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G1314-90010 - Agilent Technologies

1. Figure 19 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 Variable Wavelength Detector User Manual Using the Detector 4 Special Settings of the Detector In this chapter special settings of the G1314B VWD and G1314C VWD SL are described based on the Agilent ChemStation B 02 01 Control Settings Set up VWD Signal VWD Controls xj Lamp turn on and off of s Control Lamp pErorMethod UV lamp Fu Online Spectra J 5 C on I Take current method At Power On automatic lamp on 8 Not Ready Information Help C off at power on m Analog Output Range e Error Method take error method or current method in case of an error Cov 1 At Power On m Lamp Type Analog Output Range can be Me ara al oz set to either 100 mV or 1 V full scale see also Analog Output Settings on page 59 m Automatic Turn On I KT Jamp oak Lamp Type can be set to either Date 29722005 lt ddimmyyyy G1314 60100 standard VWD Tia ME errs lamp or 2140 0590 DAD lamps see also Exchanging a Lamp on page 85 Cancel Hep Automatic Turn On lamps can be programmed detector must be on for this e Help online help Figure 20 Detector control settings 1200 Series Var
2. 3 If required insert the interface board and fix the screws Next steps Remove the ESD strap e Reinstall the module into the stack 98 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Replacing the Detector s Firmware When required If new version solves problems of currently installed version or after exchange of the detector main board VWM 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 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 00 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 G1314C VWD SL requires firmware revision A 06 02 or above main and resident 1200 Series Variable Wavelength Detector User Manual 99 100 8 Maintenance Tests amp Calibrations The following tests are r
3. 7 Maintenance and Repair This chapter provides general information on maintenance and repair of the detector 8 Maintenance This chapter describes the maintenance of the detector 1200 Series Variable Wavelength Detector User Manual 3 Parts and Materials for Maintenance This chapter provides information on parts for maintenance Appendix This chapter provides addition information on safety legal and web 1200 Series Variable Wavelength Detector User Manual Contents 1 Introduction to the Variable Wavelength Detector Introduction to the Detector 10 Optical System Overview 11 Electrical Connections 15 Instrument Layout 17 Early Maintenance Feedback EMF 18 EMF Counter 18 Using the EMF Counters 18 2 Site Requirements and Specifications Site Requirements 22 Physical Specifications 24 Performance Specifications 25 3 Installing the Detector Unpacking the Detector 28 Optimizing the Stack Configuration 30 Installing the Detector 33 Flow Connections to the Detector 36 4 Using the Detector Setting up an Analysis 40 Before Using the System 40 Requirements and Conditions 42 1200 Series Variable Wavelength Detector User Manual Optimization of the System 44 Preparing the HPLC System 45 Running the Sample and Verifying the Results 54 Special Settings of the Detector 55 Control Settings 55 Online Spectra 56 Scanning with the VWD 57 Analog Output Settings 59 Special Setpoints 60 Peakwidth Settings 61 Optimi
4. 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 option 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 see Table 9 on page 62 Limits When you set the peak width in minutes the corresponding response time is set automatically and the appropriate data rate for signal acquisition is selected as shown in Table 9 on page 62 Peakwidth Setting 1200 Series Variable Wavelength Detector User Manual 4 4 Using the Detector Table 9 Peak Width Response Time Data Rate G1314B VWD Peak Width min Response Time sec Data Rate Hz lt 0 005 gt 0 005 gt 0 01 gt 0 025 gt 0 05 gt 0 10 gt 0 20 gt 0 40 0 12 0 12 0 25 0 5 1 0 2 0 4 0 8 0 13 74 13 74 13 74 13 74 6 87 3 43 1 72 0 86 Table 10 Peak Width Response Time Data Rate G1314C VWD SL Peak Width min Response Time sec Data
5. 8 Place the window on gasket 9 Place the peek ring on the window 10 Insert the conical springs Make sure the conical springs point towards the window Otherwise tightening the cell screw might break the window 11 Screw the cell screw into the flow cell and tighten the screw 12 Repeat the procedure for the other cell side 1200 Series Variable Wavelength Detector User Manual 91 8 92 Maintenance Next steps Reconnect the capillaries see Exchanging a Flow Cell on page 87 Perform a leak test If OK insert the flow cell Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the flow cell Replace the front cover 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Using the Cuvette Holder When required If your own standard should be used to checkout the instrument Tools required None Parts required Cuvette Holder G1314 60200 Cuvette with the standard e g NIST certified holmium oxide sample This cuvette holder can be placed instead of a flow cell in the variable wavelength detector Standard cuvettes with standards in it for example National Institute of Standards amp Technology NIST holmium oxide solution standard can be fixed in it This can be used for wavelength verifications Figure 31 Cuvette Holder 1200 Series Variable Wavelength Detector User Manual 93 8 Maintenance Preparation for this procedure are
6. Srm i a rm 418 rm gam dron G13144 B C 1100 1200 360 Srm FEE lrom 418 Sr 536 44 The variation in Measured Wavelength depends on the different Optical Bandwidth Agilent Technologies guarantees the trace ability of the specified absorb ance maxima to a National Instinute of Standards amp Technology NIST Holnimm Oxide Sobstion Standard with a lot to lottolerance of 0 3 ran The wavelength calibration filter built into the Agilent Technologies UV VIS detectors is made of this material and meets these specific ations E is therefore suitable for wavelength calibration of these detectors within the specified vravelength accuracy of the respective dete ctor over its vravelength range Juary 13 2006 1200 Series Variable Wavelength Detector User Manual 129 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 Products Chemical Analysis It will provide also the latest firmware of the Agilent 1200 Series modules for download 130 1200 Series Variable Wavelength Detector User Manual Index A absorbance Beer Lambert 67 accessory kit parts 118 Agilent ChemStation 45 LC diagnostic software 76 on internet 130 Agilent on internet 130 algea information 127 analog output range 55 59 output settings 59 ASTM environmental conditions 23 reference and conditio
7. Agilent ChemStation is the controller connect either the LAN connection to the LAN interface board in the detector If a Agilent 1200 DAD MWD EFLD is in the system the LAN should be connected to the DAD MWD FLD due to higher data load 7 Connect the analog cable 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 Security lever Interface board Analog signals APG remote RS 232C CAN GPIB Power Configuration switch Figure 8 Rear View of Detector 34 1200 Series Variable Wavelength Detector User Manual Installing the Detector 3 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 1200 Series Variable Wavelength Detector User Manual 35 3 installing the Detector Flow Connections to the Detector Preparations Parts required Detector is installed in the LC system Other modules Parts from accessory kit see Accessory Kit Contents on page 29 Two wre
8. Checklist Description Quantity Variable wavelength detector 1 Power cable 1 Flow cell As ordered User Manual 1 Accessory kit see Table 5 on page 29 1 28 1200 Series Variable Wavelength Detector User Manual Installing the Detector 3 Detector Accessory Kit Contents Table5 Accessory Kit Contents Description Part Number Quantity Accessory kit G1314 68705 CAN cable 0 5 m 5181 1516 1 PEEK outlet capillary kit 5062 8535 1 Fitting male PEEK 0100 1516 1 Hex key 1 5 mm 8710 2393 1 Hex key 4 mm 8710 2392 1 Wrench open end 1 4 5 16 inch 8710 0510 1 Wrench open end 4 mm 8710 1534 1 1200 Series Variable Wavelength Detector User Manual 29 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 path ensuring minimum delay volume 30 1200 Series Variable Wavelength Detector User Manual Solvent cabinet Vacuum degasser Pump Autosampler Column compartment Detector Figure 5 Recommended Stack Configuration Front View 1200 Series Variable Wavelength Detector User Manual Installing the Detector 3 Local User Interface 31 3 Installing the Detector Remote cable CAN Bus cable to
9. Number High pressure flow cell 10 mm 14 pl 400 bar G1314 60082 Capillary column detector SST 380 mm lg 0 17 i d G1315 87311 one side not assembled 1 Cell screw 79853 27200 Cell kit Agilent comprises G1314 65054 two windows two KAPTON gaskets and two PEEK rings 2 Ring PEEK kit quantity 2 79853 68739 3 Window quartz kit quantity 2 79853 68734 4 Gasket kit KAPTON quantity 10 G1314 65055 1 Cell screw 2 Ring PEEK 3 Window quartz 4 Gasket KAPTON 5 Cell Cover Figure 40 High Pressure Flow Cell 1200 Series Variable Wavelength Detector User Manual 115 9 Parts and Materials for Maintenance Cuvette Holder 116 Table 20 Cuvette Holder Item Description Part Number Cuvette Holder G1314 60200 For information the use of the cuvette holder refer to Using the Cuvette Holder on page 94 Figure 41 Cuvette Holder 1200 Series Variable Wavelength Detector User Manual Parts and Materials for Maintenance 9 Leak Parts Table 21 Leak Parts Item Description Part Number 3 Leak funnel 5041 8388 4 Leak funnel holder 5041 8389 5 Clip 5041 8387 6 Corrugated tubing 120 mm Ig re order 5 m 5062 2463 7 Corrugated tubing 1200 mm Ig re order 5 m 5062 2463 Figure 42 Leak Parts 1200 Series Variable Wavelength Detector User Manual 117 9 Parts and Materials for Maintenance Accessory Kit This kit contains some accessories and tools needed for the installation and repa
