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Agilent 1200 Infinity Series Diode Array Detectors

1. Autosampler a EN c S 7 E oo a i I ais Thermostat for the ALS optional Solvent cabinet Degasser optional Pump Figure 15 Recommended Two Stack Configuration for 1260 Front View Agilent 1200 Infinity Series DAD User Manual 53 3 Installing the Module Optimizing the Stack Configuration LAN to control software CAN Bus cable to Instant Pilot Thermo cable optional ae Remote cable AC Power CAN Bus cable AC Power Figure 16 Recommended Two Stack Configuration for 1260 Rear View 54 Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 Optimizing the Stack Configuration Two Stack Configuration for Agilent 1290 Infinity LC To avoid excessive height of the stack when the autosampler thermostat is added to the system it is recommended to form two stacks Some users prefer the lower height of this arr
2. p n 03394 60600 Pin 3394 Pin Agilent Signal Name Active module TTL Z 9 1 White Digital ground a NC 2 Brown Prepare run Low 3 3 Gray Start Low z NC 4 Blue Shut down Low 5 NC 5 Pink Not connected i NC 6 Yellow Power on High o 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to 3396 Series II 3395A Integrators Use the cable Agilent module to 3396A Series I integrators p n 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready Agilent 1200 Infinity Series DAD User Manual Identifying Cables 12 Agilent Module to 3396 Series III 3395B Integrators p n 03396 61010 Pin 33XX Pin Agilent Signal Name Active module TTL 9 1 White Digital ground gt NC 2 Brown Prepare run Low e 3 3 Gray Start Low m s NC 4 Blue Shut down Low e O a NC 5 Pink Not connected NC 6 Yellow Power on High o 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent Module to Agilent 35900 A D Converters p n 5061 3378 Pin 35900 A D Pin Agilent Signal Name Active module TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pink 5 Pink Not connected 6 Yellow 6
3. p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module 1 1 BCD5 20 2 2 BCD7 80 8e 7 3 3 BCD 6 40 B 4 4 BCD 4 10 5 5 BCDO 1 1e 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 238 Agilent 1200 Infinity Series DAD User Manual CAN LAN Cables Identifying Cables 12 Both ends of this cable provide a modular plug to be connected to Agilent modules CAN or LAN connectors CAN Cables p n 5181 1516 5181 1519 LAN Cables p n 5023 0203 5023 0202 Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection Agilent 1200 Infinity Series DAD User Manual 239 12 Identifying Cables RS 232 Cable Kit p n Description G1530 60600 RS 232 cable 2m RS232 61600 RS 232 cable 2 5m Instrument to PC 9 to 9 pin female This cable has special pin out and is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 5181 1561 RS 232 cable 8m 240 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 13 Appendix Safety 242 The Waste Electrical and Electronic Equipment Directive 246 Radio Inte
4. Agilent 1200 Infinity Series DAD User Manual 215 10 Maintenance Replacing the Max Light Cartridge Cell 10 Slide the cell cartridge holder completely into the module 11 Lift the two levers into the upper final position to fix the cell 12 Remove the plugs from the CELL IN and CELL OUT keep 13 Connect the inlet capillary to CELL IN left and the waste them safe tubing to CELL OUT right 216 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Replacing the Max Light Cartridge Cell 14 Close the front cover Agilent 1200 Infinity Series DAD User Manual 217 10 Maintenance Cleaning of Max Light Cartridge Cell When Low counts on Intensity Test or Cell Test failed tests Tools required Alcohol lso propanol or Ethanol Lens tissue or 0 tips Cell cleaning fluid 1 L p n 5062 8529 1 Flush the flow cell with the alcohol for some time 2 Remove the cell from the cartridge holder see Replacing the Max Light Cartridge Cell on page 213 3 Carefully clean the light inlet and outlet of the cell using lens tissue or Q tips with alcohol If Q tips are used ensure that no cotton fluff remains at the inlet or outlet Do not touch the light inlet and outlet of the cell with your fingers This will add a layer of contamination on the window and reduce the light throughput 4 Flush the flow cell with water and repeat the Intensity Test and
5. 98 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 5 Using the Module Preparing the Detector 100 Setting up the Detector with Agilent ChemStation 101 The Detector GUI 103 Control Settings 106 Method Parameter Settings 107 General Method Settings 108 Advanced Method Parameter Settings 110 Spectrum Settings 111 Other Advanced Method Parameter Settings 113 Time Table Settings 114 Instrument Curves 116 Instrument Configuration 117 Main Screens of the Detector with Agilent Instant Pilot G4208A 119 This chapter provides information on how to set up the module for an analysis and explains the basic settings ot Agilent Technologies 99 5 Using the Module Preparing the Detector 100 For best performance of the detector Let the lamp warm up and stabilize for at least one hour initial turn on of the module requires a longer time depending on the environment and the application needs refer to Specification Conditions on page 43 For high sensitivity measurements a stable environment is required refer to Environment on page 39 Prevent drafts from air condition systems Setting an appropriate reference wavelength could improve the baseline behavior Alternatively use the 1 6 uL heat exchanger from the G1316C TCC Do not work with removed front panels When the front panel of the G1316C TCC typically located below the detector is removed while the TCC i
6. Notices Agilent Technologies Inc 2010 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 64212 90010 Edition 06 2010 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn 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 merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance 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
7. 1 1467E 05 Intensity Spectrum with Flow Ce 1E 05 80000 Z o0 i 40000 20000 Figure 62 Cell Test Signals Test Failed low ratio value Cell Test Evaluation Probable cause Suggested actions 1 Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles 2 Dirty or contaminated flow cell Clean the flow cell as described in Cleaning of Max Light Cartridge Cell on page 218 184 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Quick Noise Test The quick noise test measures the noise of the detector with Max Light Cartridge Cell or with Max Light Cartridge Test Cell installed in one minute intervals over a total of 5 minutes The noise of the detector is calculated by using the maximum amplitude for all random variations of the detector signal of frequencies greater than one cycle per hour The noise is determined for 5 one minute intervals and is based on the accumulated peak to peak noise for the intervals At least seven data points per cycles are used in the calculation The cycles in the noise determination are not overlapping If the test is performed with the Max Light Cartridge Test Cell the test results are not influenced by solvent or pump effects When In case of noise and drift problem Parts required Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Preparations Detect
8. If the Agilent BootP Service program is not already installed on your PC then install it from your Agilent ChemStation DVD located in folder BootP About Agilent BootP Service The Agilent BootP Service is used to assign the LAN Interface with an IP address The Agilent BootP Service is provided on the ChemStation DVD The Agilent BootP Service is installed on a server or PC on the LAN to provide central administration of IP addresses for Agilent instruments on a LAN The BootP service must be running TCP IP network protocol and cannot run a DHCP server 74 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 How BootP Service Works When an instrument is powered on an LAN Interface in the instrument broadcasts a request for an IP address or host name and provides its hardware MAC address as an identifier The Agilent BootP Service answers this request and passes a previously defined IP address and host name associated with the hardware MAC address to the requesting instrument The instrument receives its IP address and host name and maintains the IP address as long as it is powered on Powering down the instrument causes it to lose its IP address so the Agilent BootP Service must be running every time the instrument powers up If the Agilent BootP Service runs in the background the instrument will receive its IP address on power up The Agilent LAN Interface can be set to store the IP address and will not lose the
9. 1273 0 4 0 Ref 360 0 100 0nm 1280 0 4 0 Ref 360 0 100 0 nm 250 0 100 0 Ref 360 0 100 0nm Cancel E 1190 0 nm 400 0 nm step 2 0 nm Agilent 1200 Infinity Series DAD User Manual 121 5 Using the Module Main Screens of the Detector with Agilent Instant Pilot G4208A Maintenance DAD The Maintenance screen allows EMF setup Maintenance calibrate cell lamp info logging of maintenance activities module identification blinking LED Firmware Updates can be done via the System Maintenance screen a The Diagnose screen provides access to module specific tests Lamp Intensity e Calibration e Cell Cell test No Pass Fail result 122 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 6 Optimizing the Detector Introduction 124 Optimization Overview 125 Choosing a Flow Cell 126 Optimizing for Sensitivity Selectivity Linearity and Dispersion 127 Flow Cell Path Length 127 Peak width response time 129 Sample and Reference Wavelength and Bandwidth 131 Slit Width G4212A 134 Optimizing Spectral Acquisition 136 Margin for Negative Absorbance 137 Optimizing Selectivity 138 Quantifying Coeluting Peaks by Peak Suppression 138 Ratio Qualifiers for Selective Detection of Compound Classes 140 Optimizing the Detector Regarding to the System 142 Delay Volume and Extra Column Volume 142 How to Configure the Optimum Delay Volume 142 How
10. 4 To change a parameter follows the style parameter value for example ip 134 40 28 56 Then press Enter where parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to that parameter Each parameter entry is followed by a carriage return Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 5 Use the and press Enter to list the current settings cv Telnet 134 40 30 205 L gt information about the LAN interface s MAC address initialization mode Init Mode Initialization mode is Using Stored TCP IP Properties active TCP IP settings 40 30 205 255 248 808 4 a Controllers gt no connections om TCP IP status here ready Figure 36 Telnet Current settings in Using Stored mode connected to PC with controller software e g Agilent ChemStation here not connected 6 Change the IP address in this example 192 168 254 12 and type to list current settings ev Telnet 134 40 30 205 i gt ip 192 168 284 12 change of IP setting to SNN SASS ESCO Initialization mode is Using Stored MAC Addy gt 6636D317521C Init Mode ing Stored active TCP IP settings stored TCP IP settings in non volatile memory connected to PC with controller software e g Agilent Kanbaotiass Sone OANGEAN ChemStation here not connected Figure 37 Telnet Change IP settings Agilent 1200 Infinity Series DAD User Manual 87
11. 2 Uncheck the Do you want to log BootP requests once all instruments have been added The Do you want to log BootP requests box must be unchecked when you have finished configuring instruments otherwise the log file will quickly fill up disk space 3 Click Edit BootP Addresses The Edit BootP Addresses screen appears 4 Click Add The Add BootP Entry screen appears x Mac Address Host Name IP Address Figure 29 Enable BootP logging 80 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 5 Make these entries for the instrument e MAC address e Host name Enter a Hostname of your choice The Host Name must begin with alpha characters i e LC1260 e IP address e Comment optional e Subnet mask e Gateway address optional The configuration information entered is saved in the Tab File Click OK Leave Edit BootP Addresses by pressing Close Exit BootP Settings by pressing OK After each modification of the BootP settings i e EditBootPSettings a stop or start of the BootP service is required for the BootP service to accept changes See Stopping the Agilent BootP Service on page 82 or Restarting the Agilent BootP Service on page 83 oo N OQ 10 Power cycle the Instrument OR If you changed the IP address power cycle the instrument for the changes to take effect 11 Use the PING utility to verify connectivity by opening a command window and typing Ping 10 1 1 101 for
12. 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol 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 Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF Agilent 1200 Infinity Series DAD User Manual 249 13 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 modules for download 250 Agilent 1200 Infinity Series DAD User Manual Index Index 8 bit configuration switch on board LAN 28 without On Board LAN 30 A accessory kit parts 228 accessory kit 47 advanced method parameter settings using 110 Agilent Diagnostic software 156 Agilent Lab Advisor software 156 Agilent Lab Advisor 156 Agilent ChemStation Setup 90 on internet 250 algae 249 ambient operating temperature 40 ambient non operating temperature 40 analog signal output 42 analog signal 25 analog cable 232 apg remote 26 array diode 16 astm drift 188 ASTM environmental conditions 39 automatic configuration with Bootp 74 B bandwid
