak are taken The three
36. a toothpick 1200 Series DAD and MWD Service Manual 233 12 Maintenance 9 Insert the flow cell capillaries and tighten them fingertight Use the wrench and torque adapter as described on page 235 and tighten the fittings alternately 10 Reassemble the flow cell body to the holder 11 Re install the flow cell and connect the capillaries to the union holder Next Steps 12 Perform a leak test with the flow cell outside of the detector 13 If no leak is observed install the flow cell and you are ready to work 14 Make sure that the flow cell assembly is inserted correctly and fits perfectly in the optical unit especially when PEEK capillaries are used The cell body can be fitted in two positions to allow the capillaries routed upwards or downwards depending on where the column is located Route the capillaries directly column inlet and waste assembly outlet 234 1200 Series DAD and MWD Service Manual Wrench 1200 Series DAD and MWD Service Manual Maintenance 12 With the instrument accessory kit comes a 4 mm wrench and with the Sealing Kit a special adapter Both together work as a torque wrench with pre defined torque maximum allowed torque for the cell fittings is 0 7 Nm It can be used to tight the capillary fittings at the flow cell body The wrench has to be plugged into the adapter as shown in Figure 90 Adapter DO NOT press down more than
37. and MWD Service Manual 389 A Appendix e Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides e Solutions of organic acids acetic acid formic acid and so on in organic solvents For example a 1 solution of acetic acid in methanol will attack steel e Solutions containing strong complexing agents for example EDTA ethylene diamine tetra acetic acid e Mixtures of carbon tetrachloride with 2 propanol or THF 390 1200 Series DAD and MWD Service Manual Appendix A Declaration of Conformity for HOX2 Filter Declaration of Conformity We herewith inform you dint the Holmium Oxide Glass Filter Type Hoya HY 1 Part No 79880 22711 meets the following specification of absorbance maxima positions 418 Som 3640 GISMABC 1100 1200 360 num 415 Som 36 Aum The variation m Measired Wavelength depends on the different Optical Bandwidih Agilent Technologies guarantees the traceability of the specified abyvorbamce maxuna to a National Institute of Sundards amp Technology NIST Hobmimn Oxide Solution Standard with a Jot to lot tolerance of 0 3 nm The wavelength calibration filter built into the Agilent Technologies UV VIS detectors is made of this material and tects these specifications It is therefore suitable for wavelength calibration of these detector within the spe
38. application needs a different type of flow cell or the flow cell needs repair Tools required Two 1 4 inch wrenches for capillary connections Parts required Standard flow cell 10 mm 13 pl 120 bar G1315 60022 Semi micro flow cell 6 mm 5 pl 120 bar G1315 60025 Micro flow cell 3 mm 2 pl 120 bar G1315 60025 High pressure flow cell 6 mm 1 7 pl 400 bar G1315 60015 Nano flow cell refer to Nano Flow Cell Replacing or Cleaning on page 231 Preparations Turn the lamp s off Remove the front cover 1 Press the release buttons and remove the front cover to have access to the flow cell area 2 Open the flow cell cover 1200 Series DAD and MWD Service Manual 211 12 Maintenance Note B Disconnect the flow cell inlet capillary top and the waste tubing bottom from the unions Depending on the system setup the inlet capillary might be routed directly from the module above or below to the cell and not to the capillary holder Loosen the thumb screw and remove the flow cell outlet 5 Remove the flow cell while pressing the flow cell holder capillary bottom with the union 212 1200 Series DAD and MWD Service Manual Maintenance 12 Note 6 Insert the flow cell while pressing the flow cell holder The label attached to the flow cell provides information on part number path length volume and maximu
39. are different 214 1200 Series DAD and MWD Service Manual Maintenance 12 1 Use a4 mm hex key to unscrew the window assembly 1 and remove the gasket 2 from the cell body Do not mix the gasket 6 and 7 different hole diameter Note If you want to replace the gasket only continue with step 7 Do not mix the gasket 6 and 7 They are different for standard and semi micro flow cell 2 Use a tooth pick to remove the quartz window from the window assembly push through from the screw side Note If the washers fall out of the window assembly they must be inserted in the correct order with the Teflon ring to prevent any leaks from the flow cell window 1200 Series DAD and MWD Service Manual 215 12 Maintenance Noor wohr Orientation of Flow Cell Parts NOTE Gaskets 6 and 7 have different hole diameters window screw spring washers compression washer window holder quartz window gasket light in gasket light out 8 items 2 3 4 and 5 9 10 inlet capillary 11 outlet capillary 12 holder window screw contains flow cell body 3 Assemble the washers and the window assembly in correct order Correct orientation of spring washers 2 is required 216 1200 Series DAD and MWD Service Manual Maintenance 12 5 Press the Teflon ring into the window assembly 6 Press the window asse
40. be given the opportunity to edit the configure 1200 access screen during the restart of the Agilent ChemStation After restart the serial number type you have just entered can be seen under the Instrument menu of the main user interface screen Using the Instant Pilot G2408A 1 Connect the Instant Pilot to the detector s CAN connector Turn ON the detector On the Instant Pilot s Welcome screen press More then select Maintenance Using the up down arrows select the detector where you have to change the product number or serial number Press PN SN This will display a screen where you can enter the product number and or serial number Make your changes using the information from the product label of your module 1200 Series DAD and MWD Service Manual Repairs 13 To configure the detector as G1315C DAD SL and G1315D DAD requires the correct main board version WARNING If you enter the wrong type your module might not be accessible anymore with the Agilent ChemStation and the Instant Pilot unsupported module In such a case follow the Recover Instructions on page 269 5 Press OK to highlight the complete command 6 Press Done to transfer the information into the main board s memory Press Cancel quit the process 7 Turn the detector OFF then ON again The Maintenance screen should display the correct serial number for this module 8 Ifan Agilent ChemStation is also connected restart the Agilen
41. connected correctly V Exchange fan V Exchange the detector main board 140 1200 Series DAD and MWD Service Manual Error Information 8 Open Cover The top foam has been removed The sensor on the detector main board detects when the top foam is in place If the foam is removed the fan is switched off and the error message is generated Probable Causes e The top foam was removed during operation e Foam not activating the sensor Suggested Actions Y Replace the top foam V Exchange the foam 1200 Series DAD and MWD Service Manual 141 8 Error Information Cover Violation The top foam has been removed The sensor on the detector main board detects when the top foam is in place If the foam is removed while the lamps are on or if an attempt is made to switch on the lamps with the foam removed the lamps are switched off and the error message is generated Probable Causes e The top foam was removed during operation e Foam not activating the sensor Suggested Actions V Replace the top foam V Exchange the foam 142 1200 Series DAD and MWD Service Manual Error Information 8 Detector Error Messages These errors are detector specific Visible Lamp Current The visible lamp current is missing The processor continually monitors the lamp current during operation If the current falls below the lower current limit the error message is generated Probable Causes e Visible lamp disconnected e
42. does not ignite Screwdriver POZI 1 PT3 Longlife Deuterium lamp C 2140 0820 with black cover and RFID tag Tungsten lamp G1103 60001 Turn the lamp s off CAUTION If the detector has been in use the lamp may be hot If so wait five minutes until lamp cools down 1 Press the release buttons and remove the front cover to 2 Disconnect lamp from the connector unscrew the Vis lamp left and or UV lamp right and remove the lamp Do not touch the glass bulb with your fingers have access to the lamp area 1200 Series DAD and MWD Service Manual 209 12 Maintenance 3 When replacing the Vis lamp assure that the Vis lamp is Insert the lamp Fix the screws and reconnect the lamp to inserted as shown flat edge towards the deuterium lamp connector 5 Replace the front cover Next steps 6 Reset the lamp counter as described in the user interface documentation lamps with RFID tag cannot be reset 7 Turn the lamp on and give the lamp 10 minutes to warm up 8 Performa Wavelength Verification and Recalibration on page 246 or a Holmium Oxide Test on page 247 to check the correct positioning of the UV lamp 9 Perform an Intensity Test on page 167 210 1200 Series DAD and MWD Service Manual Exchanging a Flow Cell Maintenance 12 When required If an
43. external contact 356 cables LAN cables 358 cell support 332 coupling lens 330 fan heater and sensor 334 foams and dampers 337 for maintenance 303 for repair 325 high pressure micro flow cell 313 holmium oxide filter 333 leak parts 336 main assemblies for maintenance 305 nano flow cells 319 optical unit 328 overview for maintenance 304 plastics 335 power and status 338 prep flow cell 315 317 semi micro flow cell 309 sheet metal 339 standard flow cell 307 union holder ZDV 339 PC and Agilent ChemStation Setup 71 PCMCIA 364 removing from board 272 peak width response time 111 performance optimization 106 specifications 30 photometric accuracy 110 physical specifications 29 humidity 29 line voltage and frequency 29 operating altitude 29 operation temperature 29 power consumption 29 weight and dimensions 29 power considerations 26 consumption 29 cords 26 parts 338 power supply description 378 specifications 379 1200 Series DAD and MWD Service Manual Index prep flow cell 315 317 programmable slit width 30 rear view of module 24 40 364 recalibration of wavelength 126 recyclable material 31 reference conditions ASTM 32 removing the PCMCIA Interface 272 repair introduction 201 repair parts 325 repairs 251 assembling main cover 302 cleaning the instrument 204 correction leaks 239 definition of 202 exchanging a fl
44. f Nin y Minx Lear M i A vies a T j Wf V ry W W V WY y N N A LY WV ALY ji e ie MU W a 23 LJ w tere Figure 88 Board Temperature internal detector buffer 1200 Series DAD and MWD Service Manual 199 10 Diagnostic Signals 200 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector o Service Manual e0 0 oe 11 Maintenance and Repair e e j Introduction to Maintenance and Repair 202 Warnings and Cautions 203 Cleaning the Detector 204 Using the ESD Strap 205 This chapter provides general information on repairing the detector Agg Agilent Technologies 201 11 Maintenance and Repair Introduction to Maintenance and Repair Simple Repairs Maintenance The detector is designed for easy repair The most frequent repairs such as lamp change and flow cell change can be done from the front of the detector with the detector in place in the system stack These repairs are described in Maintenance on page 207 part of the User Manual and Service Manual Exchanging Internal Parts Repair Some repairs may require exchange of defective internal parts Exchange of these parts requires removing the detector from the stack removing the covers and disassembling the detector The security lever at the power input socket prevents that the detector cover is taken off when line power is still connected These repairs are described in
45. information product number product number e serial number e serial number production date production date accumulated UV on time nominal path length of the cell actual UV lamp on time cell volume in nl number of ignitions maximum pressure in bar date of last intensity test date of last cell test This feature is available for special lamps and flow cells mentioned in chapter Parts and Materials for Maintenance on page 303 or Parts for Repairs on page 325 CompactFlash Card Slot Below the PCMCIA slot Figure 127 the detector has a CompactFlash card slot G1315C DAD and G1365C MWD only The G1315C DAD and G1365C MWD are tested with the supplied CompactFlash card only Other CompactFlash cards may vary slightly and may not work correctly 1200 Series DAD and MWD Service Manual 363 17 Hardware Information The CompactFlash card allows constant buffering of data spectra information so that in case of e a busy ChemStation that cannot take the data from the detector in time or e a lost network connection no application data of the detector is lost The G1315C DAD must be operated with the CompactFlash card due to the high data rate Otherwise an error on the ChemStation will show up PCMCIA Slot The PCMICIA slot has been removed from all detectors in November 2006 with the introduction of the G1315D DAD and G1365D MWD USB The USB connector is not active yet Will be used fo
46. installed in the LC system Parts required Other modules Parts from accessory kit see Detector Accessory Kit Contents on page 35 Two wrenches 1 4 5 16 inch for capillary connections 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 42 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 avoid breakage due to subambient conditions The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the outside and to cover the deuterium lamp Some types of the Agilent deuterium lamps show a light ring during operation This is not harmful refer to UV Radiation on page 388 The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column For details see Replacing Capillaries on a Standard Flow Cell on page 222 1200 Series DAD and MWD Service Manual Installing the Detector 3 1 Press the release buttons and remove the front cover to 2 Press the release button and open the flow cell door gain acc
47. is moved through all slit positions while the detector monitors the lamp intensity change When the slit position is changed the intensity drop move to smaller slit or intensity increase move to larger slit must be within a defined range If the intensity changes are outside the expected range the test fails Slit Test Evaluation Limit 0 7 1 3 Test Failed Probable Causes e Flow cell still installed e Old lamp e Defective slit assembly e Defective detector main board e Defective optical unit Suggested Actions V Remove the flow cell Y Run the Intensity Test on page 167 Exchange the lamp if old or defective V Exchange the slit assembly V Exchange the detector main board Y Exchange the optical unit 1200 Series DAD and MWD Service Manual Test Functions 9 Dark Current Test The dark current test measures the leakage current from each diode The test is used to check for leaking diodes which may cause non linearity at specific wavelengths During the test the slit assembly moves to the dark position cutting off all light falling onto the diode array Next the leakage current from each diode is measured and displayed graphically see Figure 70 The leakage current represented in counts for each diode should fall within the limits red bands shown in the plot see Figure 70 The evaluation report is only on the Agilent ChemStation available Dark Current Test Evaluation Limit 0 12000 counts
48. is operated at a constant voltage of approx 5 5 VDC Safety Switches If the EPP foam is removed while the instrument is still on the safety light switches are activated and the deuterium lamp and the tungsten lamp are switched off Interfaces For detailed information on interfaces LAN CAN RS 232 see Interfaces on page 367 Temperature Control The G1315C D and G1365C D detectors are equipped with a temperature control to improve the baseline stability in unstable environments e g strong variation of the temperature due to air condition systems A heater and a temperature sensor assembly have been added and are controlled by the detector main board and its firmware There are no parameters to be set for the temperature control Internal Clock without Battery There is no battery on the main board that buffers the module clock The voltage for the clock is supplied by a capacitor that provides the voltage for minimum 4 weeks After that time the clock stops and at next power on it will synchronize with the clock from the Agilent ChemStation 362 1200 Series DAD and MWD Service Manual Hardware Information 17 Lamp and Flow Cell RFID Tag The Agilent G1315C D and G1365C D are equipped with a lamp flow cell identification system This allows to write and to read lamp flow cell specific information to and from the lamp flow cell identification tag see Table 53 Table 53 RFID Tag Data Lamp information Flow cell
49. mV or 1 V output range 0 001 2 AU two outputs Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN All flow cells are equipped with RFID tags that hold cell typical information Revision B 01 03 or above G1315C G1365C Revision B 01 03 SR 2 B 02 01 SR 2 or above G1315D G1365D Revision B 01 02 or above G1315C G1365C Revision B 02 01 or above G1315D G1365D Revision B 04 02 Safety and maintenance GLP features Housing Extensive diagnostics error detection and display through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user setable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with built in holmium oxide filter All materials recyclable 1200 Series DAD and MWD Service Manual 31 2 Site Requirements and Specifications ASTM Standard Practice for Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions cell path length 10 mm time constant 1 s equal to response time 2 s flow 1 ml min LC grade Methanol slit width 4 nm Linearity measured with caffeine at 265 nm For environmental conditions
50. main board Probable Causes e Loose fittings e Broken capillary e Leaking flow cell Suggested Actions V Ensure all fittings are tight Y Exchange defective capillaries V Exchange flow cell components Additional Information Detector leak error may be caused by the Aligent 1200 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 sampler s contingency leak drain system which eventually terminates in the leak pan of the bottom module of the stack the detector With normal injection volumes and run times the output of port 4 is small and evaporates right in the sampler leak pan However the output of port 4 is significant and a substantial volume of ejected mobile phase reaches the detector leak pan There are two possible fixes Select the one which is most convenient 1 The waste drain plumbing orientation shown in step 5 on page 44 eliminates the possibility of any leak drainage from above reaching 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 itis 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
51. mode Bootp amp Store carefully because writing to the non volatile memory takes time Therefore when the detector shall obtain its parameters from a Bootp Server every time it is powered on the recommended initialization mode is Bootp Using Stored When initialization mode Using Stored is selected the parameters are taken from the non volatile memory of the detector The TCP IP connection will be established using these parameters The parameters were configured previously by one of the described methods 1200 Series DAD and MWD Service Manual LAN Configuration 4 Active Stored Parameter Parameter Figure 12 Using Stored Principle Using Default When Using Default is selected the factory default parameters are taken instead These parameters enable a TCP IP connection to the LAN interface without further configuration see Table 7 Default Active Parameter Parameter Figure 13 Using Default Principle Using the default address in your local area network may result in network problems Take care and change it to a valid address immediately Table 7 Using Default Parameters IP address 192 168 254 11 Subnet Mask 255 255 255 0 Default Gateway not specified Since the default IP address is a so called local address it will not be routed by any network device Thus the PC and the detector must reside in the same subnet 1200 Series DAD and MWD Service Manual 53 4 5
52. page 309 Micro Flow Cell on page 311 High Pressure Flow Cell on page 313 or Nano Flow Cells on page 319 4 Capillary column detector 380 mm lg 0 17 i d for details see Accessory Kit on page 323 G1315 87311 Capillary column detector 150 mm lg 0 17 i d for details see Accessory Kit on page 323 G1315 87303 5 Zero dead volume fitting 5022 6515 6 Flow cell door seal included G1315 68707 Screw special for flow cell door 5022 2112 7 Holmium oxide filter 79880 22711 8 Longlife Deuterium lamp with ID tag with black cover C version 2140 0820 9 Tungsten lamp G1103 60001 10 Leak funnel 5041 8388 11 Leak funnel holder 5041 8389 12 Clip 5041 8387 13 Corrugated tubing 120 mm lg re order 5m 5062 2463 14 Teflon Tubing flexible i d 0 8 mm flow cell to waste see Accessory Kit on page 323 5062 2462 Cable CAN to Agilent 1200 Series modules 0 5 m 5181 1516 Cable CAN to Agilent 1200 Series modules 1 m 5181 1519 LAN Communication Interface Board G1369A G1369 60001 Cross over network cable shielded 3 m long for point to point connection 5023 0203 Twisted pair network cable shielded 7 m long for hub connections 5023 0202 1200 Series DAD and MWD Service Manual 305 14 Parts and Materials for Maintenance Table 27 Maintenance Parts continued Item Description Analog cable BNC to general purpose spade lugs CompactFlash Card Kit Part Number 01046 60105 01100 68700 306 1200 Ser
53. refer to Environment on page 27 Time Constant versus Response Time According to ASTM E1657 98 Standard Practice for Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatography the time constant is converted to response time by multiplying by the factor 2 2 32 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 3 Installing the Detector Unpacking the Detector 34 Optimizing the Stack Configuration 36 Installing the Detector 39 Flow Connections to the Detector 42 This chapter provides information on unpacking checking on completeness stack considerations and installation of the detector ee Agilent Technologies 33 3 installing the Detector Unpacking the Detector Damaged Packaging CAUTION If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the detector may have been damaged during shipment If there are signs of damage please do not attempt to install the detector Delivery Checklist 34 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 Table3 Detector Checklist Description Quantity Detector CompactFlash Card Powe
54. shaft 2 Figure 118 Source Lens Achromat Assembly Parts 1200 Series DAD and MWD Service Manual 331 15 Parts for Repairs Cell Support Assembly Table 43 Cell Support Assembly Item Description Part Number Cell support assembly G1315 65202 1 Retainer ring 0510 1638 2 Washer spring wavy 3050 1591 3 Spectro window 79880 28111 4 Cell support G1315 24701 Figure 119 Cell Support Assembly Parts 332 1200 Series DAD and MWD Service Manual Parts for Repairs 15 Holmium Oxide Filter Table 44 Holmium Oxide Filter Assembly Parts Item Description Part Number 1 Holmium oxide filter motor assembly includes items G1315 68700 2 and 4 2 Holmium oxide filter lever G1315 45001 3 Holmium oxide filter 79880 22711 4 Spring 1460 1510 When the filter motor has been removed the filter lever should not be reused Use always a new filter lever to assure correct fit on the filter motor shaft Figure 120 Holmium Oxide Filter Parts 1200 Series DAD and MWD Service Manual 333 15 Parts for Repairs Fan Assembly Parts Table 45 Fan Assembly Parts Item Description Part Number 1 Fan 3160 1016 2 Heater assembly C 60W for G1315C G1365C only G1315 60013 3 Temperature sensor assembly G1315 60003 GLY a Figure 121 Fan Assembly Parts 334 1200 Series DAD and MWD Service Manual Parts for Repairs 15 Plastic Parts Table 46 Plastics Parts
55. the change of the TCP IP settings on your PC to match the detector s default parameters in a local configuration see also Using Default on page 53 General General Connect using Melee abe sect atahe opr ted deter ear FIXED IP thes Capabity Othervate you need to ask your netrrock adknmrestiator for BY Xircom CreditCard Ethernet 10 100 Modem 56 the apcropriate IP settings address Configure a D Components checked are used by this connection Upe the folowing IP access IP ackbers I 192 168 24 1 Subnet mask 25 25 28 0 Qrin guewmw Install Uninstall Properties e Intemel Protocol TCP IP Properties Bo l U __Fropettics Mt Ps Description Sathe Germa Transmission Control Protocol Intemet Protocol The default Brotemed DNS verve oul 3 wide area network protocol that provides communication ou cn k soagred edomabcaly i your network suppots across diverse interconnected networks Ademate DNS serve ihig capability Otherwise you need to ask your network administrator for IV Show icon in taskbar when connected OK Cancel automatic IP address via DHCP requires special IT setup of the network Figure 32 1200 Series DAD and MWD Service Manual the appropriate IP settings Obtain an IP address automaticaly C Use PERET ees i Oplan DNS server address automatically C Usg the following DNS serves addeesses ED Changing the TCP IP settings of the PC 4 LAN Configurat
56. together A conventional dual signal detector can only detect and quantify both compounds independently from each other if their spectra do not overlap However in most cases this is highly unlikely With a dual channel detector based on diode array technology quantifying two compounds is possible even when both compounds absorb over the whole wavelength range The procedure is called peak suppression or signal subtraction As an example the analysis of hydrochlorothiazide in the presence of caffeine is described If hydrochlorothiazide is analyzed in biological samples there is always a risk that caffeine is present which might interfere chromatographically with hydrochlorothiazide As the spectra in Figure 62 show hydrochlorothiazide is best detected at 222 nm where caffeine also shows significant absorbance It would therefore be impossible with a conventional variable wavelength detector to detect hydrochlorothiazide quantitatively when caffeine is present 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 WL1 204 nm caffeine WL2 222 nm hydrochlorothiazide WL3 260 nm reference to suppress hydrochlorothiazide WL4 282 nm reference to suppress caffeine WL3 WL4 WLI wil Wavelength nm Figure 62 Wavelength Selection for Peak Suppression With a UV visible detector based on a diode array and the correct choice of a reference wavelength setting quantitative detection is possible To suppress
57. top cover and top foam section see Removing the Top Cover and Foam on page 260 Remove optical unit see Removing the Optical Unit on page 281 1 Place the optical unit on your bench and locate the cell 2 Unscrew the two screws using a 2 5 mm hex key rotation limiter and tag reader in the flow cell area view from top 1200 Series DAD and MWD Service Manual 289 13 Repairs 3 Remove the cell rotation limiter and tag reader assembly Route the tag reader cable through the hole Insert the new tag reader assembly together with the cell rotation limiter and fix the two screws Next steps Reinstall the optical unit see Installing the Optical Unit on page 297 Reconnect all cables to the mainboard Reinstall the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 Replace the detector into the stack soo uN SO Oo Reconnect the power cable and turn on detector 290 1200 Series DAD and MWD Service Manual Repairs 13 Exchanging the Power Supply When required If defective Tools required Sc rewdriver POZI 1 PT3 Wrench 1 4 inch Wrench 5 mm Wrench 7 mm Parts required Po Preparations s wer supply 0950 2528 Turn off the lamp Switch off the detector and disconnect t
58. wavelength range from 190 950 nm a new approach is required to achieve wavelength accuracy over the full range Each spectrograph is calibrated individually The calibration data is stored in the spectrograph on an EEPROM Based on these data the built in processors calculate absorbance data with linear intervals 1 0 2 0 between data points This results in an excellent wavelength accuracy and instrument to instrument reproducibility The micro slit system makes use of the mechanical properties of silicon combined with the precise structuring capabilities of bulk micro machining It combines the required optical functions slit and shutter in a simple and compact component The slit width is directly controlled by the micro processor of the instrument and can be set as method parameter 1200 Series DAD and MWD Service Manual Introduction 1 Grating The combination of dispersion and spectral imaging is accomplished by using a concave holographic grating The grating separates the light beam into all its component wavelengths and reflects the light onto the photodiode array Diode Array The diode array is a series of 1024 individual photodiodes and control circuits located on a ceramic carrier With a wavelength range from 190 950 nm the sampling interval is lt 1 nm 1200 Series DAD and MWD Service Manual 19 1 Early Maintenance Feedback EMF 20 Maintenance requires the exchange of components which are subject to
59. were not plotted 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 7 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 126 Status Indicators 127 User Interfaces 129 Agilent LC Diagnostic Software 130 This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces ee Agilent Technologies 125 7 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 126 Status Indicators The detector is provided with two status indicators which indicate the operational state prerun run and error states of the detector The status indicators provide a quick visual check of the operation of the detector Error Messages In the event of an electronic mechanical or hydraulic failure the detector generates an error 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 Information on page 131 Test Functions A series of test functions are available for troubleshooting and operational verification after exchanging internal components see Test Functions on page 159 or Tests amp Calibrations on page 243 Wavelength Verification Recalibration Wavelength recalibr
60. will not work 1200 Series DAD and MWD Service Manual Maintenance Tests amp Calibrations The following tests are required after maintenance of lamps and flow cells e Intensity Test on page 244 e Wavelength Verification and Recalibration on page 246 e Holmium Oxide Test on page 247 e Cell Test on page 249 1200 Series DAD and MWD Service Manual 243 12 Maintenance Intensity Test The test is for the standard flow cells 10 mm and 6 mm pathlength only The nano flow cells 80 nl and 500 nl cannot be run with this test due to its low volume The intensity test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm Four spectral ranges are used to evaluate the intensity spectrum The test is used to determine the performance of the lamps and optics see also Cell Test on page 249 When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell The shape of the intensity spectrum is primarily dependent on the lamp grating and diode array characteristics Therefore intensity spectra will differ slightly between instruments Figure 94 on page 245 shows a typical intensity test spectrum Intensity Test Evaluation The Agilent ChemStation evaluates four spectral ranges automatically and displays t