10. UV Radiation 126 Solvent Information 127 Declaration of Conformity for HOX2 Filter 129 Agilent Technologies on Internet 130 Index 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 1 Introduction to the Variable Wavelength Detector Introduction to the Detector 10 Optical System Overview 11 Flow Cell 12 Electrical Connections 15 Instrument Layout 17 Early Maintenance Feedback EMF 18 This chapter gives an introduction to the detector instrument overview and internal connectors ee Agilent Technologies 1 Introduction to the Variable Wavelength Detector Introduction to the Detector The Agilent 1200 Series variable wavelength detector is designed for highest optical performance GLP compliance and easy maintenance with higher data rate 27 55Hz for fast HPLC with G1314C VWD SL see Set the Detector Parameters on page 69 deuterium lamp for highest intensity and lowest detection limit over a wavelength range of 190 to 600 nm optional flow cell cartridges standard 10 mm 14 ul high pressure 10 mm 14 ul micro 5 mm I ul semi micro 6 mm 5 ul are available and can be used depending on the application needs easy front access to lamp and flow cell for fast replacement and built in holmium oxide filter for fast wavelength accuracy verification For specifications Performance Specifications on page 25 Two version of the Agilent 1200 Se
11. bad a 70 w w V E V atsl 1 E 1 1 GB hee B On line plot window details window Figure 10 Initial ChemStation screen Method and Run Control 1200 Series Variable Wavelength Detector User Manual 45 4 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 rc cs EMG Same soro SP 2 DEFALLT D no Detal z ott ee sess g gt a 3 a 5 Figure 11 Turning on the HPLC Module 46 1200 Series Variable Wavelength Detector User Manual 12 1a Using the Detector 4 5 Purge the pump For more information see Priming and Purging the System on page 40 6 Allow the detector to warm up of at least 60 minutes to provide a stable baseline see example in Figure 12 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 VWO A Wavelengtss 284 am LAMPON LAMPON D a ee Sc a TT 2 x w s oo min Figure 12 Stabilization of Baseline 1200 Series Variable Wavelength Detector User Manual 47 4 Using the Detector 7 For the isocratic pump fill the solvent bottle with the mixture of HPLC grade bi distilled water 80 and aceton
12. from the deuterium lamp and focuses it onto the entrance slit Entrance Slit Assembly The entrance slit assembly has an exchangeable slit The standard one has a 1 mm slit For replacement and calibration purposes to optimize the alignment a slit with a hole is needed Filter Assembly The filter assembly is electromechanically actuated During wavelength calibrations it moves into the light path The filter assembly has two filters installed and is processor controlled OPEN nothing in light path CUTOFF cut off filter in light path at gt 370 nm HOLMIUM holmium oxide filter for wavelength check A photo sensor determines the correct position Cutoff filter Holmium oxide filter with cutoff filter Figure 3 Filter Assembly 1200 Series Variable Wavelength Detector User Manual 13 1 14 Introduction to the Variable Wavelength Detector Mirror Assemblies M1 and M2 The instrument contains two spherical mirrors M1 and M2 The beam adjustable is vertically and horizontally Both mirrors are identical Grating Assembly The grating separates the light beam into all its component wavelengths and reflects the light onto mirror 2 Beam Splitter Assembly The beam splitter splits the light beam One part goes directly to the sample diode The other part of the light beam goes to the reference diode Photo Diodes Assemblies Two photo diode assemblies are installed in the optical unit The sample diode assembly is loc
13. indicator is OFF and power switch light is on the detector is in a prerun condition and is ready to begin an analysis A green status indicator indicates the detector is performing an analysis run mode A yellow indicator indicates a not ready condition 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 Variable Wavelength Detector User Manual Troubleshooting and Diagnostics 6 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 13 Test Functions available 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 Wave
14. local user interface CAN Bus cable Analog detector signal 1 or 2 outputs per detector LAN to LC ChemStation location depends on detector Figure 6 Recommended Stack Configuration Rear View 32 1200 Series Variable Wavelength Detector User Manual Installing the Detector 3 Installing the Detector Preparations Locate bench space Provide power connections Unpack the detector Parts required Detector Power cord for other cables see text below and on page 118 ChemStation and or Control Module G1323B 1 Install the LAN interface board in the detector if required see Replacing the Interface Board on page 99 2 Place the detector in the stack or on the bench in a horizontal position 3 Ensure the line power switch at the front of the detector is OFF Status indicator green yellow red Line power switch with green light Figure 7 Front View of Detector The figure above shows the flow cell already installed The flow cell area is closed with a metal cover The flow cell has to be installed as described in Flow Connections to the Detector on page 36 1200 Series Variable Wavelength Detector User Manual 33 3 installing the Detector 4 Connect the power cable to the power connector at the rear of the detector 5 Connect the CAN cable to other Agilent 1200 Series modules 6 Ifa
15. path length 68 semimicro parts 113 standard parts 111 types and data 12 25 front of detector 33 G grating assembly 14 holmium oxide declaration of conformity 129 filter 13 information on cuvette holder 94 on lithium batteries 123 on radio interference 124 on solvents 127 on sound emission 125 on UV radiation 126 installation of flow connections 36 of module 33 instant pilot 75 instrument layout 17 internet 130 introduction 10 to optical system 11 isocratic test sample 54 L lamp 13 initial drift 52 intensity test 102 type 25 55 131 Index leak correcting 97 panels parts 117 line power consumption 24 voltage and frequency 24 linearity 25 26 M maintenance 83 cleaning the instrument 80 correcting leaks 97 exchanging flow cell 87 exchanging interface board 99 exchanging lamps 85 exchanging leak handling system 98 for parts see parts for maintenance 109 introduction 77 overview 84 replacing firmware 100 simple repairs 78 standard flow cell 90 using the cuvette holder 94 using the ESD strap 81 method error 55 load 48 mirror assemblies 14 negative absorbance margins 60 noise short term 25 0 online plot 52 online spectra 56 operating temperature 24 optical unit beam splitter assembly 14 entrance slit assembly 13 filter 13 filter assembly 13 flow cell 12 grating assembly 14 132 lamp 13 mirrors 1
16. test passes exchange the flow cell windows V Clean replace optical components V Exchange the lamp 1200 Series Variable Wavelength Detector User Manual 101 102 Maintenance Instrument G1314B Serial Number JP33324886 Operator Wolfgang Date 03 01 2006 Time 15 07 09 File C CHEM32 2 DIAGNOSE VWD_INT DGR VWD Intensity Spectrum Accumulated lamp on time 94 35 h Highest intensity gt 10000 cts 222615 cts Average intensity gt 5000 cts 29734 cts Lowest intensity gt 200 cts 1137 cts Figure 34 Intensity Test Report Passed Passed Passed 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Wavelength Verification Calibration Wavelength calibration of the detector is done using the zero order position and 656 nm emission line position of the deuterium lamp The calibration procedure involves two steps First the grating is calibrated on the zero order position The stepper motor step position where the zero order maximum is detected is stored in the detector Next the grating is calibrated against the deuterium emission line at 656 nm and the motor position at which the maximum occurs is stored in the detector In addition to the zero order and 656 nm alpha emission line calibration the beta emission line at 486 nm and the three holmium lines are used for the complete wavelength calibration process These holmium lines are at 360 8 nm 418 5 nm and 536 4 nm WD Wavelength Calib
17. to have access to the flow cell area Turn the lamp OFF 1200 Series Variable Wavelength Detector User Manual 87 8 Maintenance 2 Disconnect the inlet and outlet capillaries 3 Unscrew the thumb screws parallel and remove the flow cell Note If you want to maintain flow cell parts see Repairing the Flow Cells on page 90 or the information provided with your flow cell 4 Replace the flow cell and fix the thumb screws Reconnect the inlet and outlet capillaries to the flow cell 88 1200 Series Variable Wavelength Detector User Manual Maintenance 8 5 Replace the front cover Next steps To check for leaks establish a flow and observe the flow cell outside of the cell compartment and all capillary connections Insert the flow cell Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the flow cell Replace the front cover 1200 Series Variable Wavelength Detector User Manual 89 8 Maintenance Repairing the Flow Cells When required If the flow cell needs repair due to leaks or contaminations Tools required Wrench 1 4 inch for capillary connections Hexagonal wrench 4 mm Tooth picks Parts required See Standard Flow Cell on page 111 See Micro Flow Cell on page 112 See Semi micro Flow Cell on page 113 See High Pressure Flow Cell on page 115 Preparations Tu
18. 4 photodiode assemblies 14 photodiode boards 14 source lens assembly 13 optimization detector performance 66 of the system 44 overview optical path 11 optical system 11 system overview 11 P parameters detector 49 parts and materials for maintenance 109 parts for maintenance accessory kit 118 cuvette holder 116 high pressure flow cell 115 leak panels 117 micro flow cell 112 overview of maintenance parts 110 semimicro flow cell 113 standard flow cell 111 peakwidth settings 50 61 69 performance optimization 66 specifications 25 photodiode assemblies 14 boards 14 photometric accuracy 68 physical specifications 24 humidity 24 line voltage and frequency 24 operating temperature 24 power consumption 24 safety information 24 weight and dimensions 24 power considerations 22 consumption 24 cords 22 preparing the HPLC system 45 radio interference 124 rear of detector 34 recalibration of wavelength 72 reference conditions 26 repairs cleaning the instrument 80 introduction 77 of internal parts 78 overview of simple repairs 84 simple maintenance 78 simple repairs see maintenance 83 using the ESD strap 81 replacing firmware 100 response time 62 69 running the sample 54 S safety class instrument 120 general information 120 lithium batteries 123 symbols 122 sample info 53 scan range step 60 scanning 57 setting up an analysis 40