13. Exchange the UV lamp Please contact your Agilent service representative Please contact your Agilent service representative The processor monitors the UV lamp current during the ignition cycle If the lamp current does not rise above the lower limit within 2 5 seconds the error message is generated Probable cause 1 Lamp too hot Hot gas discharge lamps may not ignite as easily as cold lamps 2 Lamp disconnected 3 Defective UV lamp or non Agilent lamp 4 Defective detector main board 5 Defective power supply Agilent 1200 Infinity Series DAD User Manual Suggested actions Switch off the lamp and allow it to cool down for at least 15 minutes Ensure the lamp is connected Exchange the UV lamp Please contact your Agilent service representative Please contact your Agilent service representative 167 8 Error Information UV Heater Current The UV lamp heater current is missing During UV lamp ignition the processor monitors the heater current If the current does not rise above the lower limit within one second the error message is generated Probable cause 1 Lamp disconnected 2 Ignition started without the top foam in place 3 Defective UV lamp or non Agilent lamp 4 Defective detector main board 5 Defective power supply Calibration Values Invalid Suggested actions Ensure the UV lamp is connected Please contact your Agilent service representative Exchange the
14. Preparations 188 The ASTM noise test determines the detector noise over a period of 20 minutes The test is done with installed Max Light Cartridge Cell or Max Light Cartridge Test Cell This test does also check for the drift It is also part of the Self Test without checking for the drift If the test is performed with the Max Light Cartridge Test Cell the test results are not influenced by solvent or pump effects In case of noise and drift problem Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Detector and UV lamp must be on for at least 2 hours ASTM measurements based on specifications may require longer stabilization times When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 ASTM Drift and Noise Test 1 Run the ASTM Drift and Noise Test with the recommended user interface for further information see Online Help of user interface ASTM Drift and Noise Test Description G4212A PROO100015 Passed 7 9 2009 3 52 03 PM 7 9 2009 4 12 26 PM EERNERREREEEENEN The test performs ASTM Drift and Noise evaluation without reference cei Produet mmber ozen C C e dR omn Sonal ae vale at 254 m W Figure 66 ASTM Drift and Noise Test Signals Agilent 1200 Infinity Series DAD User Manual 189 9 Test Functions and Calibration
15. Yes Yes Yes Yes No No No No No Yes Yes Yes CAN DC OUT for CAN slaves Yes THERMOSTAT for G1330B Yes THERMOSTAT for G1330B CAN DC OUT for CAN slaves Yes Yes Yes 22 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Table1 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD LAN RS 232 Analog APG Special optional on board Remote G4212A B DAD 2 No Yes Yes 1 Yes G1315C DAD VL 2 No Yes Yes 2 Yes G1365C MWD G1315D DAD VL G1365D MWD VL G1321B FLD 2 Yes No Yes 1 Yes G1362A RID G4280A ELSD No No No Yes Yes Yes EXT Contact AUTOZERO Others G1316A C TCC 2 No No Yes No Yes G1322A DEG No No No No No Yes AUX G1379B DEG No No No Yes No No AUX G4227A Flex Cube 2 No No No No No G4240A CHIP CUBE 2 Yes No Yes No Yes CAN DC OUT for CAN slaves THERMOSTAT for G1330A B NOT USED The detector DAD MWD FLD VWD RID is the preferred access point for control via LAN The inter module communication is done via CAN e CAN connectors as interface to other modules e LAN connector as interface to the control software RS 232C as interface to a computer e REMOTE connector as interface to other Agilent products e Analog output connector s for signal output Agilent 1200 Infinity Series DAD User Manual 23 1 24 Introduction Overview Interfaces CAN The CAN is inter module communication interface It is a 2 wire serial bus system supporting high
16. on page 48 1 Remove the front cover 2 Remove the black hoods from the cell interfaces in out and store them in the plastic case provided with the Max Light Cartridge Flow Cell 60 Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 Flow Connections to the Detector 3 Locate the flow cell cartridge 4 Unlock the flow cell cartridge by pulling the lever to the front 5 The lever should be in the final down position 6 Pull the flow cell cartridge completely out towards the front Agilent 1200 Infinity Series DAD User Manual 61 3 Installing the Module Flow Connections to the Detector Remove the black hoods from the cell interfaces in out and insert the cell into the cell cartridge holder 8 Slide the cell cartridge holder completely into the module cell 10 Remove the plugs from the CELL IN and CELL OUT keep them safe 62 Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 Flow Connections to the Detector 11 Connect the inlet capillary to CELL IN left and the waste 12 Close the front cover tubing to CELL OUT right 13 Route the inlet capillary and waste tubing towards their destinations NOTE The detector should be operated with the front cover in place to protect the flow cell area against strong drafts from the outside NOTE If the flow cell is replaced by
17. s Assemblies 224 This chapter describes the maintenance of the module ee Agilent Technologies 203 10 Maintenance Warnings and Cautions WARNING Toxic flammable and hazardous solvents samples and reagents The handling of solvents samples and reagents can hold health and safety risks gt When working with these substances observe appropriate safety procedures for example by wearing goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the vendor and follow good laboratory practice gt The amount of substances should be reduced to the minimal volume required for the analysis gt Do not operate the instrument in an explosive atmosphere WARNING Eye damage by detector light 2 Eye damage may result from directly viewing the UV light produced by the lamp of the optical system used in this product gt Always turn the lamp of the optical system off before removing it WARNING Electrical shock Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened gt Do not remove the metal top cover of the module No serviceable parts inside gt Only certified persons are authorized to carry out repairs inside the module 204 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Personal injury or damage to the product Agilent is not responsible for any damages caused in wh
18. 1 1 1 Preparations Turn the pump off 64212 60008 G4212 60007 G4212 60011 Max Light Cartridge Flow Cell 10 mm V o 1 0 pl Max Light Cartridge Flow Cell 60 mm V o 4 0 pL Max Light Cartridge Test Cell The flow cell is shipped with a filling of isopropanol This is to avoid breakage due to subambient conditions In case the flow cell is not used for some time stored then flush the flow cell with iso propanol 1 Remove the front cover 2 Locate the cell area Agilent 1200 Infinity Series DAD User Manual 213 10 Maintenance Replacing the Max Light Cartridge Cell 3 Disconnect the inlet capillary to CELL IN left and the 4 Unlock the cell cartridge holder by pulling the lever to the waste tubing to CELL OUT right front front 214 Agilent 1200 Infinity Series DAD User Manual 10 Maintenance Replacing the Max Light Cartridge Cell 7 Remove the cell from the cartridge holder 8 Replace the black hoods A to the cell interfaces in out and insert plugs B for save storage The hoods and the plugs should be always in place to protect the flow cell For longer storage the flow cell should be flushed and filled with isopropanol to prevent the grow of algae Store it in the plastic case provided with the Max Light Cartridge Flow Cell 9 Remove the black hoods from the cell interfaces in out and insert the cell into the cell cartridge holder
19. Interfaces and available test functions Interface Comment Available Function Agilent Instrument Utilities Agilent Lab Advisor Agilent ChemStation Agilent Instant Pilot Maintenance tests are available All tests are available No tests available Adding of temperature lamp signals to chromatographic signals possible Some tests are available Intensity Cell WL Calibration Self Test Intensity Quick Noise ASTM Drift and Noise Cell Dark Current D A Converter Slit G4212A only WL Verification WL Calibration Test Chromatogram Tools Spectra Scan Tools Module Infos Tools Diagnostic Tools Temperature main board Temperature optical unit Lamp anode voltage Intensity WL Calibration Cell For details on the use of the interface refer to the interface documentation Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Use of Max Light Cartridge Test Cell The Test Cell Cartridge provided with every detector is recommended to be used for several tests instead of the used Max Light Cartridge Cell 10 mm o 1 ul or 60 mmo 4 ul because it allows running the test s without any influence of the rest of the system degasser pump sampler and others The results of the test cell are comparable with the Max Light Cartridge Cell 10 mmo 1 ul filled with water e g Intensity Profile Only the Absorbance value is higher on the Max Light Cartridge Cell I
20. SLW 4 RT 2s Board Temperature a Optical Temperature Figure 56 Detector Warm up 2 hour 150 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 7 Troubleshooting and Diagnostics Overview of the Module s Indicators and Test Functions 152 Status Indicators 153 Power Supply Indicator 153 Module Status Indicator 154 Available Tests vs User Interfaces 155 Agilent Lab Advisor Software 156 Overview about the troubleshooting and diagnostic features ee Agilent Technologies 151 7 Troubleshooting and Diagnostics Overview of the Module s Indicators and Test Functions Status Indicators The module is provided with two status indicators which indicate the operational state prerun run and error states of the module The status indicators provide a quick visual check of the operation of the module Error Messages In the event of an electronic mechanical or hydraulic failure the module 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 chapter Error Information Test Functions A series of test functions are available for troubleshooting and operational verification after exchanging internal components see Tests and Calibrations Diagnostic Signals The module has several signals internal temperature
21. When Parts required Preparations 180 The intensity test measures the intensity of the UV lamp over the full wavelength range 190 640 nm Four spectral ranges are used to evaluate the intensity spectrum The test is used to determine the performance of the lamp and optics see also Cell Test on page 183 When the test is started the 1 nm slit is moved into the light path automatically G4212A To eliminate effects due to absorbing solvents the test should be done with water in the Max Light Cartridge Cell or with the Max Light Cartridge Test Cell The shape of the intensity spectrum is primarily dependent on the lamp grating and diode array characteristics Therefore intensity spectra will differ slightly between instruments In case of UV lamp problem drift noise Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Lamp must be on for at least 10 minutes Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Intensity Test 1 Run the Intensity Test with the recommended user interface for further information see Online Help of user interface Intensity Test Description The test scans the Intensity spectrum generated by the UV G4212A PRO0100015 ST Passed 71912009 2 14 09 PM 719 2009 2 14 30 PM cser2 soon C cae a RO hes Irtnaty m Range 190 3500 151611 Cons hes intenstyinRanpe St 60mm 58691 Coos E Figure 59
22. and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION 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 damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions 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 correc
23. as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used Agilent 1200 Infinity Series DAD User Manual 245 13 Appendix The Waste Electrical and Electronic Equipment Directive Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all electric and electronic appliances starting with 13 August 2005 This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring and Control Instrumentation product s Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information 246 Agilent 1200 Infinity Series DAD User Manual Appendix 13 Radio Interference Cables supplied by Agilent Technologies are screened to provide optimized protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for measurements on open set ups the user has to assure that un
24. chromatographic resolution peak resolution versus sensitivity versus disk space sensitivity versus selectivity sensitivity versus linearity baseline drift due to RI effects spectral resolution sensitivity and linearity Agilent 1200 Infinity Series DAD User Manual 125 126 Optimizing the Detector Choosing a Flow Cell The Max Light Cartridge Cell with path length 10 mm and volume 0 1 0 ul covers a wide range of applications all column diameter down to at least 2 1 mm ID or even less e applications with peak dispersion Peakwidth x flow down to 2 ul example pw 0 04 min at flow 0 1 ml min gives peak dispersion of 0 04 min x 0 1 ml min 0 004 ml 4 ul If higher sensitivity is necessary the Max Light Cartridge Cell with path length 60 mm and volume 6 4 uL can be used This cell enhances the detector by lowering the limit of detection LOD by a factor of about 3 depending on the application Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Optimizing for Sensitivity Selectivity Linearity and Dispersion Flow Cell Path Length Lambert Beer s law shows a linear relationship between the flow cell path length and absorbance Absorbance log T log exCxd where T is the transmission defined as the quotient of the intensity of the transmitted light I divided by the intensity of the incident light Io is the extinction coefficient which is a char