61. 00 1 compression washer 5 spring washers 2 seal rings 1200 Series DAD and MWD Service Manual 313 14 Parts and Materials for Maintenance Figure 108 High Pressure Flow Cell Parts 314 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Prep Flow Cell SST For more details on the Preparative Flow Cells refer to the technical note that comes with the flow cells Table 32 Prep Flow Cell SST Parts Item Description Part Number AeA wo N 9a Prep Flow Cell SST 3 mm 120 bar 12 MPa with RFID Tag completely assembled includes all items below Window screw Spring washers pack of 10 Compression washer Window holder Quartz window Gasket BACK FEP Teflon 2 3 mm hole outlet side Seal kit BACK for STD flow cell qty 12 Gasket FRONT FEP Teflon 1 3 mm hole inlet side Seal kit FRONT for STD flow cell qty 12 Window assembly comprises item 1 2 3 4 5 Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 spring washers Cell repair kit semi micro includes window screw kit 4 mm kexagonal wrench and seal kits Capillary SST 250 mm length 0 5 mm i d 0 D 0 9 mm with fittings for flow cell assembled Fitting FRONT Fitting BACK Fitting 1 16 re order 10 pk Cell body 1200 Series DAD and MWD Service Manual G1315 60016 79883 22402 5062 8553 79883 28801 79883 22301 1000 0488 G1315 68711
62. 06 01 or above Otherwise the ChemStation see Performance Specifications on page 30 will not recognize modules Assure that the CompactFlash Card is installed in the rear of the detector required for operation 1 Note the MAC address of the LAN interface rear of the module under the configuration switch see Figure 5 on page 40 It s required for LAN Configuration on page 47 Place the detector in the stack or on the bench in a horizontal position Ensure the line power switch at the front of the detector is OFF Connect the power cable to the power connector at the rear of the detector Connect the CAN cable to other Agilent 1200 Series modules Connect the LAN cable e g from a Agilent ChemStation as controller to the detector s LAN connector ao oa FF Ww N 1200 Series DAD and MWD Service Manual 39 3 Installing the Detector In multi detector configurations the LAN of the G1315C D and G1365C D must be used due to its higher data load 7 Connect the analog cable s optional 8 Connect the APG remote cable optional for non Agilent 1200 Series instruments 9 Turn on power by pushing the button at the lower left hand side of the detector The status LED should be green
63. 181 1530 long life deuterium lamp G1315A B C D G1365A B C D black cover G1314A B C see note below 2140 0590 standard deuterium lamp G1315A B C D G1365A B C D G1314A4 B C see note below These lamps can be operated in the Agilent 1200 series variable wavelength detector G1314A B C as well For details about changing the configuration and information on the specifications refer to the Reference Manual of the G1314A B C section Exchanging a Lamp 186 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 Optimization Information To extend the useful life of deuterium lamps in the 1200 Series DAD MWD we recommend 1 to turn lamps off over night or when not used for gt 4 hours 2 to use an appropriate reference wavelength The above mentioned problem can be reduced by choosing the right wavelength settings The use of a reference wavelength setting close to the sample wavelength e g sample 254 4 reference 350 100 will reduce the lamp effects see figures 1 to 3 During installation familiarization of an 1200 Series DAD MWD this optimization hint should be given to the user as described in the 1200 Series DAD MWD Reference Manual s Optimization Section Examples of baselines Below are 3 examples of baseline instabilities caused by lamps Please keep in mind e the different forms of the baseline problem Periods can be a few second to hours e the significant reduction of the problem by choosi
64. 2 cts Passed Figure 94 Intensity Test Results report 1200 Series DAD and MWD Service Manual 245 12 246 Wavelength Verification and Recalibration The detector uses the alpha 656 1 nm and beta 486 nm emission lines of the deuterium lamp for wavelength calibration The sharp emission lines enable more accurate calibration than is possible with holmium oxide When verificaation is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with bubble free degassed HPLC water in the flow cell If a deviation is found and displayed it can be recalibrated by pressing Adjust The deviations are tracked in the Calibration History diagnosis buffer in the detector DAD Wavelength Calibration G1315C x Calibration history Deviation D2 Alpha D2 Beta Time Date 0 01nm D 04nm 13 19 31 16 03 2005 D2 Alpha UEEMEEp EEE EE 1 2mm 656 1nm 1 2nm D2 Beta MNNHenpern re 1 2mm 486 0nm 1 2nm Resthistoy D2 Alpha line deviation is 0 00nm D2 Beta line deviation is 0 00nm OK Cancel Help A ee Calibration settings equal to measured ones No calibration necessary Figure 95 Wavelength Verification and Recalibration Wavelength calibration should be done e after maintenance of the flow cell e lamp exchange or e after a major repair like processor board or optical unit exchange After calibration the ho
65. 200 Series DAD and MWD Service Manual 83 5 Using the Detector 7 For the isocratic pump fill the solvent bottle with the mixture of HPLC grade bi distilled water 80 and acetonitrile 70 For binary and quaternary pumps you can use separate bottles 8 Click on the Load Method button and select DEF_LC M and press OK Alternative double click on the method in the method window The default LC method parameters are transferred into the 1200 modules Load Method System z z 2j None Fer Cx Carel foEF_LC M co chem32 2 nethods OFMOCAL M OGALSTST M OGCALAS M DGCALOO1 M OGCALOQ2M zj Oriver mesere 5 E Eke EG mate Obs cer sc z ime Ub oo lt 2 dja aa Bsgu Socoowmemos LA eam MN Oe ea a eras l Sm SIO i i Q vemoca2 m W Ocustst W ooceaasm W OaM oxcacgem U OAIM Uoan W aM Q ocan DEFAULT O Q ostmrs n Q oacerst Q vocrtest m W ow orst m Q DGEAKT M W ogo Q corres W behets owocem E Adaa SPAN E 1168 hee Q onors Figure 38 Loading Default LC Method eo8b ee 88288 84 1200 Series DAD and MWD Service Manual Using the Detector 5 9 Click on the module icons Figure 39 and open the Setup of these modules Figure 40 on page 86 shows the detector settings do not change the detector parameters at this time Li a Ca a 3 2 re ge em omg Me LEE O G1Set up Pump auxiliary G
66. 254 4 Ref off NOISE INMOOS D mAU F o4 Response ime 0 05 min on OT OLN ATA a aati 044 T TT T T T T T T 0 05 4 1 6 2 2 5 3 35 mi DAD1 A Sig 254 4 Ref off NOISE INMO1 D mAU J o4 Response time 0 1 min P a 0 44 lot i 0 5 4 15 2 2 5 3 35 mit Figure 56 Influence of Response Time on Signal and Noise Figure 19 lists the filter choices of the detector To get optimum results set peak width as close as possible to a narrow peak of interest in your chromatogram Response time will the be approximately 1 3 of the peak width resulting in less than 5 peak height reduction and less than 5 additional peak dispersion Decreasing the peak width setting in the detector will result in less than 5 gain in peak height but baseline noise will increase by a factor of 1 4 for a factor of 2 response time reduction Increasing peak width response time by factor of two from the recommended setting over filtering will reduce peak height by about 20 and reduce baseline noise by a factor of 1 4 This gives you the best possible signal to noise ratio but may affect peak resolution 1200 Series DAD and MWD Service Manual 111 6 How to optimize the Detector Table 19 Peak Width Response Time Data Rate Peak Width min Response Time sec Data Rate Hz Detector lt 0 0025 0 025 80 G1315C G1365C only gt 0 0025 0 05 80 G1315C G1365C only gt 0 005 0 1 40 G1315C G1365C only gt 0 01 0 2 20 G1
67. 315 45001 ectro window 79880 28111 Filter lever G1315 45001 Preparations Turn off the lamp Switch off detector and disconnect the power cable Remove detector from stack and place it on the working bench Remove the front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 Remove the optical unit see Removing the Optical Unit on page 281 Remove the UV lamp If the filter motor was removed the filter lever should not be reused Always use a new filter lever to assure correct fit on the filter motor shaft 1200 Series DAD and MWD Service Manual 283 13 Repairs 1 Place the optical unit on your bench 2 Pull the filter motor off the shaft Keep the spring and the lever fixture in a safe place Remove the filter lever on the other side la ry ia i mv aand HH H 3 Use the 1 5 mm hexagonal key to loosen the setscrew that secures the source lens assembly Carefully slide the cell support assembly to the right by pushing it from the deuterium lamp side with a hexagonal wrench 284 1200 Series DAD and MWD Service Manual Repairs 13 5 Remove the achromat assembly 6 Use a metal blade 12 mm width 1 mm thick to unscrew the lens achromatic holder quartz window lia spring Cleaning Steps 7 Place the parts on a clean tissue 8 Remove the spring and the spectro window from th
68. 315C D and G1365C D gt 0 03 0 5 10 G1315C D and G1365C D gt 0 05 1 0 5 G1315C D and G1365C D gt 0 10 2 0 2 5 G1315C D and G1365C D gt 0 20 4 0 1 25 G1315C D and G1365C D gt 0 40 8 0 0 62 G1315C D and G1365C D gt 0 85 16 0 0 31 G1315C D and G1365C D Sample and Reference Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 to 950 nm Two lamps provide good sensitivity over the whole wavelength range The deuterium discharge lamp provides the energy for the UV range 190 to 400 nm and the tungsten lamp emits light from 400 to 950 nm for the visible and short wave near infrared If you know little about the analytes in your sample use both lamps and store all spectra over the full wavelength range This provides full information but fills up your disk space rather quickly Spectra can be used to check a peak s purity and identity Spectral information is also useful to optimize wavelength settings for your chromatographic signal The detector can compute and store at run time up to 8 signals with these properties e sample wavelength the center of a wavelength band with the width of sample bandwidth BW and optionally e reference wavelength the center of a wavelength band with the width of reference bandwidth 112 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 The signals comprises a series of data points over time with the average absorbance in the sa
69. 4 LAN Configuration The user may open a Telnet session using the default IP address and change the parameters stored in the non volatile memory of the detector He may then close the session select the initialization mode Using Stored power on again and establish the TCP IP connection using the new parameters When the detector is wired to the PC directly e g using a cross over cable or a local hub separated from the local area network the user may simply keep the default parameters to establish the TCP IP connection In the Using Default mode the parameters stored in the memory of the detector are not cleared automatically If not changed by the user they are still available when switching back to the mode Using Stored 1200 Series DAD and MWD Service Manual LAN Configuration 4 Link configuration selection Table 8 The LAN interface supports 10 or 100 Mbps operation in full or half duplex modes In most cases full duplex is supported when the connecting network device such as a network switch or hub supports IEEE 802 3u auto negotiation specifications When connecting to network devices that do not support auto negotiation the LAN interface will configure itself for 10 or 100 Mbps half duplex operation For example when connected to a non negotiating 10 Mbps hub the LAN interface will be automatically set to operate at 10 Mbps half duplex If the detector is not able to connect to the networ
70. 6 Replacing the Tag Reader Lamp 278 Removing the Optical Unit 281 Exchanging the Source Lens Achromat Assembly 283 Replacing the Holmium Oxide Filter Motor 286 Replacing the Tag Reader Flow Cell or the Cell Rotation Limiter 289 Exchanging the Power Supply 291 Exchanging the Leak Sensor 294 Replacing Status Light Pipe 296 Installing the Optical Unit 297 Replacing the Foam and the Top Cover 299 Assembling the Main Cover 302 This chapter describes the repair of the detector ot Agilent Technologies 251 13 Repairs Cautions and Warnings The following procedures require opening the main cover of the detector Always ensure the detector is disconnected from the line power when the main cover is removed The security lever at the power input socket prevents that the detector cover is taken off when line power is still connected To disconnect the detector from line unplug the power cord The power supply still uses some power even if the switch on the front panel is turned off To prevent personal injury be careful when getting in contact with sharp metal areas 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 CAUTION The electronics of the detector will not allow operation of the detec
71. 7 have different hole diameters 1 window screw 2 spring washers 3 compression washer 4 window holder 5 quartz window 6 Gasket Figure 103 Orientation of Spring Washers 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Semi Micro Flow Cell Table 29 Semi Micro Flow Cell Parts Item Description Part Number A wo N Semi micro flow cell assembly 6 mm 5 ul maximum pressure 120 bar 12 MPa with RFID tag Window screw Spring washers pack of 10 Compression washer Window holder Quartz window Gasket BACK Teflon 1 8 mm hole outlet side Gasket FRONT Teflon 1 3 mm hole inlet side Window assembly comprises item 1 2 3 4 5 Capillary IN 0 17 mm 310 mm lg including heat exchanger Capillary OUT 0 12 mm 200 mm lg Capillary OUT 0 17 mm 200 mm lg Clamp unit Screw M 2 5 4 mm lg for cell body clamp Zero dead volume fitting Cell repair kit semi micro includes window screw kit 4 mm hexagonal wrench and seal kits Seal kit BACK for semi micro flow cell qty 12 of item 6 Seal kit FRONT for semi micro flow cell qty 12 of item 7 Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 spring washers G1315 60025 79883 22402 5062 8553 79883 28801 79883 22301 1000 0488 See kits below See kits below No part number G1315 87319 G1315 87306 G1315 87302 G1315 84910 0515 1056 5022 21
72. 73 Replacing Temperature Sensor 276 Replacing the Tag Reader Lamp 278 Removing the Optical Unit 281 Exchanging the Source Lens Achromat Assembly 283 Replacing the Holmium Oxide Filter Motor 286 Replacing the Tag Reader Flow Cell or the Cell Rotation Limiter 289 Exchanging the Power Supply 291 Exchanging the Leak Sensor 294 1200 Series DAD and MWD Service Manual 11 Replacing Status Light Pipe 296 Installing the Optical Unit 297 Replacing the Foam and the Top Cover 299 Assembling the Main Cover 302 14 Parts and Materials for Maintenance Overview of Maintenance Parts 304 Standard Flow Cell 307 Semi Micro Flow Cell 309 Micro Flow Cell 311 High Pressure Flow Cell 313 Prep Flow Cell SST 315 Prep Flow Cell Quartz 317 Nano Flow Cells 319 Accessory Kit 323 15 Parts for Repairs Parts At The Rear Of The Detector 326 Optical Unit Assembly 328 Coupling Lens Assembly 330 Source Lens Achromat Assembly 331 Cell Support Assembly 332 Holmium Oxide Filter 333 Fan Assembly Parts 334 Plastic Parts 335 Leak Parts 336 1200 Series DAD and MWD Service Manual Foam Parts 337 Power and Status Light Pipes 338 Sheet Metal Kit 339 16 Identifying Cables Cable Overview 342 Analog Cables 344 Remote Cables 347 BCD Cables 352 Auxiliary Cable 354 CAN Cable 355 External Contact Cable 356 RS 232 Cable Kit 357 LAN Cables 358 17 Hardware Information Detector Main Board DADM MWDM 360 Main features 360 Firmware 361 Leak Senso
73. 84 G1315 68713 79883 68702 G1315 68710 79883 68703 1200 Series DAD and MWD Service Manual 309 14 Parts and Materials for Maintenance G Figure 104 Semi Micro Flow Cell Parts Gaskets 6 and 7 have different hole diameters 1 window screw 2 spring washers THY 5 3 compression washer WAWU N 4 window holder 5 quartz window 6 Gasket Figure 105 Orientation of Spring Washers 310 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Micro Flow Cell Table 30 Micro Flow Cell Parts Item Description Part Number Micro flow cell assembly 3 mm 2 ul G1315 60024 maximum pressure 120 bar 12 MPa with RFID tag 1 Window screw 79883 22402 2 Spring washers pack of 10 5062 8553 3 Compression washer 79883 28801 4 Window holder 79883 22301 5 Quartz window 1000 0488 6 Gasket BACK Teflon 1 8 mm hole outlet side See kits below 7 Gasket FRONT Teflon 1 3 mm hole inlet side See kits below 8 Window assembly comprises item 1 2 3 4 5 No part number 9 Capillary IN 0 12 mm 310 mm lg including heat exchanger G1315 87339 10 Capillary OUT 0 12 mm 200 mm lg G1315 87306 10 Capillary OUT 0 17 mm 200 mm lg G1315 87302 11 Clamp unit G1315 84910 Screw M 2 5 4 mm lg for cell body clamp 0515 1056 Zero dead volume fitting 5022 2184 Cell repair kit semi micro includes window screw kit 4 mm G1315 68713 kexagonal wrench and seal kits Seal kit BACK for semi m
74. 9 Compensation Sensor Short 139 Fan Failed 140 Open Cover 141 Cover Violation 142 Detector Error Messages 143 Visible Lamp Current 143 Visible Lamp Voltage 144 Calibration Values Invalid 145 Wavelength Recalibration Lost 146 Diode Current Leakage 147 Holmium Oxide Test Failed 148 UV Lamp Current 149 UV Lamp Voltage 150 UV Ignition Failed 151 UV Heater Current 152 Illegal Value From Temperature Sensor 153 Illegal Value From Air Inlet Temperature Sensor 154 Heater Failed 155 Heater Power At Limit 156 No Run Data Available In Device G1315C G1365C only 157 DSP Not Running 158 1200 Series DAD and MWD Service Manual 9 Test Functions Self test 160 Filter Test 162 Slit Test 164 Dark Current Test 165 Intensity Test 167 Holmium Oxide Test 169 Spectral Flatness Test 172 ASTM Noise Test 173 Cell Test 174 Wavelength Verification and Recalibration 176 Test Chromatogram 178 Agilent ChemStation 179 Control Module G1323B 180 Diagnosis Information on Agilent ChemStation 181 10 Diagnostic Signals Overview of Diagnostic Signals 184 Baseline problems deriving from deuterium lamps 185 Problem Description 185 Problem Verification 185 Solution 186 Optimization Information 187 Examples of baselines 187 Wander Drift Problems Due to Temperature Changes 190 Situation 190 Specifications and Conditions 191 Principle of Temperature Control 192 1200 Series DAD and MWD Service Manual 10 11 12 Setup of Detector 194 Start
75. AN Configuration 4 With Telnet Whenever a TCP IP connection to the detector is possible TCP IP parameters set by any method the parameters may be altered by opening a Telnet session 1 Open the system DOS prompt window by clicking on Windows START button and select Run Type cmd and press OK 2 Type the following at the system DOS prompt c gt telnet lt IP address gt or c gt telnet lt host name gt EY C WINDOWS system32 cmd exe C2 gt telnet 134 46 27 95 Figure 20 Telnet Starting a session where lt IP address gt may be the assigned address from a Bootp cycle a configuration session with the Handheld Controller G1323B or the default IP address see Configuration Switches on page 50 When the connection was established successfully the detector responds with the following EY C AWINDOWS system32 cmd_ exe telnet 134 40 27 95 Agilent Technologies Gi1315C PP 88860024 Figure 21 A connection to the module is made 1200 Series DAD and MWD Service Manual 63 4 64 LAN Configuration 3 Type and press enter to see the available commands E C WINDOWS system32 cmd exe telnet 134 40 27 95 Agilent Technologies G1315C PP 6688024 gt command syntax Figure 22 Telnet Commands Table9 Telnet Commands description display help info display current LAN settings set IP Address set Subnet Mask set Default Gateway exit shell Value De
76. Agilent 1200 Series Diode Array and Multiple Wavelength Detector G1315C D and G1365C D Service Manual Eee Agilent Technologies Notices Agilent Technologies Inc 2006 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61315 90112 Edition 11 06 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn Manual Structure The Service Manual G1315 90112 English contains the complete information about the Agilent 1200 Series Diode Array and Multiple Wavelength Detector It is avail able as Adobe Reader file PDF only The User Manual G1315 90012 English and its localized versions contain a subset of the Service Manual and is shipped with the detector in printed matter Latest versions of the manuals can be obtained from the Agilent web Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the impl
77. Cleaning When required If parts are contaminated or leaky Tools required Screwdriver POZI 1 PT3 Two 1 4 inch wrenches for capillary connections Parts required For parts identification refer to Nano Flow Cells on page 319 80 nl and 500 nl Preparations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 For details refer to the technical note that comes with the nano flow cell kit The quartz block can be cleaned with alcohol DO NOT touch the inlet and outlet windows at the quartz block 1200 Series DAD and MWD Service Manual 231 12 Maintenance 1 Disconnect the capillaries from the capillary holder and 2 Unscrew the cell body from the holder remove the flow cell B Unscrew the capillaries from the flow cell DO NOT use the 4 Using for example a toothpick press on the plastic part adapter at this time and slide the quartz body out of the cell housing 232 1200 Series DAD and MWD Service Manual Maintenance 12 5 The quartz body and the cell seal assembly can be separated for cleaning purpose 6 This figure shows the correct holding of the quartz body and the cell seal assembly 7 Replace the cell seal assembly onto the quartz body Always use a new seal assembly to exclude damage during disassembling 8 Slide the quartz body completely into the cell body to the front stop use for example
78. D 4 Start the run On completion of the run or when the run is stopped the test chromatogram is deactivate pas a bet innamen PaE APTIT DS DY Fy ua z i a Figure 75 Test Chromatogram on Agilent ChemStation response time 2 seconds 1200 Series DAD and MWD Service Manual 179 9 Test Functions Control Module G1323B Select the response time and stop time according to Table 21 on page 178 2 If required connect a recording device to the analog output 3 Select the function Enable test chromatogram in Tests DAD or MWD and press Execute 4 Select the Plot button in the System screen and press the Setup button 5 Select as Source the Signal DAD or MWD change the Y range to 10 to 300 mAU fit the Time Range to match Table 21 on page 178and press Done 6 Press the Start button to start the run On completion of the run or when the run is stopped the test chromatogram is deactivated 180 1200 Series DAD and MWD Service Manual Test Functions 9 Diagnosis Information on Agilent ChemStation The Agilent ChemStation provides certain information on various assemblies in the detector 1 Open the Diagnosis and change to detailed view 2 Click on the assembly of interest and select Update Variables Display Figure 76 on page 182 shows an example Table 23 on page 181 lists the assemblies which provide detailed information Table 23 Diagnosis detailed information Assembly Details Genera
79. D B Signal 254 16 Reference lt r Window DAD A Signal 254 4 Reference 360 100 x axis 15 J min Type acquired y axis range 1 mau J draw zero line J auto y adjust Offset 20 4 Fraction Colector __ p Method Settings J Show Fraction collection ticks J Use method settings Apply to Method OK Cancel Help Figure 41 Edit Signal Plot Window 1200 Series DAD and MWD Service Manual 87 5 Using the Detector The Online Plot Figure 42 on page 88 shows both the pump pressure and the detector absorbance signals Pressing Adjust the signals can be reset to the offset value and Balance would do a balance on the detector Figure 42 Online Plot Window 13 If both baselines are stable set the Y range for the detector signal to 100 mAU If you start with a new UV lamp for the first time the lamp may show initial drift for some NOTE time burn in effect 88 1200 Series DAD and MWD Service Manual Using the Detector 5 14 Select the menu item RunControl gt Sample Info and enter information about this application Figure 43 on page 89 Press OK to leave this screen KLI M Sample Info x Offline Data Analysis Operator Name Wolfgang Run Sequence peste Pause Sequence Path JE CHEMSTATION 2 DATAS x Subdirectory JISOTEST Resume Sequence Resume Injection Manual Filename Stop RunfInject Sequence Fs 1s0 01D i Prefix Counter 7 p QI
80. DGCALAS M m Sample Parameters Location vial 1 blank run if no entry Sample Name fisocratic test sample Sample Amount 0 Multiplier fi ISTD Amount fo Dilution fi Comment Isocratic test sample 1 ul 30 70 H2O Acetonitrile 1 5 ml min l Run Method OK Cancel Help Figure 43 Sample Information 15 Fill the content of an isocratic standard sample ampoule into a vial and seal the vial with a cap and place the vial into autosampler tray position 1 1200 Series DAD and MWD Service Manual 89 5 90 Using the Detector Running the Sample and Verifying the Results 1 To start a run select the menu item RunControl gt Run Method 2 This will start the 1200 modules and the online plot on the Agilent ChemStation will show the resulting chromatogram DADI A Sipa RetG00 100 1101 4 10 400003 D ral Figure 44 Chromatogram with lsocratic Test Sample Information about using the Data Analysis functions can be obtained from the Using your ChemStation manual supplied with your system 1200 Series DAD and MWD Service Manual Using the Detector 5 Special Settings of the Detector In this chapter special settings of the G1315C D and G1365C D are described based on the Agilent ChemStation B 02 01 Control Settings setup 2 DAD Controls Sia X lt Lamps turn on and off of UV ag Control p lamp Error Method and Vis lamp a8 Config
81. Defective visible lamp e Defective detector main board e Defective power supply Suggested Actions Y Ensure the visible lamp connector is seated firmly V Exchange the visible lamp V Exchange the detector main board V Exchange the power supply 1200 Series DAD and MWD Service Manual 143 8 Error Information Visible Lamp Voltage The visible lamp voltage is missing The processor continually monitors the voltage across the lamp during operation If the lamp voltage falls below the lower limit the error message is generated Probable Causes e Defective detector main board e Defective power supply Suggested Actions V Exchange the detector main board V Exchange the power supply 144 1200 Series DAD and MWD Service Manual Error Information 8 Calibration Values Invalid The calibration values read from the spectrometer ROM are invalid After recalibration the calibration values are stored in ROM The processor periodically checks if the calibration data are valid If the data are invalid or cannot be read from the spectrometer ROM the error message is generated Probable Causes e Defective detector main board e Defective optical unit Suggested Actions V Exchange the detector main board Y Exchange the optical unit 1200 Series DAD and MWD Service Manual 145 8 Error Information Wavelength Recalibration Lost Te calibration information needed for your detector to operate correctly has been lost
82. Firmware 242 Tests amp Calibrations 243 Intensity Test 244 Wavelength Verification and Recalibration 246 Holmium Oxide Test 247 Cell Test 249 This chapter describes the maintenance of the detector ot Agilent Technologies 207 12 Maintenance Overview of Maintenance The following pages describe maintenance simple repairs of the detector that can be carried out without opening the main cover Table 25 Overview of Maintenance Procedure Typical Frequency Notes Deuterium lamp or If noise and or drift exceeds your application limits or An intensity test should be performed tungsten lamp lamp does not ignite after replacement exchange Flow cell exchange If application requires a different flow cell type A holmium or wavelength calibration test should be performed after replacement Flow cell parts If leaking or if intensity drops due to contaminated flow A pressure tightness test should be Cleaning or exchange cell windows done after repair Holmium oxide filter If contaminated A holmium or wavelength calibration Cleaning or exchange test should be performed after replacement Leak sensor drying If leak has occurred Check for leaks Leak handling System If broken or corroded Check for leaks replacement 208 1200 Series DAD and MWD Service Manual Exchanging a Lamp When required Tools required Parts required Preparations Maintenance 12 If noise or drift exceeds application limits or lamp
83. Handle for clamp unit G1315 84901 5 Clamp unit G1315 84902 6 Screw M 2 5 4 mm lg for cell body clamp 0515 1056 7 Quartz body Prep Cell 0 3 mm G1315 80004 7 Quartz body Prep Cell 0 06 mm G1315 80003 The flow cell comes with two tubings 0 8 mm i d and one 0 5 mm i d so that the combination at the flow cell could be either 0 8 0 8 or 0 5 0 8 inlet outet Standard is 0 8 0 8 Depending on the system pressure lt 30 ml min or bandbroadening the inlet tubing might be changed to 0 5 mm 1200 Series DAD and MWD Service Manual 317 14 Parts and Materials for Maintenance Figure 111 Prep Flow Cell Quartz Parts 318 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Nano Flow Cells The following kits are available Table 34 Nano flow cell kits Description Part number 500 nl Flow Cell Kit G1315 68724 includes Flow cell assembly 10 mm 500 nl 5 MPa completely assembled includes items 1 2 3 4 10 11 12 13 14 15 and 16 80 nl Flow Cell Kit G1315 68716 includes Flow cell assembly 10 mm 80 nl 5 MPa completely assembled includes items 1 2 3 4 10 11 12 13 14 15 and 16 Figure 112 shows all parts delivered with the nano flow cell kits Figure 112 Content of kits 1200 Series DAD and MWD Service Manual 319 14 Parts and Materials for Maintenance 320 Table 35 lists the generic parts for both nano flow cells Table 35 Generic Parts
84. I 1 PT3 ESD kit Preparations The power supply the fan and the processor board are already installed The fan must be installed in the correct orientation to ensure correct cooling and operation of the detector see Replacing Fan Parts on page 273 1 Check that the three shock absorbers and the leak sensor 2 Carefully insert the optical unit into the instrument holding cable are placed correctly the one hand at back of the heat sink r HAHAHAHAH ES HHHHHHHHHHHHHHHHHHH 1200 Series DAD and MWD Service Manual 297 13 Repairs 3 Reconnect all cables to the detector main board optical Replace the two rubber shock absorbers holmium oxide filter motor ID cell ID lamp Next steps Reinstall the flow cell cover see Correcting Leaks on page 239 Reinstall the flow cell see Exchanging a Flow Cell on page 211 Reinstall the lamps see Exchanging a Lamp on page 209 Reinstall the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 Replace detector into the stack oN OO CI 0 Reconnect the power cable and turn on the detector If a new optical is installed or a new detector main board perform a Wavelength Verification and Recalibration on page 176 to add the recalibration parameters into the detector main
85. MWD Service Manual Repairs 13 3 Replace the leak sensor assembly into the leak pan 4 5 Next steps Reconnect the leak sensor cable to the detector main board Replace the optical unit see Installing the Optical Unit on page 297 Replace the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 Replace the detector into the stack Reconnect the cables Turn on the detector 1200 Series DAD and MWD Service Manual 295 13 Repairs Replacing Status Light Pipe When required If part was broken or removed Tools required Screwdriver POZI 1 PT3 Parts required Status light pipe 5041 8384 Preparations Turn off the lamp Switch off the detector and disconnect the power cable e Remove detector from stack and place it on working bench e Remove front cover top cover and metal cover see Removing the Top Cover and Foam on page 260 do not remove the foam 1 The status light pipe is clipped into the top cover Next steps 2 Replace the top cover see Replacing the Foam and the Top Cover on page 299 3 Replace the detector into the stack and reconnect the cables and capillaries a N Turn on the detector 296 1200 Series DAD and MWD Service Manual Repairs 13 Installing the Optical Unit When required When repairs have been completed Tools required Screwdriver POZ
86. MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 5 Using the Detector Setting up an Analysis 76 Before Using the System 76 Requirements and Conditions 78 Optimization of the System 80 Preparing the HPLC System 81 Running the Sample and Verifying the Results 90 Special Settings of the Detector 91 Control Settings 91 Configuration Settings 92 Online Spectra DAD only 93 Run Recovery Settings G1315C G1365C only 94 Analog Output Settings 97 Spectrum Settings DAD only 98 Peakwidth Settings 100 Slit Settings 102 Margin for Negative Absorbance Settings 103 Optimizing the Detector 103 Special Setups with Multiple DAD MWDs_ 104 This chapter provides information on how to set up the detector for an analysis and explains the basic settings ee Agilent Technologies 75 5 Using the Detector Setting up an Analysis This chapter can be used for e preparing the system e to learn the set up of an HPLC analysis and e to use it as an instrument check to demonstrate that all modules of the system are correctly installed and connected It is not a test of the instrument performance e Learn about special settings Before Using the System Solvent Information Observe recommendations on the use of solvents in chapter Solvents in the pump s reference manual Priming and Purging the System When the solvents have been exchanged or the pumping system has been
87. REMOTE connector as interface to other Agilent products e Analog Output connector s for signal output and e Interface slot for specific interfacing external contacts BCD LAN and so on For identification and location of the connectors Electrical Connections on page 23 1200 Series DAD and MWD Service Manual 367 17 Hardware Information WARNING Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations see Cable Overview on page 342 Analog Signal Output The analog signal output can be distributed to a recording device For details refer to the description of the module s main board LAN Interface The LAN interface is used to connect the module with a computer The settings of configuration switch determines the LAN operation of your module The switches are preset to a default and recognized by the operating software from Aligent Technologies For details see LAN Configuration on page 47 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 368 1200 Series DAD and MWD Service Manual Hardware Information 17 Remote Interface The APG remote connector may be used in combination with other analytical instruments from Aligent Technologies if you want to use features such as common shut down
88. Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 8 Error Information What Are Error Messages 132 General Error Messages 133 Detector Error Messages 143 This chapter describes the meaning of detector error messages and provides information on probable causes and suggested actions how to recover from error conditions ot Agilent Technologies 131 8 Error Information What Are Error Messages Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention before the analysis can be continued for example repair or exchange of consumables is necessary In the event of such a failure the red status indicator at the front of the detector is switched on and an entry is written into the detector logbook 132 1200 Series DAD and MWD Service Manual Error Information 8 General Error Messages General error messages are generic to all Agilent 1200 series HPLC modules Timeout The timeout threshold was exceeded Probable Causes The analysis was completed successfully and the timeout function switched off the pump as requested e A not ready state was present during a sequence or multiple injection run for a period longer than the timeout threshold Suggested Actions V Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required 1200
89. Temperature Control In Figure 81 the principle of temperature control is shown The fan draws the air in from the rear of the instrument A heater element heats the air and the air stream blows across the optical unit s casting back to the rear of the instrument The temperature control mechanism heater fan temperature sensors processor assures a stable temperature of the optical unit approx 30 C at the flow cell If the detector environment is far away from normal laboratory temperatures but inside the allowed ambient operating temperature 0 55 C 32 131 F the setpoint is automatically adapted to a value near this temperature detector front Ambient sensor optical unit heater fan detector main board optical temp sensor air flow Figure 81 Air flow and sensors in the detector Warm up of detector Give the optical unit enough time to warm up and stabilize The G1315C D and G1365C D detector is temperature controlled After turn on of the detector it goes through a cycle of different states see Figure 82 0 to 0 5 minutes the heater control is OFF and the heater element runs at 0 duty cycle 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 e 0 5 to 1 minutes the heater control is OFF and the heater element runs at 66 duty cycle This first minute is used as self test of the heater functionality e 1 to 30 minutes the heater control is OFF and the heater element runs at 40 d
90. White Digital ground 2 Brown 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 350 1200 Series DAD and MWD Service Manual Identifying Cables 16 Agilent 1200 to HP 1090 LC or Signal Distribution Module Connector Pin Pin Signal Name Active 01046 60202 HP 1090 Agilent 1200 TTL 1 1 White Digital ground NC 2 Brown Prepare run Low p 8 4 3 Gray Start Low 7 LA e 7 4 Blue Shut down Low m 45 8 5 Pink Not connected 2 NI NC 6 Yellow Power on High 3 7 Red Ready High 5 Key 6 8 Green Stop Low NC 9 Black Start request Low Agilent 1200 to General Purpose Connector Pin Pin Signal Name Active 01046 60201 Universal Agilent 1200 TTL 1 White Digital ground i a 2 Brown Prepare run Low au 3 Gray Start Low ae ua a 4 Blue Shut down Low E 5 Pink Not connected a 6 Yellow Power on High z lo 7 Red Ready High 8 Green Stop Low 9 Black Start request Low 1200 Series DAD and MWD Service Manual 351 16 Identifying Cables BCD Cables One end of these cables provides a 15 pin BCD connector to be connected to the Agilent 1200 Series modules The other end depends on the instrument to be connected to Agilent 1200 to Gen
91. a Run and Evaluate 196 Internal Board Temperature 199 Maintenance and Repair Maintenance Introduction to Maintenance and Repair 202 Simple Repairs Maintenance 202 Exchanging Internal Parts Repair 202 Warnings and Cautions 203 Cleaning the Detector 204 Using the ESD Strap 205 Overview of Maintenance 208 ExchangingaLamp 209 Exchanging a Flow Cell 211 Maintenance of Standard Semi Micro or Micro Flow Cell 214 Maintenance of High Pressure Flow Cell 219 Replacing Capillaries on a Standard Flow Cell 222 Replacing Capillaries on a Semi Micro Micro and High Pressure Flow Cell 227 Nano Flow Cell Replacing or Cleaning 231 Cleaning or Exchanging the Holmium Oxide Filter 236 Correcting Leaks 239 Replacing Leak Handling System Parts 240 Replacing the CompactFlash Card G1315C G1365C only 241 Replacing the Detector s Firmware 242 1200 Series DAD and MWD Service Manual Tests amp Calibrations 243 Intensity Test 244 Wavelength Verification and Recalibration 246 Holmium Oxide Test 247 Cell Test 249 13 Repairs Cautions and Warnings 252 Cleaning or Replacing Coupling Lens Assembly 254 Cleaning or Replacing Cell Support Window 257 Removing the Top Cover and Foam 260 Exchanging the Detector Main Board 263 Changing the Product Number and Serial Number 267 Using the Agilent ChemStation 267 Using the Instant Pilot G2408A 268 Using the Control Module G1323B 270 Removing the PCMCIA Interface 272 Replacing Fan Parts 2
92. across the temperature compensation sensor NTC on the detector main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable Causes Defective detector main board Suggested Actions V Exchange the detector main board Compensation Sensor Short The ambient compensation sensor NTC on the detector main board in the detector has failed short circuit The resistance across the temperature compensation sensor NTC on the detector main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor falls below the lower limit the error message is generated Probable Causes e Defective detector main board Suggested Actions V Exchange the detector main board 1200 Series DAD and MWD Service Manual 139 8 Error Information Fan Failed The cooling fan in the detector has failed The hall sensor on the fan shaft is used by the detector main board to monitor the fan speed If the fan speed falls below two revolutions second for more than five seconds the error message is generated Probable Causes e Fan cable disconnected e Defective fan e Defective detector main board Suggested Actions V Ensure the fan is
93. ailed The UV lamp failed to ignite The processor monitors the UV lamp current during the ignition cycle If the lamp current does not rise above the lower limit within 2 5 seconds the error message is generated Probable Causes e Lamp too hot Hot gas discharge lamps may not ignite as easily as cold lamps Lamp not connected e Defective UV lamp or non Agilent lamp e Defective detector main board e Defective power supply Suggested Actions V Switch off the lamp and allow it to cool down for at least 15 minutes V Ensure the lamp is connected V Exchange the UV lamp V Exchange the detector main board V Exchange the power supply 1200 Series DAD and MWD Service Manual 151 8 Error Information UV Heater Current The UV lamp heater current is missing During UV lamp ignition the processor monitors the heater current If the current does not rise above the lower limit within one second the error message is generated Probable Causes e UV Lamp not connected e Ignition started without the top foam in place e Defective UV lamp or non Agilent lamp e Defective detector main board e Defective power supply Suggested Actions V Ensure the UV lamp is connected V Replace the top foam and turn on the lamp V Exchange the UV lamp V Exchange the detector main board V Exchange the power supply 152 1200 Series DAD and MWD Service Manual Error Information 8 Illegal Value From Temperature Sensor This
94. ain board fan The heater is clipped into the fan assembly temperature sensor and heater and pull the fan assembly If the fan is defective unclip the heater assembly from the fan as described in the next steps 1200 Series DAD and MWD Service Manual 273 13 Repairs 2 To unclip the heater from the fan use a pair of pliers squeeze the clips and push them through the hole Repeat this with the three remaining clips 3 Position the heater assembly and clip the heater onto the fan The cables should be oriented towards the left corner The fan must be installed in the correct orientation see arrow on the top foam to ensure optimum cooling and operation of the detector The direction of air flow is from the rear towards the front 274 4 Insert the fan assembly into its location 1200 Series DAD and MWD Service Manual Repairs 13 5 Reconnect the fan and heater to the main board see figure Next Steps below for location 6 Reinstall the top foam section top cover and front cover see Replacing the Foam and the Top Cover on page 299 7 Replace the detector into the stack 8 Reconnect cables capillaries and turn on detector 1200 Series DAD and MWD Service Manual 275 13 Repairs Replacing Temperature Sensor When required If the sensor is defective Tools required Screwdriver POZI 1 PT3 a pair of pliers Parts required Temperature sensor asse
95. ale Figure 129 RS 232 Cable 1200 Series DAD and MWD Service Manual 371 17 Hardware Information Setting the 8 bit Configuration Switch The G1315C D and G1365C D have a new main board platform that differs from the other modules Therefore the use of the 8 bit configuration switch has been changed Refer to the module specific reference manual in case you need detailed information on an other 1200 module The 8 bit configuration switch is located at the rear of the module Switch settings provide configuration parameters for LAN serial communication protocol and instrument specific initialization procedures ON 12 3 4 5 6 7 8 H c axe NC gt REMOTE om oa OO s O ee L_Je oe Son CAN CAN f asza USB o _LAN 7 N El O H idol I E O O ete h a JA E ANALOG ANALOG SS SS SS Sd I SS i 2 COMPACT FLASH K 2 C D E D M s c gt Toyo a c c C gt gt JC gt bi A 2C JC 5 SC one x J A 2 co ae aes ae oe Mg A NY C C Yi Figure 130 Location of Configuration Switches G1315C D and G1365C D To perform any LAN configuration SW1 and SW2 must be set to OFF See also Configuration Switches on page 50 372 1200 Series
96. ate see Wavelength Verification and Recalibration on page 246 and repeat the test Y Run the cell test see Wavelength Verification and Recalibration on page 246 If the test fails exchange the flow cell windows V Clean optical components with alcohol and lint free cloth V Exchange the UV lamp Instrument G1315C Serial Number PPO00000024 Operator Date Time 08 File C CHEM32 2 DIAGNOSE DAD FILTER2 DGR Holmium Filter Spectrum Adsorbance 3 X Holmium Filter Test Results Specification Measured Result Wavelength 1 261 0 nz 360 262 nm 360 5 nm Passed Wavelengsh 2 453 7 nz 452 7 454 7 nm 452 4 nm Passed Wavelength 2 536 7 nz 35 7 537 7 nm 526 8 nm Passed Figure 96 Holmium Oxide Test Results report 248 1200 Series DAD and MWD Service Manual Maintenance 12 Cell Test The cell test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm once with the flow cell installed and once with the flow cell removed The resulting intensity ratio is a measure of the amount of light absorbed by the flow cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell This test should be performed inititially with a n
97. ath ensuring minimum delay volume 36 1200 Series DAD and MWD Service Manual Installing the Detector 3 Vacuum degasser Pump Local User Interface Autosampler Column compartment Detector Figure 3 Recommended Stack Configuration Front View 1200 Series DAD and MWD Service Manual 37 3 38 Installing the Detector Remote cable CAN Bus cable to local user interface CAN Bus cable AC power Analog detector signal 1 or 2 outputs per LAN to LC detector ChemStation location depends on detector Figure 4 Recommended Stack Configuration Rear View 1200 Series DAD and MWD Service Manual Installing the Detector 3 Installing the Detector Preparations Locate bench space Provide power connections Unpack the detector Parts required Detector Power cord LAN cable cross over or twisted pair network cable e for other cables see below and section Cable Overview in the Service Manual e ChemStation and or Instant Pilot G4208A or Control Module G1323B with the appropriate revisions see Performance Specifications on page 30 e Other 1100 1200 modules must have firmware A 06 01 or above Before adding a G1315C D and G1365C D into an existing system assure that the existing modules have been updated to firmware revision A
98. ation is recommended after exchange of lamps and flow cells maintenance of flow cells repair of internal components and ona regular basis to ensure correct operation of the detector The detector uses the deuterium alpha and beta emission lines for wavelength calibration see Wavelength Verification and Recalibration on page 176 or Wavelength Verification and Recalibration on page 246 Diagnostic Signals The detector has several signals internal temperatures voltages and currents of lamps that can be used for diagnosing baseline problems see Diagnostic Signals on page 183 1200 Series DAD and MWD Service Manual Troubleshooting and Diagnostics 7 Status Indicators Two status indicators are located on the front of the detector The lower left indicates the power supply status the upper right indicates the detector status Status indicator green yellow red A CN Line power switch with green light Figure 66 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch When the indicator is illuminated green the power is ON 1200 Series DAD and MWD Service Manual 127 7 128 Troubleshooting and Diagnostics Detector Status Indicator The detector status indicator indicates one of four possible detector conditions When the status indicator is OFF and power switch light is on the detector is in a prerun condition and is r
99. board s memory 298 1200 Series DAD and MWD Service Manual Repairs Replacing the Foam and the Top Cover When required When all repairs have been completed Tools required Screwdriver POZI 1 PT3 Prerequisites The detector is open and other procedures have been carried out Preparations The optical unit power supply the fan and the detector main board are already installed 13 1 Route the lamp connector cables through the hole inthe 2 Insert the foam and make sure that the foam is installed foam correctly 1200 Series DAD and MWD Service Manual 299 13 Repairs 3 Press the lamp cables into the foam channel and reconnect the lamp connectors to the front panel 4 Reconnect the lamps 5 Slide the top plate towards the rear and fix the top plate screws Ensure correct fit with Z plane 6 Replace the cover 300 1200 Series DAD and MWD Service Manual Repairs 13 7 Replace waste funnel assembly and the front panel Next steps 8 Replace the detector into the stack 9 Reconnect the hydraulic connections 10 Reconnect the power cable and turn on the detector 1200 Series DAD and MWD Service Manual 301 13 Repairs Assembling the Main Cover When required If cover is broken Tools required None Parts required Plastics kit 5062 9985 includes base top left and right Preparations The plastics kit is not assembl
100. chapter provides information on how to set up the detector for an analysis and explains the basic settings 6 How to optimize the Detector This chapter provides information on how to optimize the detector 7 Troubleshooting and Diagnostics This chapter gives an overview about the troubleshooting and diagnostic features and the different user interfaces 1200 Series DAD and MWD Service Manual 3 10 11 12 13 14 15 17 Annex A Error Information This chapter describes the meaning of detector error messages and provides information on probable causes and suggested actions how to recover from error conditions Test Functions This chapter describes the detector s built in test functions Diagnostic Signals This chapter describes the detector s built in diagnostic signals Maintenance and Repair This chapter provides general information on repairing the detector Maintenance This chapter describes the maintenance of the detector Repairs This chapter describes the repair of the detector Parts and Materials for Maintenance This chapter provides information on parts for maintenance Identifying Cables This chapter provides information on cables used with the 1200 series of HPLC modules Hardware Information This chapter describes the detector in more detail on hardware and electronics Appendix This chapter provides addition information on safety legal and web 1200 Series DAD an
101. cified wavelength accuracy of the respective detector over is wavelength range September 15 2006 Texas foi nia Engineering Manager PIN 89550 90501 Revision F 3 Agilent T ies munana momen ee 1200 Series DAD and MWD Service Manual 391 A Appendix Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Select Life Sciences amp Chemical Analysis Solutions under Support It will provide also the latest firmware of the Agilent 1200 series modules for download 392 1200 Series DAD and MWD Service Manual Index A accessory kit 35 accessory kit parts 323 achromat parts 332 source lens 18 Agilent ChemStation Setup 71 on internet 392 algae information 389 alpha and beta line 176 246 analog signal output 31 361 368 APG remote interface 369 array 18 ASTM environmental conditions 27 noise test ChemStation only 173 reference 32 automatic configuration with Bootp 56 baseline problems deriving from deuterium lamps 185 specifications and conditions 191 wander drift problems due to temperature changes 190 Beer Lambert law 109 bench space 27 beta and alpha line 176 246 board layout and connectors 365 Bootp 51 amp Store 51 automatic configuration 56 initialization modes 51 service 56 storing the settings permanently 61 using default 53 using default parame
102. ct the optical bandwidth of the Sidney detector the narrower the slit the smaller the optical bandwidth a Configuration of the instrument but the lower its sensitivity The smaller the of Run Recovery optical bandwidth the higher the spectral resolution Fu Online Spectra To set the slit width display the drop down list and select an ae snfsesatlun appropriate slit width from the list rm Slit 4 nm m Margin for negat im Figure 52 Slit Settings 102 1200 Series DAD and MWD Service Manual Using the Detector 5 Margin for Negative Absorbance Settings 1 To change the settings select Setup Detector Signals 2 In the section Margin for Negative Absorbance change the value according to your needs CeTSet up DAD Signals Use this field to modify the detector s signal handling to increase of Control the margin for negative absorbance Use this option if for a5 Configuration example your solvent gradient produces a decreasing baseline of Run Recovery absorbance and for GPC analyses fy Online Spectra Limits 100 to 4000 mAU 8 Not Ready Information amp Help Margin for negative Absorbance fi 00 mAU Figure 53 Margin for Negative Absorbance The higher the value the greater the baseline noise Set this value only if you expect negative absorbance greater than 100 mAU Optimizing the Detector Additional theoretical information can be found in chapter How to op
103. d MWD Service Manual Content 1 Introduction Introduction to the Detector 16 Optical System 17 Early Maintenance Feedback EMF 20 Instrument Layout 22 Electrical Connections 23 2 Site Requirements and Specifications Site Requirements 26 Physical Specifications 29 Performance Specifications 30 3 Installing the Detector Unpacking the Detector 34 Damaged Packaging 34 Delivery Checklist 34 Optimizing the Stack Configuration 36 Installing the Detector 39 Flow Connections to the Detector 42 Setting up the LAN access 45 4 LAN Configuration What you have to do first 48 TCP IP parameter configuration 49 Configuration Switches 50 Initialization mode selection 51 1200 Series DAD and MWD Service Manual Link configuration selection 55 Automatic configuration with Bootp 56 Configuring the Agilent Bootp service program 56 Storing the settings permanently with Bootp 61 Manual Configuration 62 With Telnet 63 With the Instant Pilot G4208A 67 With the Handheld Controller G1323B 68 PC and Agilent ChemStation Setup 71 PC Setup for Local Configuration 71 Agilent ChemStation Setup 72 5 Using the Detector Setting up an Analysis 76 Before Using the System 76 Requirements and Conditions 78 Optimization of the System 80 Preparing the HPLC System 81 Running the Sample and Verifying the Results 90 Special Settings of the Detector 91 Control Settings 91 Configuration Settings 92 Online Spectra DAD only 93 Run Rec
104. e holder 9 Clean with alcohol and lint free cloth or replace the spectro window To clean use dry air only or use a new one 10 Replace all parts into the holder and tighten the lens achromatic with the metal blade Do not clean the achromatic lens with any liquid 11 Replace the achromat assembly move it completely into the optical and fix the setscrew Next steps 12 Reinstall the Holmium Filter assembly see Replacing the Holmium Oxide Filter Motor on page 286 1200 Series DAD and MWD Service Manual 285 13 Repairs Replacing the Holmium Oxide Filter Motor When required If defective Tools required Screwdriver POZI 1 PT3 hexagonal key 3 mm Parts required Filter motor assembly G1315 68700 includes filter lever G1315 45001 and spring 1460 1510 For others see Holmium Oxide Filter on page 333 Preparations Turn off the lamp e Switch off the detector and disconnect the power cable Remove detector from stack and place it on working bench Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 e Remove optical unit see Removing the Optical Unit on page 281 If the filter motor was removed the filter lever should not be reused Always use a new filter lever to assure correct fit on the filter motor shaft 286 1200 Series DAD and MWD Service Manual Repairs 13 1 Place the optical unit on your bench 2 Pull
105. e lt Not Set gt Temperature Control ON Use UV lamp anyway Use cell anyway OV 1V output range OV 1V_ output range Stays off at power on Stays off at power on 134 40 27 95 255 255 248 0 LAN Def Gateway 134 40 24 1 Figure 26 Instant Pilot LAN Configuration 5 Press the Edit button perform the required changes and press the Done button 6 Leave the screen by pressing the Exit button 1200 Series DAD and MWD Service Manual 67 4 68 LAN Configuration With the Handheld Controller G1323B To configure the TCP IP parameters before connecting the detector to the network the Handheld Controller G1323B with firmware B 04 02 or above can be used 1 Press F5 Views select System and press the Enter key 2 Press F2 Configure select the module where the LAN cable is installed and press the Enter key Figure 27 Time BERET ide Ready Fri 16 20 Module Message ld Date Time AHPLG System 2 Quat Pump Records Figure 27 Select module 3 Press F1 LAN Figure 28 Ready Options Analog voltage range Out 1 7 scale Out2 1 0 full scale At Power On O turn UY lamp on O turn VIS lamp on Figure 28 Select LAN 1200 Series DAD and MWD Service Manual LAN Configuration 4 4 After the Handheld Controller was reading out the LAN interface you will get an overview of the LAN settings LAN Status Page The informati
106. e controlled activities 4 SHUT DOWN L System has serious problem for example leak stops pump Receiver is any module capable to reduce safety risk 5 Not used 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 activities 9 START REQUEST L Request to start injection cycle for example by start key on any module Receiver is the autosampler 1200 Series DAD and MWD Service Manual Hardware Information 17 RS 232C The RS 232C connector is used to control the instrument from a computer through RS 232C connection using the appropriate software This connector can be activated by the configuration switch not on G1315C D and G1365C D The RS 232C is designed as DCE Data Communication Equipment with a 9 pin male SUB D type connector The pins are defined as follows Table 57 RS 232C Connection Table 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 Instrument PC RX 2 2 RX TX 3 X 3 TX DTR 4 4 DTR GND 5 5 GND DSR 6 6 DSR RTS 7 7 RTS CTS 8 X 8 CTS RI 9 9 RI DB9 DB9 DB9 DB9 Male Female Female M
107. e data is recovered from disk 1200 Series DAD and MWD Service Manual 95 5 Using the Detector Set up DAD Signals of Control a Configuration oo Run Recovery fy Online Spectra Help oD Manual Run Recovery in case of permanent communication failures DAD Run Recovery G1315C x r Run Recovery see Note No Run data available in device below Last Run Start Time Datafile E CHEMSTATIONS2 DATASRECOV D Status READY Start a recover After a recover 96 Dose He DAD Run Recovery G1315C x r Run Recovery Last Run Start Time Thu Feb 24 10 16 07 2005 E CHEMSTATIONS2 DATA RECOV D Datafile Status READY RUN RECOVERY IN PROGRESS Start F Close Help DAD Run Recovery G1315C x r Run Recovery Last Run Start Time Thu Feb 24 10 16 07 2005 Datafile E CHEMSTATION 2 DATA RECOV D Status DONE Close Help Manual Run Recovery in case of permanent communication failures Figure 48 When during recovery an error Method Sequence stopped appears the instrument logbook shows an entry No Run data available in device In this case refer to No Run Data Available In Device G1315C G1365C only on page 157 1200 Series DAD and MWD Service Manual P EC CHEM3 BATCH QI DeaLs QI pecat QI DECAL QI pecat QI DECAL QI DGCAL QI DECAL Pl arra 1200 Seri Using the Detector Analog Output Settings T
108. e ees el Signal Y range Offset VAS TENGE z ites A 2 10 Tis aut adjust Dimai hts B 2 20 a E c 2 30 K 20 40 Gi GIGS L 20 50 M 5 60 Figure 84 Selecting online plot signals 4 Let the detector equilibrate for about 30 to 60 minutes The Y range for signals A B C and M may require higher values when the lamps have been turned on NOTE 1200 Series DAD and MWD Service Manual 195 10 Diagnostic Signals Start a Run and Evaluate 1 Do Start baseline runs for 1 to 2 hours during the time where the user experiences the problems not run shorter runs Typical effects from air condition systems run at cycles of 15 to 20 minutes Look for a correlation between the temperature signal and the baseline If you see no correlation to the temperature signal see also Baseline problems deriving from deuterium lamps on page 185 3 Determine the rate of temperature change Look for trends which prevail for 5 minutes or longer Turbulences around one minute or less can be ignored Figure 85 shows an example where the detector s temperature control is ON normal operation The ambient temperature of 25 degree C varies by 2 degree C The baseline is stable Signal 254 4 ref OFF Signal 254 4 360 100 Board Temperature Optical Temperature Figure 85 Example plot optical unit temperature control ON 196 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 Figure 86
109. e filter test checks the correct operation of the filter assembly When the test is started the holmium oxide filter is moved into position During filter movement the absorbance signal is monitored As the edge of the filter passes through the light path an absorbance maximum is seen Once the filter is in position the absorbance maximum of holmium oxide is determined Finally the filter is moved out of the light path During movement an additional absorbance maximum is expected as the edge of the filter passes through the light path The test passes successfully if the two maxima resulting from the edge of the filter assembly during filter movement are seen and the absorbance maximum of holmium oxide is within the limits Figure 69 Filter Test Results report Filter Test Evaluation Test Failed Probable Causes e Filter assembly Clever and filter not installed e Defective filter motor 1200 Series DAD and MWD Service Manual Test Functions 9 Suggested Actions V Install the filter assembly V Exchange the filter motor Holmium Oxide Maximum out of Limits Probable Causes Holmium oxide filter not installed e Dirty or contaminated filter Suggested Actions V Install the holmium oxide filter V Exchange the holmium oxide filter 1200 Series DAD and MWD Service Manual 163 9 Test Functions Slit Test 164 The slit test verifies correct operation of the micromechanical slit During the test the slit
110. e humidity described in Table 1 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 30 is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 C hour 1 8 F hour Turbulences around one minute or less can be ignored Do not store ship or use your detector under conditions where temperature fluctuations could cause condensation within the detector Condensation will damage the system electronics If your detector was shipped in cold weather leave it in its box and allow it to warm up slowly to room temperature to avoid condensation 1200 Series DAD and MWD Service Manual 27 2 Site Requirements and Specifications NOTE The G1315C D and G1365C D are designed to operate in a typical electromagnetic environment EN61326 1 where RF transmitters such as mobile phones should not be used in close proximity 28 1200 Series DAD and MWD Service Manual Site Requirements and Specifications 2 Physical Specifications Table 1 Physical Specifications G1315C D and G1365C D Type Weight Dimensions width x depth x height Specification 11 5 kg 26 lbs