19. 4 Using the Detector WD Signal System 2 xl m Signal m Time Wavelength Stoptime 254 nm ee min Peakwidth Responsetime Posttime bom 2 W ot Hmn m Timetable Line Time Table Graphic r Analog Output Zero Offset 5 E Attenuation 1000 mAU r Store additionally T Signal w o Reference IT Reference only m Autobalance IV Prerun IT Postrun m Special Setpoints Setup Figure 15 50 1 signal with individual wavelength setting stop and post time can be set if required peakwidth depends on the peaks in the chromatogram see page 61 time table for programmable actions during the run Zero Offset Limits 1 to 99 in steps of 1 Attenuation Limits 0 98 to 4000 mAU at discrete values for either 100 mV or 1 V full scale additional signals can be stored with the normal signal for diagnostics autobalance to zero absorbance on the analog output plus offset at begin and or end of run see Special Setpoints on page 60 Detector Settings default 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 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 VWD A Signal 254 as signals Change the Y range for the VWD to 1 m
20. 8 1200 Series Variable Wavelength Detector User Manual 107 8 Maintenance 108 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 9 Parts and Materials for Maintenance Overview of Maintenance Parts 110 Standard Flow Cell 111 Micro Flow Cell 112 Semi micro Flow Cell 113 High Pressure Flow Cell 115 Cuvette Holder 116 Leak Parts 117 Accessory Kit 118 This chapter provides information on parts for maintenance ee Agilent Technologies 109 9 Parts and Materials for Maintenance Overview of Maintenance Parts Table 15 Maintenance Parts Item Description Part Number Cable CAN assembly 0 5 m 5181 1516 Cable CAN assembly 1 m 5181 1519 Interface board BCD External Contacts G1351 68701 LAN Communication Interface board G1369A or G1369 60001 Control Module G1323B Note The G1314C VWD SL can be operated with a G1323B just G1323 67001 in standard mode as G1314B no higher data rate available or Instant Pilot G4208A G4208 67001 Deuterium lamp G1314 60100 Standard flow cell 10 mm 14 ul additional flow cell parts see page 111 G1314 60086 Micro flow cell 5 mm 1 ul additional flow cell parts see page 112 G1314 60081 High pressure flow cell 10 mm 14 ul additional flow cell parts see page 115 G1314 60082 Semi micro flow cell 6 mm 5 ul additional flow cell parts see page 113 G1314 60083 Cuvette Holder G1314 60200 Front cover 5065 9982 Leak handling
21. 8 Replacing Leak Handling System Parts When required lfthe parts are corroded or broken Tools required None Parts required Leak funnel 5061 3356 Leak funnel holder 5041 8389 Leak tubing 120 mm 0890 1711 Remove the front cover to have access to the leak handling system Pull the leak funnel out of the leak funnel holder Pull the leak funnel with the tubing out of its location Replace the leak funnel and or the tubing Insert the leak funnel with the tubing in its position Insert the leak funnel into the leak funnel holder NJ oo FW HN Replace the front cover Leak funnel holder _ Leak funnel s i Leak tubing Leak plan FE Waste outlet Leak sensor assembly Figure 33 Replacing Waste Handling System Parts 1200 Series Variable Wavelength Detector User Manual 97 8 Maintenance Replacing the Interface Board When required detector Part required When defective or for installation of the board or for all repairs inside the Interface board BCD G1351 68701 with external contacts and BCD outputs LAN Communication Interface board G1369A or G1369 60001 Tools required None 1 Install the ESD strap Move the power lock across the power inlet ESD strap B LEZ E BEDE T a BEES 8 ds Bee TE x ets a A FS BULLET IN SM Ay Ay power lock D iy 2 If required unscrew and remove the interface board Place the board on the ESD kit
22. 80 0 19 mm 5 4 8 High Pressure flow cell 14 ul G1314 60082 10 mm 10 00 0 19 mm 6 5 75 68 However you have to be aware that there are additional tolerance of gasket thickness and its compression ratio which is supposed to be very small in comparison with the machining tolerance 1200 Series Variable Wavelength Detector User Manual Set the Detector Parameters How to optimize the detector 5 1 Set peakwidth as close as possible to the width at half height of a narrow peak of interest Table 12 Peakwidth Settings Peakwidth at half height Rise time 10 90 Data rate Module lt 0 00125 minutes lt 0 031 seconds 54 96 Hz G1314C 0 00125 minutes 0 031 seconds 27 48 Hz G1314C 0 0025 minutes 0 062 seconds 13 74 Hz G1314C 0 005 minutes 0 125 seconds 13 74 Hz G1314B G1314C 0 01 minutes 0 25 seconds 13 74 Hz G1314B G1314C 0 025 minutes 0 50 seconds 13 74 Hz G1314B G1314C 0 05 minutes 1 second 6 87 Hz G1314B G1314C 0 1 minutes 2 seconds 3 43 Hz G1314B G1314C 0 2 minutes 4 seconds 1 72 Hz G1314B G1314C 0 4 minutes 8 seconds 0 86 Hz G1314B G1314C 2 Choose the sample wavelength at a longer wavelength than the cut off wavelength of the mobile phase at a wavelength where the analytes have strong absorptivity if you want to get the lowest possible detection limit at a wavelength with moderate absorptivity if you work with high concentrations and preferably where the spectrum is flat for bett
23. AU 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 A A A A Edit Signal Plot OEFAULT O Available Signals Selected Signals Quaternary Pump Pressure uaternary Pump Flow uaternary Pump 4 uaternary Pump B uaternary Pump C uaternary Pump D olumn Thermostat Temperature l olumn Thermostat Temperature ri WD B Signal w o Reference at 254 VWD A Absorbance at 254 nm Add gt En Adatav 1 1 GB hee Window CVWD 4 Absorbance at 254 nm x axis 15 d min Type acquired y axis range 1 mau TF draw zero line T auto y adjust Offset 10 B Yo Fraction Colector p Method Settings FF Show Fraction collection ticks J Use method settings Apply to Method OK Figure 16 Edit Signal Plot Window Cancel Help 1200 Series Variable Wavelength Detector User Manual 51 4 Using the Detector The Online Plot Figure 17 on page 52 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 17 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 52 1200 Se
24. Agilent 1200 Series Variable Wavelength Detector G1314B G1314 SL User 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 electronic storage and retrieval or translation into a foreign language without prior agreement and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61314 90010 Edition 02 06 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn Germany Manual Structure The User Manual G1314 90010 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 The Service Manual G1314 90110 English contains the complete information about the Agilent 1200 Series Variable Wavelength Detector It is available as Adobe Reader file PDF only 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 implied warranties of merchantabilit
25. Rate Hz lt 0 00125 gt 0 00125 gt 0 0025 gt 0 005 gt 0 01 gt 0 025 gt 0 05 gt 0 10 gt 0 20 gt 0 40 lt 0 031 0 031 0 062 0 12 0 25 0 5 1 0 2 0 4 0 8 0 55 27 5 13 74 13 74 13 74 13 74 6 87 3 43 1 72 0 86 62 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 Optimizing the Detector Additional theoretical information can be found in chapter How to optimize the detector on page 65 1200 Series Variable Wavelength Detector User Manual 63 4 Using the Detector 64 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 5 How to optimize the detector Optimizing the Detector Performance 66 This chapter gives hints on how to select the detector parameters and the flow cell att Agilent Technologies 65 5 How to optimize the detector Optimizing the Detector Performance The detector has a variety of parameters that can be used to optimize 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 a rule of thumb for optimizing the detector parameters Match the Flow Cell to the Column Figure 26 recommends the flow cell that matches the column used If more than one selection is appropriate use the larger flow cell to get the best detection limit Use the smaller flow cell for best peak resol
26. Remove the normal flow cell e Have cuvette with standard available 1 Locate the cuvette holder on the desk 2 Unscrew the bracket 3 Insert the cuvette with the sample into the holder The clear side of the cuvette must be visible Light path Clear side Next steps Reset the lamp counter as described in the User Interface documentation Turn the lamp ON e Give the lamp more than 10 minutes to warm up Perform Wavelength Verification Calibration on page 104to check the correct positioning of the lamp 94 1200 Series Variable Wavelength Detector User Manual Maintenance 8 4 Replace the bracket and fix the cuvette 5 Install the cuvette holder in the instrument Next steps Perform your verification 1200 Series Variable Wavelength Detector User Manual 95 8 Maintenance Correcting Leaks When required If a leakage has occurred in the flow cell area or at the capillary connections Tools required Tissue Two 1 4 inch wrenches for capillary connections Parts required None 1 Remove the front cover 2 Use tissue to dry the leak sensor area Observe the capillary connections and the flow cell area for leaks and correct if required 4 Replace the front cover Leak plane yk Waste outlet Leak sensor assembly Figure 32 Drying the Leak Sensor 96 1200 Series Variable Wavelength Detector User Manual Maintenance