25. serial number serial number production date production date accumulated UV on time in hours nominal path length of the cell in mm actual UV lamp on time in hours cell volume 0 in ul number of ignitions maximum pressure in bar date of last intensity test date of last cell test The pressure value is always displayed in bar even if the user interface uses other units e g PSI Serial Number and Firmware Revision The user interface provides module specific information that is stored in the main board These are for example the serial number firmware revision 224 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual J 6 eec 11 e Parts and Materials for Maintenance J Overview of Maintenance Parts 226 Accessory Kits 228 This chapter provides information on parts for maintenance ot Agilent Technologies 225 11 Parts and Materials for Maintenance Overview of Maintenance Parts Item p n 1 5190 0917 2 G4212 60008 3 G4212 60007 4 G4212 60011 5 5067 4660 6 5062 2462 7 5067 4691 8 5041 8388 9 5041 8389 10 5063 6527 11 G4212 40027 12 G4208A Description Long life Deuterium lamp 8 pin with RFID tag Max Light Cartridge Flow Cell 10 mm V o 1 0 pl Max Light Cartridge Flow Cell 60 mm V o 4 0 pL Max Light Cartridge Test Cell Inlet Capillary SST 0 12 mm I D 220 mm long Teflon Tubing flexible i d 0 8 mm o d 1 6 mm 2 m re ord
26. use lamp tag 5190 0917 compatible without continuous heating 5190 0916 compatible continuous heating Automatic Tum On Tum on at wernina x A Non original Agilent lamp used You may be using the device outside of the guaranteed specification Coxe _cm_ 106 Lamps can be turned ON OFF At Power On automatic lamp on at power on Analog Output Range can be set to either 100 mV or 1 V full scale 1 V default UV lamp Tag Automatic detects a lamp with RFID tag If no RFID tag lamp is used UV lamp not ready is displayed and it cannot be ignited A compatible mode has to be selected based on the used lamp see Non RFID tag lamp information below Automatic Turn On The module can be turned on at a specified date time If Turn UV lamp on at power on is set the lamp is turned on as well Non RFID tag lamp In case a non RFID tag lamp is used the user interface will show this when selecting a compatible mode You may operate the detector outside of the guaranteed specification Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Setting up the Detector with Agilent ChemStation Method Parameter Settings NOTE These settings are available via Menu Instrument Setup Instrument Method or via right click on the active area of the detector GUI The Instrument Curves tab is not shown when opening the method parameter settings via right mouse click on the detector GUI
27. 88 4 LAN Configuration 7 When you have finished typing the configuration parameters type exit and press Enter to exit with storing parameters ex C WINDOWS system32 cmd exe Agilent Technologies G4212A PR66160015 exit Connection to host lost GENS Figure 38 Closing the Telnet Session If the Initialization Mode Switch is changed now to Using Stored mode the instrument will take the stored settings when the module is re booted In the example above it would be 192 168 254 12 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Manual Configuration With the Instant Pilot G4208A To configure the TCP IP parameters before connecting the module to the network the Instant Pilot G4208A can be used 1 From the Welcome screen press the More button 2 Select Configure 3 Press the DAD button 4 Scroll down to the LAN settings lt Not Set gt Use lamp tag settings OV 1V_ output range Stays off at power on 40 28 56 255 255 255 0 LAN Def Gateway 134 40 24 1 x Cancel Valid from 0 to 255 JR 16 08 Figure 39 Instant Pilot LAN Configuration Edit mode 5 Press the Edit button only visible if not in Edit mode perform the required changes and press the Done button 6 Leave the screen by clicking Exit Agilent 1200 Infinity Series DAD User Manual 89 4 LAN Configuration PC and Agilent ChemStation Setup PC and Agilent ChemStation Setup PC Setup for Local Con
28. Broad band universal detection Narrow band selective detection e Sensitivity for a specific analyte Broad band or universal detection works by having a wide bandwidth to detect any species with absorbance in that range For example to detect all absorbing molecules between 200 nm and 300 nm set a signal at 250 nm witha bandwidth of 100 nm The disadvantage is that sensitivity will not be optimal for any one of those molecules Narrow band or selective detection is used most often The UV spectrum for a particular molecule is examined and an appropriate absorbance maximum is selected If possible the range where solvents absorb strongly should be avoided below 220 nm for methanol below 210 nm for acetonitrile For example in Figure 54 on page 146 anisic acid has a suitable absorbance maximum at 252 nm A narrow bandwidth of 4 nm to 12 nm generally gives good sensitivity and is specific for absorbance in a narrow range Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 The narrow band can be optimized for sensitivity for a specific molecule As the bandwidth is increased the signal is reduced but so is the noise and there will be an optimum for best S N As an approximate guide this optimum is often close to the natural bandwidth at half height of the absorption band in the UV spectrum In the anisic acid example this is 30 nm The analytical wavelength is usually set at a wavelength maximum to increase sensiti
29. C C SSCSC d ee Dzaba tne Devan orem Absckte 02 Aipha Une Devan onem C Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Wavelength Calibration The detector uses the alpha 656 1 nm and beta 486 nm emission lines of the deuterium lamp for wavelength calibration The sharp emission lines enable more accurate calibration than is possible with holmium oxide When recalibration is started the 1 nm slit is moved into the light path automatically G4212A The gain is set to zero On completion of the scan the alpha and beta line deviations in nm are displayed These values indicate how far the detector calibration deviates from the actual positions of the alpha and beta emission lines After calibration the deviation is zero To eliminate effects due to absorbing solvents install the Max Light Cartridge Test Cell before starting the test When The detector is calibrated at the factory and under normal operating conditions should not require recalibration However it is advisable to recalibrate after maintenance flow cell or UV lamp after repair of components in the optical unit after exchange of the optical unit or main board after significant environmental condition changes temperature humidity ata regular interval at least once per year for example prior to an Operational Qualification Performance Verification procedure and when chromatographic results in
30. IP address if power cycled Situation Cannot Establish LAN Communication If a LAN communication with BootP service cannot be established check the following on the PC e Is the BootP service started During installation of BootP the service is not started automatically Does the Firewall block the BootP service Add the BootP service as an exception e Is the LAN Interface using the BootP mode instead of Using Stored or Using Default modes Agilent 1200 Infinity Series DAD User Manual 75 4 76 LAN Configuration Installation of BootP Service Before installing and configuring the Agilent BootP Service be sure to have the IP addresses of the computer and instruments on hand 1 2 3 Log on as Administrator or other user with Administrator privileges Close all Windows programs Insert the Agilent ChemStation software DVD into the drive If the setup program starts automatically click Cancel to stop it 4 Open Windows Explorer 5 Go to the BootP directory on the Agilent ChemStation DVD and double click BootPPackage msi If necessary click the Agilent BootP Service icon in the task bar The Welcome screen of the Agilent BootP Service Setup Wizard appears Click Next The End User License Agreement screen appears Read the terms indicate acceptance then click Next The Destination Folder selection screen appears Install BootP to the default folder or click Browse to choose another location Click
31. Intensity Test Results Figure 60 Intensity Test Signals Agilent 1200 Infinity Series DAD User Manual 181 9 182 Test Functions and Calibration Test Failed Intensity Test Evaluation Probable cause 1 Absorbing solvent or air bubble in flow cell 2 Incorrect calibration 3 Dirty or contaminated flow cell 4 Dirty or contaminated optical components 5 Old UV lamp 6 Defect optical unit Suggested actions Ensure the flow cell is filled with water and free from air bubbles Repeat test with Max Light Cartridge Test Cell and compare results Recalibrate and repeat the test Run the cell test If the test fails flush the flow cell See also Cleaning of Max Light Cartridge Cell on page 218 Please contact your Agilent service representative t Exchange the UV lamp If the test fails with Max Light Cartridge Test Cell and new UV lamp please contact your Agilent service representative If only one range fails and the application does not require this range the lamp may not be changed Agilent 1200 Infinity Series DAD User Manual Cell Test When Parts required Preparations Test Functions and Calibration 9 The cell test measures the intensity of the UV lamp over the full wavelength range 190 690 nm once with the Max Light Cartridge Cell installed and once with the Max Light Cartridge Test Cell The resulting intensity ratio is a measure of the amount of light a
32. Next The default location for installation is C Program Files Agilent BootPService 10 Click Install to begin installation Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 11 Files load when finished the BootP Settings screen appears BootP Settings BootP Tab File Create Tab File Edit BootP Addresses Logging B BootP Log File Ed SAT Ts Default Settings Subnet mask 0 03 10 10 Gateway 0 0 0 0 Cancel Help Figure 27 BootP Settings screen 12 In the Default Settings part of the screen if known you can enter the subnet mask and gateway Defaults can be used The default subnet mask is 255 255 255 0 The default gateway is 10 1 1 101 13 On the BootP Settings screen click OK The Agilent BootP Service Setup screen indicates completion 14 Click Finish to exit the Agilent BootP Service Setup screen 15 Remove the DVD from the drive This completes installation 16 Start the BootP service On the Windows desktop select Start gt Control Panel gt Services Select the Agilent BootP Service and click Start Agilent 1200 Infinity Series DAD User Manual 77 4 LAN Configuration Two Methods to Determine the MAC Address Enabling logging to discover the MAC address using BootP If you want to see the MAC address select the Do you want to log BootP requests check box 1 Open BootP Settings from Start gt All Programs gt Agilent BootP S
33. Please contact your Agilent service representative Links 2 Detector is exposed to illegal ambient Verify that the ambient conditions are within the conditions allowed range Agilent 1200 Infinity Series DAD User Manual 169 8 Error Information Illegal Value From Air Inlet Temperature Sensor This temperature sensor located on the detector main board delivered a value outside the allowed range The parameter of this event equals the measured temperature in 1 100 centigrade As a result the temperature control is switched off Probable cause Suggested actions 1 The temperature sensor is defect Please contact your Agilent service representative 2 Detector is exposed to illegal ambient Verify that the ambient conditions are within the conditions allowed range Heater Failed Every time the deuterium lamp or the tungsten lamp is switched on or off a heater self test is performed If the test fails an error event is created As a result the temperature control is switched off Probable cause Suggested actions 1 Defective connector or cable Please contact your Agilent service representative 2 Defective heater Please contact your Agilent service representative 170 Agilent 1200 Infinity Series DAD User Manual Error Information 8 Heater Power At Limit The available power of the heater reached either the upper or lower limit This event is sent only once per run The parameter determines which limit has been hit 0 m
34. Stack Configuration 53 Installing the Detector 57 Flow Connections to the Detector 60 Initial Recalibration 64 This chapter provides information on unpacking checking on completeness stack considerations and installation of the module ee Agilent Technologies 45 3 Installing the Module Unpacking the Module Damage to the module CAUTION 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 instrument may have been damaged during shipment Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your site and initiate appropriate actions CAUTION Condensation Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation 46 Agilent 1200 Infinity Series DAD User Manual Delivery Checklist In