111. eady to begin an analysis A green status indicator indicates the detector is performing an analysis run mode A yellow indicator indicates a not ready condition 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 set point 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 problem which affects correct operation of the detector Usually an error condition requires attention e g leak defective internal components An error condition always interrupts the analysis A red blinking indicator indicates that the module is in resident mode e g during update of main firmware 1200 Series DAD and MWD Service Manual Troubleshooting and Diagnostics 7 User Interfaces Depending on the user interface the available tests vary All test descriptions are based on the Agilent ChemStation as user interface Some descriptions are only available in the Service Manual Table 20 Test Functions avaible vs User Interface Test ChemStation Instant Pilot Control Module G4208A G1323B Selftest Yes No No Filter Yes No No Slit Yes No Yes D A Converter Yes No No Test Chromatogram Yes C No Yes Wavelength Calibration Yes Yes M Yes Lamp Intensity Yes Yes D Yes Holmium Yes Yes D Yes Cell Yes Yes D N
112. ectral information For spectra options see Spectrum Settings on page 99 Range Only the wavelength range where the compounds in your sample absorb contains information that is useful for purity checks and library searches Reducing the spectrum storage range saves disk space Step Most substances have broad absorbance bands Display of spectra peak purity and library search works best if a spectrum contains 5 to 10 data points per width of the absorbance bands For anisic acid the example used before a step of 4 nm would be sufficient However a step of 2 nm gives a more optimal display of the spectrum Threshold Sets the peak detector Only spectra from peaks higher than threshold will be stored when a peak controlled storage mode is selected 118 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 Margin for Negative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative about 100 mAU In some special case for example when gradient with absorbing solvents are used the baseline may drift to more negative values Only for such cases increase the margin for negative absorbance to avoid overflow of the analog to digital converter 1200 Series DAD and MWD Service Manual 119 6 How to optimize the Detector Optimizing Selectivity 120 Quantifying Coeluting Peaks by Peak Suppression In chromatography two compounds may often elute
113. ed The plastics kit contains all parts but it is not assembled WARNING In case you insert the left or right side in the opposite position you may not be able to remove the side from the top part 1 Place the top part on the bench and insert the left and right 2 Replace the cover side into the top part 302 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 14 Parts and Materials for Maintenance Overview of Maintenance Parts 304 Standard Flow Cell 307 Semi Micro Flow Cell 309 Micro Flow Cell 311 High Pressure Flow Cell 313 Prep Flow Cell SST 315 Prep Flow Cell Quartz 317 Nano Flow Cells 319 Accessory Kit 323 This chapter provides information on parts for maintenance ee Agilent Technologies 303 14 Parts and Materials for Maintenance Overview of Maintenance Parts Figure 101 Maintenance Parts 304 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Table 27 Maintenance Parts Item Description Part Number 1 Front cover 5065 9982 2 Instant Pilot G4208A firmware revision B 01 02 or above for G1315C G1365C and B 02 01 or G4208 67001 above for G1315D G1365D Control Module G1323B firmware revision must be B 04 02 or above G1323 67011 3 Flow Cells with ID tag For details see Standard Flow Cell on page 307 Semi Micro Flow Cell on
114. ell path length and 120 bar 1760 psi pressure maximum Micro 2 ul volume 3 mm cell path length and 120 bar 1760 psi pressure maximum High pressure 1 7 pl volume 6 mm cell path The UV lamp is equipped with RFID tag that holds lamp typical information See note on page 32 See note on page 32 See note on page 32 Self calibration with deuterium lines verification with holmium oxide filter Programmable in steps of 1 nm Programmable slit See Optimization Overview on page 107 All flow cells are equipped with RFID tags that hold cell typical information length and 400 bar 5880 psi pressure maximum 500 nano 0 5 pl volume 10 mm cell path length and 50 bar 725 psi pressure maximum 80 nano 0 5 pl volume 10 mm cell path length and 50 bar 725 psi pressure maximum 30 1200 Series DAD and MWD Service Manual Site Requirements and Specifications 2 Table 2 Performance Specifications G1315C D and G1365C D continued Type Specification Comments Flow Cells Control and data evaluation Local Control Analog outputs Communications Prep SST 3 mm cell path length and 120 bar 1760 psi pressure maximum Prep Quartz 0 3 mm mm cell path length and 20 bar 293 psi pressure maximum Prep Quartz 0 06 mm mm cell path length and 20 bar 293 psi pressure maximum Agilent ChemStation for LC 32 bit Agilent Instant Pilot G4208A or Control Module G1323B Recorder integrator 100
115. emoving the PCMCIA Interface on page 272 264 1200 Series DAD and MWD Service Manual Repairs 13 REMOTE ANALOG LAN USB RS 232 CAN CAN 2 1 J l l ise me PCMCIA CONFIG 4 See note on page 264 PWS OOO LEAK O Oo a O00 enj Eeto res HOLM TEMP ID CELL OPTICAL ID LAMP HEATER FAN Figure 99 Location of Connectors on Detector Main Board 1200 Series DAD and MWD Service Manual 265 13 Table 26 Connections on the main board see Figure 99 on page 265 266 Connector Description Connector Description PCMCIA removed in November 2006 OPTICAL connects to optical unit LAN connects to LAN interface ID CELL connects to ID reader of flow cell USB for future use FAN connects to the fan REMOTE remote control TEMP connects to temperature sensor CAN inter module communication HEATER connects to heater ANALOG signal to plotter or data system HOLM connects to stepper motor PWS connects to power supply ID LAMP connects to ID reader of UV lamp LEAK connects to leak sensor 7 Install the new detector main board and reconnect the connectors Assure that the board is fitted correctly into the board recess in the rear panel 8 Refit the nuts at the REMOTE RS 232 and analog connector
116. eral Purpose Connector Wire Color Pin Signal Name BCD Digit G1351 81600 Agilent 1200 Green 1 BCD5 20 Violet 2 BCD7 80 I Blue 3 BCD 6 40 E Yellow 4 BCD 4 10 ker Se Black 5 BCD 0 1 Se SS Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 not connected 14 not connected 15 5V Low 352 1200 Series DAD and MWD Service Manual Identifying Cables 16 Agilent 1200 to 3396 Integrators Connector Pin Pin Signal Name BCD Digit 03396 60560 3392 3 Agilent 1200 1 1 BCD 5 20 ES 2 BCD7 80 se ds 3 3 BCD 6 40 to 4 4 BCD 4 10 o 5 5 BCDO 1 1e 6 6 BCD3 8 O 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 1200 Series DAD and MWD Service Manual 353 16 Identifying Cables Auxiliary Cable 354 One end of this cable provides a modular plug to be connected to the Agilent 1200 Series vacuum degasser The other end is for general purpose Agilent 1200 Series Degasser to general purposes Connector Color Pin Signal Name G1322 61600 Agilent 1200 White 1 Ground Brown 2 Pressure signal Za Green 3 ae eee j Yellow 4 n D Grey 5 DC 5VIN Pink 6 Vent 1200 Series DAD and MWD Service Manual Identifying Cables 16 CAN Cable Both ends of this cable provide a modular plug to be connected to Agilent 1200 Series module s CAN bus connect
117. ess 0A3AD3AAA838S Init Mode Using Stored Initialization mode is Using Stored TCP IP Properties active IP Address 134 46 27 95 Subnet Mask 255 255 248 0 active TCP IP settings Gateway 134 46 24 1 stored Address 134 40 27 99 255 248 8 Gateway stored TCP IP settings in non volatile memory Controllers no connections connected to PC with controller software e g Agilent ChemStation here not connected Figure 24 Telnet Change IP settings 1200 Series DAD and MWD Service Manual 65 4 LAN Configuration 7 When you have finished typing the configuration parameters type exit and press Enter to exit with storing parameters EY C WINDOWS system32 cmd exe Agilent Technologies G1315C PP 88660024 gt exit Connection to host lost Cz gt Figure 25 Closing the Telnet Session If the Initialization Mode Switch is changed now to Using Stored mode the instrument will take the stored settings when the module is re booted In the example above it would be 134 40 27 99 66 1200 Series DAD and MWD Service Manual LAN Configuration 4 With the Instant Pilot G4208A To configure the TCP IP parameters before connecting the detector to the network the Instant Pilot G4208A can be used 1 From the Welcome screen press the More button 2 Select Configure 3 Press the DAD MWD button 4 Scroll down to the LAN settings Configure DAD Symbolic Nam
118. ess to the flow cell area 3 Insert the flow cell 4 Connect the flow cell capillaries to the capillary holder top is inlet bottom is outlet 1200 Series DAD and MWD Service Manual 43 3 Installing the Detector 5 If another Agilent 1200 Series module is positioned on top of the detector route the tubing assembly waste from the accessory kit behind the capillary holder and connect the top end to the other module s waste outlet To other module as 6 Connect the capillary from the column to the capillary holder top Connect the teflon waste tubing to the flow cell outlet fitting bottom and the corrugated waste tubing to the leak outlet leaks 8 Insert the flow cell close the cover and replace the front cover The installation of the detector is complete now 1200 Series DAD and MWD Service Manual Installing the Detector 3 Setting up the LAN access Please follow the instructions in LAN Configuration on page 47 1200 Series DAD and MWD Service Manual 45 3 Installing the Detector 46 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 4 LAN Configuration What you
119. est to check the proper function 11 Replace the flow cell cover see Correcting Leaks on page 239 12 Replace both lamps 13 Replace the front cover 1200 Series DAD and MWD Service Manual 259 13 Repairs Removing the Top Cover and Foam When required For all repairs inside the detector Tools required Screwdriver POZI 1 PT3 Screwdriver Parts required Depends on the work inside and the following procedures Preparations Turn off the detector Disconnect the power cable Disconnect capillaries e Remove detector from stack and place it on the working bench 1 Press the release buttons and remove the front cover 2 Move the power lock across the power inlet and lift the Unclip the waste funnel assembly clips of the cover 260 1200 Series DAD and MWD Service Manual Repairs 13 3 Lift the cover up and slide it towards the rear f Unscrew the screws at the rear of the top plate slide the plate towards the front and remove it Remove the two lamp connectors towards the back by depressing their connector tabs with a screwdriver 1200 Series DAD and MWD Service Manual 261 13 Repairs 7 While removing the top foam section completely route the lamp cables through the hole in the foam Dell T at LY Zi E Aut WWWe ttt Note Do not connect a power plug to the detec
120. et capillary with heat exchanger 7 Take the new inlet capillary and bend it 90 about 35 mm 8 Bend the capillary again by 90 as shown below from its end Aga ss NS Q Y N 5 y pa ge 224 1200 Series DAD and MWD Service Manual Maintenance 12 9 Insert the capillary into the hole between fixing screw and the inlet fitting 10 The capillary lays in the grove and should be tied around the body in the grove 5 times 11 Insert the fixing screw the grove Screw Inlet capillary with heat so that the capillary cannot leave LO HI KORY UY WINS 12 Carefully insert the RFID tag into the new heat exchanger Shown is the default orientation See Note on page 219 1200 Series DAD and MWD Service Manual 225 12 Maintenance 13 Fix the heat exchanger to the clamp unit and the flow cell body to the heat exchanger 14 Fix the inlet capillary to the flow cell body handtight first Then do a 1 4 turn with a 4 mm wrench 15 Check for a centered holder vs hole If required adjust with the holder screws Next steps 16 Reconnect the capillaries see Exchanging a Flow Cell on page 211 17 Perform a leak test 18 Insert the flow cell 19 Replace the front cover 20 Perform a Wavelength Verification and Recalibration on page 246 ora Holm
121. ety of parameters that can be used to optimize performance Depending on whether signal or spectral data need to be optimized different settings are recommended The following sections describe optimization for e signal sensitivity selectivity and linearity e spectral sensitivity and resolution DAD only and e disk space required for storing data The information in this chapter should be seen as a basic introduction to diode array detector technics Some of these technics may not be available in the instrument firmware or the user interfaces Control Module and or Agilent Chemstation How to Get the Best Detector Performance The information below will guide you on how to get the best detector performance Follow these rules as a start for new applications It gives rules of thumb for optimizing detector parameters 1200 Series DAD and MWD Service Manual Optimization Overview Table 17 Optimization Overview How to optimize the Detector 6 Parameter Impact 1 4 Selection of flow cell Choose flow cell according to used column see Figure 54 Connection of flow cell For flow rates from 0 5 ml min connect column using the zero dead volume fittings of the detector For small column i d e g 1 mm the inlet capillary of the micro flow cell can be connected directly to the column Setting the peak width response time Use peak width according Figure 54 as starting point Set the peak width close to the width
122. ew detector flow cell The values should be kept for later reference comparison Cell Test Evaluation The Agilent ChemStation calculates the intensity ratio automatically The intensity ratio typically between 0 5 and 0 7 for new standard flow cells is dependent on the degree of contamination of the flow cell windows and on the type of flow cell used Figure 97 Cell Test Results report with no flow cell inserted This test can be used for the standard flow cells only The nano flow cells will give very low values due to their design 1200 Series DAD and MWD Service Manual 249 12 Maintenance Test Failed low ratio value Probable Causes e Absorbing solvent or air bubble in flow cell e Dirty or contaminated flow cell Suggested Actions V Ensure the flow cell is filled with water and free from air bubbles Y Exchange the flow cell windows 250 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 13 Repairs Cautions and Warnings 252 Cleaning or Replacing Coupling Lens Assembly 254 Cleaning or Replacing Cell Support Window 257 Removing the Top Cover and Foam 260 Exchanging the Detector Main Board 263 Changing the Product Number and Serial Number 267 Using the Agilent ChemStation 267 Using the Instant Pilot G2408A 268 Using the Control Module G1323B 270 Removing the PCMCIA Interface 272 Replacing Fan Parts 273 Replacing Temperature Sensor 27
123. f the cell used for the measurement Therefore flow cells with longer path lengths yield higher signals Although noise usually increases little with increasing path length there is a gain in signal to noise ratio For example in Figure 55 the noise increased by less than 10 but a 70 increase in signal intensity was achieved by increasing the path length from 6 mm to 10 mm When increasing the path length the cell volume usually increases in our example from 5 13 ul Typically this causes more peak dispersion As Figure 55 demonstrates this did not affect the resolution in the gradient separation in our example As a rule of thumb the flow cell volume should be about 1 3 of the peak volume at half height To determine the volume of your peaks take the peak width as reported in the integration results multiply it by the flow rate and divide it by 3 1200 Series DAD and MWD Service Manual 109 6 How to optimize the Detector Analysis of pesticide standard g 6 mm optical path length E 10 mm optical path lengt 3 lt Time min Figure 55 Influence of Cell Path Length on Signal Height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards To check photometric accuracy of the Agilent 1200 DAD MWD it is necessary to have more precise information on path lengths of the flow cells The correct response is expected response correction factor
124. ger check your entries 6 Press Exit Manager and OK to exit the Agilent Bootp Service 7 Now turn on the module with the detector wait about 30 60 seconds and view the LogFile see Figure 18 It should display the request from the detector with the hardware MAC address 02 03 05 16 33 56 PM Status BOOTP Request received at outer most layer Status BOOTP Request received from hardware adire 00300300658 Status found 134 40 27 95 WADI1171 Status Host IP Address is 134 40 29 56 Status Reply to BOOTP Request has been sent Status BOOTP Request finished processing at outer most layer Figure 18 LogFile the detector has received the parameter 1200 Series DAD and MWD Service Manual 59 4 60 LAN Configuration When using this Bootp mode the parameters are not written into the non volatile memory of the detector If you delete this Bootp Configuration the Bootp Manager will show up as shown in Figure 15 on page 57 Bootp mode If you want to store your parameters permanently on the detector for use without the Agilent Bootp service refer to Storing the settings permanently with Bootp on page 61 1200 Series DAD and MWD Service Manual LAN Configuration 4 Storing the settings permanently with Bootp If you want to change parameters of the detector using the Bootp follow the instructions below 1 2 Turn off the detector Change the detector s settings of the Configuration Switch to Bootp amp
125. h capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column 1200 Series DAD and MWD Service Manual 219 12 Maintenance 1 Use a4 mm hex key to unscrew the window assembly 1 and remove the gasket 2 from the cell body If you want to replace the gasket only continue with step 7 on page 217 2 Use a tooth pick to remove the quartz window from the window assembly Note If the washers fall out of the window assembly they must be inserted in the correct order with the Teflon ring to prevent any leaks from the flow cell window 220 1200 Series DAD and MWD Service Manual Maintenance 12 Orientation of Flow Cell Parts 1 window assembly contains 6 items 2 3 4 5 and 6 2 seal ring D quartz window compression washer spring washers window holder window screw inlet capillary outlet capillary OI PAO Bw 3 Follow the procedure Maintenance of Standard Semi Micro or Micro Flow Cell on page 214 for reassembling 1200 Series DAD and MWD Service Manual 221 12 Maintenance Replacing Capillaries on a Standard Flow Cell When required If the capillary is blocked Tools required Two 1 4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see Standard Flow Cell on page 307 Preparations Turn the lamp s off Remove t
126. have to do first 48 TCP IP parameter configuration 49 Configuration Switches 50 Initialization mode selection 51 Link configuration selection 55 Automatic configuration with Bootp 56 Configuring the Agilent Bootp service program 56 Storing the settings permanently with Bootp 61 Manual Configuration 62 With Telnet 63 With the Instant Pilot G4208A 67 With the Handheld Controller G1323B 68 Manual Configuration 62 PC and Agilent ChemStation Setup 71 This chapter provides information on connecting the detector to the Agilent ChemStation PC ot Agilent Technologies 47 4 LAN Configuration What you have to do first The G1315C D and G1365C D have an on board LAN communication interface 1 Note the MAC Media Access Control address for further reference The MAC or hardware address of the LAN interfaces is a world wide unique identifier No other network device will have the same hardware address The MAC address can be found on a label at the rear of the detector underneath the configuration switch see Figure 8 Sie aaa Ae eT Part number of the detector main board MAC 000001000001 Revision Code Vendor Year and Week of assembly Made in Germany MAC address Country of Origin Figure 7 MAC Label 2 Connect the instrument s LAN interface see Figure 8 to a the PC network card using a crossover network cable point to point or b ahub or switch using a standard LAN cable
127. he chromatogram see page 100 autobalance to zero absorbance on the analog output plus offset at begin and or end of run mechanical slit width can be changed for further optimization see page 102 margin for negative absorbance see page 103 Under More additional diagnostic signals can be added for troubleshooting purpose see section Diagnostic Signals in the Service Manual time table for programmable actions during the run NOTE The Agilent G1315C D and G1365C D time table can contain a maximum of 60 rows 1200 Series DAD and MWD Service Manual Using the Detector 5 11 Pump the water acetonitrile 30 70 mobile phase through the column for 10 minutes for equilibration 12 Click the button and select Change to open the Signal Plot information Select the Pump Pressure and the DAD A Signal 254 4 as signals Change the Y range for the DAD to 1 mAU and the offset to 20 and the pressure offset to 50 The X axis range should be 15 minutes Press OK to exit this screen Ln nnn SCC ee G 2 Pl ie mg Ma LTD O Edit Signal Plot DEFAULT O Available Signals Selected Signals uaternary Pump Flow DAD Signal 254 4 Reference 360 aternary Pump A 4d Quaternary Pump Pressure Add gt 2 uaternary Pump B aes uaternary Pump oC D uaternary Pump D E atah lad olumn Thermostat Temperature le E116Bhee 5 L olumn Thermostat Temperature ri A
128. he front cover Remove the flow cell see Exchanging a Flow Cell on page 211 All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column The fittings at the flow cell body are special types for low dead volumes and not compatible with other fittings When retightening the fittings make sure that they are carefully tightened handtight plus 1 4 turn with a wrench Otherwise damage of the flow cell body or blockage may result 222 1200 Series DAD and MWD Service Manual Maintenance 12 1 Identify the inlet and outlet capillaries To replace the inlet 2 After replacing the outlet capillary fix it handtight first capillary continue with step 3 Then do a 1 4 turn with a 4 mm wrench Outlet 3 To replace the inlet capillary use a 4 mm wrench for the 4 Unscrew the cell body from the heat exchanger and the fitting heat exchanger from the clamp unit 1200 Series DAD and MWD Service Manual 223 12 Maintenance 5 Use a small flat screw driver to carefully lift off the RFID 6 Unscrew the fixing screw and unwrap the inlet capillary tag Shown is the default orientation See Note on from the grove in the flow cell body page 219 Screw Inl
129. he limits for each range the measured intensity counts and passed or failed for each spectral range see Figure 94 on page 245 The evaluation report is only on the Agilent ChemStation available Test Failed Probable Causes e Absorbing solvent or air bubble in flow cell e Dirty or contaminated flow cell e Dirty or contaminated optical components achromat windows e Old or non Agilent lamp 244 1200 Series DAD and MWD Service Manual Maintenance 12 Suggested Actions V Ensure the flow cell is filled with water and free from air bubbles Y Run the cell test see Cell Test on page 249 If the test fails exchange the flow cell windows V Clean optical components with alcohol and lint free cloth V Exchange the lamp Instrument G61315 Serial Number 200000024 Operator Wolfgang Date 25 02 2005 Time 14 53 05 Pile C CHEM32 2 DIAGNOSE DAD_INT2 DGR Intensity Test Results Accumulated UV lamp on time 23 77 h Lowest intensity in range 190nm 220nm gt 2000 cts 18695 crs Passed Lowest i ity in range 221nm 350nm gt 5000 cts 26848 cts Passed Lowest int in range 3S5inm 00nm gt 2000 cts 16593 cts Passed Lowest intensity in range 50lnm 950nm gt 6000 cts 15767 cts Passed Highest intensity in range 190nm 350nm lt 450000 cts 4508 cts Passed Highest intensity in range 700nm 50nm lt 300000 cts 69968 cts Passed Highest intensity for the D2 alpha line lt 1200000 cts 15920
130. he power cable Remove detector from stack and place it on working bench Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 Remove the fan assembly see Replacing Fan Parts on page 273 Remove the detector main board see Exchanging the Detector Main Board on page 263 Remove optical unit see Removing the Optical Unit on page 281 The repair level of the power supply assembly is exchanging the complete assembly No serviceable parts are inside 1200 Series DAD and MWD Service Manual 291 13 Repairs 1 Carefully remove the bottom foam part by sliding it out towards the rear 2 Unscrew the power supply at the rear of the module 3 Press down the power switch light pipe to remove it from the coupler Power switch light pipe 4 Remove the power supply completely Re use the coupler on the new power supply Coupler inside The repair level of the power supply assembly is exchange of the complete assembly No serviceable parts 292 1200 Series DAD and MWD Service Manual Repairs 13 5 Insert the power supply into its location and fix it with the screws at the rear panel LAN Usa o 3 o o le le Decs J COMPACT FLASH amp 6 Press down and clip in the power switch light pipe into the power supply Power switch light pipe 7 Re
131. he test should be done with water in the flow cell The shape of the intensity spectrum is primarily dependent on the lamp grating and diode array characteristics Therefore intensity spectra will differ slightly between instruments Figure 71 on page 168 shows a typical intensity test spectrum Intensity Test Evaluation The Agilent ChemStation evaluates four spectral ranges automatically and displays the limits for each range the measured intensity counts and passed or failed for each spectral range see Figure 71 on page 168 The evaluation report is only on the Agilent ChemStation available Test Failed Probable Causes e Absorbing solvent or air bubble in flow cell e Dirty or contaminated flow cell e Dirty or contaminated optical components achromat windows e Old or non Agilent lamp 1200 Series DAD and MWD Service Manual 167 9 Test Functions Suggested Actions V Ensure the flow cell is filled with water and free from air bubbles V Run the cell test see Cell Test on page 174 If the test fails exchange the flow cell windows V Clean optical components with alcohol and lint free cloth V Exchange the lamp Instrument G61315 Serial Number 200000024 Operator Wolfgang Date 25 02 2005 Time 14 53 05 Pile C CHEM32 2 DIAGNOSE DAD_INT2 DGR Intensity Test Results Accumulated UV lamp on time 23 77 h Lowest intensity in range 190nm 220nm gt 2000 cts 18695 crs Passed Lowe
132. his resident section of the firmware is identical for all Agilent 1200 series modules Its properties are e the complete communication capabilities CAN and RS 232C e memory management e ability to update the firmware of the main system Main System Its properties are e the complete communication capabilities CAN LAN and RS 232C e memory management e 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 e run synchronization through APG remote e error handling e diagnostic functions e or module specific functions like internal events such as lamp control filter movements raw data collection and conversion to absorbance 376 1200 Series DAD and MWD Service Manual Hardware Information 17 Firmware Updates Firmware updates can be done using your user interface e handheld control module with files from a PC card or e PC and Firmware Update Tool with local files on the hard disk The file naming conventions are PPPPRVVV_XX dlb where PPPP is the product number for example 1315 for the G1315 DAD R the firmware revision for example B for the G1315C DAD VVV is the revision number for example 101 is revision 1 01 XX is the build number of the firmware For instructions on firmware updates refer to Replacing the Detector s Firmware on page 242 Update of main system can be done
133. i Set up DAD Signals of Control beds ett a Configuration of Control of Run Recovery B Not Ready Information ees amp Help 8 Not Ready Information B ors Help Figure 39 Open the module menu 10 Enter the pump parameters mentioned under Conditions on page 79 1200 Series DAD and MWD Service Manual 85 5 Using the Detector x m Signals m Time Store Sample Bw Reference Bw Stoptime as Pump al ae AW m Jaso fioo S nm d no Limit Z B fase fe feso fo gnm Postime of Sf mn O M fao B faeo fioo 4 nm gt ml 230 fie faso fico 4 nm r Reguired Lamps e faso fie faso froo 2 nm M uv T Vis F fox fie feo foo 2f nm a 280 fis jeo foo 4 ann m Peakwidth Responsetime HI e0 fie feo fioo 2 nm f gt 01 mnes xi m Spectrum m Autobalance ae None IV Pren I Postrun Range EN to o nm Step fzo nm ee Threshold fi oo mal dnm m Margin for negative Absorbance neta gt to Lines 0 100 ai Cancel s Line Time Sig Sam Bw Rei Bw Store Specta Threaha S C imet Append Ca Table C Graphic Carcel Figure 40 DAD Timetable System 2 xj Heb Detector parameter default up to 8 signals A to H with individual wavelength settings can be selected spectrum settings see page 98 stop and post time can be set if required depending on the application the lamps can be selected one or both peak width depends on the peaks in t
134. iation 388 initialization mode selection 51 installation accessory kit 35 bench space 27 delivery checklist 34 environment 27 flow connections 42 of flow cell and capillaries 42 of the detector 39 physical specifications 29 power considerations 26 power cords 26 site requirements 26 unpacking 34 instrument layout 22 intensity test 167 interfaces analog signal output 368 APG remote 369 CAN 368 overview 367 RS 232C 371 internet 392 introduction optical unit parts 18 L lamp and flow cell identification 363 lamp control 361 lamps 18 LAN automatic configuration with Bootp 56 Bootp 51 Bootp amp Store 51 Bootp service 56 cables 358 configuration 47 configuration switches 50 factory default settings 50 1200 Series DAD and MWD Service Manual Index initialization mode selection 51 link configuration selection 55 manual configuration 62 manual configuration with handheld controller 68 manual configuration with telnet 63 PC and Agilent ChemStation Setup 71 storing the settings permanently 61 TCP IP parameter configuration 49 using default 53 using default parameters 53 using stored 52 what you have to do first 48 leak correcting 239 parts 336 sensor 361 line voltage and frequency 29 linear range 30 linearity measurements 32 link configuration selection 55 local control 31 location of connectors 265 M MAC address 48 location of label 40 mai
135. icro flow cell qty 12 of item 6 79883 68702 Seal kit FRONT for semi micro flow cell qty 12 of item 7 G1315 68710 Window screw kit includes 2 quartz windows 2 compression 79883 68703 washers 2 window holders 2 window screws and 10 spring washers 1200 Series DAD and MWD Service Manual 311 14 Parts and Materials for Maintenance NOTE Gaskets 6 and 7 have different hole diameters Figure 106 Micro Flow Cell Parts 1 window screw 2 spring washers 3 compression washer 4 window holder 5 quartz window 6 Gasket Figure 107 Orientation of Spring Washers 312 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 High Pressure Flow Cell Table 31 High Pressure Flow Cell Parts Item Description Part Number High pressure flow cell assembly 6 mm 1 7 ul G1315 60015 maximum pressure 400 bar 40 MPa with RFID tag 1 Window assembly comprises items 2 3 4 5 and 6 2 Seal ring 79883 27101 3 Quartz window 1000 0953 4 Compression washer 79883 28802 5 Spring washers pack of 10 5062 8553 6 Window screw 79883 22404 7 Capillary IN 0 12 mm 290 mm Ig including heat exchanger G1315 87325 8 Capillary OUT 0 12 mm 200 mm lg G1315 87306 9 Clamp unit G1315 84901 Screw M 2 5 4 mm lg for cell body clamp unit 0515 1056 Capillary 0 12 mm 150 mm lg G1315 87312 Capillary 0 17 mm 380 mm lg G1315 87311 High Pressure Cell Repair Kit includes 1 quartz window 79883 687