27. and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with built in holmium oxide filter Housing All materials recyclable ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions cell path length 10 mm response time 2 s flow 1 ml min LC grade methanol Linearity measured with caffeine at 265 nm 26 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 3 Installing the Detector Unpacking the Detector 28 Optimizing the Stack Configuration 30 Installing the Detector 33 Flow Connections to the Detector 36 This chapter describes the installation of the detector ee Agilent Technologies 27 3 Installing the Detector Unpacking the Detector Damaged Packaging If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the detector may have been damaged during shipment CAUTION If there are signs of damage please do not attempt to install the detector Delivery Checklist Ensure all parts and materials have been delivered with the detector The delivery checklist is shown below Please report missing or damaged parts to your local Agilent Technologies sales and service office Table 4 Variable Wavelength Detector
28. are available for troubleshooting and operational verification after exchanging internal components see Test Functions in the Service Manual Wavelength Verification Recalibration Wavelength recalibration is recommended after repair of internal components and on a 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 Calibration on page 104 Diagnostic Signals The detector has several signals internal temperatures voltages and currents of lamps that can be used for diagnosing baseline problems see Diagnosis Signals in the Service Manual 1200 Series Variable Wavelength Detector User Manual Troubleshooting and Diagnostics 6 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 green yellow red Line power switch with green light Figure 28 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 Variable Wavelength Detector User Manual 73 6 74 Troubleshooting and Diagnostics Detector Status Indicator The detector status indicator indicates one of four possible detector conditions When the status
29. ated on the left side of the optical unit The reference diode assembly is located in the front of the optical unit Photo Diode ADC analog to digital converter The photo diode current is directly converted to 20 bit digital data direct photo current digitalization The data is transferred to the detector main board VWM The photo diode ADC boards are located close to the photo diodes 1200 Series Variable Wavelength Detector User Manual Introduction to the Variable Wavelength Detector 1 Electrical Connections The GPIB connector G1314B only is used to connect the detector with a computer The address and control switch module next to the GPIB connector determines the GPIB address of your detector The switches are preset to a default address and is recognized once after power is switched ON 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 One analog output provides signals for integrators or data handling systems The interface board slot is used for external contacts and BCD bottle number output or LAN connections 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 RS 232C connector may be used to control t
30. ccording 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 impaired 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 fuse holders must be avoided 1200 Series Variable Wavelength Detector User 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 c
31. cess to the lamp area Turn the lamp OFF 1200 Series Variable Wavelength Detector User Manual 85 8 Maintenance 4 Unscrew the lamp cover and remove it 5 Unscrew disconnect and replace the lamp Insert fix and reconnect the lamp ER __ E m 1 ETT ei PER ET fT R I T q Des 4 i 2 Ny f amp j 6 Replace the lamp cover 7 Replace the front cover en O m G NINE i Pe E amp Next steps Reset the lamp counter as described in the User Interface documentation Turn the lamp ON e Give the lamp more than 10 minutes to warm up Perform Wavelength Verification Calibration on page 104 to check the correct positioning of the lamp 86 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Exchanging a Flow Cell When required If 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 G1314 60086 10 mm 14 ul 40 bar Micro flow cell 5 mm 1 pl 40 bar G1314 60081 Semimicro flow cell 6 mm 5 pl 40 bar G1314 60083 High pressure flow cell 10 mm 14 pl 400 bar G1314 60082 Preparations for this procedure 1 Press the release buttons and remove the front cover
32. condensation 1200 Series Variable Wavelength Detector User Manual 23 2 Site Requirements and Specifications Physical Specifications Table2 Physical Specifications Type Weight Dimensions height x width x depth Specification Comments 11 kg 25 Ibs 140 x 345 x 435 mm 5 5 x 13 5 x 17 inches Line voltage Line frequency Power consumption 100 240 VAC 10 Wide ranging capability 50 or 60 Hz 5 220 VA 85 W 290 BTU 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 Non condensing Up to 2000 m 6500 ft Up to 4600 m 14950 ft For storing the instrument Installation Category II Pollution Degree 2 For indoor use only 24 1200 Series Variable Wavelength Detector User Manual Site Requirements and Specifications 2 Performance Specifications Table 3 Performance Specifications Agilent 1200 Series Variable Wavelength Detector Type Specification Comments Detection type Light source Wavelength range Short term noise ASTM Drift Linearity Wavelength accuracy Band width Flow cells Control and data evaluation Analog outputs Double beam photometer Deuterium lamp 190 600 nm 0 75 x 10 AU at 254 nm 3 x 104 AU hr at 254 nm gt 2 AU 5 upper l
33. crew 2 Conical Springs 3 Ring SST 4 Gasket 1 5 Window Quartz 6 Gasket 2 Figure 38 Micro Flow Cell 112 1200 Series Variable Wavelength Detector User Manual Parts and Materials for Maintenance 9 Semi micro Flow Cell Table 18 Semi micro Flow Cell Assembly Item Description Part Number Semi micro flow cell assembly 6 mm 5 ul 40 bar G1314 60083 1 Cell screw 79853 27200 Semi micro cell kit consisting of G1314 65056 two windows two 1 standard gaskets one 1 semi micro gasket and one 2 semi micro gasket 2 Conical springs pack of 10 79853 29100 3 Ring SST pack of 2 79853 22500 4 PTFE 1 standard gasket pack of 10 79853 68743 5 Quartz window pack of 2 79853 68742 6 Semi micro 1 gasket PTFE pack of 10 G1314 65057 7 Semi micro 2 gasket PTFE pack of 10 G1314 65058 Inlet capillary 400 mm long 0 12 mm i d 5021 1823 The semi micro 1 and 2 gaskets items 6 and 7 look very similar Do not mix them up 1200 Series Variable Wavelength Detector User Manual 113 9 Parts and Materials for Maintenance 1 Cell screw 2 Conical springs 3 Ring SST 4 Gasket 1 5 Quartz window 6 Semi micro gasket 1 7 Semi micro gasket 2 Figure 39 114 Semi micro Flow Cell 1200 Series Variable Wavelength Detector User Manual Parts and Materials for Maintenance 9 High Pressure Flow Cell Table 19 High Pressure Flow Cell Assembly Item Description Part
34. d 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 Halogenated solvents or mixtures which form radicals and or acids for example 2CHCl13 Og 2COClg 2ZHCI1 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 Variable Wavelength Detector User Manual 127 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 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 128 1200 Series Variable Wavelength Detector User Manual Appendix A Declaration of Conformity for HOX2 Filter Declaration of Conformity We herewith infomn you that the Holmium Oxide Glass Filter Type Hoya HY 1 Part No 79380 22711 meets the following specification of absorbance maxima positions Pee pian tue aa Accura Pal Bese ame A Irm 554 mo 0 O 79853C 1050 fm
35. d it could damage the detector 80 1200 Series Variable Wavelength Detector User Manual Maintenance and Repair 7 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 29 Using the ESD Strap 1200 Series Variable Wavelength Detector User Manual 81 7 Maintenance and Repair 82 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual e 6 Gee 8 e Maintenance S Overview of Maintenance 84 Exchanging a Lamp 85 Exchanging a Flow Cell 87 Repairing the Flow Cells 90 Using the Cuvette Holder 94 Correcting Leaks 97 Replacing Leak Handling System Parts 98 Replacing the Interface Board 99 Replacing the Detector s Firmware 100 Tests amp Calibrations 101 Intensity Test 102 Wavelength Verification Calibration 104 Holmium Oxide Test 105 This chapter describes the maintenance of the detector ee Agilent Technologies 83 8 Maintenance Overview of Maintenance The following pages describe maintenance simple repairs of the detector that can be ca
36. e purge valve Pump for approximately 10 minutes before starting your application 1200 Series Variable Wavelength Detector User Manual 41 4 Using the Detector Requirements and Conditions What You Will Need Table 7 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 Table7 What you will need 1200 system Pump plus degassing Autosampler Detector standard flow cell installed Agilent ChemStation B 02 01 and above or Instant Pilot G4208 A 01 01 and above optional for basic operation or Control Module G1323B B 04 02 and above optional for basic operation see note below System should be correctly set up for LAN communication with the Agilent ChemStation Column Zorbax Eclipse XDB C18 4 6 x 150 mm 5 um Part No 993967 902 or Part No 5063 6600 Standard Part No 01080 68704 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl 0 03 wt o terphenyl in methanol The G1314C VWD SL can be operated with a G1323B Control Module just in standard mode as G1314B no higher data rate selection is available 42 1200 Series Variable Wavelength Detector User Manual Conditions Using the Detector 4 A single injection of the isocratic test standard is made under the conditions given in Table 8 Table8 Conditions Flow Stoptime Solvent Temperature Wavelength Injection Volume 1 5 ml minute 8
37. e specific operating conditions of the instrument Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially no EMF limit should be set When instrument performance indicates maintenance is necessary take note of the values displayed by lamp 1200 Series Variable Wavelength Detector User Manual Introduction to the Variable Wavelength Detector 1 counters Enter these values or values slightly less than the displayed values 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 Variable Wavelength Detector User Manual 19 1 20 Introduction to the Variable Wavelength Detector 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 2 Site Requirements and Specifications Site Requirements 22 Physical Specifications 24 Performance Specifications 25 This chapter gives information on environmental requirements physical and performance specifications ot Agilent Technologies 21 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 see Table 2 on page 24 It accepts any li