35. Switches to additional instrument signals for troubleshooting Toggles to Advanced Settings actual window Toggles to Timetable Settings Opens the Time table graph 20 10 min 2 0 s response ime 25 Hz Stogtine Postime T mu em ox aw c e _ Agilent 1200 Infinity Series DAD User Manual 107 5 Using the Module General Method Settings Signals Signals Use Wave Band Reference Reference Signal length width Wavelength Bandwidth Signal A v 2540 40 gt v 3600 gt 1000 nm Signal B v 2100 40 gt v 3600 100 0 nm Signal C v 2140 40 gt v 3600 gt 1000 nm Signal D v 2300 40 gt v 3600 1000 nm Signal E v 2600 lt 40 gt vV 3600 1000 nm Signal F nm Signal G nm Signal H nm Peakwidth Peakwidth gt 0 10 min 2 0 s response time 2 5 H2 v Stoptime 108 lt 0 0016 min 0 016s response time 160 H2 gt 0 0016 min 0 03s response time 160 Hz gt 0 003 min 0 062 s response time 80 Hz J gt 0 006 min 0 12 s response time 40 H2 gt 0 012 min 0 25 s response time 20 Hz gt 0 025 min 0 5 s response time 10 H2 mn gt 0 05 min 1 0 s response time 5 Hz gt 0 10 min 2 0 s response time 2 5 H2 gt 0 20 min 4 0 s response time 1 25 Hz gt 0 40 min 8 0 s response time 0 62 H2 gt 0 85 min 16 0 s response time 0 31 H2 Up to 8 individual signals can be set For each of the signals the wavelength and bandwidth can be s
36. TCP IP parameter configuration 67 telnet configuration 85 temperature sensor 164 test function astm drift 188 D A converter 198 test functions 152 test cell usage 1 5 test function celltest 183 conditions 176 DAC 198 dark current 200 failing 177 intensity test 180 introduction 1 74 max light cartridge 175 noise 188 quick noise test 185 self test 178 slit 191 test cell cartridge 175 wavelength calibration 195 wavelength verification 193 time table settings using 114 time constant versus response time 43 Agilent 1200 Infinity Series DAD User Manual Index timeout 159 troubleshooting error messages 152 158 status indicators 152 153 U unpacking 46 user interfaces 155 using advanced method parameter settings 110 control settings 106 detector 100 general method settings 108 GUI 103 Instant Pilot 119 instrument configuration 117 instrument curves 116 method parameter settings other advanced method parameter 113 spectrum settings 111 time table settings 114 V voltage range 40 W warm up of detector 149 warnings and cautions 204 waste electrical and electronic equipment 246 wavelength and bandwidth optimization 144 wavelength recalibration lost 169 wavelength calibration 195 wavelength verification test 193 wavelength accuracy 41 bunching 41 range 41 WEEE directive 246 weight 40 Agilent 1200 Infinity Series DAD User Manual 255
37. Test Example of Integrator Plot The test can be started via the command line 1 To start the test TEST DAC 1 Reply RA 00000 TEST DAC 1 2 To stop the test TEST DAC 0 Reply RA 00000 TEST DAC 0 Test Failed D A Converter DAC Test Evaluation The noise on the step should be less than 3 uV Probable cause 1 Bad cable or grounding problem between detector and external device 2 Defective detector main board Agilent 1200 Infinity Series DAD User Manual Suggested actions Check or replace the cable Please contact your Agilent service representative 199 9 Test Functions and Calibration Dark Current Test The dark current test measures the leakage current from each diode The test is used to check for leaking diodes which may cause non linearity at specific wavelengths During the test the slit assembly moves to the dark position cutting off all light falling onto the diode array Next the leakage current from each diode is measured and displayed graphically The leakage current represented in counts for each diode should fall within the limits When In case of problem 1 Run the Dark Current Test with the recommended user interface for further information see Online Help of user interface Test Name Dark Current Test Description The test measures the dark current from the detector optic Module G4212A PRO0100015 Status Passed Start Time 7 9 2009 3 04 21 PM Stop Time 7 9 2009 3 04
38. Test Failed ASTM Noise Test Evaluation Probable cause Suggested actions 1 Insufficient lamp warm up time Allow detector and UV lamp turned on for at least 2 hours 2 Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles 3 Dirty or contaminated flow cell Flush flow cell Clean the flow cell as described in Cleaning of Max Light Cartridge Cell on page 218 4 Old UV lamp Exchange the UV lamp 5 Environment not according to specifications Improve environment 190 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Slit Test G4212A The slit test verifies correct operation of the micromechanical slit During the test the slit is moved through all slit positions while the detector monitors the lamp intensity change When the slit position is changed the intensity drop move to smaller slit or intensity increase move to larger slit must be within a defined range If the intensity changes are outside the expected range the test fails When In case of problems Parts required Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Preparations Lamp must be on for at least 10 minutes When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required 1 Run the Slit Test with the recommended user interface for further information see Online Help of user
39. UV lamp Please contact your Agilent service representative Please contact your Agilent service representative The calibration values read from the spectrometer ROM are invalid After recalibration the calibration values are stored in ROM The processor periodically checks if the calibration data are valid If the data are invalid or cannot be read from the spectrometer ROM the error message is generated Probable cause 1 Defective connector or cable 2 Defective PDA optical unit Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Agilent 1200 Infinity Series DAD User Manual Error Information 8 Wavelength Recalibration Lost The calibration information needed for your detector to operate correctly has been lost During calibration of the detector the calibration values are stored in ROM If no data is available in the spectrometer ROM the error message is generated Probable cause Suggested actions 1 The detector is new Recalibrate the detector 2 The detector has been repaired Please contact your Agilent service representative Illegal Value From Temperature Sensor This temperature sensor delivered a value outside the allowed range The parameter of this event equals the measured temperature in 1 100 centigrade As a result the temperature control is switched off Probable cause Suggested actions 1 Dirty or defective sensor
40. all modules The module should be operated in a horizontal position 38 Agilent 1200 Infinity Series DAD User Manual Site Requirements and Specifications 2 Environment CAUTION Your module will work within the specifications at ambient temperatures and relative humidity described in Table 12 on page 40 ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification refer also to Specifications on page 41 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 Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation This module is designed to operate in a typical electromagnetic environment i e where RF transmitters such as mobile telephones may not be used in close proximity Agilent 1200 Infinity Series DAD User Manual 39 2 Site Requiremen
41. are available For testing of the detector a Max Light Cartridge Test Cell is available The optical principle of the Max Light Cartridge cell is based on opto fluidic waveguides Nearly 100 light transmission is achieved by utilizing total internal reflection in a non coated silica fiber Compromising refractive index and thermal effects are almost completely eliminated resulting in significantly less baseline drift T yf Agilent ourLet G4212 60008 Figure 3 Max Light Cartridge Flow Cell Agilent 1200 Infinity Series DAD User Manual 13 1 Introduction Optical System Slit Assembly Programmable Slit G4212A The micro slit system makes use of the mechanical properties of silicon combined with the precise structuring capabilities of bulk micro machining It combines the required optical functions slit and shutter in a simple and compact component The slit width is directly controlled by the micro processor of the instrument and can be set as method parameter Figure 4 Slit Assembly The slit width influences the spectral resolution and noise 14 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Absorbance mAU 0 6 0 5 0 4 0 3 0 2 0 1 0 230 240 250 260 270 280 nm PA 2 ia fat ill 4nm Oceania 8nm Noise level Figure 5 Influence of slitwidth on resolution and noise level Fixed Slit G4212B The fixed slit combines the required optical functions slit and sh
42. are taken continuously as for All but only every second spectrum is stored other spectra are discarded This reduces the amount of data storage necessary Range defines the wavelength range for spectral storage Limits 190 to 650 nm in steps of 1 nm for both low and high values The high value must be greater than the low value by at least 2 nm 111 5 Using the Module Step Step defines the wavelength resolution for spectral storage Limits 0 10 to 100 00 nm nm in steps of 0 1 nm Threshold The threshold is the height in mAU of the smallest expected peak The peak detector ignores any peaks which are lower than the threshold value and does not save spectra Limits 0 001 to 1000 00 mAU in steps of 0 001 mAU 112 Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Other Advanced Method Parameter Settings Analog Ouiput This screen part of the Advanced Method Settings shows Oait the default settings Zero Offset ox Altenuation 1000 mau Magn for negative Absorbance sa 100 mAU 4 7j na Autobalance Lamps on required for aquisition V Pieun v UV Lamp Postun Analog Output The Range can be set to either 100 mV or 1 V full scale see Control Settings on page 106 Zero Offset 1 to 99 in steps of 1 5 equal to 50 mV Attenuation 0 98 to 2000 mAU at discrete values for either 100 mV or 1 V full scale Margin for Negative Absorbance Use this field to modify the detector s signal handling to increas
43. be used to bring the module into a defined mode with default parameter settings CAUTION Loss of data Forced cold start erases all methods and data stored in the non volatile memory Exceptions are diagnosis and repair log books which will not be erased gt Save your methods and data before executing a forced cold start If you use the following switch settings and power the instrument up again a forced cold start has been completed Table 11 Forced Cold Start Settings without on board LAN Mode Select SW1 sw2 SW3 sw4 SW5 SW6 SW7 Sws LAN TEST BOOT 1 1 0 0 0 0 0 1 No LAN TEST BOOT 1 1 0 0 1 0 0 1 34 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 2 Site Requirements and Specifications Site Requirements 36 Physical Specifications 40 Performance Specifications 41 Specifications 41 Specification Conditions 43 This chapter provides information on environmental requirements physical and performance specifications ee Agilent Technologies 35 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the module Power Consideration The module power supply has wide ranging capabilities and accepts any line voltage in the range mentioned in Table 12 on page 40 Consequently there is no voltage selector in the rear of the module There are also no externally accessible fuses because automatic e
44. interface Test Name Slit Test Description The test performs a slit test Module G4212A PRO0100015 Status Passed Start Time 7 9 2009 2 19 17 PM Stop Time 7 9 2009 2 19 56 PM ET Test Procedure m Result T Name Value WH 1 Check Prerecuistes Cell Product Number 4212 60011 72 Inet spoed Celor Test Cet C Cid ates at Y 2 PefomSh Tet cette tos 7 ad Seeds mee oc Setettesk Ci Figure 67 Slit Test Results Agilent 1200 Infinity Series DAD User Manual 191 9 Test Functions and Calibration Slit Test G4212A Figure 68 Slit Test Signals Test Failed Slit Test Evaluation Probable cause Suggested actions 1 Max Light Cartridge Cell still installed Install Max Light Cartridge Test Cell 2 Old lamp Run the Intensity Test Exchange the lamp if old or defective 3 Defective slit assembly Please contact your Agilent service representative 4 Defective detector main board Please contact your Agilent service representative 5 Defective optical unit Please contact your Agilent service representative 192 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Wavelength Verification Test When Parts required Preparations The detector uses the alpha 656 1 nm and beta 486 nm emission lines of the UV lamp for wavelength calibration The sharp emission lines enable accurate calibration When verification is started the 1 nm slit is moved into the light path automati
45. leaking or if intensity drops due to contaminated flow A wavelength calibration test should be cell performed after replacement Leak sensor drying If leak has occurred Check for leaks Leak handling System If broken or corroded replacement Check for leaks Agilent 1200 Infinity Series DAD User Manual 207 10 Maintenance Cleaning the Module The module 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 as liquid may drip into the module WARNING Liquid dripping into the electronic compartment of your module Liquid in the module electronics can cause shock hazard and damage the module gt Do not use an excessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings 208 Agilent 1200 Infinity Series DAD User Manual Maintenance Replacing the Deuterium Lamp When If noise or drift exceeds application limits or lamp does not ignite Tools required Screwdriver POZI 1 PT3 Parts required p n Description 1 5190 0917 Long life Deuterium lamp 8 pin with RFID tag Preparations Turn the lamp off WARNING Injury by touching hot lamp If the detector has been in use the lamp may be hot gt If so wait for lamp to cool down 10 1 Remove the front cover 2 Locate the lamp area Agilent 1200 Infinity Series DAD User Manua