136. ied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connec tion with the furnishing use or per formance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this 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 those rights customarily provided to end user Customers of Software Agilent provides this customary commercial license in Software and technical data pursuant to FAR 12 211 Technical Data and FAR 12 212 Computer Software and for Department of Defense purchases DFARS 252 227 7015 Technical Data Commercial Items and DFARS 227 7202 3 Rights in Commercial Computer Software or Computer Software Documentation If a federal government or other public sector Customer has a need for rights not conveyed under these terms it must negotiate with Agilent to establish acceptable terms in a written agreement executed by all relevant parties Safety Notices
137. ies DAD and MWD Service Manual Parts and Materials for Maintenance 14 Standard Flow Cell Table 28 Standard Flow Cell Parts Item Description Part Number A wo N Standard flow cell assembly 10 mm 13 ul maximum pressure 120 bar 12 MPa with RFID tag Window screw Spring washers pack of 10 Compression washer Window holder Quartz window Gasket BACK Teflon 2 3 mm hole outlet side Gasket FRONT Teflon 1 3 mm hole inlet side Window assembly comprises item 1 2 3 4 5 Capillary IN 0 17 mm 590 mm lg including heat exchanger Capillary OUT 0 17 mm 200 mm lg Clamp unit Screw M 2 5 4 mm lg for cell body clamp Zero dead volume fitting Cell repair kit STD includes window screw kit 4 mm hexagonal wrench and seal kit Seal kit BACK for STD flow cell qty 12 of item 6 Seal kit FRONT for STD flow cell qty 12 of item 7 Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 spring washers G1315 60022 79883 22402 5062 8553 79883 28801 79883 22301 1000 0488 See kits below See kits below No part number G1315 87321 G1315 87302 G1315 84910 0515 1056 5022 2184 G1315 68712 G1315 68711 G1315 68710 79883 68703 1200 Series DAD and MWD Service Manual 307 14 Parts and Materials for Maintenance NOTE Gaskets 6 and 7 have different hole diameters 308 Figure 102 Standard Flow Cell Parts Gaskets 6 and
138. illary fix it handtight first Then do a 1 4 turn with a 4 mm wrench 3 To replace the inlet capillary use a 4 mm wrench for the fitting Unscrew the cell body from the heat exchanger and the heat exchanger from the clamp unit 228 1200 Series DAD and MWD Service Manual Maintenance 12 5 Use a small flat screw driver to carefully lift off the RFID tag Shown is the default orientation See Note on page 219 6 Carefully insert the RFID tag into the new heat exchanger Shown is the default orientation See Note on page 219 7 Fix the new heat exchanger to the clamp unit and the heat exchanger to the cell body 8 Fix the inlet capillary to the flow cell body handtight first Then do a 1 4 turn with a 4 mm wrench 1200 Series DAD and MWD Service Manual 229 12 Maintenance 9 Check for a centered holder vs hole If required adjust with the holder screws Next steps 10 Reconnect the capillaries see Exchanging a Flow Cell on page 211 11 Perform a leak test 12 Insert the flow cell 13 Replace the front cover 14 Perform a Wavelength Verification and Recalibration on page 246 or a Holmium Oxide Test on page 247 to check the correct positioning of the flow cell 230 1200 Series DAD and MWD Service Manual Maintenance 12 Nano Flow Cell Replacing or
139. in 2 Flush all tubes with at least 30 ml of solvent 3 Set flow to required value of your application and close the purge valve Pump for approximately 10 minutes before starting your application 1200 Series DAD and MWD Service Manual 77 5 78 Using the Detector Requirements and Conditions What You Will Need Table 11 lists the items you need to have for the set up of the analysis Some of these are optional not required for the basic system Table 11 What you will need 1200 system Column Standard Pump plus degassing Autosampler Detector standard flow cell installed Agilent ChemStation or Instant Pilot G4208 optional for basic operation or e Control Module G1323B optional for basic operation with with the appropriate revisions see Performance Specifications on page 30 System should be correctly set up for LAN communication with the Agilent ChemStation Zorbax Eclipse XDB C18 4 6 x 150 mm 5 um Part No 993967 902 or Part No 5063 6600 Part No 01080 68704 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl 0 03 wt o terphenyl in methanol 1200 Series DAD and MWD Service Manual Conditions Using the Detector 5 A single injection of the isocratic test standard is made under the conditions given in Table 12 Table 12 Conditions Flow Stoptime Solvent Temperature Wavelength Injection Volume 1 5 ml minute 8 minutes
140. in the detector The detector s local memory is too small to store the data 94 The detector supports run buffering which means that an amount of run data uv and ch files is stored in a storage medium CompactFlash Card in the detector until either it is overwritten or the detector undergoes a power cycle If there is a temporary network failure or the PC is not able to constantly take the data the stored data is transferred to the ChemStation automatically when the network connection is restored or the PC can take the data so that no loss of data occurs If there is a permanent network failure the Run Recovery dialog box Figure 48 on page 96 allows you to restore the stored data to the data directory From there you can copy the files to the directory where the files are corrupted or not complete On very large recovery files it may take a long time to restore it to the Agilent ChemStation A sequence will be stopped in case of a network problem When during recovery an error Method Sequence stopped appears the instrument logbook shows an entry No Run data available in device In this case refer to No Run Data Available In Device G1315C G1365C only on page 157 1200 Series DAD and MWD Service Manual Using the Detector 5 Automated Run Recovery in case of temporary communication failures Table 14 Automated Run Recovery in case of temporary communication failures Situation Reaction On ChemS
141. in the resident system only Update of the resident system can be done in the main system only main FW update Resident System Main System resident FW update Figure 131 Firmware Update Mechanism 1200 Series DAD and MWD Service Manual 377 17 Hardware Information The Main Power Supply Assembly The main power supply comprises a closed assembly no onsite repair possibility The power supply provides all DC voltages used in the module except for the voltages supplied by the lamp power supply to the deuterium and tungsten lamps in the detectors The line voltage can vary in a range from 100 240 volts AC 10 and needs no manual setting MPS 36V m 36V not used supply line i 24V gt primary D voltage circuits 424V 45A 5V switching gt 45V 3A regulator linear voltage gt 15 3A regulators gt 15V 3A Figure 132 Main Power Supply MPS Block diagram WARNING 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 378 1200 Series DAD and MWD Service Manual Hardware Information 17 No accessible hardware fuse is needed because the main power supply is safe against any short circuits or overload conditions on the output lines When overload conditions occur the power supply turns off all output voltages
142. ing recommendations on the use of solvents Flow Cell Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell Prevent any crystallization of buffer solutions This will lead into a blockage damage of the flow cell If the flow cell is transported while temperatures are below 5 degree C it must be assured that the cell is filled with alcohol Aqueous solvents in the flow cell can built up algae Therefore do not leave aqueous solvents sitting in the flow cell Add small of organic solvents e g Acetonitrile or Methanol 5 Solvents Brown glass ware can avoid growth of algae Always filter solvents small particles can permanently block the capillaries Avoid the use of the following steel corrosive solvents e Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on e High concentrations of inorganic acids like nitric acid sulfuric acid especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel e Halogenated solvents or mixtures which form radicals and or acids for example 2CHCls Op 32COCly 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol 1200 Series DAD
143. install bottom foam part Slide it in underneath the leak drain Next steps 8 Reinstall the processor board see Exchanging the Detector Main Board on page 263 9 Reinstall the fan assembly see Replacing Fan Parts on page 273 10 Reinstall the optical unit see Installing the Optical Unit on page 297 11 Reinstall the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 12 Replace detector into the stack 13 Reconnect the power cable and turn on the detector 1200 Series DAD and MWD Service Manual 293 13 Repairs Exchanging the Leak Sensor When required Tools required Parts required Preparations If defective Screwdriver POZI 1 PT3 Leak sensor assembly 5061 3356 Turn off the lamp Switch off the detector and disconnect the power cable Remove detector from stack and place it on working bench Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 Remove optical unit see Removing the Optical Unit on page 281 board 1 Disconnect the leak sensor cable from the detector main 2 Remove the leak sensor assembly from the leak pan ia on rm 294 1200 Series DAD and
144. ion Agilent ChemStation Setup 1 Start the Configuration Editor of the Agilent ChemStation Select Instrument System 2 Device Configuration Instrument Type Modular 3D LC 1090 LC System m Modules 1100 System Access LC Data Analysis onl Modular 3D LC System x r Selected Modules GPIB Instrument Name System 2 Initially Start Instrument Session C Yes C No OK Cancel Help Initial Screen Window Size Normal C Ic C Full scre Device Address Cancel Help Identify by Host Name iene Modular 3D LC m Modules IP Address fi 34 40 27 95 C GPIB LAN Cancel Help 1100 Modular System Ln a GPIB Address 1100 System Access i i CR rm Selected Modules 1100 System Delete 1100 System Access IP 134 40 27 95 Cancel Help Figure 33 Changing the TCP IP settings of the Agilent ChemStation 72 1200 Series DAD and MWD Service Manual LAN Configuration 4 2 Adda TCP IP connection to communicate with the detector Use the IP address of the detector If using a corporate LAN IP addresses need to be supplied by the responsible IT department Also the LAN needs to be able to handle additional traffic 3 Save the configuration close the Configuration Editor and start the Agilent ChemStation 1200 Series DAD and MWD Service Manual 73 4 LAN Configuration 74 1200 Series DAD and
145. irements 26 slit test 164 slit width 30 115 specifications analog signal output 31 communications 31 control and data evaluation 31 diode width 30 flow cell 30 GLP features 31 linear range 30 noise and drift ASTM 30 performance 30 physical 29 programmable slit width 30 safety and maintenance 31 wavelength accuracy 30 wavelength bunching 30 wavelength range 30 spectra acquisition 118 settings 99 396 spectral flatness test 172 spectrograph 18 diodes pernm 18 stack configuration 36 38 front view 36 rear view 38 standard flow cell dimensions 110 parts 307 storing the settings permanently 61 T TCP IP parameter configuration 49 telnet commands 64 configuration 63 temperature control 362 temperature control principle 192 test chromatogram 178 Agilent ChemStation 179 Control Module 180 test functions 126 tests ASTM noise ChemStation only 173 dark current 165 filter 162 flow cell ChemStation only 174 holmium oxide 169 247 intensity 167 overview 184 slit 164 spectral flatness ChemStation only 172 test chromatogram 178 time constant versus response time 32 time table 86 troubleshooting error messages 126 132 status indicators 126 127 Tungsten lamp voltage control 362 U union holder ZDV parts 339 unpacking 34 USB 364 uv radiation 388 V variable entrance slit 18 verification and recalibration of wavelength 176
146. ise is reduced by a factor of approximately 2 5 whereas the signal is about 75 of a 4 nm wide band The signal to noise ratio for a 30 nm bandwidth is twice that for a 4 nm bandwidth in our example Bandwidth 30 nm 12 nm 4nm Figure 58 Influence of Bandwidth on Signal and Noise Because the detector averages absorbance values that are calculated for each wavelength using a wide bandwidth does not negatively impact linearity The use of a reference wavelength is highly recommended to further reduce baseline drift and wander induced by room temperature fluctuations or refractive index changes during a gradient An example of the reduction of baseline drifts is shown in Figure 59 for PTH amino acids Without a reference wavelength the chromatogram drifts downwards due to refractive index changes induced by the gradient This is almost completely eliminated by using a reference wavelength With this technique PTH amino acids can be quantified in the low picomole range even in a gradient analysis 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 Lud a og e 1 pmol each I cc J q T Gn a a EE a Wavelength 267 nm Reference 380 nm Wavelength 267 nm No reference Time min Grad 0 02 m KH2P04 ACN from 12 ACN to 45 ACN in 12 min Figure 59 Gradient Analysis of PTH Amino Acids 1 pmol each with and without Refer ence Slit Width The detector has a variable sl
147. it at the entrance of the spectrograph This is an effective tool to adapt the detector to changing demand of different analytical problems A narrow slit provides spectral resolution for analytes with very fine structures in the absorbance spectrum An example of such a spectrum is benzene The five main absorbance bands fingers are only 2 5 nm wide and just 6 nm apart from each other 1200 Series DAD and MWD Service Manual 115 6 How to optimize the Detector Figure 60 Benzene at 1 4 and 16 nm slit width A wide slit uses more of the light shining through the flow cell This gives lower baseline noise as shown in Figure 61 DAD1 A Sig 254 4 Ref off NOISEVINMANM D maAU A o Slit width 1 nm 0 2 0 4 T T T T T T T 41 15 2 25 3 35 min DAD1 A Sig 254 4 Ref off NOISEVINM4NM D mAU Slit width 4 nm 02 0 4 T T T T T T T 0 5 4 15 2 25 3 35 mit DAD1 A Sig 254 4 Ref off NOISE INMIGNM D mAU o Slit width 16 nm as 0 4 eee SS 05 4 15 Zz 25 3 35 mir Figure 61 Influence of the Slit Width on Baseline Noise However with a wider slit the spectrograph s optical resolution its ability to distinguish between different wavelengths diminishes Any photodiode receives light within a range of wavelength determined by the slit width This explains why the fine spectral structure of benzene disappears when using a 16 nm wide slit 116 1200 Series DAD and MWD Service Manua
148. ium Oxide Test on page 247 to check the correct positioning of the flow cell 226 1200 Series DAD and MWD Service Manual Maintenance 12 Replacing Capillaries on a Semi Micro Micro and High Pressure Flow Cell When required If the capillary is blocked Tools required Two 1 4 inch wrenches for capillary connections Wrench 4 mm for capillary connections Screwdriver Pozi 1 PT3 Parts required For parts see Semi Micro Flow Cell on page 309 Micro Flow Cell on page 311 or High Pressure Flow Cell on page 313 Preparations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column The fittings at the flow cell body are special types for low dead volumes and not compatible with other fittings When retightening the fittings make sure that they are carefully tightened handtight plus 1 4 turn with a wrench Otherwise damage of the flow cell body or blockage may result 1200 Series DAD and MWD Service Manual 227 12 Maintenance 1 Identify the inlet and outlet capillaries Inlet capillary Outlet capillary 2 After replacing the outlet cap
149. ization Specifying a signal ratio that is typical for the sample class is one way of selectively plotting only those peaks that are of interest The signal output remains at zero so long as the ratio is out of the user specified ratio range When the ratio falls within the range the signal output corresponds to the normal absorbance giving single clear peaks on a flat baseline An example is shown in Figure 64 and Figure 65 122 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 Select 2 characteristic wavelengths Signal WL1 WL2 20 o Terphenyl Biphenyl WL2 WL1 Scaled Wavelength nm Figure 64 Wavelength Selection for Ratio Qualifiers Signals at 250 nm Biphenyl o Terphenyl No selectivity With ratio qualifier 250 222 nm 3 5 20 Time min Figure 65 Selectivity by Ratio Qualifiers In a four component mixture only biphenyl was recorded The other three peaks were suppressed because they did not meet the ratio qualifier criterion and therefore the output was set to zero The characteristic wavelengths 249 nm A and 224 nm Ag were found from the spectra shown in Figure 64 1200 Series DAD and MWD Service Manual 123 6 124 How to optimize the Detector The ratio range was set at 2 2 4 2 2 10 Only when the ratio between 249 and 224 nm was within this range is the signal plotted Of all four peaks only the third fulfilled the criterion Figure 65 The others
150. k through auto negotiation you can manually set the link operating mode using link configuration switches on the detector Link Configuration Switches SW3 SW4 SW5 Link Configuration OFF speed and duplex mode determined by auto negotiation ON 1 2 l l l I I ON OFF OFF manually set to 10 Mbps half duplex ON OFF ON manually set to 10 Mbps full duplex E ee ee R ON ON OFF manually set to 100 Mbps half duplex ON ON ON manually set to 100 Mbps full duplex 1200 Series DAD and MWD Service Manual 55 4 LAN Configuration Automatic configuration with Bootp When automatic configuration with Bootp is selected and the LAN interface is powered on it broadcasts a BOOTP Bootstrap Protocol request that contains its MAC hardware address A BOOTP server daemon searches its database for a matching MAC address and if successful sends the corresponding configuration parameters to the detector as a BOOTP reply These parameters become the active TCP IP parameters immediately and the TCP IP connection can be established Configuring the Agilent Bootp service program All examples shown in this chapter will not work in your environment You need your own IP Subnet Mask and Gateway addresses Assure that the detector configuration switch is set properly The setting should be either Bootp or Bootp amp Store see Table 6 on page 51 Assure that the detector connected to the network is powered off If the Agilen
151. l How to optimize the Detector 6 Furthermore the absorbance is no longer strictly linear with concentration for wavelengths at a steep slope of a compound s spectrum Substances with fine structures and steep slopes like benzene are very rare In most cases the width of absorbance bands in the spectrum is more like 30 nm as with anisic acid see Figure 57 In most situations a slit width of 4 nm will give the best results Use a narrow slit 1 or 2 nm if you want to identify compounds with fine spectral structures or if you need to quantify at high concentrations gt 1000 mAU with a wavelength at the slope of the spectrum Signals with a wide bandwidth can be used to reduce baseline noise Because digital bandwidth is computed as average of absorbance there is no impact on linearity Use a wide 8 or 16 nm slit when your sample contains very small concentrations Always use signals with bandwidth at least as wide as the slit width 1200 Series DAD and MWD Service Manual 117 6 How to optimize the Detector Optimizing Spectral Acquisition DAD only Storage of all spectra consumes a lot of disk space It is very useful to have all spectra available during optimization of a method or when analyzing unique samples However when running many samples of the same type the large size of data files with all spectra may become a burden The detector provides functions to reduce the amount of data yet retaining the relevant sp
152. l Product number firmware revision manufacturing date of intsrument or if replaced of main board serial number accumulated on time spectrometer serial number Vis lamp Accumulated on time actual on time lamp switch on accumulated on time switches switch on voltage current lamp current lamp voltage current UV lamp Accumulated on time actual on time lamp ignitions Holmium Filter Flow Cell Micro Slit accumulated on time reset ignition voltage current lamp voltage lamp voltage current Available with ID tag lamp only product number serial number production date last intensity test Filter movements filter moves reset log Available with ID tag flow cells only Product number production date pathlength max pressure serial number volume last cell test Slit movements filter moves reset log 1200 Series DAD and MWD Service Manual 181 9 Test Functions Diode Array Detector UY Lamp Details of UV lamp Accum UV On Time 179 83h Accum On Time Reset Show with RFID tag UV Lamp On Time 0 00h Ignition Voltage Current Show Number of Ignitions 70 UV Lamp Voltage __ Show Product Number 2140 0820 UV Lamp Volt Current Show Serial Number 213913 Last Intensity Test 02 01 2006 Production Date 08 10 2004 Copyto Memo Pad Send Changes Cancel Changes Diode Array Detector Cell Details of flow cell with RFID tag Product Number G1315 60022 Serial Numbe
153. lamp emits light over the 190 nm to approximately 800 nm wavelength range The light source for the visible and SWNIR wavelength range is a low noise tungsten lamp This lamp emits light over the wavelength range 470 950 nm The achromat receives the light from both lamps and focuses it so that the beam passes through the flow cell The holmium oxide filter is electromechanically actuated During the holmium filter test it moves into the light path The cell support window assembly separates the holmium filter area from the flow cell area The optical unit has a flow cell compartment for easy access to flow cells A variety of optional flow cells can be inserted using the same quick simple mounting system The flow cell can be removed to check the optical and electronic performance of the detector without having influences from the flow cell The spectrograph material is ceramic to reduce thermal effects to a minimum The spectrograph consists of the spectrograph lens the variable entrance slit the grating and the photodiode array with front end electronics The spectrograph lens refocuses the light beam after it has passed through the flow cell The sampling interval of the diode array is lt 1 nm over the wavelength range 190 950 nm Depending on the wavelength this varies from 1 0 to 1 25 diodes per nanometer for example a diode every 0 8 to 1 nm For a small wavelength range the small non linearity could be neglected With the
154. ling System Parts When required If the parts are corroded or broken Tools required None Parts required Leak funnel 5061 3388 Leak funnel holder 5041 8389 Leak tubing 120 mm 0890 1711 Preparations Remove the front cover 1 Pull the leak funnel out of the leak funnel holder 2 Pull out the leak funnel with the tubing 3 Insert the leak funnel with the tubing in its position 4 Insert the leak funnel into the leak funnel holder Leak funnel and holder Leak tubing Figure 92 Replacing Leak Handling System Parts 5 Replace the front cover 240 1200 Series DAD and MWD Service Manual Maintenance 12 Replacing the CompactFlash Card G1315C G1365C only When required If defective Tools required None Parts required CompactFlash Card Kit 01100 68700 Preparations Turn the detector OFF and have access to the rear of the detector The G1315C DAD SL and G1365C MWD SL is equipped with a CompactFlash card This CompactFlash card is required for the operation of the detector data buffering DO NOT use other types of CompactFlash cards Only CompactFlash cards supplied with the detector or as replacement with above part number are tested with the detector 1 Remove the CompactFlash card by pulling it out of its slot in the rear of the detector 2 Install the new CompactFlash card into the slot 3 Turn the detector ON Figure 93 Replacing SanDisk CompactFlash card 1200 Series DAD and MWD Service Ma
155. lmium oxide test see Holmium Oxide Test on page 247 provides verification of wavelength accuracy at three additional wavelengths 1200 Series DAD and MWD Service Manual Maintenance 12 Holmium Oxide Test The holmium oxide test uses three characteristic absorbance maxima of the built in holmium oxide filter to verify wavelength accuracy see also Wavelength Verification and Recalibration on page 246 When the test is started the 1 nm slit is moved into the light path automatically To eliminate effects due to absorbing solvents the test should be done with water in the flow cell See also Declaration of Conformity for HOX2 Filter on page 391 Holmium Oxide Test Evaluation Limits 361 0 nm 360 0 362 0 nm 1nm 453 7 nm 452 7 454 7 nm 1nm 536 7 nm 535 7 537 7 nm 1nm The test is evaluated by the instrument and the measured maxima are displayed automatically The test fails if one or more of the maxima lies outside of the limits see Figure 96 on page 248 The evaluation report is only on the Agilent ChemStation available Test Failed Probable Causes e Absorbing solvent or air bubble in flow cell Incorrect calibration e Dirty or contaminated flow cell e Dirty or contaminated optical components achromat windows e Old or non Agilent lamp 1200 Series DAD and MWD Service Manual 247 12 Maintenance Suggested Actions Y Ensure the flow cell is filled with water Y Recalibr
156. m pressure If you want to replace flow cell parts see Maintenance of Standard Semi Micro or Micro Flow Cell on page 214 or Maintenance of High Pressure Flow Cell on page 219 7 Insert the flow cell capillaries into the union holder top is Note inlet bottom is outlet Tighten the thumb screw and To check for leaks establish a flow and observe the Reconnect the waste tubing bottom to the union flow cell outside of the cell compartment and all capillary connections inlet y i outlet y waste thumbscrew Next steps 8 Performa Wavelength Verification and Recalibration on page 246 or Holmium Oxide Test on page 247 to check the correct positioning of the flow cell 9 Replace the front cover 1200 Series DAD and MWD Service Manual 213 12 Maintenance Maintenance of Standard Semi Micro or Micro Flow Cell When required If the flow cell needs repair due to leaks or contaminations reduced light throughput Tools required Two 1 4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks Parts required For parts see Standard Flow Cell on page 307 Semi Micro Flow Cell on page 309 or Micro Flow Cell on page 311 Preparations Turn the flow off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 The gaskets used in the standard and semi micro micro flow cell
157. may be hot If so wait five minutes until lamp cools down 1 Remove both lamps see Exchanging a Lamp on page 209 Use the 1 5 mm hex key to loosen the setscrew that secures the lens assembly 254 1200 Series DAD and MWD Service Manual Repairs 13 3 Carefully slide the lens assembly to the right into the deuterium lamp area by pushing it from the tungsten lamp side with the hex key 4 Remove the lens assembly completely 5 The assembly may be disassembled using a pair of pliers to remove the retainer ring 6 The lens may be cleaned or the complete assembly must be exchanged Retainer ring Washer i A __ Lens support S 1200 Series DAD and MWD Service Manual 255 13 Repairs 7 Insert the rebuilt or new lens assembly and slide it into its 8 Align the lens assembly with the wall of the deuterium holder lamp area Fix the setscrew that secures the lens assembly Next steps 9 Replace both lamps 10 Perform an intensity test to check the proper function 11 Replace the front cover 256 1200 Series DAD and MWD Service Manual Repairs 13 Cleaning or Replacing Cell Support Window When required Tools required Parts required Preparations This window is located between the holmium oxide filter and the flow cell It may be replaced when the transmission of light is reduced and a lamp exchange or a wind
158. mbly G1315 60003 Preparations Turn off the lamp e Switch off the detector and disconnect the cables and capillaries e Remove detector from stack and place it on the working bench e Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 1 Disconnect the temperature sensor connector from the 2 The temperature sensor is clipped into the foam behind the optical main board T a ee ae Ty 276 1200 Series DAD and MWD Service Manual Repairs 13 3 Insert the temperature sensor and reconnect it to the main board see figure below for location Next Steps Reinstall the top foam section top cover and front cover see Replacing the Foam and the Top Cover on page 299 Replace the detector into the stack Reconnect cables capillaries and turn on detector 1200 Series DAD and MWD Service Manual 277 13 Repairs Replacing the Tag Reader Lamp When required If defective Tools required Screwdriver POZI 1 PT3 hexagonal key 2 5 mm Parts required Tag reader assembly lamp G1315 60006 Preparations Turn off the lamp Switch off the detector and disconnect the power cable Remove detector from stack and place it on working bench Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 two screws nea
159. mbly onto the new or cleaned quartz window 7 Insert a new gasket 6 7 and the window assembly 1 into the cell body Assure that the gasket is on the bottom Do not mix the gasket 6 and 7 different hole diameter 8 Using a 4 mm hex key tighten the window screw hand tight plus a quarter turn 1200 Series DAD and MWD Service Manual 217 12 Maintenance Next steps 9 Reconnect the capillaries see Exchanging a Flow Cell on page 211 10 Perform a leak test 11 Insert the flow cell 12 Replace the front cover 13 Perform a Wavelength Verification and Recalibration on page 246 or a Holmium Oxide Test on page 247 to check the correct positioning of the flow cell 218 1200 Series DAD and MWD Service Manual Maintenance 12 Maintenance of High Pressure Flow Cell When required Tools required Parts required Preparations If the flow cell needs repair due to leaks or contaminations reduced light throughput Two 1 4 inch wrenches for capillary connections hexagonal key 4 mm Tooth picks For parts see High Pressure Flow Cell on page 313 Turn the flow off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have bot
160. ment may still be charged even though 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 When working with solvents please observe appropriate safety procedures e g goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 1200 Series DAD and MWD Service Manual 383 A Appendix Safety Symbols Table 62 shows safety symbols used on the instrument and in the manuals Table 62 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage g Indicates dangerous voltages Indicates a protected ground terminal a Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in I this product WARNING A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met CAUTION A caution alerts you to situations that co