38. egative absorbance margins 60 online plot 52 online spectra 56 peakwidth setting 50 peakwidth settings 61 preparing the HPLC system 45 priming and purging the system 40 requirements and conditions 42 response time 62 running the sample 54 sample info 53 scan range step 60 scanning 57 setting up an analysis 40 setup of detector 49 signal plot 51 signal polarity 60 special setpoints 50 60 special settings 55 stable baseline 47 stop and post time 50 stop flow condition 56 the cuvette holder 94 the detector 39 time table 50 turn on 46 typical chromatogram 44 warm up 47 zero offset 50 UV radiation 126 Ww warm up 47 warnings and cautions 79 wavelength accuracy 25 calibration 104 range 190 600 nm 25 recalibration 72 1200 Series Variable Wavelength Detector User Manual weight 24 Z zero offset 50 Index 133 Index 134 1200 Series Variable Wavelength Detector User Manual www agilent com In This Book This manual contains the technical reference information about the Agilent 1200 Series variable wavelength detector The manual describes the following e introcduction and specifications e installation e using and optimizing e troubleshooting overview e maintenance e parts identification e safety and related information Agilent Technologies 2006 Printed in Germany 02 06 G1314 90010 Agilent Technologies
39. equired after maintenance of lamps and flow cells e Intensity Test on page 102 e Wavelength Verification Calibration on page 104 e Holmium Oxide Test on page 105 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Intensity Test The intensity test measures the intensity of the deuterium lamp over the full VWD wavelength range 190 600 nm The test can be used to determine the performance of the lamp and to check for dirty or contaminated flow cell windows When the test is started 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 characteristics Therefore intensity spectra will differ slightly between instruments Figure 34 shows a typical intensity test spectrum Intensity Test Evaluation Agilent ChemStation only The Agilent ChemStation evaluates three values automatically and displays the limits for each value the average the minimum and the maximum of all data points and passed or failed for each value Test Failed Probable Causes e Absorbing solvent in flow cell e Dirty or contaminated flow cell e Dirty or contaminated optical components source lens mirrors grating Old or non Agilent lamp Suggested Actions Y Ensure the flow cell is filled with water V Repeat the test with the flow cell removed If the
40. er linearity 3 Consider to use time programming to further optimization The G1314C VWD SL can be operated with a G1323B just in standard mode as G1314B no higher data rate selection is available 1200 Series Variable Wavelength Detector User Manual 69 5 How to optimize the detector 70 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 6 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 72 Status Indicators 73 User Interfaces 75 Agilent LC Diagnostic Software 76 Overview about the troubleshooting and diagnostic features ee Agilent Technologies 71 6 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 72 Status Indicators The detector is provided with two status indicators which indicate the operational state prerun run and error states of the detector The status indicators provide a quick visual check of the operation of the detector see page 51 Error Messages In the event of an electronic mechanical or hydraulic failure the detector generates an error message in the user interface 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 Troubleshooting and Diagnostics in the Service Manual Test Functions A series of test functions
41. esults The test is passed successfully when all three wavelengths are within 1 nm of the expected value This indicates the detector is calibrated correctly The test results are currently available on the Agilent ChemStation only ChemStation revisions below B 01 xx show a limit of 2 nm It should read 1 nm If the test shows a value greater than 1 nm perform a recalibration 1200 Series Variable Wavelength Detector User Manual Maintenance 8 GNOSE VWD_HOLM DGR N 1 i 1 a iene 0 7 oe S oy 200 300 400 500 600 Wavelength nm VWD Holmium Test Results Specification Measured Result Deviation from wavelength 1 360 8 nm 1 1 nm 0 0 nm Passed Deviation from wavelength 2 418 5 nm 1 1 nm 0 1 nm Passed Deviation from wavelength 3 536 4 nm 1 1 nm 0 0 nm Passed Figure 36 Holmium Test Report Holmium Oxide Test Failed Probable Causes e Detector not calibrated Dirty or defective flow cell Dirty or defective holmium oxide filter Optical misalignment 1200 Series Variable Wavelength Detector User Manual 105 8 Maintenance Suggested Actions Y Re calibrate the detector V Repeat the test with the flow cell removed If the test is OK exchange the flow cell components V Run the holmium oxide filter test If the test fails exchange the filter assembly Y Realign the optical components 106 1200 Series Variable Wavelength Detector User Manual Maintenance
42. flow cell area against strong drafts from the outside 38 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 4 Using the Detector Setting up an Analysis 40 Before Using the System 40 Requirements and Conditions 42 Optimization of the System 44 Preparing the HPLC System 45 Running the Sample and Verifying the Results 54 Special Settings of the Detector 55 Control Settings 55 Online Spectra 56 Scanning with the VWD 57 Analog Output Settings 59 Peakwidth Settings 61 Optimizing the Detector 63 This chapter provides information on how to set up the detector for an analysis and explains the basic settings ee Agilent Technologies 39 4 Using the Detector Setting up an Analysis This chapter can be used for e preparing the system to learn the set up of an HPLC analysis and 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 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 turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the solvent reservo
43. he module from a computer through a RS 232C connection This connector is activated and can be configured with the configuration switch See your software documentation for further information e The power input socket accepts a line voltage of 100 240 volts AC 10 with a line frequency of 50 or 60 Hz Maximum power consumption is 220 VA There is no voltage selector on your module because the power supply has 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 the module cover from being 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 Variable Wavelength Detector User Manual 15 1 Introduction to the Variable Wavelength Detector Security lever Slot for interface board serial number DEmanufactured in Germany 62006 01week of last major change 00130number of unit product number serial number 613148 VWD SL Serial No 2 Agilent Technologies Agilent Vechnotogers 76337 Waiddronn Made in Germany Figure 4 CAN GPIB Configuration s
44. ht see Table 2 on page 24 allow to place the instrument on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inch 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 specifications at ambient temperatures and relative humidity as described in Table 2 on page 24 ASTM drift tests require a temperature change below 2 C hour 3 6 F hour measured over one hour period Our published drift specification refer also to Performance Specifications on page 25 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
45. iable Wavelength Detector User Manual 55 4 Using the Detector Online Spectra 1 To view the online spectra select Online Spectra NOTE This online spectrum is taken during a stop flow condition only while the peak is kept in the flow cell see Scanning with the VWD on page 57 2 Not Ready Information B B 100 00 1000 0 Figure 21 Online Spectra Window 2 Change the absorbance and wavelength range according your needs 56 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 Scanning with the VWD Access to the scan feature is only possible during run 1 Set up a run Start a run While running on the baseline select from the menu Instrument More VWD Blank Scan see Figure 22 on page 57 A background scan is stored in the memory a System 2 File RunControl instrument Method Sequence View Abort Help a 8 Met Of Pump coe SECU Injector _ Navigation Bar Set up Column Thermostat Set up VWD Signal EKG CACHEMS More Pune 5 En AFCDE More Injector gt E BATCH More Column Thermostat gt ER DEF LEA N Control Step 1 Blank Scan scan of the background 5 DGNOI ER INSTPE __ Snapshot B LOADT System On B ROBUS System Off solvent is stored in the memory Sample Scan Blank Scan Step 2 Sample Scan scan of the peak of interest is taken while the peak stays in the Gh ROUTI 7 TE flow cell st
46. ijn batterijen geleverd Wanneer deze leeg zijn moet u ze niet weggooien maar inleveren als KCA 1200 Series Variable Wavelength Detector User Manual 123 A Appendix Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises 124 1200 Series Variable Wavelength Detector User 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 At Operator Position e Normal Operation According to ISO 7779 1988 EN 27779 1991 Type Test 1200 Series Variable Wavelength Detector User Manual 125 A Appendix UV Radiation 126 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 Hygie
47. imit 1nm 6 5 nm typical Standard 14 ul volume 10 mm cell path length and 40 bar 588 psi pressure maximum High pressure 14 ul volume 10 mm cell path length and 400 bar 5880 psi pressure maximum Micro 1 ul volume 5 mm cell path length and 40 bar 588 psi pressure maximum Semi micro 5 pl volume 6 mm cell path length and 40 bar 588 psi pressure maximum Agilent ChemStation for LC Recorder integrator 100 mV or 1 V output range 0 001 2 AU one output See NOTE on page 26 See NOTE on page 26 See NOTE on page 26 Self calibration with deuterium lines verification with holmium oxide filter Can be repaired on component level 1200 Series Variable Wavelength Detector User Manual 25 2 Site Requirements and Specifications Table3 Performance Specifications Agilent 1200 Series Variable Wavelength Detector continued Type Specification Comments Communications Controller area network CAN GPIB for G1314B only GPIB RS 232C APG Remote ready start stop and shut down signals LAN optional Safety and maintenance Extensive diagnostics error detection and display through control module and Agilent ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user settable limits