46. limits If the current increases above the upper limit the error message is generated Probable cause 1 Defective flow sensor 2 Leak sensor incorrectly routed being pinched by a metal component Agilent 1200 Infinity Series DAD User Manual Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative 161 8 Error Information Leak Sensor Open The leak sensor in the module has failed open circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current falls outside the lower limit the error message is generated Probable cause Suggested actions 1 Leak sensor not connected to the main Please contact your Agilent service board representative 2 Defective leak sensor Please contact your Agilent service representative 3 Leak sensor incorrectly routed being Please contact your Agilent service pinched by a metal component representative Compensation Sensor Open The ambient compensation sensor NTC on the main board in the module has failed open circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the senso
47. nm wide slit Furthermore the absorbance is no longer strictly linear with concentration for wavelengths at a steep slope of a compound s spectrum Substances with fine structures and steep slopes like benzene are very rare In most cases the width of absorbance bands in the spectrum is more like 30 nm as with anisic acid Figure 45 on page 132 In most situations a slit width of 4 nm will give the best results Use a narrow slit 1 or 2 nm if you want to identify compounds with fine spectral structures or if you need to quantify at high concentrations gt 1000 mAU with a wavelength at the slope of the spectrum Signals with a wide bandwidth can be used to reduce baseline noise Because digital bandwidth is computed as average of absorbance there is no impact on linearity Use a wide 8 nm slit when your sample contains very small concentrations Always use signals with bandwidth at least as wide as the slit width Agilent 1200 Infinity Series DAD User Manual 135 136 Optimizing the Detector Optimizing Spectral Acquisition Storage of all spectra consumes a lot of disk space It is very useful to have all spectra available during optimization of a method or when analyzing unique samples However when running many samples of the same type the large size of data files with all spectra may become a burden The detector provides functions to reduce the amount of data yet retaining the relevant spectral information
48. or Cell Test 5 If tests fail again the flow cell might be replaced if the chromatographic performace cannot be accepted If the cleaning with the alcohol did not improve you may use Cell cleaning fluid 1 L p n 5062 8529 218 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Storage of Max Light Cartridge Cell 1 Flush the Max Light Cartridge Flow Cell with iso propanol or methanol and insert the plugs into the cell inlet and outlet see Replacing the Max Light Cartridge Cell on page 213 2 Remove the Max Light Cartridge Cell from the cartridge holder of the detector 3 Replace the black hoods that secure the cell light inlet and outlet 4 Store the Max Light Cartridge Cell in plastic case provided with the Max Light Cartridge Flow Cell Agilent 1200 Infinity Series DAD User Manual 219 10 Maintenance Drying the Leak Sensor Drying the Leak Sensor When If leak has occurred Tools required Tissue Preparations Turn the pump off 1 Remove the front cover 2 Locate the leak sensor area 3 Dry the leak sensor and the area around Check loose 4 Close the front cover fittings at the flow cell Note that the leak sensor does not touch the panel clearance of about 1 mm 220 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Replacing Leak Handling System Parts Replacing Leak Handling System Parts When If the parts are corroded or broken Tools required Tiss
49. speed data communication and real time requirement LAN The modules have either an interface slot for an LAN card e g Agilent G1369A B LAN Interface or they have an on board LAN interface e g detectors G1315C D DAD and G1365C D MWD This interface allows the control of the module system via a connected PC with the appropriate control software If an Agilent detector DAD MWD FLD VWD RID is in the system the LAN should be connected to the DAD MWD FLD VWD RID due to higher data load If no Agilent detector is part of the system the LAN interface should be installed in the pump or autosampler RS 232C Serial The RS 232C connector is used to control the module from a computer through RS 232C connection using the appropriate software This connector can be configured with the configuration switch module at the rear of the module Refer to Communication Settings for RS 232C There is no configuration possible on main boards with on board LAN These are pre configured for e 19200 baud e 8 data bit with no parity and one start bit and one stop bit are always used not selectable The RS 232C is designed as DCE data communication equipment with a 9 pin male SUB D type connector The pins are defined as Agilent 1200 Infinity Series DAD User Manual Introduction 1 Table 2 RS 232C Connection Table Pin Direction Function 1 In DCD 2 In RxD 3 Out TxD 4 Out DTR 5 Ground 6 In DSR 7 Out RTS 8 In
50. threshold Agilent 1200 Infinity Series DAD User Manual Suggested actions Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required Check the logbook for the occurrence and source of a not ready condition Restart the analysis where required 159 160 Error Information Shut Down An external instrument has generated a shut down signal on the remote line The module continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable cause Suggested actions 1 Leak detected in another module witha CAN Fix the leak in the external instrument before connection to the system restarting the module 2 Leak detected in an external instrument with Fix the leak in the external instrument before a remote connection to the system restarting the module 3 Shut down in an external instrument witha Check external instruments for a shut down remote connection to the system condition Remote Timeout A not ready condition is still present on the remote input When an analysis is started the system expects all not ready conditions for example a not ready condition during detector balance to switch to run conditions within one minute of starting the analysis If a not ready condition is still present on the remote line after one minute the error message is generated Probable cause Sugg
51. www agilent com In This Book This manual contains technical reference information about the Agilent 1290 Infinity Diode Array Detector G4212A and the Agilent 1260 Infinity Diode Array Detector G4212B introduction and specifications e installation e using and optimizing troubleshooting and diagnose e maintenance e parts identification safety and related information Agilent Technologies 2010 Printed in Germany 06 2010 G4212 90010 EE Agilent Technologies
52. 0 Table 8 Data Bit Settings without on board LAN Switch 6 Data Word Size 0 7 Bit Communication 1 8 Bit Communication Table9 Parity Settings without on board LAN Switches Parity 7 8 0 0 No Parity 1 0 Odd Parity 1 1 Even Parity One start bit and one stop bit are always used not selectable Per default the module will turn into 19200 baud 8 data bit with no parity Agilent 1200 Infinity Series DAD User Manual Introduction 1 Special Settings The special settings are required for specific actions normally in a service case The tables include both settings for modules with on board LAN and without on board LAN They are identified as LAN and no LAN Boot Resident Firmware update procedures may require this mode in case of firmware loading errors main firmware part If you use the following switch settings and power the instrument up again the instrument firmware stays in the resident mode It is not operable as a module It only uses basic functions of the operating system for example for communication In this mode the main firmware can be loaded using update utilities Table 10 Boot Resident Settings without on board LAN Mode Select SW1 sw2 SW3 SW4 SW5 SW6 SW7 Swe LAN TEST BOOT 1 1 1 0 0 0 0 0 No LAN TEST BOOT 1 1 0 0 1 0 0 0 Agilent 1200 Infinity Series DAD User Manual 33 1 Introduction Forced Cold Start A forced cold start can
53. 0 Infinity DAD Idle B te Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Setting up the Detector with Agilent ChemStation EMF Status shows Offline gray Ok No Maintenance required EMF warning Maintenance or check might be required yellow EMF warning Maintenance required red Important The EMF settings can be accessed via the Agilent Lab Advisor or the Instant Pilot only The limit s can be changed Based on the limit the User Interface displays the above status RFID tag information is displayed when moving with the mouse cursor on to the tag attached to the flow cell or lamp The information provides flow cell and lamp related information like e Part number e Production date Serial number and other details Lamp tag information Burn time 93 3h Minimum lifetime 2000 0h Number of ignitions 10 Product Number 5190 0917 Serial Number 824337 Production Date 4 9 2009 8 23 53 AM Tested Date 7 16 2009 1 50 04 PM Intensity et test 37275 counts Cell tag information Cell Name Max Light Cell Product Number 64212 60008 Serial Number 10PP042325 Production Date 2 5 2009 12 49 06 PM Optical path length 10 0mm Cell Volume 0 1 0pL Maximum pressure 60 bar Tested Date 7 10 2009 1 44 52 PM Cell Revision 0 105 5 Using the Module Control Settings 151 Lamps At Power On uv On Tum UV lamp on Off Analog Output Range Output 1 01y 1v UV Lamp Tag Automatic
54. 1 xX x xX 100 MBit half duplex 1 1 0 x X X 100 MBit full duplex 1 1 1 Xx x xX Bootp x xX x 0 0 0 Bootp amp Store Xx X X 0 0 1 Using Stored x X x 0 1 0 Using Default Xx xX xX 0 1 1 TEST 1 1 System NVRAM Boot Resident System 1 x Revert to Default Data Coldstart X X X 1 Legend 0 switch down 1 switch up x any position When selecting the mode TEST the LAN settings are Auto Negotiation amp Using Stored For explanation of Boot Resident System and Revert to Default Data Coldstart refer to Special Settings on page 33 Agilent 1200 Infinity Series DAD User Manual 29 1 Introduction Setting the 8 bit Configuration Switch without On Board LAN The 8 bit configuration switch is located at the rear of the module Modules that do not have their own LAN interface e g the TCC can be controlled through the LAN interface of another module and a CAN connection to that module Figure 10 Configuration switch settings depend on configured mode All modules without on board LAN e default is ALL DIPS DOWN best settings Bootp mode for LAN e for boot test modes DIPS 1 2 must be UP plus required mode Switch settings provide configuration parameters for GPIB address serial communication protocol and instrument specific initialization procedures With the introduction of the Agilent 1260 Infinity all GPIB interfaces have been removed The preferred communication is LAN The following tables represe
55. 2 Manual Configuration 84 With Telnet 85 With the Instant Pilot G4208A 89 PC and Agilent ChemStation Setup 90 PC Setup for Local Configuration 90 Agilent ChemStation Setup 93 This chapter provides information on connecting the module to the Agilent ChemStation PC ot Agilent Technologies 65 4 LAN Configuration What You Have to Do First The module has an on board LAN communication interface 1 Note the MAC Media Access Control address for further reference The MAC or hardware address of the LAN interfaces is a world wide unique identifier No other network device will have the same hardware address The MAC address can be found on a label at the rear of the module underneath the configuration switch see Figure 21 on page 66 G4212 65800 Mga Part number of the detector main board B 01 XX 0925 Revision Code Vendor Year and Week of assembly MAC 000001000001 MAC address Made in Germany Country of Origin Figure 20 MAC Label 2 Connect the instrument s LAN interface see Figure 21 on page 66 to the PC network card using a crossover network cable point to point or a hub or switch using a standard LAN cable LAN interface MAC label Protuct Nos Gaara ET Seda Mo OCh TONNE p gt igan baatesen AIN Aetas A y Made ia Germany Figure 21 Location of LAN interfaces and MAC label 66 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 TCP IP param
56. 2 5 2 5 2 5 2 5 2 5 gt 0 20 40 1 25 1 25 1 25 1 25 1 25 gt 0 40 8 0 0 625 0 62 0 625 0 625 0 625 gt 0 85 16 0 0 3125 0 31 0 3125 0 3125 0 3125 1 2 64212A only 130 Values in the User Interface may be rounded The maximum spectra scan rate depends on the data points per scan see Table 21 on page 130 Running at 160 Hz the spectra scan data rate is reduced automatically if the spectra scan data rate is more than 251 points scan Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Sample and Reference Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 to 640 nm A UV lamp provides good sensitivity over the whole wavelength range If you know little about the analytes in your sample store all spectra over the full wavelength range This provides full information but fills up your disk space rather quickly Spectra can be used to check a peak s purity and identity Spectral information is also useful to optimize wavelength settings for your chromatographic signal The detector can compute and store at run time up to 8 signals with these properties e sample wavelength the center of a wavelength band with the width of sample bandwidth BW and optionally e reference wavelength the center of a wavelength band with the width of reference bandwidth The signals comprises a series of data points over time with the average absorbance in the sample wav