161. meters obtained become the active parameters immediately They are not stored to the non volatile memory of the detector Therefore the parameters are lost with the next power cycle of the detector Bootp Active Server Parameter Figure 10 Bootp Principle Bootp amp Store When Bootp amp Store is selected the parameters obtained from a Bootp Server become the active parameters immediately In addition they are stored to the non volatile memory of the detector Thus after a power cycle they are still available This enables a kind of bootp once configuration of the detector 1200 Series DAD and MWD Service Manual 51 4 52 LAN Configuration Example The user may not want to have a Bootp Server be active in his network all the time But on the other side he may not have any other configuration method than Bootp In this case he starts the Bootp Server temporarily powers on the detector using the initialization mode Bootp amp Store waits for the Bootp cycle to be completed closes the Bootp Server and powers off the detector Then he selects the initialization mode Using Stored and powers on the detector again From now on he is able to establish the TCP IP connection to the detector with the parameters obtained in that single Bootp cycle Bootp Active Server Parameter Non Volatile RAM Stored Parameter Figure 11 Bootp amp Store Principle Use the initialization
162. mp tag not ready and analysis is r Cell Tag disabled ci C use UV lamp anyway e Cell tag for Agilent flow cells with Ce Coll arpney RFID tags If no RFID tag cell is used detector icon will become grey cell tag not ready and analysis is Cancel Help disabled e Help online help PEMA Celtag The detector status shows Cell tag in aan OA VisLamp Off yellow in case the flow cell with the E sreda RFID tag is not inserted The detector MA 2544 360 100 icon is gray and the system is not ready T B 25416 360100 Tc 2108 360 100 Store Sam Bw Ref Bw Figure 46 Detector configuration settings If the flow cell temperature is critical for your chromatography you may set the Temperature Control to off This will lower the optical unit and flow cell temperature by some degree C For more details see Principle of Temperature Control on page 192 1200 Series DAD and MWD Service Manual Using the Detector Online Spectra DAD only 1 To view the online spectra during the run select Online Spectra a Not Ready Information a J l i J l i Figure 47 Online Spectra Window 2 Change the absorbance and wavelength range according your needs 1200 Series DAD and MWD Service Manual 5 93 5 Using the Detector Run Recovery Settings G1315C G1365C only CAUTION For this recovery mode the CompactFlash Card must be
163. mpaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuseholders must be avoided 1200 Series DAD and MWD Service Manual CAUTION Appendix A The operator of this instrument is advised that if the equipment is used in a manner not specified in this manual the protection provided by the equipment may be impaired Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided as much as possible When inevitable this should be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instru
164. mple wavelength band minus the average absorbance of the reference wavelength band Signal A in the detector default method is set to sample 250 100 reference 360 100 that is the average absorbance from 200 300 nm minus the average absorbance from 300 400 nm As all analytes show higher absorbance at 200 300 nm than at 300 400 nm this signal will show you virtually every compound which can be detected by UV absorbance Many compounds show absorbance bands in the spectrum Figure 57 shows the spectrum of anisic acid as an example To optimize for lowest possible detectable concentrations of anisic acid set the sample wavelength to the peak of the absorbance band that is 252 nm and the sample bandwidth to the width of the absorbance band that is 30 nm A reference of 360 100 is adequate Anisic acid does not absorb in this range If you work with high concentrations you may get better linearity above 1 5 AU by setting the sample wavelength to a valley in the spectrum like 225 nm for anisic acid Anisic acid sample wavelength 252 nm Reference bandwidth 100 nm 30 nm bandwidth Absorbance mAU Reference wavelength 360 Wavelength nm Figure 57 Optimization of Wavelength Setting 1200 Series DAD and MWD Service Manual 113 6 114 How to optimize the Detector A wide bandwidth has the advantage of reducing noise by averaging over a wavelength range compared to a 4 nm bandwidth the baseline no
165. n volatile memory or initialized with known default values The initialization mode is selected by the configuration switch see Figure 9 on page 50 1200 Series DAD and MWD Service Manual 49 4 LAN Configuration Configuration Switches The configuration switch can be accessed at the rear of the detector see Figure 9 ON 12 3 4 5 6 7 8 Figure 9 Location of Configuration Switches The detector is shipped with all switches set to OFF as shown above To perform any LAN configuration SW1 and SW2 must be set to OFF Table5 Factory Default Settings Initialization Init Mode Bootp all switches down For details see Bootp on page 51 Link Configuration speed and duplex mode determined by auto negotiation for details see Link configuration selection on page 55 50 1200 Series DAD and MWD Service Manual LAN Configuration 4 Initialization mode selection The following initialization init modes are selectable Table 6 Initialization Mode Switches SW6 SW7 SW8_Init Mode OFF OFF OFF Bootp OFF OFF ON Bootp amp Store ON 1 2 i l i i I l OFF ON OFF Using Stored 3 4 5 6 7 8 OFF ON ON Using Default Bootp When the initialization mode Bootp is selected the detector tries to download the parameters from a Bootp Server The para
166. nd MWD Service Manual 323 14 Parts and Materials for Maintenance Figure 113 Waste Tubing Parts 9 0 This end is 3 pre installed aces Figure 114 Inlet Capillary Column Detector Parts 324 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 15 Parts for Repairs Parts At The Rear Of The Detector 326 Optical Unit Assembly 328 Coupling Lens Assembly 330 Source Lens Achromat Assembly 331 Cell Support Assembly 332 Holmium Oxide Filter 333 Fan Assembly Parts 334 Plastic Parts 335 Leak Parts 336 Foam Parts 337 Power and Status Light Pipes 338 Sheet Metal Kit 339 This chapter provides information on parts for repair ee Agilent Technologies 325 15 Parts for Repairs Parts At The Rear Of The Detector 2 4 HED C REMOTE on ones lone L E 2 C C C C d JC gt om D D a C je c gt xe Mi i CAN CAN Seay USB LAN ZX GONFIG ae A RAS 232 fe f KH AG Oo Z A a A ee fe nr A al ANALOG ANALOG Se as i 3 COMPACT FLASH le gt C c 3 c gt gt gt gt a c G gt C C D i c gt i 4 C C gt C ls c C 2 le a JE Ne N jas My pG gt 5C A
167. nd power the instrument up again the instrument firmware stays in the resident mode It is not operable as a detector It only uses basic functions of the operating system for example for communication In this mode the main firmware can be loaded using update utilities Table 59 Stay Resident Settings Mode Select sw 1 SW 2 SW 3 SW 4 SsW5 SW 6 SW7 SW 8 TEST BOOT 1 1 1 0 0 0 0 0 374 1200 Series DAD and MWD Service Manual Hardware Information 17 Forced Cold Start Settings A forced cold start can be used to bring the module into a defined mode with default parameter settings CAUTION Forced cold start erases all methods and data stored in the non volatile memory Exceptions are diagnose and repair log books which will not be erased If you use the following switch settings and power the instrument up again a forced cold start has been completed Table 60 Forced Cold Start Settings Mode Select sw 1 SW 2 SW 3 SW 4 SW5 SW 6 SW7 SW 8 TEST BOOT 1 1 0 0 0 0 0 1 To return to normal operation set switches back to your default configuration settings 1200 Series DAD and MWD Service Manual 375 17 Hardware Information Firmware Description The firmware of the instrument consists of two independent sections e anon instrument specific section called resident system e an instrument specific section called main system Resident System T
168. ndividual battery 360 1200 Series DAD and MWD Service Manual Hardware Information 17 Firmware For an outline of the firmware see Firmware Description on page 376 Leak Sensor The detector has 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 Fan Drive The operation of the fan is controlled by the main processor and runs with constant revolution The fan produces a sense signal which is derived from the revolution This sense signal is used for diagnostics Analog Signal Outputs There are two independent analog outputs 0 1 V or 0 100 mV full scale For analog cables refer to Analog Cables on page 344 Deuterium Lamp Filament and Current Control Before ignition the deuterium lamp filament control circuit provides a constant voltage of 2 5 VDC to the filament of the deuterium lamp After ignition the filament heating is turned off Then the constant current source of 320 mA at an operating voltage of about 85 VDC for stable operating conditions and light emission of the deuterium lamp If the deuterium lamp failed to ignite the whole sequence is repeated after a wait sequence for cooling down If the deuterium lamp still does not ignite an error message occurs 1200 Series DAD and MWD Service Manual 361 17 Hardware Information Tungsten Lamp Voltage Control The tungsten lamp
169. ng 50 um i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 PEEK coated fused silica capillary Outlet 50 um G1315 87328 alternative includes Outlet capillary 120 mm long 50 um i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 11 Cell Housing 500 nl G1315 27703 12 Cell Seal Assembly 500 nl G1315 87101 13 Quartz Body 500 nl G1315 80001 Sealing Kit includes items 10 12 QTY 2 and 7 QTY 5 G1315 68715 1200 Series DAD and MWD Service Manual 321 14 Parts and Materials for Maintenance Table 37 lists the specific parts for the 80 nl flow cell Table 37 Specific 80 nl Flow Cell Parts Item Description Part Number 80 nl Flow Cell Kit G1315 68716 1 PEEK coated fused silica capillary Inlet 50 pm G1315 87323 pre mounted to cell includes Inlet capillary 400 mm long 50 um i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 PEEK coated fused silica capillary Outlet 50 um G1315 87328 pre mounted to cell includes Outlet capillary 120 mm long 50 um i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 1 PEEK coated fused silica capillary Inlet 25 pm G1315 87313 alternative includes Inlet capillary 200 mm long 25 pm i d with pre fixed ferrules 4 and fittings 3 plus one PEEK Fitting FT 5 2 PEEK coated fused silica capillary Outlet 25 um G1315 87318 alternative incl
170. ng an appropriate reference wavelength Used wavelength settings e Window 1 shows the baseline when a reference wavelength setting of 350 100 would be used window 2 minus window 3 e Window 2 Sample wavelength 250 100 Ref OFF e Window s3 Sample wavelength 350 100 Ref OFF 1200 Series DAD and MWD Service Manual 187 10 Diagnostic Signals Figure 77 Example with regular appearing spikes L 5 i 415 zu zs Figure 78 Example that might generate the impression the pumping system is the source problem 188 1200 Series DAD and MWD Service Manual A z 1 A LI zs st 75 iret ert ARP U z 1 A z5 se 7s irs AHP A z 1 A L zs sa z5 Figure 79 Example of stepping with period gt 2 hours 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 189 10 Diagnostic Signals Wander Drift Problems Due to Temperature Changes Situation The most frequent cause of ambient temperature fluctuations are unstable laboratory air conditioning systems Other causes include direct sunshine or drafts from open doors and windows These temperature changes cause baseline wander which can make reproducible integration of trace level peaks difficult or impossible TDADT A Sige254 10 Reto K14_DADWAD_RSI 00D Dp DADI B Sige254 10 Refeott N UN DATATPZSADSNANDERO1 D ABST amp Temperature R4 DAD WAD NEIGE OF J SADOI A Tempemture NANDATATPZSAOSWAN DERO D f map a 83
171. ng conditions the radio interference limits are still met within the premises 386 1200 Series DAD and MWD Service Manual Appendix A Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB e Sound Pressure Lp lt 70 dB A e At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 1200 Series DAD and MWD Service Manual 387 A Appendix UV Radiation This information is only valid for UV lamps without cover e g 2140 0590 and 2140 0813 Emissions of ultraviolet radiation 200 315 nm from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs Threshold Limit Values according to the American Conference of Governmental Industrial Hygienists Table 63 UV Radiation Limits Exposure day Effective Irradiance 8 hours 0 1 uW cm 10 minutes 5 0 uW cm Typically the radiation values are much smaller than these limits Table 64 UV Radiation Typical Values Position Effective Irradiance Lamp installed 50 cm distance Average 0 016 W cm Lamp installed 50 cm distance Maximum 0 14 W cm 388 1200 Series DAD and MWD Service Manual Appendix A Solvent Information Observe the follow
172. nnector to the detector main board is seated firmly V Exchange heater assembly 1200 Series DAD and MWD Service Manual 155 8 156 Error Information Heater Power At Limit The available power of the heater reached either the upper or lower limit This event is sent only once per run The parameter determines which limit has been hit 0 means upper power limit hit excessive ambient temperature drop 1 means lower power limit hit excessive ambient temperature increase Probable Causes e Ambient conditions have changed too much during the run so that optimum results may not be guaranteed Suggested Actions V Verify that the reproducibility of your results is not affected V Expose the detector to more stable ambient conditions 1200 Series DAD and MWD Service Manual Error Information 8 No Run Data Available In Device G1315C G1365C only In a very rare case the capacity of the CompactFlash Card is not sufficient This could happen for example when the interrupt of LAN communication takes longer and the detector uses special settings e g full data rate at 80 Hz plus full spectra plus all signals during data buffering Probable Causes e CompactFlash Card is full Suggested Actions Y Correct communication problem Y Reduce data rate Method Instrument run started 09 44 46 11 20 05 1200 DAD 1 Power on 10 07 24 11 20 05 1200 DAD 1 UV lamp on 10 07 24 11 20 05 1200 DAD 1 Vis lamp on 10 07 24 11 20 05 1200
173. ns 1200 Series DAD and MWD Service Manual 343 16 Identifying Cables Analog Cables One end of these cables provides a BNC connector to be connected to Agilent 1200 Series modules The other end depends on the instrument to which connection is being made Agilent 1200 to 3390 2 3 Integrators Connector Pin Pin Signal Name 01040 60101 3390 2 3 Agilent 1200 1 Shield Ground 2 Not connected 8 3 Center Signal 2 ees ETNE egy 4 Connected to pin 6 KE ai 5 Shield Analog a i BENA 6 Connected to pin 4 7 Key 8 Not connected 34 1200 Series DAD and MWD Service Manual Identifying Cables 16 Agilent 1200 to 3394 6 Integrators Connector Pin Pin Signal Name 35900 60750 3394 6 Agilent 1200 1 Not connected 2 Shield Analog 3 Center Analog GIN Agilent 1200 to BNC Connector Connector Pin Pin Signal Name 8120 1840 BNC Agilent 1200 Shield Shield Analog Center Center Analog 1200 Series DAD and MWD Service Manual 345 16 Identifying Cables Agilent 1200 to General Purpose Connector Pin Pin Signal Name 01046 60105 3394 6 Agilent 1200 1 Not connected 2 Black Analog 3 Red Analog en ae 346 1200 Series DAD and MWD Service Manual Remote Cables Identifying Cables 16 One end of these cables provides a Agilent Technologies APG Analytical Products
174. nstrument performance indicates maintenance is necessary take note of the values displayed by lamp counters Enter these values or values slightly less than the displayed values 1200 Series DAD and MWD Service Manual Introduction 1 as EMF limits and then reset the EMF counters to zero The next time the EMF counters exceed the new EMF limits the EMF flag will be displayed providing a reminder that maintenance needs to be scheduled 1200 Series DAD and MWD Service Manual 21 1 Introduction Instrument Layout 22 The industrial design of the detector incorporates several innovative features It uses Agilent s E PAC concept for the packaging of electronics and mechanical assemblies This concept is based upon the use of expanded polypropylene EPP layers of foam plastic spacers in which the mechanical and electronic boards components of the detector are placed This pack is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are e virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly e the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations e the plastic layers help cushion the electronic and mechanical parts from physical shock and e the metal inner cabinet shields the internal electronics from
175. nt showing the not ready condition Suggested Actions V Ensure the instrument showing the not ready condition is installed correctly and is set up correctly for analysis V Exchange the remote cable V Check the instrument for defects refer to the instrument s reference documentation 1200 Series DAD and MWD Service Manual 135 8 Error Information Synchronization Lost During an analysis the internal synchronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration If one or more of the modules is no longer recognized as being connected to the system the error message is generated Probable Causes e CAN cable disconnected e Defective CAN cable e Defective main board in another module Suggested Actions V Ensure all the CAN cables are connected correctly V Switch off the system Restart the system and determine which module or modules are not recognized by the system 136 1200 Series DAD and MWD Service Manual Error Information 8 Leak A leak was detected in the detector The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the detector
176. ntenance feedback 20 introduction 201 overview 208 parts 303 manual configuration of LAN 62 of LAN with handheld controller 68 message compensation sensor open 139 compensation sensor short 139 cover violation 142 diode current leakage 147 fan failed 140 holmium oxide test failed 148 ignition without cover 141 leak 137 leak sensor open 138 leak sensor short 138 remote timeout 135 394 shutdown 134 synchronization lost 136 time out 133 uv heater current 152 uv ignition failed 151 uv lamp current 149 uv lamp voltage 150 visible lamp current 143 visible lamp voltage 144 wavelength calibration failed 145 nano flow cells dimensions 110 parts 319 negative absorbance 119 noise and drift ASTM 30 0 operating altitude 29 operation temperature 29 optical unit parts 328 optimization choosing a flow cell 108 detector performance 106 for sensitivity selectivity linearity dispersion 109 how to get the best performance 106 margins for negative absorbance 119 of selectivity 120 of the system 80 overview 107 peak width 111 sample and reference wavelength 112 slit width 115 spectra acquisition 118 P parts identification accessory kit 323 achromat source lens 332 at rear of detector 326 cable overview 342 cables 341 cables analog 344 cables APG remote 347 cables auxiliary 354 cables BCD 352 cables CAN 355 cables
177. nterface The PCMICIA slot has been removed from all detectors in November 2006 with the introduction of the G1315D DAD and G1365D MWD Follow the procedure below when installing a main board of the G1315C DAD SL or G1365C MWD SL with a PCMCIA interface into a detector that does not have the slit in the cabinet 1 Place the main board on the ESD protection kit 2 Locate the two screws that fix the PCMCIA interface on the board unscrew 5 lt i By nN a cut Figure 100 Removing the PCMCIA Interface 3 Unscrew the two screws 1 5 mm hexagonal key from the opposite side of the board 4 Carefully remove the metal part of the PCMCIA interface Using a wire cutting pliers cut the thin metal part from the black rear 272 1200 Series DAD and MWD Service Manual Replacing Fan Parts When required Tools required Parts required Preparations Repairs 13 If the fan is defective or noisy or the heater fails Screwdriver POZI 1 PT3 a pair of pliers Fan assembly 3160 1016 heater assembly G1315 60013 Turn off the lamp e Switch off the detector and disconnect the cables and capillaries Remove detector from stack and place it on the working bench e Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 out of its location 1 Disconnect the connectors from the m
178. nual 241 12 Replacing the Detector s Firmware 242 When required If new version solves problems of currently installed version or after exchange of the detector main board DADM or MWDM the version on board is older than previous installed one Tools required LAN RS 232 Firmware Update Tool or Instant Pilot G4208A or Control Module G1323B Parts required Firmware tools and documentation from Agilent web site Preparations Read update documentation provided with the Firmware Update Tool The installation of older firmware might be necessary e to keep all systems on the same validated revision or e if third part control software requires a special version To upgrade downgrade the detector s firmware the following steps have to be performed 1 Download the module s firmware the LAN RS 232 FW Update Tool Version 2 4 or above and the documentation from the Agilent web http www chem agilent com scripts cag_firmware asp 2 Load the firmware into the detector as described in the documentation The initial firmware revision of the G1315C DAD and the G1365C MWD is B 01 01 main and resident No further downgrade is possible The initial firmware revision of the G1315D DAD and the G1365D MWD is B 01 04 main and resident No further downgrade is possible When using the G1315C D and G1365C D in a system all other modules must be upgraded to firmware revision 6 x or above main and resident Otherwise the communication
179. o Dark Current Yes Yes D No C via command M section Maintenance D section Diagnose The Agilent Control Module G1323B does not do any calculations So there will be no reports generated with passed failed information 1200 Series DAD and MWD Service Manual 129 7 Troubleshooting and Diagnostics Agilent LC Diagnostic Software 130 The Agilent LC diagnostic software is an application independent tool that provides troubleshooting capabilities for the Agilent 1200 Series modules It provides for all 1200 Series LC the possibility of a first guided diagnostic for typical HPLC symptoms and a status report stored as Adobe Acrobat pdf or as a printable file to assist users evaluating the instrument state At the introduction following modules will be fully supported by the software including module tests and calibrations as well as injector steps and maintenance positions e Agilent 1200 Series binary pump SL G1312B e Agilent 1200 Series high performance autosampler SL G1367B e Agilent 1200 Series thermostatted column compartment SL G1316B e Agilent 1200 Series diode array detector SL G1315C With further releases of the diagnostic software all Agilent 1200 Series HPLC modules will be fully supported This diagnostic software provides tests and diagnostic features that may differ from the descriptions in this manual For details refer to the help files provided with the diagnostic software 1200 Series DAD and MWD
180. o change the Output Range of the analog outputs see Control Settings on page 91 1 To change the offset and the attenuation select Analog Outputs 2 Change the ranges for absorbance and wavelength according your needs DAD Analog Outputs System 2 xj 5 Set up Pump Set up Injector Set up Column Thermostat Set up DAD Signals More Pump More Injector More Column Thermostat More DAD Analog Outp Control Configuration Run Recovery Output 1 Output 2 Zero Offset E 5 Attenuation 1000 m u 1000 mAU x System On Zero Offset Limits 1 to 99 in steps of 1 System OFF Attenuation Limits 0 98 to 2000 mAU at discrete values for either 100 mV or 1 V full scale Revisions amp Serial s Columns Configure 1100 1200 Access Figure 49 Analog Output Settings 3 Change the values if required es DAD and MWD Service Manual 97 5 Using the Detector Spectrum Settings DAD only To change the Spectra settings open 1 To change the Spectra settings select Setup Detector Signals 2 In the section Spectrum click on the drop down list and chose a parameter Table 15 on page 99 shows the possible parameters 3 Change the Range Step width and Threshold according to your needs Set up DAD Signals DAD Signals System 2 DAD Signals System 2 ag Control m Signals Signals ai Configuration
181. of a narrow peak of interest in your chromatogram Setting wavelength and bandwidth Sample wavelength Never miss a peak by the use of a browser wavelength like 250 nm with 100 nm bandwidth Select specific wavelength with reduced bandwidth if you need selectivity e g 250 10 nm and 360 100 nm as reference wavelength Set the sample wavelength to a peak or valley in the spectrum to get best linearity for high concentrations Reference wavelength Select the reference wavelength with broad bandwidth 30 100 nm wavelength range where your analytes have little or no absorbance e g sample at 254 nm reference at 320 nm peak resolution versus sensitivity chromatographic resolution peak resolution versus sensitivity versus disk space sensitivity versus selectivity sensitivity versus linearity baseline drift due to RI effects 1200 Series DAD and MWD Service Manual 107 6 How to optimize the Detector Table 17 Optimization Overview continued Parameter Impact 5 Setting the slit width Use 4 nm slit for normal applications spectral resolution sensitivity and Use narrow slit e g 1 nm if your analytes have narrow absorbance linearity bands and for high concentrations Use a wide slit e g 16 nm to detect very low concentrations Optimizing spectral acquisition DAD only Select spectra acquisition mode according to your needs see Spectrum Set
182. of lamp life This may only be observed when operating at very sensitive detection levels see Figure 77 to Figure 79 Without or with inappropriate reference wavelength such lamp instabilities show up as baseline problems even earlier and stronger Lamp instabilities come in many different forms The period may vary from a few seconds to hours Some extreme examples are shown in Figure 77 to Figure 79 Problem Verification If an 1200 Series DAD or MWD shows baseline problems the following steps to diagnose whether the lamp is the cause of the baseline instability 1 Ensure that the detector has been properly optimized see next page 2 Take the flow cell out of the detector to remove any influence of the flow system If the baseline continues to show the problem the lamp should be replaced 1200 Series DAD and MWD Service Manual 185 10 Diagnostic Signals If the baseline is stable without cell inserted look for other possible causes of the problem for example dirty flow cell column sampler pump etc Solution Replace the lamp after problem verification Table 24 Deuterium lamps used in 1200 series DAD MWD detectors Part Number Description usable in 2140 0820 long life deuterium lamp with RFID tag G1315A B C D G1365A B C D black cover G1314A B C see note below RFID tag info used in G1315C D and G1365C D only 2140 0813 long life deuterium lamp G1315A B C D G1365A B C D G1314A B C see note below 5
183. omponents see Using the ESD Strap on page 205 1 Use a5 mm wrench to unscrew the REMOTE and the RS 232 nuts 2 Use a 15 mm wrench to unscrew the nuts of the ANALOG connectors 3 Unscrew the screw left of the Compact Flash Card slot 1200 Series DAD and MWD Service Manual 263 13 Repairs aC JC CAN E COMPACT FLASH D Figure 98 Unscrew nuts and screws 4 Disconnect all connectors from the detector main board When removing connectors counter hold with one hand on connector J13 5 Remove the detector main board Place the board on the ESD kit 6 On the new board check the switch setting of address switch S1 see Setting the 8 bit Configuration Switch on page 372 An incorrect switch setting for example TEST BOOT may cause the module to turn in a basic mode yellow or red flashing status light In such a case turn off the module reset the address switches and turn on the module again The PCMCIA interface has been removed on all detectors with the introduction of the G1315D DAD and G1365D MWD Main boards for the G1315C DAD SL and G1365C MWD SL may still have the interface If used for replacements in a detector without the opening in the cabinet refer to R
184. on corresponds to the information in Figure 23 on page 65 Init Mode Bootp Server 134 40 29 56 Figure 29 Diode Array and Multiple Wavelength Detector Status Page In Figure 30 on page 69 the complete listing is shown For explanations refer to Figure 23 on page 65 LAN Status Page MAC Address 0030d30A080B Init Mode Bootp Bootp Server 134 40 29 56 TCP IP Properties active IP Address 134 40 25 220 Subnet Mask 255 255 248 0 Def Gateway 0 0 0 0 stored IP Address 134 40 25 220 Subnet Mask 255 255 248 0 Def Gateway 134 40 24 1 Controllers no connections Figure 30 LAN interface Status Page complete 1200 Series DAD and MWD Service Manual 69 4 LAN Configuration 5 To change the TCP IP settings press F1 Service IP Address KEZ 40 25 220 Subnet Mask 255 255 248 0 Default Gateway 134 40 24 1 6 Move to the parameter you want to change enter the new value and press Enter 7 If you completed your changes press Done to leave the Service section 8 Press F6 Done and restart the module by pressing OK The module is going to be restarted The control module will be rebooted too Do you want to proceed SC ae Figure 31 Re boot screen 70 1200 Series DAD and MWD Service Manual LAN Configuration 4 PC and Agilent ChemStation Setup PC Setup for Local Configuration This procedure describes
185. ons V Ensure the lamps are switched on V Ensure the flow cell is inserted correctly and is free from contamination cell windows buffers etc Y Exchange the filter assembly V Exchange the achromat assembly Y Exchange the optical unit 1200 Series DAD and MWD Service Manual Error Information 8 UV Lamp Current The UV lamp current is missing The processor continually monitors the anode current drawn by the lamp during operation If the anode current falls below the lower current limit the error message is generated Probable Causes e UV lamp disconnected e Defective UV lamp or non Agilent lamp e Defective detector main board e Defective power supply Suggested Actions V Ensure the UV lamp connector is seated firmly V Exchange the UV lamp V Exchange the detector main board V Exchange the power supply 1200 Series DAD and MWD Service Manual 149 8 150 Error Information UV Lamp Voltage The UV lamp anode voltage is missing The processor continually monitors the anode voltage across the lamp during operation If the anode voltage falls below the lower limit the error message is generated Probable Causes e Defective UV lamp or non Agilent lamp e Defective detector main board e Defective power supply Suggested Actions V Exchange the UV lamp V Exchange the detector main board V Exchange the power supply 1200 Series DAD and MWD Service Manual Error Information 8 UV Ignition F
186. or Description PCMCIA has been removed OPTICAL connects to optical unit LAN connects to LAN interface ID CELL connects to ID reader of flow cell USB for future use FAN connects to the fan REMOTE remote control TEMP connects to temperature sensor CAN inter module communication HEATER connects to heater ANALOG signal to plotter or data system HOLM connects to stepper motor PWS connects to power supply ID LAMP connects to ID reader of UV lamp LEAK connects to leak sensor 1200 Series DAD and MWD Service Manual Interfaces Hardware Information 17 The Agilent 1200 Series modules provide the following interfaces Table 55 Agilent 1200 Series Interfaces Interface Type Pumps Autosampler DA Detector DA Detector VW Detector Thermostatted Vacuum MW Detector G1315C D RI Detector Column Degasser FL Detector MW Detector Compartment G1365C D CAN Yes Yes Yes Yes Yes Yes No LAN on board No No No Yes No No No GPIB Yes Yes Yes No Yes Yes No RS 232C Yes Yes Yes Yes Yes Yes No Remote Yes Yes Yes Yes Yes Yes Yes Analog Yes No 2x 2x 1x No Yes Interface board Yes Yes Yes No Yes No No LAN BCD Ext The vacuum degasser will have a special connector for specific use For details see description of main board e CAN connectors as interface to other Agilent 1200 Series modules e LAN connector as interface to the Agilent ChemStation e GPIB connector as interface to the Agilent ChemStation e RS 232C as interface to a computer e