48. ir 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 40 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 Table 6 Choice of Priming Solvents for Different Purposes Activity Solvent Comments After an installation Isopropanol Best solvent to flush air out of the When switching between reverse Isopropanol 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 Isopropanol 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 min 2 Flush all tubes with at least 30 ml of solvent 3 Set flow to required value of your application and close th
49. ir of the detector Table 22 Accessory Kit Parts Description Part Number Accessory kit G1314 68705 Corrugated tubing to waste re order 5 m 5062 2463 Peek outlet capillary kit i d is 0 25 mm PEEK 5062 8535 Fitting male PEEK quantity 1 0100 1516 Hex key 1 5 mm 8710 2393 Hex key 4 mm 8710 2392 Wrench open end 1 4 5 16 inch 8710 0510 Wrench open end 4 mm 8710 1534 118 1200 Series Variable Wavelength Detector User Manual This chapter provides addition information on safety legal and web Agilent 1200 Series Variable Wavelength Detector User Manual A Appendix General Safety Information 120 Lithium Batteries Information 123 Radio Interference 124 Sound Emission 125 UV Radiation 126 Solvent Information 127 Declaration of Conformity for HOX2 Filter 129 Agilent Technologies on Internet 130 ee Agilent Technologies 119 A Appendix General Safety Information 120 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 Agilent 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 a
50. is driven directly by a stepper motor This configuration allows fast change of the wavelength The cutoff filter is moved into the lightpath above 370 nm to reduce higher order light Deuterium lamp Lens Mirror M1 Sample diode l Flow cell Grating Mirror M2 Beam splitter Reference diode Figure 1 Optical Path of the Variable Wavelength Detector 1200 Series Variable Wavelength Detector User Manual 11 1 Introduction to the Variable Wavelength Detector Flow Cell A variety of flow cell cartridges can be inserted using the same quick and simple mounting system Figure 2 Cartridge Type Flow Cell Table 1 Flow Cell Data STD Semi micro High Pressure Micro Maximum pressure 40 4 40 4 400 40 40 4 bar MPa Path length 10 conical 6 conical 10 conical 5 mm Volume 14 5 14 1 ul Inlet i d 0 17 0 17 0 17 0 1 mm Inlet length 750 750 750 555 mm Outlet i d 0 25 0 25 0 25 0 25 mm Outlet length 120 120 120 120 mm Materials in contact with SST quartz SST quartz SST quartz SST quartz solvent PTFE PEEK PTFE Kapton PTFE 12 1200 Series Variable Wavelength Detector User Manual Introduction to the Variable Wavelength Detector 1 Lamp The light source for the UV wavelength range is a deuterium lamp As a result of plasma discharge in a low pressure deuterium gas the lamp emits light over the 190 to 600 nm wavelength range Source Lens Assembly The source lens receives the light
51. itrile 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 2 22 h iil 53 DEF LC M OEMULALI M DEMOCAL M DGALSTST M OGCALAS M OGCALOQ1M OGCALOQ2M Method Sequence View Abert Help sammes OBB kgl cerae Q enoc QI OGssTsT AM Q oscaasm foo V oxncgim Y caog WOK caog W Onon aos DEFAULT D W occurs W oscerrst 4 W OG TEST M W OGLOTSTM W OGEAKT M Q DNEM W oaet Q ostesT W OGywooc m E Adaa QJ tsockam E1168 hee Y moror Be s88B8888388 Figure 13 Loading Default LC Method 48 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 9 Click on the module icons Figure 14 and open the Setup of these modules Figure 15 on page 50 shows the detector settings do not change the detector parameters at this time DEFAULT D CS Set up Pump Set up VWD Signal Sony amp Control e Q Data Curves H one Spedra reee 8 Not Ready Information B Not Ready Information Help Figure 14 Open the module menu 10 Enter the pump parameters mentioned under Conditions on page 43 1200 Series Variable Wavelength Detector User Manual 49
52. le 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 WARNING To prevent personal injury be careful when getting in contact with sharp metal areas WARNING 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 for example the ESD wrist strap from the accessory kit when handling electronic boards and components see Using the ESD Strap on page 81 WARNING 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 AG 1200 Series Variable Wavelength Detector User Manual 79 7 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 WARNING Do not let liquid drip into the detector It could cause shock hazard an
53. length Calibration Yes Yes M Yes Lamp Intensity Yes Yes D Yes Holmium Yes Yes D Yes Cell Yes Yes D No 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 Variable Wavelength Detector User Manual 75 6 Troubleshooting and Diagnostics Agilent LC Diagnostic Software 76 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 Agilent 1200 Series binary pump SL G1312B Agilent 1200 Series high performance autosampler SL G1367B Agilent 1200 Series thermostatted column compartment SL G1316B 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 descri
54. lues for either 100 mV or 1 V full scale At Power On m Lamp Type a131 4 60100 I Tum lamp on m Automatic Turn On I Tum lamp on at lt dd rim ypyp gt lt hhemmiss gt OK Cancel Help of Control Signal Time gt f Analog Output fy Online Spectra r wavelength Stoptime Zero Offset Not Ready Information i as Pump 4 mi x Help 254 kom no Limit MM ER Peakwidth Responsetime Posttime Attenuation gt O1min 2s v ot min 1000 7 mau Figure 23 Analog Output Settings 3 Change the values if required 1200 Series Variable Wavelength Detector User Manual 59 4 Using the Detector Special Setpoints 1 To change the offset and the attenuation select VWD Signal More Special Setpoints set up vWD Signal E gt VD Special Setpoints System 2 x of Control Eu Online Spectra Margin for negative Absorbance piam 8 Not Ready Information Help Signal Polarity Positive Negative I Enable analysis when lamp is off Restore Defaults Scan Range fig0 to 400 nm Step ER nm m l Cancel Figure 24 Spectra Window Help Margin for negative Absorbance Use this field to modify the detector s signal handling to increase the margin for negative absorbance Use this option if for example your solvent gradient produces a decreasing baseline absorbance and fo
55. minutes 100 30 water 70 Acetonitrile Ambient sample 254 nm Tul 1200 Series Variable Wavelength Detector User Manual 43 4 Using the Detector Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 9 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 R D0 100 1401840 ON D mau 4 Figure 9 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 63 or Optimizing in the your module s Reference Manual 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 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 B 02 01 If the pump autosampler thermostatted column compartment and detector are found the ChemStation screen should look like shown in Figure 10 The System status is red Not Ready System status Latte o wren Bag oer e s EME axa No M TE O DEFAULT o ais w ro Dotai
56. nches 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 using toxic or hazardous solvents 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 1 Press the release buttons and remove the front cover to have access to the flow cell area 36 2 Remove the metal cover and install the flow cell Tighten the cell screws 1200 Series Variable Wavelength Detector User Manual Installing the Detector 3 3 Assemble the column detector capillary Depending on the flow cell type it may be a PEEK or SST capillary 4 Connect the newly assembled fitting of the capillary to the inlet connector 5 Connect the other end of the capillary to the column 6 Connect the PEEK waste capillary to the outlet connector 1200 Series Variable Wavelength Detector User Manual 37 3 Installing the Detector 7 Establish a flow and observe for leakage 8 Replace the front cover The installation of the detector is now complete The detector should be operated with the front cover in place to protect the
57. ne voltage in the above mentioned range 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 CAUTION Make sure to have easy access to the power cable of the instrument in order to disconnect the instrument from line Power Cords Different power cords are offered as options with the detector The female end of the 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 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 22 1200 Series Variable Wavelength Detector User Manual Site Requirements and Specifications 2 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 weig
58. nists Table 24 UV Radiation Limits Exposure day Effective Irradiance 8 hours 0 1 uW cm 10 minutes 5 0 W cm Typically the radiation values are much smaller than these limits Table 25 UV Radiation Typical Values Position Effective Irradiance Lamp installed 50 cm distance average 0 016 uW cm Lamp installed 50 cm distance maximum 0 14 uW cm 1200 Series Variable Wavelength Detector User Manual Appendix A Solvent Information Observe the following 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 High concentrations of inorganic acids like nitric aci