57. 41 PM PETTITTE p Test Procedure p Result J i Name Value WY 1 Check Prerequisites Cell Product Number G4212 60011 9 2 Patom Dak Cineni Test 3 Evaluate Data Cell Type 10 mmj pl Lamp Type Automatic Mode Dark Current Minimum 7698 Counts Dark Current Average 7726 Counts Figure 73 Dark Current Test Results 200 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Dark Current Test Figure 74 Dark Current Test Signals Test Failed Dark Current Test Evaluation Probable cause Suggested actions 1 Defective slit assembly stray light Run the Self Test on page 178 2 Defective detector main board Please contact your Agilent service representative 3 Defective PDA optical unit Please contact your Agilent service representative Agilent 1200 Infinity Series DAD User Manual 201 9 Test Functions and Calibration Dark Current Test 202 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual ee 10 e Maintenance J Warnings and Cautions 204 Introduction to Maintenance 206 Overview of Maintenance 207 Cleaning the Module 208 Replacing the Deuterium Lamp 209 Replacing the Max Light Cartridge Cell 213 Cleaning of Max Light Cartridge Cell 218 Storage of Max Light Cartridge Cell 219 Drying the Leak Sensor 220 Replacing Leak Handling System Parts 221 Replacing Module Firmware 223 Information from Module
58. Agilent 1200 Infinity Series DAD User Manual 95 4 LAN Configuration PC and Agilent ChemStation Setup 12 The left column shows the modules that could be configured You may select the module manually from the list We use the Auto Configuration mode Click on Yes aerate eerie Qs Driers EG sewo raw ae Agilent 1100 1200 1290 Series LC Auto Configuraliar 4 14 Click on OK The selected module is shown now in the right window with serial number In addition all other modules connected via CAN to the detector are shown as well 96 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 PC and Agilent ChemStation Setup 15 Click on OK to continue the ChemStation loading instrument Configuration Agilent 1100 1200 1230 Series LC Agilent 1100 1200 1290 Series LC Qs SH 040 1642124 PRONS Dros or eo GG anne of cshnecone 16 You may see the details of the module by selecting the module and clicking on Configure 1100 1200 1290 DAD Configuration Instrument 1 Under Connection Settings you may change the IP Hostname of the module may require a re start of the ChemStation After successful load of the ChemStation you should see the module s as active item in the graphical user interface GUID Agilent 1200 Infinity Series DAD User Manual 97 4 LAN Configuration PC and Agilent ChemStation Setup nil D NotReady Instrument 0 00 0 00 Not Ready
59. CTS 9 In RI Instrument PC DCD 1 1 DCD RX 2 2 RX TX 3 xX 3 TX DTR 4 aF 4 DTR GND 5 X 5 GND DSR 6 6 DSR RTS 7 X 7 RTS CTS 8 8 CTS RI 9 9 RI DB9 DB9 DB9 DB9 Male Female Female Male Figure 8 RS 232 Cable Analog Signal Output The analog signal output can be distributed to a recording device For details refer to the description of the module s main board Agilent 1200 Infinity Series DAD User Manual 25 1 26 Introduction APG Remote The APG Remote connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features as common shut down prepare and so on Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements The subminiature D connector is used The module provides one remote connector which is inputs outputs wired or technique To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the system s critical parts in case any module detects a serious problem To detect whether all participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines In addition PREPARE and START REQUES
60. Detector Previous Absolute D2 Alpha Line Deviation Previous Absolute D2 Beta Line Deviation O iLO absckte 02 Aiha une Doran o psm D2 Beta Line Calibrate Detector with Wavelength Verificati Figure 70 Wavelength Calibration Results 196 Agilent 1200 Infinity Series DAD User Manual Wavelength Recalibration Fails Probable cause 1 Absorbing solvent or air bubble in Max Light Cartridge Cell 2 Dirty or contaminated Max Light Cartridge Cell 3 Old UV lamp 4 Dirty or contaminated optical components Test Functions and Calibration Suggested actions Repeat calibration with Max Light Cartridge Test Cell and compare results Ensure the Max Light Cartridge Cell is filled with water e Recalibrate Exchange the UV lamp Run the Cell Test If the test fails flush the flow cell See also Cleaning of Max Light Cartridge Cell on page 218 If the test fails with Max Light Cartridge Test Cell and new UV lamp the optical unit must be replaced Agilent 1200 Infinity Series DAD User Manual 9 197 9 Test Functions and Calibration D A Converter DAC Test When Preparations 198 The detector provides analog output of chromatographic signals for use with integrators chart recorders or data systems The analog signal is converted from the digital format by the digital analog converter DAC The DAC test is used to verify correct operation of the digital analog converter b
61. For spectra options see Spectrum Settings on page 111 Range Only the wavelength range where the compounds in your sample absorb contains information that is useful for purity checks and library searches Reducing the spectrum storage range saves disk space Step Most substances have broad absorbance bands Display of spectra peak purity and library search works best if a spectrum contains 5 to 10 data points per width of the absorbance bands For anisic acid the example used before a step of 4 nm would be sufficient However a step of 2 nm gives a more optimal display of the spectrum Threshold Sets the peak detector Only spectra from peaks higher than threshold will be stored when a peak controlled storage mode is selected Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Margin for Negative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative about 100 mAU In some special case for example when gradient with absorbing solvents are used the baseline may drift to more negative values Only for such cases increase the margin for negative absorbance to avoid overflow of the analog to digital converter Agilent 1200 Infinity Series DAD User Manual 137 6 Optimizing the Detector Optimizing Selectivity Quantifying Coeluting Peaks by Peak Suppression In chromatography two compounds may often elute together A conventional dual sig
62. If the test fails also then start with proposed actions mentioned in the details of the tests Agilent 1200 Infinity Series DAD User Manual 9 177 9 Test Functions and Calibration Self Test The self test runs a series of individual tests described on the next pages and evaluates the results automatically The following tests are run e Slit Test e Dark Current Test e Intensity Test e Wavelength Verification Test e ASTM Noise Test a simplified version of the ASTM Drift and Noise Test without testing the Drift When For complete detector check Parts required Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Preparations Lamp must be on for at least 10 minutes For noise test a longer warm up time may be required gt 2 hours When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required 178 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 Self Test 1 Run the Self Test with the recommended user interface for further information see Online Help of user interface m calredstnmbe SS feraizwoon C ce C OY C mati de fseteanesk idm foakcurent Mmm __ _ dve cs C rreaconts Lowest rtenaty n Range E owes ienaty a Range 221 01 ale comts Figure 58 Self Test Results Agilent 1200 Infinity Series DAD User Manual 179 9 Test Functions and Calibration Intensity Test
63. Manual Optimizing the Detector 6 Warm up of the Detector Give the optical unit enough time to warm up and stabilize gt 60 minutes The detector is temperature controlled After turn on of the detector it goes through a cycle of different states 0 to 0 5 minutes the heater control is OFF and the heater element runs at 0 duty cycle 0 5 to 1 minutes the heater control is OFF and the heater element runs at 66 duty cycle This first minute is used as self test of the heater functionality 1 to 30 minutes the heater control is OFF and the heater element runs at 40 duty cycle e After 30 minutes the heater control is ON and is working with optimized parameters to get the optical unit into the optimal temperature window stabilized This cycle starts e when the detector is turned off on e when the lamp is turned off on to ensure that the temperature control operates in a defined control range The times to stabilize the baseline may vary from instrument to instrument and depends on the environment The example below was done under stable environmental conditions The figures below show the first two hours of a detector warm up phase The lamp was turned on immediately after turn on of the detector Agilent 1200 Infinity Series DAD User Manual 149 6 Optimizing the Detector Warm up of the Detector Baseline 230 4 360 100 SLW 4 RT 2s _ 4st Figure 55 Detector Warm up hour Baseline 230 4 360 100
64. OK to save the configuration 92 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Agilent ChemStation Setup This procedure describes the Agilent ChemStation B 04 02 setup for the 1290 Infinity system using the 1290 Infinity DAD G4212A as the interfacing module The LAN must be connected to detector due to high data load on communication to Control Software 1 Open the ChemStation Configuration Editor Joiz File Configure Utilities Help Instrment 1 LC 3D Data Analysis orly 2 Select from the menu Configure Instruments 3 Select Modular 3D LC System 4 Give the Instrument a name Agilent 1200 Infinity Series DAD User Manual 93 4 LAN Configuration PC and Agilent ChemStation Setup 5 Click on OK Select Instrument mitialy Start Instrument Session EVES 5 No 94 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 PC and Agilent ChemStation Setup 7 Click on OK The Configuration Editor shows now the new instrument 8 If required change under Configure Path the folder locations 9 Save the current configuration via File Save Configuration editor o File Configure Utilities Help instrment 1 4 Nodular 3D LC System LC System Access Recess Point 10 Exit the Configuration Editor 11 Start the Agilent ChemStation During first startup or when the system configuration has changed a notification shows up
65. Off Get Ready 2 System Get Ready 3 System Clear Errors Reset of Errors 4 DAD Balance Balance 1 System Set Defaults 5 More 2 Controller Format USB 3 DAD Spectrum Take Spectrum DAD G4212A PROO100015 o wN Method Sequence Status Logbook Mores Agilent 1200 Infinity Series DAD User Manual 119 5 Using the Module Main Screens of the Detector with Agilent Instant Pilot G4208A The System Info screen list details of the detector Firmware revision On time LAN settings Main Board information Lamp RFID tag Information Flow cell RFID tag Information USING STORED s 192 168 254 11 0030D317521C TYPE G4212 65800 REV BE MFG ZZ SER M 3190 0917 824337 G4212 60011 200PP00015 Configure DAD The Configuration screen allows to configure Symbolic name of module Temperature control Lamp and cell RFID tag use Analog Output range Use lamp tag settings UV lamp at power on OV 1V_ output range LAN settings Stays off at power on 192 168 254 11 255 255 255 0 LAN Def Gateway 255 255 255 255 Done Enter up to 30 characters eT 16 43 120 Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Main Screens of the Detector with Agilent Instant Pilot G4208A Method DEFAULT all 5 The Method screen lists all method parameters of the detector These can be edited ef 360 0 100 0 nm
66. SSSSS CC YWW SSSSS Format country of manufacturing DE Germany e JP Japan e CN China year and week of last major manufacturing change e g 820 could be week 20 of 1998 or 2008 real serial number Serial Number Information 1260 Infinity The serial number information on the instrument labels provide the following information CCXZZ00000 cC X ZZ 00000 Agilent 1200 Infinity Series DAD User Manual Format Country of manufacturing DE Germany Alphabetic character A Z used by manufacturing Alpha numeric code 0 9 A Z where each combination unambiguously denotes a module there can be more than one code for the same module Serial number 21 1 introduction Interfaces Table1 Agilent 1200 Infinity Series Interfaces Module CAN LAN BCD optional LAN on board RS 232 Analog The Agilent 1200 Infinity Series modules provide the following interfaces APG Special Remote Pumps G1310B Iso Pump G1311B Quat Pump G1311C Quat Pump VL G1312B Bin Pump G1312C Bin Pump VL 1376A Cap Pump G2226A Nano Pump G4220A B Bin Pump G1361A Prep Pump Samplers G1329B ALS G2260A Prep ALS G1364B FC PS G1364C FC AS G1364D FC uS G1367E HiP ALS G1377A HiP micro ALS G2258A DL ALS G4226A ALS Detectors G1314B VWD VL G1314C VWD VL G1314E F VWD Yes No Yes Yes Yes Yes Yes No No Yes No No No No No Yes Yes Yes Yes Yes