187. ors Agilent 1200 module to module 0 5 m 5181 1516 Agilent 1200 module to module 1 m 5181 1519 Agilent 1200 module to control module G1323 81600 1200 Series DAD and MWD Service Manual 355 16 Identifying Cables External Contact Cable One end of this cable provides a 15 pin plug to be connected to Agilent 1200 Series module s interface board The other end is for general purpose Agilent 1200 Series Interface Board to general purposes Connector Color Pin Signal Name G1103 61611 Agilent 1200 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 ee ee Red 8 EXT 4 ie _ 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 yellow 15 Not connected 356 1200 Series DAD and MWD Service Manual Identifying Cables 16 RS 232 Cable Kit This kit contains a 9 pin female to 9 pin female Null Modem printer cable and one adapter Use the cable and adapter to connect Aligent Technologies instruments with 9 pin male RS 232 connectors to most PCs or printers Agilent 1200 module to PC RS 232 Cable Kit 34398As Instrument PC RX 2 2 RX TX 3 X 3 TX DTR 4 4 DTR GND 5 gt 5 enD DSR 6 6 DSR RTS 7 7 RTS CTS 8 m 8 CTS RI 9 9 RI DB9 DB9 DB9 DB9 Male Female Female Male 1200 Series DAD and MWD Service Manual 357 16 Identifying Cables LAN Cables
188. overy Settings G1315C G1365C only 94 Analog Output Settings 97 Spectrum Settings DAD only 98 Peakwidth Settings 100 Slit Settings 102 Margin for Negative Absorbance Settings 103 Optimizing the Detector 103 1200 Series DAD and MWD Service Manual Special Setups with Multiple DAD MWDs 104 Two detectors of same type e g G1315C D and G1315C D 104 Two detectors of similar type e g G1315C D and G1315A B 104 6 How to optimize the Detector Optimizing the Detector Performance 106 Optimization Overview 107 Optimizing for Sensitivity Selectivity Linearity and Dispersion 109 Flow Cell Path Length 109 Peak width response time 111 Sample and Reference Wavelength and Bandwidth 112 Slit Width 115 Optimizing Spectral Acquisition DAD only 118 Margin for Negative Absorbance 119 Optimizing Selectivity 120 Quantifying Coeluting Peaks by Peak Suppression 120 Ratio Qualifiers for Selective Detection of Compound Classes 122 7 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 126 Status Indicators 127 Power Supply Indicator 127 Detector Status Indicator 128 User Interfaces 129 Agilent LC Diagnostic Software 130 1200 Series DAD and MWD Service Manual 8 Error Information What Are Error Messages 132 General Error Messages 133 Timeout 133 Shutdown 134 Remote Timeout 135 Synchronization Lost 136 Leak 137 Leak Sensor Open 138 Leak Sensor Short 138 Compensation Sensor Open 13
189. ow cell 211 exchanging alamp 209 exchanging holmium oxide filter 239 exchanging internal parts 252 exchanging leak sensor 294 exchanging main board DAM 263 exchanging power supply 291 exchanging the achromat 283 flow cell rotation limiter 289 installing optical unit 297 introduction 202 of the detector 207 251 removing the optical unit 281 removing top cover and foam 260 replacing cell support window 257 replacing CompactFlash card 241 replacing coupling lens 254 replacing fan parts 273 replacing filter motor 286 replacing firmware 242 replacing foam and top cover 299 replacing leak handling system 240 replacing semi micro flow cell capillaries 227 replacing status light pipe 296 replacing STD flow cell capillaries 222 replacing tag reader flow cell 289 the high pressure flow cell 219 the standard semi micro flow cell 214 using the ESD strap 205 395 Index warnings and cautions 202 response time peak width 111 response time versus time constant 32 RFID 363 RS 232C cable kit to PC 357 communication settings 374 interface 371 Run 94 run recovery automatic 95 manual 96 no run data available in 157 S safety switches 362 sample and reference wavelength 112 selectivity optimization 120 semi micro flow cell dimensions 110 parts 309 sensor parts 334 serial number entered on control module 270 entered on instant pilot 268 sheet metal parts 339 site requ
190. ow cleaning does not improve the light throughput Screwdriver POZI 1 PT3 hexagonal key 1 5 mm Pointed pair of pliers Cell support window 79880 28111 Cell support window assembly G1315 65202 For other parts see Cell Support Assembly on page 332 Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 1 Unscrew the six screws and remove the flow cell cover 2 If not already in this position move the holmium oxide filter down 1200 Series DAD and MWD Service Manual 257 13 Repairs 3 Use the 1 5 mm hex key to loosen the setscrew that 4 Carefully slide the assembly to the right into the flow cell secures the cell support assembly compartment by pushing it from the holmium oxide filter side Remove the cell support assembly completely 6 The assembly may be disassembled using a pair of pliers to remove the retainer ring IN Pd 258 1200 Series DAD and MWD Service Manual Repairs 13 Insert the rebuilt or new assembly and slide it in until it is 7 The window may be cleaned or the complete assembly must be exchanged _ Retainer ring fO E H Washer a S TN C4 Vi f J stopped by the filter lever Next steps 9 Leave slight clearance for movement of the filter lever fix the setscrew between both the lens assembly and the filter lever and 10 Perform a filter t
191. prepare and so on Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements The subminiature D connector is used The module provides one remote connector which is inputs outputs wired or technique To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the system s critical parts in case any module detects a serious problem To detect whether all participating modules are switched on or properly 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 Typical values are TTL high out 2 4V in 2 0V TTL low out 0 4V in 0 8V Depending on the load the values can vary 1200 Series DAD and MWD Service Manual 369 17 370 Hardware Information Table 56 Remote Signal Distribution Pin Signal Description 1 DGND Digital ground 2 PREPARE L Request to prepare for analysis for example calibration detector lamp on Receiver is any module performing pre analysis activities 3 START L Request to start run timetable Receiver is any module performing run tim
192. purpose spade lugs 01046 60105 Remote 3390 integrator 01046 60203 cables 3392 3 integrators 3394 integrator 3396A Series I integrator 3396 Series Il 3395A integrator see page 349 3396 Series Ill 3395B integrator Agilent 1200 1100 1050 modules 1046A FLD 1046A FLD 35900A A D converter 1090 liquid chromatographs Signal distribution module 01046 60206 01046 60210 03394 60600 03396 61010 5061 3378 5061 3378 5061 3378 01046 60202 01046 60202 1200 Series DAD and MWD Service Manual Identifying Cables 16 Table 51 Cables Overview continued Type Description Part Number BCD 3396 integrator 03396 60560 cables General purpose spade Lugs G1351 81600 Auxiliary Agilent 1200 Series vacuum degasser G1322 61600 CAN Agilent 1200 module to module 0 5 m 5181 1516 cables Agilent 1200 module to module 1 m 5181 1519 Agilent 1200 module to control module G1323 81600 External Agilent 1200 Series interface board to general purpose G1103 61611 contacts GPIB Agilent 1200 module to Agilent ChemStation 1 m 10833A cable Agilent 1200 module to Agilent ChemStation 2 m 10833B RS 232 Agilent 1200 module to a computer 34398A cable This kit contains a 9 pin female to 9 pin female Null Modem printer cable and one adapter LAN cable Cross over network cable shielded 3 m long 5023 0203 for point to point connection Twisted pair network cable shielded 7 m long 5023 0202 for hub connectio
193. r 361 Fan Drive 361 Analog Signal Outputs 361 Deuterium Lamp Filament and Current Control 361 Tungsten Lamp Voltage Control 362 Safety Switches 362 Interfaces 362 Temperature Control 362 Internal Clock without Battery 362 Lamp and Flow Cell RFID Tag 363 1200 Series DAD and MWD Service Manual 13 14 A Appendix CompactFlash Card Slot 363 PCMCIA Slot 364 USB 364 Board Layout and Connectors 365 Interfaces 367 Analog Signal Output 368 LAN Interface 368 CAN Interface 368 Remote Interface 369 RS 232C 371 Setting the 8 bit Configuration Switch 372 LAN Settings 374 RS 232C Communication Settings 374 Boot Resident Settings 374 Forced Cold Start Settings 375 Firmware Description 376 Firmware Updates 377 The Main Power Supply Assembly 378 General Safety Information 382 The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 385 Radio Interference 386 Sound Emission 387 UV Radiation 388 Solvent Information 389 Declaration of Conformity for HOX2 Filter 391 Agilent Technologies on Internet 392 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 1 Introduction Introduction to the Detector 16 Optical System 17 Early Maintenance Feedback EMF 20 Instrument Layout 22 Electrical Connections 23 This chapter gives an introduction to the detector instrument overview and internal connectors ee Agilent Technologies
194. r DE515H0876 Production Date 22 09 2005 Path Length 10 mm Volume 13000 nl Max Pressure 120 bar Last Cell Test 22 09 2005 Copy to Memo Pad Send Changes Cancel Changes Figure 76 Diagnosis screen in Agilent ChemStation detailed view 182 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 10 Diagnostic Signals Overview of Diagnostic Signals 184 Baseline problems deriving from deuterium lamps 185 Wander Drift Problems Due to Temperature Changes 190 Internal Board Temperature 199 This chapter describes the detector s built in diagnostic signals ee Agilent Technologies 183 10 Diagnostic Signals Overview of Diagnostic Signals The detector has several signals internal temperatures voltages and currents of lamps that can be used for diagnosing problems These can be e baseline problems deriving from deuterium lamps e wander drift problems due to temperature changes These signals can be used in addition to the normal baseline signal to determine whether correlation to temperature or voltage current of the lamp 184 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 Baseline problems deriving from deuterium lamps Problem Description With the low noise of the 1200 Series Diode Array Detector G1315C D or Multiple Wavelength Detector G1365C D some deuterium lamps may cause periodic baseline instabilities at the end
195. r cable Cross over network cable Twisted pair network cable Flow cell User Manual Accessory kit see Table 4 on page 35 1 1 installed G1315C G1365C only 1 1 1 As ordered 1 1 1200 Series DAD and MWD Service Manual Installing the Detector 3 Detector Accessory Kit Contents Table4 Accessory Kit Contents Description Part Number Quantity Accessory kit G1315 68705 Teflon Tubing flexible i d 0 8 mm flow cell to waste 5062 2462 2m re order 5m Corrugated tubing to waste re order 5 m 5062 2463 1 2m Fitting male PEEK 0100 1516 2 Capillary column detector G1315 87311 1 380 mm long 0 17 mm i d includes Ferrule front 1 16 SST re order pack of 10 5180 4108 2 Ferrule back 1 16 SST re order pack of 10 5180 4114 2 Fitting 1 16 SST re order pack of 10 5061 3303 2 Capillary column cell G1315 87303 1 150 mm long 0 17 mm i d CAN cable 5181 1516 1 Wrench open end 1 4 5 16 inch 8710 0510 1 Wrench open end 4 mm 8710 1534 1 Hex key 4 mm 15 cm long T handle 8710 2392 1 Hex key 1 5 mm 10 cm long straight handle 8710 2393 1 or kit 5062 2418 1 16 Fittings and Ferrules front back 10 PK 1200 Series DAD and MWD Service Manual 35 3 Installing the Detector Optimizing the Stack Configuration If your detector is part of a complete Agilent 1200 Series system you can ensure optimum performance by installing the following configuration This configuration optimizes the system flow p
196. r future enhancements 9 f REMOTE ZIE CD CD CD A c CT D OL JO S555 connie CAN GAN i a USB _LAN OO Lee Bile ANALOG ANALOG Le e a Sa COMPACT FLASH p D TE C SaaS 2 J J Ag gt gt UUUUUUY A Ne L D Figure 127 Rear View of Detector 364 1200 Series DAD and MWD Service Manual Hardware Information 17 Board Layout and Connectors REMOTE ANALOG LAN USB RS 232 CAN CAN 2 1 i IEAI LU PCMCIA CONFIG o See infos on z page 364 PWS a OOO LEAK o O a 000 ze EERO HOLM TEMP ID CELL OPTICAL ID LAMP HEATER FAN Figure 128 Main Board Layout and Connectors 1200 Series DAD and MWD Service Manual 365 17 Hardware Information Table 54 lists the connectors on the main board Table 54 Connections on the main board see Figure 128 on page 365 366 Connector Description Connect
197. r the hydraulic connection 1 Loosen the screw on the left side of the z plane and the 2 Slide the z plane to the front and remove it from the module 278 1200 Series DAD and MWD Service Manual Repairs 13 3 Carefully pull the isolation seal above the UV lamp to the Unscrew the two screws using a 2 5 mm hex key and front to have access to the tag reader the figure shows remove the tag reader assembly the lamps and the isolation seal removed 5 Disconnect the tag reader connector from the mainboard 6 Replace the tag reader assembly and fix the two screws and reconnect the tag reader connector to the mainboard 1200 Series DAD and MWD Service Manual 279 13 Repairs 7 Ensure that the isolation seal fits correctly 8 Install the z plane 9 Fix the screw on the left side of the z plane and the two screws near the hydraulic connection Next steps 10 Reinstall the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 11 Replace the detector into the stack 12 Reconnect the power cable and turn on detector 280 1200 Series DAD and MWD Service Manual Repairs 13 Removing the Optical Unit When required For all repairs inside the optical unit Tools required Screwdriver POZI 1 PT3 Parts required Optical unit G1315 69002 exchange assembly or Individ
198. reboot of the module Using the Agilent ChemStation Module serial numbers are entered by typing specific commands on the command line at the bottom of the main user interface screen 1 To enter a module serial number type the following command into the command line print sendmodule ndad Ser YYYYYYYYYY print sendmodule nmwd ser YYYYYYYYYY Where YYYYYYYYYY is the 10 character serial number of the module in question The first two characters are letters which should be capitalized The reply line will respond with RA 0000 SER followed by the module serial number you just entered 1200 Series DAD and MWD Service Manual 267 13 268 Repairs To change the type of the module use the following command print sendmodule ndad TYPE XXXXX print sendmodule nmwd TYPE XXXXX Where XXXXxX is the 5 character product number of the module e g G1315C To configure the detector as G1315C DAD SL and G1315D DAD requires the correct main board version WARNING If you enter the wrong type your module will not be accessible anymore In such a case see Changing the Product Number and Serial Number on page 267 or Using the Control Module G1323B on page 270 for recovering 2 Turn OFF the module then ON again Then restart the Agilent ChemStation If the serial number you have just entered is different than the original module serial number you will
199. s 9 Fix the three screws at the rear panel 10 Reinstall the top foam section top cover and front cover see Replacing the Foam and the Top Cover on page 299 11 Replace detector into the stack and reconnect the cables and capillaries If a new detector main board is installed update the serial number information of the detector in the user interface see procedure below 12 Check the firmware revision of the module If the firmware revision is older than the current firmware revision of the module update the firmware using the standard firmware update procedure see Replacing the Detector s Firmware on page 242 The initial firmware revision of the G1315C DAD and the G1365C MWD is B 01 01 main and resident No further downgrade is possible The initial firmware revision of the G1315D DAD and the G1365D MWD is B 01 04 main and resident No further downgrade is possible 1200 Series DAD and MWD Service Manual Repairs 13 Changing the Product Number and Serial Number When required If main board has been replaced Tools required User interface Parts required none Preparations Turn the detector on e Start the user interface When the main board has to be replaced the new board does not have a serial number For some modules e g pumps or autosamplers the type has to be changed multiple usage boards Use the information from the serial number plate of your module The changes become active after the
200. scription displays syntax and descriptions of commands displays current LAN settings ip lt X X X X gt sets new ip address sm lt X X X X gt sets new subnet mask gW lt X X X X gt sets new default gateway exit exits shell and saves all changes 4 To change a parameter follows the style parameter value for example ip 134 40 27 230 then press Enter where parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to that parameter Each parameter entry is followed by a carriage return 1200 Series DAD and MWD Service Manual LAN Configuration 4 5 Use the and press Enter to list the current settings EJ C WINDOWS system32 cmd exe telnet 134 40 27 95 gt 7 LAN Status Page information about the LAN interface MAC address initialization mode Initialization mode is Using Stored TCP IP Properties active IP Address 134 40 27 95 l Subnet Mask 255 255 248 0 active TCP IP settings Def Gateway 134 40 24 1 Pict litte drat TCP IP status here ready ha connections connected to PC with controller software e g Agilent ChemStation here not connected Figure 23 Telnet Current settings in Using Stored mode 6 Change the IP address in this example 134 40 27 99 and type to list current settings d exe telnet 134 40 27 95 lt P 134 40 27 99 change of IP setting to LAN Status Page MAC Addr
201. sesses g On line plot window details window Figure 35 Initial ChemStation screen Method and Run Control 1200 Series DAD and MWD Service Manual 81 5 Using the Detector 4 Turn on the detector lamp pump and autosampler by clicking the System On button or the buttons below the module icons on the graphical user interface GUI After some time the pump thermostatted column compartment and detector module will turn to green 2 P Tumen the uv lamp of the DAD Module 7 Ce Evsa 1 1 GB hee coSt8 888388 E Figure 36 Turning on the HPLC Module 82 1200 Series DAD and MWD Service Manual Using the Detector 5 5 Purge the pump For more information see Priming and Purging the System on page 76 6 Allow the detector to warm up of at least 60 minutes to provide a stable baseline see example in Figure 37 and Table 13 For reproducible chromatography the detector and lamp should be on for at least one hour Otherwise the detector baseline may still drift depending on the environment See also section Wander Drift Problems Due to Temperature Changes on page 190 DADI A agrata Remand 100 TER PRAMONO D 2 w a Figure 37 Stabilization of Baseline both lamps turned on at the same time Table 13 Baseline drift after lamp turn on example from Figure 37 Time minutes Drift mAU hr 17 20 2 6 27 30 0 8 37 40 0 4 47 50 0 2 57 60 lt 0 2 1
202. shown here Figure 90 Wrench plus Torque Adapter 235 12 Maintenance Cleaning or Exchanging the Holmium Oxide Filter When required If holmium oxide filter is contaminated Tools required Screwdriver POZI 1 PT3 Screwdriver flat blade Two 1 4 inch wrenches for capillary connections A pair of tweezers Parts required Holmium oxide filter 79880 22711 Preparations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 211 See also Declaration of Conformity for HOX2 Filter on page 391 The glass tends to build a film on its surface even under normal environmental conditions This is a phenomenon which can be found also on the surface of several other glasses and has something to do with the composition of the glass There is no indication that the film has an influence on the measurement Even in the case of a thick film which scatters the light remarkably no shift of the peak positions is to be expected A slight change in the absorbance might be possible Other components within the light path lenses windows are also changing their behavior over the time 236 1200 Series DAD and MWD Service Manual Maintenance 12 1 Unscrew the six screws and remove the flow cell cover 2 If not already in this position move the filter up ee i y 3 While releasing the holder with a screw driver at the top Note carefully remove
203. shows an example where the detector s temperature control has been turned off no regulation The ambient temperature of 25 degree C varies by 2 degree C The baseline is instable Signal 254 4 ref OFF pe a 2 Signal 254 4 360 100 a SRS Board Temperature Optical Temperature Figure 86 Example plot optical unit temperature control OFF 1200 Series DAD and MWD Service Manual 197 10 Diagnostic Signals Figure 87 on page 198 shows an example where the UV lamp is periodically stepping There is no correlation visible on the temperature signals Therefore it is a lamp problem Signals top to bottom baseline 254 4 ref off baseline 254 4 360 100 main board temperature optical unit temperature UV lamp voltage orFwh Figure 87 Example plot Lamp is stepping 198 1200 Series DAD and MWD Service Manual Diagnostic Signals 10 Internal Board Temperature An on board temperature sensor on the detctor main board provides the actual temperature on the board This information is running continuously into a buffer from which it can be retrieved as last 12 hours plot Agilent ChemStation Diagnosis Detector Details view Temperature History BR ode Array Detector Lernmrereture History anita x A AP Ad Vi detector ON sos lamp turned ON detector ON lamp OFF 20 i I MA n ms a E Ah Am TAS
204. sorbing solvent or air bubble in flow cell e Incorrect calibration e Dirty or contaminated flow cell 1200 Series DAD and MWD Service Manual 169 9 Test Functions e Dirty or contaminated optical components achromat windows e Old or non Agilent lamp Suggested Actions Y Ensure the flow cell is filled with water V Recalibrate see Wavelength Verification and Recalibration on page 176 and repeat the test V Run the cell test see Cell Test on page 174 If the test fails exchange the flow cell windows V Clean optical components with alcohol and lint free cloth V Exchange the UV lamp 170 1200 Series DAD and MWD Service Manual Test Functions 9 Instrument G1315 Serial Number PPooooOd2 Operator Wolfgang Date 25 02 2005 Time 14 30 08 Pile C CHEM22 2 DIAGNOSE DAD FILTER2 DGR Holmium Filter Spectrum Holmium Filter Test Results Specification Measured Result Wavelengsh 1 261 0 nz 360 262 nm 360 9 nm Passed Wavelength 2 453 7 nz 452 7 454 7 nm 452 4 nm Passed Wavelength 2 536 7 nm 35 7 537 7 nm 526 8 nm Passed Figure 72 Holmium Oxide Test Results report 1200 Series DAD and MWD Service Manual 171 9 Test Functions Spectral Flatness Test 172 The spectral flatness test determines the maximum noise in mAU on the spectrum The test is run with the flowcell removed to eliminate effects due to absorbing solvent or a dirty flowcell First a detector balance is done Ne
205. spectra acquisition types mentioned above are also referred to as peak controlled spectra acquisition The peak detection is done by the detector firmware based on the threshold and peakwidth parameters you set for the DAD If you want to use peak controlled spectra storage make sure that you set these parameters to recognize all the peaks of interest The integration algorithm also includes peak detection based on the threshold and peakwidth parameters set in the integration events Spectra are taken continuously as for All but only every second spectrum is stored other spectra are discarded This reduces the amount of data storage necessary Spectra are taken continuously depending on the setting of the Peakwidth Eight spectra are acquired per Peakwidth The acquisition time for one spectrum is slightly less than the Peakwidth divided by 8 that is greater than or equal to 0 01s and less than or equal to 2 55s If there are no peaks in Signal A there are no spectra You cannot process spectra present in other signals Range defines the wavelength range for spectral storage Limits 190 to 950 nm in steps of 1 nm for both low and high values The high value must be greater than the low value by at least 2 nm Step defines the wavelength resolution for spectral storage Limits 0 10 to 100 00 nm in steps of 0 1 nm The threshold is the height in mAU of the smallest expected peak The peak detector ignores any peaks which are lower than
206. st i ity in range 221nm 350nm gt 5000 cts 26848 cts Passed Lowest int in range 3S5inm 00nm gt 2000 cts 16593 cts Passed Lowest intensity in range 50lnm 950nm gt 6000 cts 15767 cts Passed Highest intensity in range 190nm 350nm lt 450000 cts 4508 cts Passed Highest intensity in range 700nm 50nm lt 300000 cts 69968 cts Passed Highest intensity for the D2 alpha line lt 1200000 cts 159202 cts Passed Figure 71 Intensity Test Results report 168 1200 Series DAD and MWD Service Manual Test Functions 9 Holmium Oxide Test The holmium oxide test uses three characteristic absorbance maxima of the built in holmium oxide filter to verify wavelength accuracy see also Wavelength Verification and Recalibration on page 176 When the test is started the 1 nm slit is moved into the light path automatically To eliminate effects due to absorbing solvents the test should be done with water in the flow cell See also Declaration of Conformity for HOX2 Filter on page 391 Holmium Oxide Test Evaluation Limits 361 0 nm 360 0 362 0 nm 1nm 453 7 nm 452 7 454 7 nm 1nm 536 7 nm 535 7 537 7 nm 1nm The test is evaluated by the instrument and the measured maxima are displayed automatically The test fails if one or more of the maxima lies outside of the limits see Figure 72 on page 171 The evaluation report is only on the Agilent ChemStation available Test Failed Probable Causes e Ab
207. t Bootp Service program is not already installed on your PC then install it from your Agilent ChemStation CD ROM located in folder Bootp The screens refer to version B 01 0x 56 1200 Series DAD and MWD Service Manual LAN Configuration 4 1 The Agilent Bootp Service is placed in the start up group and automatically is started during the boot process of the PC 2 Open the Bootp Settings window Figure 14 and enter the default settings for your setup Bootp Settings location of LogFile and TabFile Figure 14 Bootp Service Settings 3 Launch the Manager It will open the Bootp Manager screen see Figure 15 This shows all network hardware that has been added initially empty Figure 15 Bootp Manager 1200 Series DAD and MWD Service Manual 57 4 LAN Configuration 4 Select Add to enter the enter the module specific information see Figure 16 MAC address from label on the instrument host name IP address comment instrument name location subnet mask if different gateway if required Figure 16 Bootp Manager Enter your parameter 58 1200 Series DAD and MWD Service Manual LAN Configuration 4 5 Press OK The parameter are added to the Bootp Manager see Figure 16 and added to the TabFile see Figure 14 on page 57 Bootp Manager x Hardware Address HostName IP Address Subnet Mask 003043080838 WADIT171 134 40 27 95 PP024 255 255 248 0 0 0 0 0 Figure 17 Bootp Mana
208. t ChemStation now as well Recover Instructions 1 Turn off the detector 2 Change the 8 bit Configuration Switch to Resident see Boot Resident Settings on page 374 3 Turn the detector on 4 Re do steps 2 to 5 of Changing the Product Number and Serial Number on page 267 and correct the type information Enter the product number without R 5 Turn the detector off 6 Change the 8 bit Configuration Switch back to default settings see Setting the 8 bit Configuration Switch on page 372 7 Turn the detector ON again The Maintenance screen should display the correct type for this module 1200 Series DAD and MWD Service Manual 269 13 270 Repairs Using the Control Module G1323B Connect the control module to the detector Turn ON the detector On the control module press System F5 then Records F4 Using the up down arrows make sure that the detector is highlighted Press FW Update F5 then m This will display a box which says Update Enter Serial Press Enter This will display the box labeled Serial Letters and numbers are created using the up and down arrows Into the box labeled Serial enter the 10 character serial number for the detector When the 10 character serial number is entered press Enter to highlight the complete serial number Then press Done F6 Turn the detector OFF then ON again The Records screen should display the correct serial number for this module
209. tation All OK Run in progress Data Analysis e Run Rawdata Run Elapsed run time is running Spectra counter is running UY Lamp On Vis Lamp On Z Spectra 54 Data are stored on PC and on card V A 2544 360 100 V B 25416 360100 LAN breaks Run in progress Data Analysis eee Fawdsia ME Error Power Fail Elapsed run time stops Spectra counter stops Data continues to be stored on card UV Lamp On Spectra 146 VA 2544 360 100 V B 25416 360 100 Vis Lamp On LAN recovers e Run in progress Data Analysis Run Rawdata Rawdata e Error Power Fail cleared Elapsed run time continues at actual time Spectra counter continues Data continues to be stored ion PC and on card ChemStation tries already to add missing data depends on the data load U Lamp On Z Spectra 290 VA 2544 360 100 V B 25416 360100 Vis Lamp On Stop time elapsed e Run in progress Data Analysis Prerun Rawdata PEM Rawda Elapsed run time stops Spectra counter continues ChemStation continues to ads missing data UV Lamp On IZ Spectra 380 VA 2544 360 100 V B 25416 360100 Vis Lamp On Run ends Ready Run finished kz SM Prerun Ready U Lamp On Vis Lamp On IZ Spectra MA 2544 360 100 V B 25416 360 100 If the detector status window is not opened you will realize only the Power Fail error and the long Run In Progress information until th
210. ted 1200 Series DAD and MWD Service Manual Identifying Cables 16 START and STOP are connected via diodes to pin 3 of the 3394 connector Agilent 1200 to 3396A Integrators Connector Pin Pin Signal Name Active 03394 60600 3394 Agilent 1200 TTL 9 1 White Digital ground O NC 2 Brown Prepare run Low gt J gt 3 3 Gray Start Low NC 4 Blue Shut down Low o NC 5 Pink Not connected i E NC 6 Yellow Power on High Eo 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent 1200 to 3396 Series II 3395A Integrators Use the cable 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready 1200 Series DAD and MWD Service Manual 349 16 Identifying Cables Agilent 1200 to 3396 Series III 3395B Integrators Connector Pin Pin Signal Name Active 03396 61010 33XX Agilent 1200 TTL 9 1 White Digital ground cn NC 2 Brown Prepare run Low i 15 3 3 Gray Start Low NC 4 Blue Shut down Low o NC 5 Pink Not connected i NC 6 Yellow Power on High oe 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent 1200 to HP 1050 HP 1046A or Agilent 35900 A D Converters Connector Pin Pin Signal Name Active 5061 3378 HP 1050 Agilent 1200 TTL 1 White 1