59. ns 26 attenuation 50 autobalance 50 automatic turn on 55 band width 6 5 nm 25 battery safety information 123 beam splitter 14 Beer Lambert law 67 bench space 23 boards photodiode boards ADC 14 C cable connecting APG remote 32 connecting CAN 32 connecting GPIB 32 connecting LAN 32 connecting the analog 34 connecting the APG remote 34 connecting the CAN 34 connecting the ChemStation 32 connecting the LAN 34 connecting the power 32 34 CAN 33953353533535 connecting interface 34 cautions and warnings 79 chromatogram 44 configuration stack 30 connector locations at rear 34 control module G1323B 10 75 correction factors for flow cells 68 cutoff filter 13 cuvette holder 94 D data rate 62 69 declaration of conformity 129 delivery checklist 28 detection type 25 diagnostic signals 72 dimensions 24 drift 25 47 initial 52 E electrical connections descriptions of 15 EMF early maintenance feedback 18 enable analysis when lamp is off 60 entrance slit assembly 13 environment 23 error messages 72 ESD electrostatic discharge strap 81 exchange interface board 99 F features 10 GLP 26 instrument layout 17 safety and maintenace 26 firmware updates 100 flow cell 12 choosing 66 1200 Series Variable Wavelength Detector User Manual Index correction factors 68 cuvette holder parts 116 high pressure parts 115 micro parts 112
60. op flow condition J a SEQDC Revisions amp Serial s LER seqsu Columns Online Spectrum Sample Scan minus Ea STATIE Blank Scan Configure 1100 1200 Access Figure 22 Taking Online Spectra 4 When the peak of interest enters the flow cell stop the flow set flow rate to zero or open the purge valve and wait a few moments to stabilize the concentration Turning off the pump would stop the run and no access to the sample scan is possible 1200 Series Variable Wavelength Detector User Manual 57 4 Using the Detector 5 Select from the menu Instrument More VWD Sample Scan A sample scan is taken in the range defined under Special Setpoints on page 60 and the Online Spectra window see Online Spectra on page 56 displays the result Sample Scan minus Blank Scan 58 1200 Series Variable Wavelength Detector User Manual Using the Detector 4 Analog Output Settings 1 To change the Output Range of the analog outputs select VWD Control 2 To change the offset and the attenuation select VWD Signal More ea VWD Control SS Xl Analog Output Range can be of Control m Lamp Error Method set to either 100 mV or 1 V full fy Online Spectra scale Take current method B Not Ready Information Help C off i P r Analog Output Range Zero Offset can be set to either 100 mV or 1 V full scale Cov 1 Attenuation Limits 0 98 to 4000 mAU at discrete va
61. otes 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 Variable Wavelength Detector User Manual In This Manual This manual covers the Agilent 1200 Series Variable Wavelength Detectors G1314B Agilent 1200 Series VWD G1314 Agilent 1200 Series VWD SL 1 Introduction to the Variable Wavelength Detector This chapter gives an introduction to the detector instrument overview and internal connectors 2 Site Requirements and Specifications This chapter gives information on environmental requirements physical and performance specifications 3 Installing the Detector This chapter describes the installation of the detector 4 Using the Detector This chapter provides information on how to set up the detector for an analysis and explains the basic settings 5 How to optimize the detector This chapter gives hints on how to select the detector parameters and the flow cell
62. overs 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 instrument 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 1200 Series Variable Wavelength Detector User Manual 121 A Appendix Safety Symbols Table 23 shows safety symbols used on the instrument and in the manuals Table 23 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage Indicates dangerous voltages Indicates a protected gro
63. parts see page 117 110 1200 Series Variable Wavelength Detector User Manual Parts and Materials for Maintenance 9 Standard Flow Cell Table 16 Standard Flow Cell Assembly Item Description Part Number Standard Flow Cell 10 mm 14 ul 40 bar Cell screw kit quantity 2 2 Conical spring kit quantity 10 3 Ring 1 PEEK kit quantity 2 4 Gasket 1 small hole KAPTON quantity 10 5 Window quartz kit quantity 2 6 Gasket 2 large hole KAPTON quantity 10 7 Ring 2 PEEK kit quantity 2 G1314 60086 G1314 65062 79853 29100 G1314 65065 G1314 65063 79853 68742 G1314 65064 G1314 65066 1 Cell Screw 2 Conical Springs 3 Ring 1 PEEK 4 Gasket 1 small hole 5 Window Quartz 6 Gasket 2 large hole 7 Ring 2 PEEK Figure 37 Standard Flow Cell 1200 Series Variable Wavelength Detector User Manual 111 9 Parts and Materials for Maintenance Micro Flow Cell Table 17 Micro Flow Cell Assembly Item Description Part Number Micro flow cell 5 mm 1 pl 40 bar G1314 60081 Capillary column detector SST 400 mm lg 0 12 i d 5021 1823 1 Cell screw 79853 27200 Cell kit micro comprises G1314 65052 two windows two gaskets 1 and two gaskets 2 2 Conical spring kit quantity 10 79853 29100 3 Ring SST kit quantity 2 79853 22500 4 Window quartz kit quantity 2 79853 68742 5 Gasket 1 PTFE quantity 10 79853 68743 Gasket 2 PTFE quantity 10 G1314 65053 1 Cell S
64. ptions in this manual For details refer to the help files provided with the diagnostic software 1200 Series Variable Wavelength Detector User Manual Agilent 1200 Series Variable Wavelength Detector User Manual 7 Maintenance and Repair Introduction to Maintenance and Repair 78 Warnings and Cautions 79 Cleaning the Detector 80 Using the ESD Strap 81 This chapter provides general information on maintenance and repair of the detector ot Agilent Technologies 77 7 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 83 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 Repair in the Service Manual 78 1200 Series Variable Wavelength Detector User Manual Maintenance and Repair 7 Warnings and Cautions WARNING To prevent personal injury the power cab
65. r example from 5 13 ul Typically this causes more peak dispersion As Figure 27 on page 68 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 Variable Wavelength Detector User Manual 67 5 How to optimize the detector Absorbance Analysis of pesticide standard 6 mm optical path length 10 mm optical path length Time min Figure 27 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 Series VWD it is necessary to have more precise information on path lengths of the VWD flow cells The correct response is expected response correction factor Please find below the details of the Agilent 1200 Series VWD flow cells Table 11 Correction factors for Agilent 1200 Series VWD flow cells Flow cell type Cell Part number Path length Path length Correction volume nominal actual factor Standard flow cell 14 ul G1314 60086 10 mm 10 15 0 19 mm 10 10 15 Semi micro flow cell 5 ul G1314 60083 6mm 6 10 0 19 mm 6 6 10 Micro flow cell Tul G1314 60081 5mm 4
66. r GPC analyses Limits 100 to 4000 mAU Signal Polarity can be switched to negative if required Enable analysis when lamp is off if the VWD is not used in a dual detector setup lamp off the not ready condition is not stopping the analysis Scan Range Step Used for stop flow scanning see Scanning with the VWD on page 57 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 60 1200 Series Variable Wavelength Detector User Manual Using the Detector Peakwidth Settings Do not use peak width shorter than necessary see also Set the Detector Parameters on page 69 1 To change the Peakwidth settings select Setup Detector Signals 2 In the section Peakwidth Responsetime click on the drop down list 3 Change the Peakwidth according to your needs SE Set up VWD Signal of Control fy Online Spectra 8 Not Ready Information Help WD Signal System 2 m Signal Wavelength 254 nm Peakwidth Responsetime gt O1min 2s i lt 0 00125 min lt 0 03s gt 0 00125 min 0 03 s m Tin gt 0 0025 min 0 06 s gt 0 005 min 0 12 gt 0 01 min 0 25 s gt 0 025 min 0 5 s gt 0 05 min gt 0 1min 2 s Figure 25 Peakwidth enables you to select the peak width response time for your analysis The peak width is defined as the width of a peak
67. ration System 2 xj iii Deviation HUU 12nm Zero order 12nm Max Deviation UHENT 12nm Reference lines 12nm Calibration history Deviation Zero order Ref lines Time Date 8 8nm O 8nm 21 55 49 07 02 1970 0 0nm Oinm 11 40 47 04 01 2006 Zero order deviation is 0 0nm Max deviation reference lines 0 0nm Adjust OK Cancel Calibration settings equal to measured one no calibration necessary Figure 35 Wavelength Verification Calibration The wavelength verification calibration takes about 2 5 minutes and is disabled within the first 10 minutes after ignition of the lamp because initial drift may distort the measurement When the lamp is turned ON the 656 nm emission line position of the deuterium lamp is checked automatically 1200 Series Variable Wavelength Detector User Manual 103 8 Maintenance Holmium Oxide Test 104 This test verifies the calibration of the detector against the three wavelength maxima of the built in holmium oxide filter The test displays the difference between the expected and measured maxima Figure 36 shows a holmium test spectrum The test uses the following holmium maxima e 360 8 nm 418 5 nm 536 4 nm See also Declaration of Conformity for HOX2 Filter on page 129 When to do the Test after recalibration e as part of the Operational Qualification Performance Verification procedure or e after flow cell maintenance or repair Interpreting the R
68. ries Variable Wavelength Detector User Manual Using the Detector 4 14 Select the menu item RunControl gt Sample Info and enter information about this application Figure 18 on page 53 Press OK to leave this screen SAL M Sample Info x Offline Data Analysis Operator Name Wolfgang r Data File Path JE CHEMSTATION Z DATAS x Subdirectory ISOTEST _ s Resume Injection Run Sequence F Pause Sequence Resume Sequence Manual Filename Stop RunjInject Sequence 150 O1D li Prefix Counter z p QI DGCALAS 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 H Run Method OK Cancel Help Figure 18 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 Variable Wavelength Detector User Manual 53 4 54 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 8192544 Ref 600 100 0 1101 8 10 440003 D gt MAN