67. T may be issued The signal levels are defined as e standard TTL levels 0 V is logic true 5 0 V is false e fan out is 10 e input load is 2 2 kOhm against 5 0 V and e output are open collector type inputs outputs wired or technique All common TTL circuits operate with a 5 V power supply A TTL signal is defined as low or L when between 0 V and 0 8 V and high or H when between 2 0 V and 5 0 V with respect to the ground terminal Agilent 1200 Infinity Series DAD User Manual Introduction 1 Table 3 Remote Signal Distribution Pin Signal Description 1 DGND Digital ground 2 PREPARE L Request to prepare for analysis for example calibration detector lamp on Receiver is any module performing pre analysis activities 3 START L Request to start run timetable Receiver is any module performing run time controlled activities 4 SHUT DOWN L System has serious problem for example leak stops pump Receiver is any module capable to reduce safety risk 5 Not used 6 POWER ON H All modules connected to system are switched on Receiver is any module relying on operation of others 7 READY H System is ready for next analysis Receiver is any sequence controller 8 STOP L Request to reach system ready state as soon as possible for example stop run abort or finish and stop injection Receiver is any module performing run time controlled activities 9 START REQUEST L Request to start injection cy
68. Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low Agilent 1200 Infinity Series DAD User Manual 235 12 Identifying Cables Agilent Module to General Purpose p n 01046 60201 Pin Universal Pin Agilent Signal Name Active module TTL 1 White Digital ground A O 1 2 B oo Brown Prepare run Low o0 pe DE KEY 3 Gray Start Low o0 e lea 4 Blue Shut down Low BE om 5 Pink Not connected oOo 0 6 Yellow Power on High Ss O 18 7 Red Ready High 8 Green Stop Low 9 Black Start request Low 236 Agilent 1200 Infinity Series DAD User Manual BCD Cables Identifying Cables 12 One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The other end depends on the instrument to be connected to Agilent Module to General Purpose p n G1351 81600 Wire Color Pin Agilent Signal Name BCD Digit module Green 1 BCD 5 20 Violet 2 BCD7 80 4 Blue 3 BCD 6 40 m Yellow 4 BCD 4 10 SS Black 5 BCD 0 1 ay Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 notconnected 14 notconnected 15 5V Low Agilent 1200 Infinity Series DAD User Manual 237 12 Identifying Cables Agilent Module to 3396 Integrators
69. a different flow cell it should be flushed with isopropanol and the CELL IN and CELL OUT should be closed with the plugs Agilent 1200 Infinity Series DAD User Manual 63 3 Installing the Module Initial Recalibration 64 The detector has been calibrated with a factory flow cell initially After installation of the detector with the delivered or a new Max Light Cartridge flow cell and an initial warm up of at least 2 hours a recalibration should be performed Wavelength Calibration on page 195 This recalibration will correct slight changes due to e significant environmental condition changes temperature humidity during transport and storage e significant environmental condition changes temperature humidity in final location and e variances between factory test cell and the installed flow cell Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 4 LAN Configuration What You Have to Do First 66 TCP IP parameter configuration 67 Configuration Switch 68 Initialization mode selection 69 Link configuration selection 73 Automatic Configuration with BootP 74 About Agilent BootP Service 74 How BootP Service Works 75 Situation Cannot Establish LAN Communication 75 Installation of BootP Service 76 Two Methods to Determine the MAC Address 78 Assigning IP Addresses Using the Agilent BootP Service 79 Changing the IP Address of an Instrument Using the Agilent BootP Service 8
70. acteristic of a given substance under a precisely defined set of conditions of wavelength solvent temperature and other parameters C mol L is the concentration of the absorbing species and d cm is the path length of the cell used for the measurement The detector can now output the signal in two forms 1 In Absorbance divide by the path length AU cm that is then similar to x C Advantage samples with same concentration have same peak height also at cells with different path lengths The upper limit of concentration the linearity limit of the detector is then seen at about 2 AU path length so for the 6 cm Max Light Cartridge Cell the linearity limit is 333 mAU cm 2 In AU that is equal to e x C x d like normal done in the past now for recalculation to your concentration C the path length must be considered 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 When increasing the path length the cell volume could increase Depending on the peak volume this could cause more peak dispersion Agilent 1200 Infinity Series DAD User Manual 127 6 Optimizing the Detector 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 div
71. angement even without the autosampler thermostat A slightly longer capillary is required between the pump and autosampler See Figure 17 on page 55 and Figure 18 on page 56 Instant Pilot Detector m Column compartment 0000 0000 0000 0 Se ee eee Solvent cabinet 5 n gt SLE O nem e E L ela a a a SS S es E j ss TSS Autosampler Thermostat for the ALS optional Figure 17 Recommended Two Stack Configuration for 1290 Front View Agilent 1200 Infinity Series DAD User Manual 55 3 Installing the Module Optimizing the Stack Configuration LAN to LC ChemStation CAN Bus cable to Instant Pilot Analog detector signal optional tit D UMN CAN Bus cable Thermo cable optional AC Power Figure 18 Recommended Two Stack Configuration for 1290 Rear View 56 Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 Installing the Detector Parts required Software required Preparations Description 1 Detector 1 Power cord 1 LAN cable cross over or twisted pair network cable Other cables see below and section Cable Overview on page 230 Instant Pilot and or ChemStation with the appropriate revisions see Table 13 on page 41 Locate bench space Provide power connections Unpack the module Module is partially energized when switched off as long as the power cord is plugged in Repair wor
72. artridge Cell 213 Cleaning of Max Light Cartridge Cell 218 Storage of Max Light Cartridge Cell 219 Drying the Leak Sensor 220 Replacing Leak Handling System Parts 221 Replacing Module Firmware 223 Information from Module s Assemblies 224 11 Parts and Materials for Maintenance 225 Overview of Maintenance Parts 226 Accessory Kits 228 12 Identifying Cables 229 Cable Overview 230 Analog Cables 232 Remote Cables 234 BCD Cables 237 CAN LAN Cables 239 RS 232 Cable Kit 240 13 Appendix 241 Safety 242 The Waste Electrical and Electronic Equipment Directive 246 Radio Interference 247 Sound Emission 248 Flow Cell 249 Agilent Technologies on Internet 250 Agilent 1200 Infinity Series DAD User Manual Contents 8 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 1 Introduction Overview of the Module 10 Optical System 11 Lamp 12 Max Light Cartridge Flow Cell 13 Slit Assembly 14 Grating and Diode Array 16 Early Maintenance Feedback 17 Instrument Layout 18 Electrical Connections 19 Rear view of the module 20 Information on Instrument Serial Number 21 Interfaces 22 Overview Interfaces 24 Setting the 8 bit Configuration Switch 28 Communication Settings for RS 232C 31 Special Settings 33 This chapter gives an introduction to the detector instrument overview and internal connectors ee Agilent Technologies 1 introduction Overview of the Module The detector is designed for hi
73. at 265 nm 1nm 2 400 nm G4212A 1 2 4 8 nm G4212B 4 nm 0 5nm up to 160 Hz G4212A or 80 Hz G4212B up to 160 Hz G4212A or 80 Hz G4212B Max Light Cartridge Cell 10 mm V o 1 0 pl 60 bar 870 psi pressure maximum Max Light Cartridge Cell 60 mm V o 4 0 pL 60 bar 870 psi pressure maximum Max Light Cartridge Test Cell Equipped with RFID tag that holds lamp typical information see Specification Conditions below see Specification Conditions below see Specification Conditions below After recalibration with deuterium lines Programmable in steps of 1 nm Programmable slit Fixed slit pH range 1 0 12 5 solvent dependent Cartridge type equipped with RFID tags that holds cell typical information Agilent 1200 Infinity Series DAD User Manual 41 2 Site Requirements and Specifications Table 13 Performance Specifications G4212A B Type Specification Comments Control and data evaluation Local Control Test and diagnostic software Analog outputs Communications Safety and maintenance GLP features Housing Data System 1 Agilent ChemStation for LC 2 EZChrom Elite 3 MassHunter Agilent Instant Pilot G4208A Agilent LabAdvisor Recorder integrator 100 mV or 1 V output range 0 001 2 AU one output Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN Extensive diagnostics error detection and displa
74. ation 101 Diagnostic software 156 dimensions 40 diode width 41 drift ASTM and noise 41 E electrical connections descriptions of 19 electronic waste 246 EMF early maintenance feedback 17 environment 39 error messages fan failed 163 uv heater current 168 uv ignition failed 167 error messages compensation sensor open 162 compensation sensor short 163 cover violation 165 diode current leakage 166 252 heater power at limit 171 heater failed 170 ignition without cover 164 164 illegal value from air inlet sensor 1 0 illegal value from heater sensor 169 leak sensor open 162 leak sensor short 161 leak 164 remote timeout 160 shut down 160 synchronization lost 161 timeout 159 uv lamp current 166 uv lamp voltage 167 wavelength calibration failed 168 wavelength recalibration lost 169 extra column volume description 142 F fan failed 163 features safety and maintenance 42 firmware updates 223 upgrade downgrade 223 flow cell max light cartridge 13 solvent information 249 flow cell correction factors 128 Max Light cartridge flow cell 143 Max Light high sensitivity cell 143 specifications 41 flow connections 60 60 frequency range 40 G general error messages 159 general method settings using 108 GLP features 42 grating 16 GUI detector 103 H humidity 40 initialization mode selection 69 installation accessory kit 47 bench space 38 delivery checklist 47 detector 5 7 environmen
75. bsorbed by the Max Light Cartridge Test Cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the 1 nm slit is moved into the light path automatically G4212A only On the G4212B the 4 nm fixed slit is used This test should be performed initially with a new detector flow cell The values should be kept for later reference comparison In case of low intensity or noise and drift problem Description 1 Max Light Cartridge Cell filled with water or 1 Max Light Cartridge Test Cell Lamp must be on for at least 10 minutes When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required 1 Run the Cell Test with the recommended user interface for further information see Online Help of user interface Test Name Cell Test Description The test compares the lamp intensity the Max Light Cell and the Max Light Test Cell The intensity ratio is an indicator of Module G4212A PR00100018 the amount of light absorbed by the flow cell Status Passed Start Time 7 14 2009 1 40 44 PM Stop Time 7 14 2009 1 41 46 PM Test Procedure Result Name Value Y 1 Check Prerequisites Cell Product Number 4212 60008 Fe erences Y 3 Scanintensly Spectrum 4 Insert supported Cel WY 5 Scanintensiy Spectum ei ee Figure 61 Cell Test Results Agilent 1200 Infinity Series DAD User Manual 183 9 Test Functions and Calibration Cell Test 2 ee e e ce
76. cally The test is run with the Max Light Cartridge Cell or with Max Light Cartridge Test Cell installed If the test is performed with the Max Light Cartridge Test Cell the test results are not influenced by solvent or pump effects The detector is calibrated at the factory and under normal operating conditions should not require recalibration However it is advisable to recalibrate after repair of components in the optical unit after exchange of the optical unit or main board after replacing the Max Light Cartridge Cell or UV lamp after significant environmental condition changes temperature humidity at a regular interval at least once per year for example prior to an Operational Qualification Performance Verification procedure and when chromatographic results indicate the detector may require recalibration Description Max Light Cartridge Test Cell or Max Light Cartridge Cell Lamp must be on for at least 10 minutes When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required Agilent 1200 Infinity Series DAD User Manual 193 194 Test Functions and Calibration Wavelength Verification Test 1 Run the Wavelength Verification Test with the recommended user interface for further information see Online Help of user interface Figure 69 Wavelength Verification Test G4212A PR00100015 Passed 7 9 2009 1 50 40 PM 7 9 2009 1 51 03 PM Wavelength Verification Results pssst