211. temperature sensor delivered a value outside the allowed range The parameter of this event equals the measured temperature in 1 100 centigrade As a result the temperature control is switched off Probable Causes e The sensor is defect e Detector is exposed to illegal ambient conditions Suggested Actions V Ensure the connector to the detector main board is seated firmly Y Verify that the ambient conditions are within the allowed range V Exchange temperature sensor assembly 1200 Series DAD and MWD Service Manual 153 8 154 Error Information Illegal Value From Air Inlet Temperature Sensor This temperature sensor located on the detector main board delivered a value outside the allowed range The parameter of this event equals the measured temperature in 1 100 centigrade As a result the temperature control is switched off Probable Causes e The sensor is defect e Detector is exposed to illegal ambient conditions Suggested Actions V Verify that the ambient conditions are within the allowed range V Exchange detector main board 1200 Series DAD and MWD Service Manual Error Information 8 Heater Failed Every time the deuterium lamp or the tungsten lamp is switched on or off a heater self test is performed If the test fails an error event is created As a result the temperature control is switched off Probable Causes Defective connector or cable e Defective heater Suggested Actions V Ensure the co
212. ter provides addition information on safety legal and web ee Agilent Technologies 381 A Appendix General Safety Information 382 The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Aligent Technologies assumes no liability for the customer s failure to comply with these requirements General This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards This instrument is designed and certified as a general purpose laboratory instrument for research and routine application only It is not certified for in vitro or medical applications Operation Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all 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 i
213. ters 53 using stored 52 C cable connecting APG remote 38 connecting CAN 38 connecting the ChemStation 38 connecting the power 38 overview and identification 342 CAN interface 368 cell support parts 332 choosing a flow cell 108 clock 362 CompactFlash card 363 configuration switch default settings 372 description and factory settings 372 configuration switches 50 control and data evaluation 31 correction factors for flow cells 110 coupling lens parts 330 D DADM MWDM analog signal output 361 CompactFlash card 363 diagnostic A D converter 362 fan drive 361 features 360 firmware 361 firmware description 376 interfaces 362 internal clock 362 lamp control 361 layout and connectors 365 leak sensor 361 location of connectors 265 overview 361 PCMCIA 364 safety switches 362 temperature control 362 Tungsten lamp voltage control 362 USB 364 damper parts 337 dark current test 165 1200 Series DAD and MWD Service Manual Index data evaluation and control 31 data recovery DRC 16 94 delivery checklist 34 diagnostic signals principle of temperature control 192 setup of detector 194 specifications and conditions 191 start a run and evaluate 196 warm up of detector 192 dimensions and weight 29 diode array 18 19 width 30 drift ASTM and noise 30 DSP not running 158 E EMF early maintenance feedback 20 entrance slit 18 environment 27 error messages
214. the power supply has a wide ranging capability There are no externally accessible fuses because automatic electronic fuses are implemented in the power supply The security lever at the power input socket prevents that the detector cover is taken off when line power is still connected WARNING Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations 1200 Series DAD and MWD Service Manual 23 1 Introduction ae REMOTE e 4 E D 3 C C gt 4 gt Cc C 3 i B C amp B a 3 Co gt C conia 2AN i ANALOG ANALOG SS 1 2 COMPACT FLASH IE De pIa D4 gt gt gt C 2 C J DEG 2 3 pid D C FE J C Jie B C p Dien hi RE FE D a gt C p pia C p O Die a pE 3 serial number DE manufactured in Germany 6 2006 01 week of last major change 00130 number of unit product number G1315C DAD SL G1315C DAD SL Serial No Serial No serial number ont Agilent Technologies Agilent Technotegies 16337 Weldbroan Made in Germany Figure 2 24
215. the filter motor off the shaft Keep the spring and the lever fixture in a safe place Remove the filter lever on the other side 3 Before installing the filter motor press the filter lever in 4 While counter holding the filter lever insert the filter from the other side motor onto the filter shaft until it clicks into the final position 1200 Series DAD and MWD Service Manual 287 13 Repairs Next steps Check that the filter lever is moveable Reinstall the optical unit see Installing the Optical Unit on page 297 Reconnect the filter motor cable to connector J18 on the detector main board Reinstall the front cover top cover and top foam section see Replacing the Foam and the Top Cover on page 299 Replace the detector into the stack oon SO A 0 Reconnect the power cable and turn on detector 288 1200 Series DAD and MWD Service Manual Repairs 13 Replacing the Tag Reader Flow Cell or the Cell Rotation Limiter When required If defective Tools required Screwdriver POZI 1 PT3 Hexagonal key 2 5 mm Tweezers Parts required Tag reader assembly flow cell G1315 60005 Cell rotation limiter G1315 26100 Screws M3 8 mm lg 0515 1040 Preparations Turn off the lamp Switch off the detector and disconnect the power cable Remove detector from stack and place it on working bench Remove front cover
216. the holmium oxide filter e Do not scratch the holmium oxide filter The holmium oxide filter can be cleaned with alcohol and a lint free cloth 1200 Series DAD and MWD Service Manual 237 12 Maintenance While releasing the holder with a screw driver carefully Replace the flow cell cover and fix the six screws insert the holmium oxide filter Next steps 6 Perform a holmium oxide test see Holmium Oxide Test on page 247 to check the proper function of the holmium oxide filter 7 Insert the flow cell see Exchanging a Flow Cell on page 211 o Replace the front cover 9 Turn on the flow 238 1200 Series DAD and MWD Service Manual Correcting Leaks When required Tools required Parts required Preparations Maintenance 12 If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections Tissue Two 1 4 inch wrenches for capillary connections None Remove the front cover 1 Use tissue to dry the leak sensor area and the leak pan 2 Observe the capillary connections and the flow cell area for leaks and correct if required Leak pan Leak sensor assembly Figure 91 Observing for Leaks 3 Replace the front cover 1200 Series DAD and MWD Service Manual 239 12 Maintenance Replacing Leak Hand
217. the threshold value and does not save spectra Limits 0 001 to 1000 00 mAU in steps of 0 001 mAU Usable for modes Apex Baselines Apex Slopes Baselines and All in Peak 1200 Series DAD and MWD Service Manual 99 5 Using the Detector Peakwidth Settings Do not use peak width shorter than necessary Do not use 0 025 sec response time no filtering high noise and no need actually ultra fast LC doesn t deliver peaks lt 0 0025 min lt 0 15 sec 1 To change the Peakwidth settings select Setup Detector Signals 2 In the section Peakwidth Responsetime click on the drop down list Change the Peakwidth according to your needs PE Set up DAD Signals of Control 28 Configuration os Run Recovery Fu Online Spectra 3 Wot Ready Information Help r Peakwidth Responsetime gt 01 min 2 s gt 0 005 min 0 1 s lt gt 0 01 min 0 2 s Peakwidth enables you to select the peak width response time for your analysis The peak width is defined as the width of a peak in minutes at half the peak height Set the peak width to the narrowest expected peak in your chromatogram The peak width sets the optimum response time for your detector The peak detector ignores any peaks that are considerably narrower or wider than the peak width setting The response time is the time between 10 and 90 of the output signal in response to an input step function When the All spectrum storage op
218. timize the Detector on page 105 1200 Series DAD and MWD Service Manual 103 5 Using the Detector Special Setups with Multiple DAD MWDs The G1315C D and G1365C D detectors are based on the same new hardware electronic platform The G1315A B and G1365A B detectors are based on the old hardware electronic platform Two detectors of same type e g G1315C D and G1315C D If you have two G1315C D DAD or G1365C D MWD in the same system then you can rearrange the order in the menu Instrument Configure 1200 Access to assign a specific detector as detector 1 and 2 The diagnostics tests and 00 PV should be done with only one detector configured Two detectors of similar type e g G1315C D and G1315A B If you have similar detectors in the same system the G1315C D will be automatically always detector 2 while the G1315A B is detector 1 independent from its location in the stack This cannot be changed 104 1200 Series DAD and MWD Service Manual Agilent 1200 Series Diode Array and Multiple Wavelength Detector Service Manual 6 How to optimize the Detector Optimizing the Detector Performance 106 Optimization Overview 107 Optimizing for Sensitivity Selectivity Linearity and Dispersion 109 Optimizing Selectivity 120 This chapter provides information on how to optimize the detector ee Agilent Technologies 105 6 How to optimize the Detector Optimizing the Detector Performance 106 The detector has a vari
219. tings on page 99 Set the spectral wavelength range for colorless samples 190 400 nm is sufficient Set step to 4 nm for normal use set small step and slit width if high resolution of spectra with fine structure is wanted Typical column Typical peak Recommended flow cell length width T lt 5 cm 0 025 min Micro or Semi nano 10 cm 0 05 min Semi mirco High pressure flow cell flow cell for pressures 20 cm 0 1 min Standard above 100 bar flow cell gt 40 cm 0 2 min Typical flow 0 01 0 2 0 2 0 4 0 4 0 4 1 5ml min 0 01 5 rate ml min ml min ml min ml min Internal column diameter 0 5 1 mm 2 1 mm 3 0 mm 4 6 mm 108 Figure 54 Choosing a Flow Cell in HPLC 1200 Series DAD and MWD Service Manual How to optimize the Detector 6 Optimizing for Sensitivity Selectivity Linearity and Dispersion Flow Cell Path Length Lambert Beer s law shows a linear relationship between the flow cell path length and absorbance I Absorbance logT log C d where T is the transmission defined as the quotient of the intensity of the transmitted light I divided by the intensity of the incident light Io is the extinction coefficient which is a characteristic of a given substance under a precisely defined set of conditions of wavelength solvent temperature and other parameters C is the concentration of the absorbing species usually in g l or mg l and d is the path length o
220. tion 1 Optical System The optical system of the detector is shown in Figure 1 Its illumination source is a combination of a deuterium arc discharge lamp for the ultraviolet UV wavelength range and a tungsten lamp for the visible VIS and short wave near infrared SWNIR wavelength range The image of the filament of the tungsten lamp is focused on the discharge aperture of the deuterium lamp by means of a special rear access lamp design which allows both light sources to be optically combined and share a common axis to the source lens The achromat source lens forms a single focused beam of light through the flow cell Each cell room and lamp are separated by a quartz window which can be cleaned or replaced In the spectrograph light is being dispersed onto the diode array by a holographic grating This allows simultaneous access to all wavelength information ell support window Tungsten lamp Coupling lens Deuterium lamp Diode array Achromat source lens iode array Holmium oxide filter Figure 1 Optical System of the Detector 1200 Series DAD and MWD Service Manual 17 1 Introduction Lamps Achromat Source Lens Holmium Oxide Filter Cell Support Window Flow Cell Compartment Spectrograph Variable Entrance 18 Slit System The light source for the UV wavelength range is a deuterium lamp with a shine through aperture As a result of plasma discharge in low pressure deuterium gas the
221. tion is selected then spectra are acquired continuously depending on the setting of the peak width The time specified by the peak width is used as a factor in the acquisition of spectra The acquisition time for one spectrum is slightly less than the peak width divided by 8 that is the acquisition time is between 0 0125 seconds 80 Hz and 3 2 seconds Limits When you set the peak width in minutes the corresponding response time is set automatically and the appropriate data rate for signal and spectra acquisition is selected as shown in Table 16 on page 101 Figure 51 Peakwidth Setting 100 1200 Series DAD and MWD Service Manual Using the Detector 5 Table 16 Peak Width Response Time Data Rate Peak Width min Response Time sec Data Rate Hz Detector lt 0 0025 0 025 80 G1315C G1365C only gt 0 0025 0 05 80 G1315C G1365C only gt 0 005 0 1 40 G1315C G1365C only gt 0 01 0 2 20 G1315C D and G1365C D gt 0 03 0 5 10 G1315C D and G1365C D gt 0 05 1 0 5 G1315C D and G1365C D gt 0 10 2 0 2 5 G1315C D and G1365C D gt 0 20 4 0 1 25 G1315C D and G1365C D gt 0 40 8 0 0 62 G1315C D and G1365C D gt 0 85 16 0 0 31 G1315C D and G1365C D 1200 Series DAD and MWD Service Manual 101 5 Using the Detector Slit Settings 1 To change the Slit settings select Setup Detector Signals 2 In the section Slit click on the drop down list 3 Change the Slit width according to your needs The Slit group allows you to sele
222. tions Self test 160 The DAD self test see Self test Results report on page 161 runs a series of individual tests and evaluates the results automatically The following tests are run e Filter Test Slit Test e Dark Current Test Intensity Test e Wavelength Calibration Test Holmium Test e Spectral Flatness Test e ASTM Noise Test optional The self test can be run once or repetitively When set up to run repetitively the tests run in series continually until stopped by the user Running the test repetitively is useful when troubleshooting problems which occur intermittently The ASTM noise test determines the detector baseline noise 254nm while pumping water at 1ml min The test requires approximately 20 minutes to run and can be included or excluded from the self test sequence as required Setup of the self test is done in the Self Test dialog box Select either Single Test or Repetitive Tests Check the ASTM Noise Test checkbox to include the noise test in the self test 1200 Series DAD and MWD Service Manual Test Functions 9 Agilent G1315 Self Test Results Slittest_ 108 Passed Min intensity 221nm 350r gt 5000cts _ 26341 cts Passed Holmiumtest o nm 0 30 nm Passed Figure 68 Self test Results report For details refer to the individual tests on the following pages 1200 Series DAD and MWD Service Manual 161 9 Test Functions Filter Test 162 Th
223. tor module after removing the top covers and foams A safety light switch on the main board will turn off the lamps immediately to avoid the operation with removed covers An error Cover Open will be generated status lamp will light red and the logbook will show an error message 262 1200 Series DAD and MWD Service Manual Repairs 13 Exchanging the Detector Main Board CAUTION When required Tools required Parts required Preparations If detector main board is defective or for repair on other assemblies Screwdriver POZI 1 PT3 Hexagonal wrenches 5 mm and 15 mm Detector main board DADM MW M depends on product G1315 66560 for G1315C DAD SL G1315 69560 exchange assembly for G1315C DAD SL G1365 66560 for G1365C MWD SL G1365 69560 exchange assembly for G1365C MWD SL G1315 66565 for G1315D DAD G1315 69565 exchange assembly for G1315D DAD G1365 66565 for G1365D MWD G1365 69565 exchange assembly for G1365D MWD Turn off the detector Disconnect the power cable Disconnect capillaries Remove detector from stack and place it on the working bench Remove the front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 Electronic boards and components are sensitive to electrostatic discharge ESD In order to prevent damage always use an ESD protection for example the ESD wrist strap from the accessory kit when handling electronic boards and c
224. tor when the top cover and the top foam are removed A safety light switch on the main board will inhibit the operation of the fan immediately Voltages for the other electronic components will be turned off after 30 seconds The status lamp will lit red and an error will be logged into the logbook of the user interface Always operate the detector with the top covers in place Electronic boards and components are sensitive to electrostatic discharge ESD In order to prevent damage always use an ESD protection when handling electronic boards and components see Using the ESD Strap on page 205 252 1200 Series DAD and MWD Service Manual Repairs 13 WARNING Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product Always turn off the deuterium lamp before removing the deuterium lamp 1200 Series DAD and MWD Service Manual 253 13 Repairs Cleaning or Replacing Coupling Lens Assembly When required The coupling lens assembly is located between the tungsten and the deuterium lamp It may be replaced when light transmission is reduced and a lamp exchange or window cleaning does not improve the light throughput Tools required Screwdriver POZI 1 PT3 hexagonal key 1 5 mm A pointed pair of pliers Parts required Coupling lens assembly G1103 68001 Preparations Turn the lamp s off Remove the front cover CAUTION If the detector has been in use the lamp
225. turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the solvent reservoir vacuum degasser when available in the system and the pump Solvents containing volatile ingredients will slightly lose these Therefore priming of the pumping system is required before starting an application 76 1200 Series DAD and MWD Service Manual Using the Detector 5 Table 10 Choice of Priming Solvents for Different Purposes Activity Solvent Comments After an installation lsopropanol Best solvent to flush air out of the When switching between reverse lsopropanol phase and normal phase both times After an installation Ethanol or Methanol To clean the system when using buffers Bidistilled water After a solvent change Bidistilled water After the installation of normal phase Hexane 5 lsopropanol seals P N 0905 1420 system Best solvent to flush air out of the system Alternative to lsopropanol second choice if no lsopropanol is available Best solvent to re dissolve buffer crystals Best solvent to re dissolve buffer crystals Good wetting properties The pump should never be used for priming empty tubings never let the pump run dry Use a syringe to draw enough solvent for completely filling the tubings to the pump inlet before continuing to prime with the pump 1 Open the purge valve of your pump by turning it counterclockwise and set flow rate to 3 5 ml m
226. ual parts depending on the following procedures Preparations Turn off the lamp e Switch off detector and disconnect power cable e Remove detector from stack and place it on the working bench e Remove front cover top cover and top foam section see Removing the Top Cover and Foam on page 260 1 Remove the two rubber shock absorbers 2 Disconnect the cable to the optical unit to the holmium oxide filter motor from the detector main board 1200 Series DAD and MWD Service Manual 281 13 Repairs Slide the z plane to the front and remove it from the 3 Loosen the screw on the left side of the z plane and the module two screws near the hydraulic connection Wy Np f VOY UUU i 1 YOY tC fff sk Sy ys f 5 Remove the optical unit from the instrument holding the 6 Place the optical on a clean bench one hand at back of the heat sink 282 1200 Series DAD and MWD Service Manual Repairs 13 Exchanging the Source Lens Achromat Assembly When required Th e source lens achromat assembly might be cleaned or replaced when the transmission of light is reduced and a lamp exchange or new spectro wi Tools required Sc ndows do not improve the light throughput rewdriver POZI 1 PT3 hexagonal key 1 5 mm A pointed pair of pliers Parts required So G1 Sp urce lens achromat assembly G1315 65201 includes filter lever
227. udes Outlet capillary 600 mm long 25 pm i d with pre fixed ferrules 4 and fitting 3 plus one PEEK Fitting FT 5 11 Cell Housing 80 nl G1315 27704 12 Cell Seal Assembly 80 nl G1315 42301 13 Quartz Body 80 nl G1315 80002 Sealing Kit 80 nl cell includes items 10 12 QTY 2 7 QTY 5 and G1315 68725 Lite Touch Sleeves QTY 5 322 1200 Series DAD and MWD Service Manual Parts and Materials for Maintenance 14 Accessory Kit This kit contains some accessories and tools needed for the installation and repair of the detector Table 38 Accessory Kit Parts Item Description Part Number Accessory kit Corrugated tubing to waste re order 5 m 1 Teflon Tubing flexible i d 0 8 mm flow cell to waste re order 5m 2 Fitting male PEEK Oty 1 3 Capillary column detector 380 mm lg 0 17 i d includes items 4 5 and 6 not assembled Capillary column detector 150 mm lg 0 17 i d 4 Ferrule front 1 16 SST qty 2 re order pack of 10 5 Ferrule back 1 16 SST qty 2 re order pack of 10 6 Fitting 1 16 SST qty 2 re order pack of 10 Hex key set 1 5 mm Wrench open end 1 4 5 16 inch Wrench open end 4 mm G1315 68705 5062 2463 5062 2462 0100 1516 G1315 87311 61315 87303 5180 4108 5180 4114 5061 3303 8710 0641 8710 0510 8710 1534 or kit 5062 2418 1 16 Fittings and Ferrules front back 10 PK For item number refer to Figure 113 and Figure 114 1200 Series DAD a
228. uld cause a possible loss of data Do not proceed beyond a caution until you have fully understood and met the indicated conditions 384 1200 Series DAD and MWD Service Manual Appendix A The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all Electric and Electronic appliances from 13 August 2005 This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex this product is classed as a Monitoring and Control instrumentation product Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information 1200 Series DAD and MWD Service Manual 385 A Appendix Radio Interference Never use cables other than the ones supplied by Aligent Technologies to ensure proper functionality and compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and or used for measurements on open set ups the user has to assure that under operati
229. unctions Wavelength Verification and Recalibration 176 The detector uses the alpha 656 1 nm and beta 486 nm emission lines of the deuterium lamp for wavelength calibration The sharp emission lines enable more accurate calibration than is possible with holmium oxide When verificaation is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with bubble free degassed HPLC water in the flow cell If a deviation is found and displayed it can be recalibrated by pressing Adjust The deviations are tracked in the Calibration History diagnosis buffer in the detector DAD Wavelength Calibration G1315C x Calibration history Deviation D2 Alpha D2 Beta Time Date 0 01nm O 04nm 13 19 31 16 03 2005 D2 Alpha UEEEEEp EEE EH 1 2mm 656 1nm 1 2nm D2 Beta MNNHengereee 1 2nm 486 0nm 1 2nm Resethistoy D2 Alpha line deviation is 0 00nm D2 Beta line deviation is 0 00nm OK Cancel Help Sd se Calibration settings equal to measured ones No calibration necessary Figure 74 Wavelength Verification and Recalibration Wavelength calibration should be done e after maintenance of the flow cell e lamp exchange or e after a major repair like processor board or optical unit exchange see also Replacing the Detector s Firmware on page 242 1200 Series DAD and MWD Service Manual Test Functions 9
230. uration l of Run Recovery Uv Vis J Take current method At Power On automatic lamp on fy Online Spectra Clon A at power on A faa fsatiation C off off Analog Output Range Error Method take error method or current method in case of an Eee On Output 1 Output 2 error rine D ot II Analog Output Range can be ORE aiy set to either 100 mV or 1 V full J Tum Vis lamp on scale see also Analog Output Settings on page 97 poma tunin Automatic Turn On lamps can Tum required lames on at be programmed detector must be on for this Date ddimm yppyy 28 12 2005 Help online help Time 2 47 42 hh mm ss p P OK Cancel Help Figure 45 Detector control settings 1200 Series DAD and MWD Service Manual 91 5 Using the Detector Configuration Settings Qe Set up DAD Signals i ion E F st cali e Temperature Control the optical uni La IP g DAD Configuration System 2 x Te t Control th pt t a8 Control m Temperature control is kept on constant temperature and Si ei gt O Temperature control on improves the baseline stability in os Run Recovery i e Seatin c vai unstable environments See also Temperature control of note below B Not Ready Information Help p UV lamp Tag UV lamp tag for Agilent lamps with use UV lamp only if RFID Tag is available RFID tags If no RFID tag lamp is 92 used detector icon will become grey la
231. uty cycle after 30 minutes the heater control is ON and is working with optimized parameters to get the optical unit into the optimal temperature window stabilized Tol pea p se hewn nee ene TD PIAA Re IO NOH DAO wanae Nei an ne A 1 baseline 254 4 ref off 2 baseline 254 4 360 100 3 main board temperature 4 optical unit temperature ge 5 UV lamp voltage t T 2 2 n 2 2 i Figure 82 Example of warm up cycle and corresponding diagnostic signals detector and both lamps turned on at room temperature of 23 C start run after 4 minutes NOTE The times to stabilize the baseline may vary from instrument to instrument and depends on your environment Above example was done under stable environmental conditions 1200 Series DAD and MWD Service Manual 193 10 Diagnostic Signals Setup of Detector 1 Remove the flow cell to eliminate problems from the flow system 2 Use the following detector settings all parameter not mentioned should stay on default values as shown DAD Signals G1315C r Signals Store Sample Bw Reference Bw Time Stoptime 120 00 min M 254 a faso fioo 4 nm a fsa fe of frm ostime ot min cM fro fs of nm 230 je 260 f100 E nm Required Lamps Ef feso fie co fioo nm K uv M Vis FT f fie 360 fioo 4 nm ar jeo fis eo fioo 4 eee lil Peakwidth Responsetime H feo fie faeo froo S nm gt O1 mn E Spectrum i Autobalance Store
232. w cell installed and once with the flow cell removed The resulting intensity ratio is a measure of the amount of light absorbed by the flow cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell This test should be performed inititially with a new detector flow cell The values should be kept for later reference comparison Cell Test Evaluation The Agilent ChemStation calculates the intensity ratio automatically The intensity ratio typically between 0 5 and 0 7 for new standard flow cells and 0 1 to 0 3 for new mico and high pressure cells is dependent on the degree of contamination of the flow cell windows and on the type of flow cell used Figure 73 Cell Test Results report with no flow cell inserted 1200 Series DAD and MWD Service Manual Test Functions 9 This test can be used for the standard flow cells only The nano flow cells will give very low values due to their design Test Failed low ratio value Probable Causes e Absorbing solvent or air bubble in flow cell e Dirty or contaminated flow cell Suggested Actions V Ensure the flow cell is filled with water and free from air bubbles V Exchange the flow cell windows 1200 Series DAD and MWD Service Manual 175 9 Test F
233. wW warm up of detector 192 wavelength accuracy 30 bunching 30 range 30 recalibration 126 verification and recalibration 176 weight and dimensions 29 1200 Series DAD and MWD Service Manual www agilent com In This Book This manual contains technical reference information about the Agilent 1200 Series diode array and multiple wavlength detectors G1315C D and G1365C D The manual describes the following e introcduction and specifications e installation e using and optimizing e troubleshooting and diagnose e maintenance and repair e parts identification e hardware information e safety and related information Agilent Technologies 2006 Printed in Germany Edition 10 06 G1315 90112 EE Agilent Technologies
234. wear or stress Ideally the frequency at which components are exchanged should be based on the intensity of usage of the detector and the analytical conditions and not on a predefined time interval The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user selectable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters The detector provides two EMF counters for the lamps The counters increment increments with lamp use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded The counters can be reset to zero after the lamp is exchanged The detector provides the following EMF counters e Deuterium Lamp On Time e Tungsten Lamp On Time Using the EMF Counters The user settable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements The useful lamp burn time is dependent on the requirements for the analysis high or low sensitivity analysis wavelength etc therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument 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 i
235. xt a spectrum no flowcell is taken Theoretically the spectrum should be flat however in practice noise is superimposed on the spectrum The amplitude of the noise is a measure of the optical and electronic performance This test is part of the detector self test only see Self test on page 160 Spectral Flatness Evaluation Limit is lt 0 002 AU Test Failed Probable causes e Old lamp e Defective DAM board e Defective optical unit Suggested Actions Y Run the Intensity Test V Exchange the lamp if old or defective V Exchange the DAM board V Exchange the optical unit 1200 Series DAD and MWD Service Manual Test Functions 9 ASTM Noise Test The ASTM noise test determines the detector noise over a period of 20 minutes The test is done with the flowcell removed so the test results are not influenced by solvent or pump effects On completion of the test the noise result is displayed automatically This test is part of the detector self test only see Self test on page 160 ASTM Noise Test Evaluation Limit is 0 02 mAU Test Failed Probable causes e Insufficient lamp warm up time e Old lamp Suggested Actions V Allow lamp to warm up for at least 1 hour V Exchange the lamp 1200 Series DAD and MWD Service Manual 173 9 Test Functions Cell Test 174 The cell test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm once with the flo
236. y All z PM Prerun J Postrun Range 200 to 750 nm Step 20 T nm Sli Threshold LOO maw 4mm E Total Lines 0 Timetable Cancel Margin to negative Absorbance foo mAL Help More Additional Signals Store Signal Name K IV Board Temperature E IV Optical Unit Temperature M IV UY Lamp Anode Voltage OK Cancel Help Figure 83 194 Setting up the detector Do not run shorter runs than 60 minutes Typical effects from air condition systems run at cycles of 15 to 20 minutes Both lamps should be on IMPRORTANT For factory evaluations spectra should be taken as well for at least 1 2 cycles 200 750nm You may use a time table for this The More button opens the additional diagnostic signals For temperature related problems at least Board Temperature and Optical Unit Temperature signals are required 1200 Series DAD and MWD Service Manual 3 In the ChemStation Online Plot window select the following signals and use the settings according the table Edit Signal Plot DAD D Signal 230 16 Reference 360 AD F Signal 280 16 Reference 360 AD G Signal 280 16 Reference 360 AD H Signal 280 16 Reference 360 DAD A Signal 254 4 Reference 360 DAD B Signal 254 4 Reference Off DAD C Signal 750 4 Reference Off DAD K Board Temperature DAD L Optical Unit Temperature Diagnostic Signals DAD M UY Lamp Anode Yoltage Pe ETI E Se

Agilent 1200 Series Diode Array and Multiple Wavelength Detector

Contents

Download Pdf Manuals

Related Search

Related Contents