69. ries variable wavelength detector are available G1314B VWD 1200 Series Variable Wavelength Detector standard version G1314C VWD SL 1200 Series Variable Wavelength Detector SL high data rates for fast HPLC The G1314C VWD SL can be operated with a G1323B Control Module just in standard mode as G1314B no higher data rate selection is available 10 1200 Series Variable Wavelength Detector User Manual Introduction to the Variable Wavelength Detector 1 Optical System Overview The optical system of the detector is shown in Figure 1 Its radiation source is a deuterium arc discharge lamp for the ultraviolet UV wavelength range from 190 to 600 nm The light beam from the deuterium lamp passes through a lens a filter assembly in position none cut off or holmium oxide an entrance slit a spherical mirror M1 a grating a second spherical mirror M2 a beam splitter and finally through a flow cell to the sample diode The beam through the flow cell is absorbed depending on the solutions in the cell in which UV absorption takes place and the intensity is converted to an electrical signal by means of the sample photodiode Part of the light is directed to the reference photodiode by the beam splitter to obtain a reference signal for compensation of intensity fluctuation of the light source A slit in front of the reference photodiode cuts out light of the sample bandwidth Wavelength selection is made by rotating the grating which
70. rn off the flow Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 87 The shown cell parts will differ depending upon the flow cell type For detailed parts schematics refer to above mentioned pages 1 Cell Screw 1 2 Conical Springs 3 Ring 1 PEEK 4 Gasket 1 small hole 5 Window Quartz 6 Gasket 2 large hole 7 Cell cover assembly 8 Ring 2 PEEK Figure 30 Standard Flow Cell 90 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Disassembling 1 Unscrew the cell screw using a 4 mm hexagonal wrench the Flow Cell 2 Remove the SST rings using a pair of tweezers 3 Use adhesive tape to remove the peek ring the window and the gasket Do not use tweezers to remove windows as the surfaces can easily be scratched CAUTION y 4 Repeat step 1 through step 3 for the other window keep the parts separate otherwise they could be mixed Cleaning the Flow 5 Pour isopropanol into the cell hole and wipe clean with a piece of lint free Cell Parts cloth 6 Clean the windows with ethanol or methanol Dry it with a piece of lint free cloth Always use new gaskets Reassembling the 7 Hold the flow cell cassette horizontally and place gasket in position Flow Cell Ensure both cell holes can be seen through the holes of gasket The semi micro 1 and 2 gaskets items 6 and 7 Semi micro Flow Cell on page 114 look very similar Do not mix them up
71. rried out without opening the main cover Table 14 Simple Repairs Procedures Typical Frequency Notes Deuterium lamp If noise and or drift exceeds your application limits or A VWD test should be performed after exchange lamp does not ignite replacement Flow cell exchange If application requires a different flow cell type A VWD test should be performed after replacement Cleaning 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 Leak sensor drying If leak has occurred Check for leaks Leak handling system If broken or corroded Check for leaks replacement 84 1200 Series Variable Wavelength Detector User Manual Maintenance 8 Exchanging a Lamp When required lf noise or drift exceeds application limits or lamp does not ignite Tools required Screwdriver POZI 1 PT3 Parts required Deuterium lamp G1314 60100 If you want to use the Agilent DAD lamp instead of the VWD lamp you have to change the lamp settings in the VWD Configuration to lamp type 2140 0590 This ensures that the DAD lamp s filament heating is operated like in the DAD The instrument specifications are based on the VWD lamp WARNING If the detector has been in use the lamp may be hot If so wait five minutes for lamp to cool down Preparations for this procedure 1 Press the release buttons and remove the front cover to have ac
72. settings analog output settings 59 peakwidth 61 setup of detector 49 signal plot 51 polarity 60 signals additional diagnostics 50 diagnostic 72 site requirements 22 bench space 23 environment 23 power considerations 22 power cords 22 solvent information 127 sound emission 125 source lens assembly 13 special setpoints 50 60 1200 Series Variable Wavelength Detector User Manual special settings 55 specifications performance 25 physical 24 spectra online 56 stable baseline 47 stack configuration 30 32 rear view 32 standards 24 status indicators 72 74 stop time post time 50 stop flow condition 56 T test functions 72 tests holmium oxide holmium oxide test 105 intensity of lamp 102 wavelength calibration 104 time table 50 troubleshooting Agilent LC diagnostic software 76 diagnostic signals 72 error messages 72 overview 72 status indicator 74 status indicators 72 73 test functions 72 user interfaces 75 turn on automatic 55 U unpacking 28 user interfaces ChemStation Control Module Instant Pilot 75 using additional signals diagnostics 50 Agilent ChemStation 45 analog output range 55 analog output settings 59 at power on 55 attenuation 50 autobalance 50 automatic turn on 55 data rate 62 detector parameters 49 drift 47 EMF 18 enable analysis when lamp is off 60 error method 55 isocratic test sample 54 lamp type 55 load method 48 n
73. t itself 1200 Series Variable Wavelength Detector User Manual 17 1 Introduction to the Variable Wavelength Detector Early Maintenance Feedback EMF 18 Maintenance requires the exchange of components which are subject to wear or stress Ideally the frequency at which components are exchanged should be based on the intensity of usage of the instrument 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 Counter The detector module provides a EMF counter for the lamp The counter 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 counter can be reset to zero after the lamp is exchanged The detector provides the following EMF counters e Deuterium Lamp On Time Using the EMF Counters The user settable EMF limits for the EMF counter enables 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 and so on therefore the definition of the maximum limits need to be determined based on th
74. und terminal o gt Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product amp WARNING A warning alerts you to situations that could cause physical injury or damage to the equipment Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A caution alerts you to situations that could cause a possible loss of data Do not proceed beyond a caution until you have fully understood and met the indicated conditions 122 1200 Series Variable Wavelength Detector User Manual Appendix A Lithium Batteries Information Danger of explosion if battery is incorrectly replaced Replace only with the same or equivalent type recommended by the equipment manufacturer Lithium batteries may not be disposed off into the domestic waste Transportation of discharged Lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries Lithium batteri Eksplosionsfare ved fejlagtig handtering Udskiftning ma kun ske med batteri af samme fabrikat og type Lever det brugte batteri tilbage til leverand ren Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten Brukt batteri returneres appararleverandoren Bij dit apparaat z
75. ution Typical peak Recommended flow cell width 0 025 min Semi micro 0 05 min flow cell Standard 0 1 min flow cell Typical flow rate 0 05 0 2 ml min 0 2 0 4 ml min 0 4 0 8 ml min 1 2 ml min Internal column diameter Figure 26 Choosing a Flow Cell 66 1200 Series Variable Wavelength Detector User Manual How to optimize the detector 5 Flow Cell Path Length Lambert Beer s law shows a linear relationship between the flow cell path length and absorbance 1 Absorbance logT log g C d where T is the transmission defined as the quotient of the intensity of the transmitted light divided by the intensity of the incident light Ip 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 of 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 27 on page 68 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 ou
76. witch 613148 VWD SL Serial No CE sms X safety standards LAU 002251 ICES NMB ON oe configuration switch wo 120 220 210 v Voltage range mavas nower consumption frequency Rear View of Detector Electrical Connections and Label NOTE The G1314C VWD SL has no GPIB connector 16 1200 Series Variable Wavelength Detector User Manual Introduction to the Variable Wavelength Detector 1 Instrument Layout The industrial design of the module 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 foam plastic spacers in which the mechanical and electronic boards components of the module 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 virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations the plastic layers help cushion the electronic and mechanical parts from physical shock and the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrumen
77. y 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 accordance 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 CAUTION A CAUTION notice den
78. zing the Detector 63 5 How to optimize the detector Optimizing the Detector Performance 66 Match the Flow Cell to the Column 66 Set the Detector Parameters 69 6 Troubleshooting and Diagnostics Overview of the Detector s Indicators and Test Functions 72 Status Indicators 73 Power Supply Indicator 73 Detector Status Indicator 74 User Interfaces 75 Agilent LC Diagnostic Software 76 7 Maintenance and Repair Introduction to Maintenance and Repair 78 Simple Repairs Maintenance 78 Exchanging Internal Parts Repair 78 Warnings and Cautions 79 1200 Series Variable Wavelength Detector User Manual Cleaning the Detector 80 Using the ESD Strap 81 8 Maintenance Overview of Maintenance 84 ExchangingaLamp 85 Exchanging a Flow Cell 87 Repairing the Flow Cells 90 Using the Cuvette Holder 94 Correcting Leaks 97 Replacing Leak Handling System Parts 98 Replacing the Interface Board 99 Replacing the Detector s Firmware 100 Tests amp Calibrations 101 Intensity Test 102 Wavelength Verification Calibration 104 Holmium Oxide Test 105 9 Parts and Materials for Maintenance Overview of Maintenance Parts 110 Standard Flow Cell 111 Micro Flow Cell 112 Semi micro Flow Cell 113 High Pressure Flow Cell 115 Cuvette Holder 116 Leak Parts 117 1200 Series Variable Wavelength Detector User Manual Accessory Kit 118 A Appendix General Safety Information 120 Lithium Batteries Information 123 Radio Interference 124 Sound Emission 125

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