77. cle for example by start key on any module Receiver is the autosampler Special Interfaces Some modules have module specific interfaces connectors They are described in the module documentation Agilent 1200 Infinity Series DAD User Manual 27 1 introduction Setting the 8 bit Configuration Switch Setting the 8 bit Configuration Switch On Board LAN The 8 bit configuration switch is located at the rear of the module Switch settings provide configuration parameters for LAN serial communication protocol and instrument specific initialization procedures All modules with on board LAN e g G1315 65C D G1314D E F G4212A B G4220A e Default is ALL switches DOWN best settings Bootp mode for LAN e For specific LAN modes switches 3 8 must be set as required e For boot test modes switches 1 2 must be UP plus required mode Figure 9 Location of Configuration Switch example shows a G4212A DAD To perform any LAN configuration SW1 and SW2 must be set to OFF For details on the LAN settings configuration refer to chapter LAN Configuration 28 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Table 4 8 bit Configuration Switch with on board LAN Mode Function SW 1 SW 2 SW 3 SW 4 SW 5 SW 6 SW7 SW 8 LAN 0 0 Link Configuration Init Mode Selection Auto negotiation 0 xX x x x x 10 MBit half duplex 1 0 0 X X xX 10 MBit full duplex 1 0
78. cribes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions 9 Test Functions and Calibration This chapter describes the tests for the module 10 Maintenance This chapter describes the maintenance of the module 11 Parts and Materials for Maintenance This chapter provides information on parts for maintenance 12 Identifying Cables This chapter provides information on cables used with the Agilent 1260 Infinity 1290 Infinity LC modules 13 Appendix This chapter provides addition information on safety legal and web 4 Agilent 1200 Infinity Series DAD User Manual Contents Contents 1 Introduction 9 Overview of the Module 10 Optical System 11 Early Maintenance Feedback 17 Instrument Layout 18 Electrical Connections 19 Interfaces 22 Setting the 8 bit Configuration Switch 28 2 Site Requirements and Specifications 35 Site Requirements 36 Physical Specifications 40 Performance Specifications 41 3 Installing the Module 45 Unpacking the Module 46 Optimizing the Stack Configuration 48 Installing the Detector 57 Flow Connections to the Detector 60 Initial Recalibration 64 4 LAN Configuration 65 What You Have to Do First 66 TCP IP parameter configuration 67 Configuration Switch 68 Initialization mode selection 69 Link configuration selection 73 Automatic Configuration with BootP 74 Manual Configuration 84 PC and Agi
79. d is not compatible with connecting printers and plotters It s also called Null Modem Cable with full handshaking where the wiring is made between pins 1 1 2 3 3 2 4 6 5 5 6 4 7 8 8 7 9 9 RS 232 cable 8m Agilent 1200 Infinity Series DAD User Manual 231 12 Identifying Cables Analog Cables One end of these cables provides a BNC connector to be connected to Agilent modules The other end depends on the instrument to which connection is being made Agilent Module to 3394 6 Integrators p n 35900 60750 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Shield Analog 3 Center Analog 10 10 A0 Agilent Module to BNC Connector p n 8120 1840 Pin BNC Pin Agilent Signal Name module m Ay Shield Shield Analog a _ EO Center Center Analog 232 Agilent 1200 Infinity Series DAD User Manual Agilent Module to General Purpose Identifying Cables 12 p n 01046 60105 Pin 3394 6 Pin Agilent Signal Name module 1 Not connected 2 Black Analog 3 Red Analog _ ee Agilent 1200 Infinity Series DAD User Manual 233 12 Identifying Cables Remote Cables 234 O O JNE One end of these cables provides a Agilent Technologies APG Analytical Products Group remote connector to be connected to Agilent modules The other end depends on the instrument to be connected to Agilent Module to 3396A Integrators
80. d with the Firmware Update Tool To upgrade downgrade the module s firmware carry out the following steps 1 Download the required module firmware the latest LAN RS 232 FW Update Tool and the documentation from the Agilent web http www chem agilent com scripts cag_firmware asp 2 To load the firmware into the module follow the instructions in the documentation Table 26 Module Specific Information G4212A B G4212A 1290 DAD G4212B 1260 DAD Initial firmware main B 06 23 B 06 30 and resident Compatibility with When using the G4212A in a system all other When using the G4212B in a system all other 1100 1200 1260 129 modules must have firmware revision A 06 1x or modules must have firmware revision A 06 3x or 0 series modules B 06 1x and above main and resident B 06 3x and above main and resident Otherwise the communication will not work Otherwise the communication will not work Conversion to N A N A emulation Agilent 1200 Infinity Series DAD User Manual 223 10 Maintenance Information from Module s Assemblies Lamp and Flow Cell RFID Tag The detector is equipped with a UV lamp and flow cell identification system using RFID radio frequency identification tags attached to the assemblies and RFID tag readers at the optical unit The table below lists all parameters stored in the RFID tag Table 27 RFID Tag Data Lamp information Flow cell information product number product number
81. der operating conditions the radio interference limits are still met within the premises Agilent 1200 Infinity Series DAD User Manual 247 13 Appendix 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 Sound Pressure Lp lt 70 dB A e At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 248 Agilent 1200 Infinity Series DAD User Manual Appendix 13 Flow Cell To protect optimal functionality of your flow cell e Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell Use of Solvents Observe the following recommendations on the use of solvents e Brown glass ware can avoid growth of algae e Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography method allows replace 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 2CHCly O gt gt 2COCl
82. dicate the detector may require recalibration Parts required Description 1 Max Light Cartridge Test Cell or 1 Max Light Cartridge Cell Preparations Detector lamp must be on for more than 1 hour When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required Agilent 1200 Infinity Series DAD User Manual 195 9 Test Functions and Calibration Wavelength Calibration NOTE If the detector is operated in a lab environment that differs at average from the final test environment 25 C then the detector should be recalibrated for this temperature NOTE If the detector was repaired opened covers the wavelength calibration can be done 10 minutes after lamp on A final wavelength calibration should be repeated after complete warm up of the detector 1 Run the Wavelength Calibration with the recommended user interface for further information see Online Help of user interface Test Name Wavelength Calibration Description The wavelength calibration procedure enables you to check the calibration of the diode array in the detector Module G4212A PR00100015 Calibration means adjusting the assignment of diodes to specific wavelengths and is done using the two deuterium Status Passed emission lines at 486 0 nm and 656 1 nm Start Time 7 9 2009 1 59 26 PM Stop Time 7 9 2009 1 59 50 PM PITT TTT TTT Test Procedure WZ 1 Check Prerequisites Y 2 Ion Tet ced Y 3 Wavengh Veiteaten a Y 4 Calibrate
83. e application conditions The dispersion volume is fractionally increased compared to the standard cell Agilent 1200 Infinity Series DAD User Manual 143 144 Optimizing the Detector Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 nm to 640 nm using diode array detection A UV lamp provides good sensitivity over the whole wavelength range The diode array detector DAD can simultaneously compute and send to the data system up to eight chromatographic signals and the full range spectra at every time point A multi wavelength detector MWD processes only the chromatographic signals A UV chromatogram or signal is a plot of absorbance data versus time and is defined by its wavelength and bandwidth The wavelength indicates the center of the detection band e The bandwidth defines the wavelength range over which the absorbance values are averaged to give the result at each time point For example a signal at wavelength 250 nm with a bandwidth of 16 nm will be an average of the absorbance data from 242 nm to 258 nm Additionally a reference wavelength and reference bandwidth can be defined for each signal The average absorbance from the reference bandwidth centered on the reference wavelength will be subtracted from its equivalent value at the signal wavelength to produce the output chromatogram The signal wavelength and bandwidth can be chosen so that they are optimized for
84. e the margin for negative absorbance Use this option if for example your solvent gradient produces a decreasing baseline absorbance and for GPC analyses Limits 100 to 4000 mAU The higher the value the greater the baseline noise Set this value only if you expect negative absorbance greater than 100 mAU Slit G4212A You can select the optical bandwidth 1 2 4 or 8 nm of the detector the narrower the slit the smaller the optical bandwidth of the instrument but the lower its sensitivity The smaller the optical bandwidth the higher the spectral resolution Autobalance Defines whether a balance is performed prior to a run and or after a run has finished Lamp on required for analysis If unchecked the lamp will be turned off after the analysis has finished Agilent 1200 Infinity Series DAD User Manual 113 5 Using the Module Setting up the Detector with Agilent ChemStation Time Table Settings Timetable window 114 You may set up time events to change functions with their parameters over the run time Add lines as required Time Limits 0 00 to 99999 00 minutes in steps of 0 01 min Via the buttons in the bottom area time table lines can be added removed cut copied pasted or completely cleared You may set up time events to change functions with their parameters over the run time Add lines as required Limits 0 00 to 99999 00 minutes in steps of 0 01 min Based on the chosen function a cer
85. eans upper power limit hit excessive ambient temperature drop 1 means lower power limit hit excessive ambient temperature increase Probable cause Suggested actions 1 Ambient conditions have changed too much Verify that the reproducibility of your results during the run so that optimum results may is not affected not be guaranteed Expose the detector to more stable ambient conditions Agilent 1200 Infinity Series DAD User Manual 171 8 Error Information Detector Error Messages 172 Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual J 6 ee 9 e Test Functions and Calibration J Introduction 174 Use of Max Light Cartridge Test Cell 175 Conditions of Detector 176 Failing a Test 177 Self Test 178 Intensity Test 180 Test Failed 182 Cell Test 183 Test Failed low ratio value 184 Quick Noise Test 185 Test Failed 187 ASTM Drift and Noise Test 188 Test Failed 190 Slit Test G4212A 191 Test Failed 192 Wavelength Verification Test 193 Wavelength Calibration 195 Wavelength Recalibration Fails 197 D A Converter DAC Test 198 Test Failed 199 Dark Current Test 200 Test Failed 201 This chapter describes the tests for the module ot Agilent Technologies 173 9 Test Functions and Calibration Introduction 174 All tests are described based on the Agilent Lab Advisor Software B 01 03 Other user interfaces may not provide any test or just a few Table 23
86. elength band minus the average absorbance of the reference wavelength band Signal A in the detector default method is set to sample 254 0 4 reference 360 0 100 that is the average absorbance from 252 256 nm minus the average absorbance from 310 410 nm As all analytes show higher absorbance at 252 256 nm than at 310 410 nm this signal will show you virtually every compound which can be detected by UV absorbance Many compounds show absorbance bands in the spectrum Figure 45 on page 132 shows the spectrum of anisic acid as an example To optimize for lowest possible detectable concentrations of anisic acid set the sample wavelength to the peak of the absorbance band that is 252 nm and the sample bandwidth to the width of the absorbance band that is 30 nm A reference of 360 100 is adequate Anisic acid does not absorb in this range If you work with high concentrations you may get better linearity above 1 5 AU by setting the sample wavelength to a valley in the spectrum like 225 nm for anisic acid Agilent 1200 Infinity Series DAD User Manual 131 132 Optimizing the Detector 58 isic aci sample wavelength 252 nm Anisic acid 421 Reference bandwidth 100 nm 5 lt 324 o o n gt 284 E 30 nm 2 bandwidth z Reference wavelength 360 i 220 248 260 280 388 328 342 360 388 482 Wavelength nm Figure 45 Optimization of Wavelength Setting A wide bandwidth has the advantage of reducin
87. ent BootP Service assigns the Hardware MAC address of the instrument to an IP address Determining the MAC address of the instrument using BootP Service 1 Power cycle the Instrument 2 After the instrument completes self test open the log file of the BootP Service using Notepad The default location for the logfile is C Documents and Settings All Users Application Data Agilent BootP LogFile The logfile will not be updated if it is open The contents will be similar to the following 02 25 10 15 30 49 PM Status BootP Request received at outermost layer Status BootP Request received from hardware address 0010835675AC Error Hardware address not found in BootPTAB 0010835675AC Status BootP Request finished processing at outermost layer 3 Record the hardware MAC address for example 0010835675AC Agilent 1200 Infinity Series DAD User Manual 79 4 LAN Configuration 4 The Error means the MAC address has not been assigned an IP address and the Tab File does not have this entry The MAC address is saved to the Tab File when an IP address is assigned 5 Close the log file before turning on another instrument 6 Uncheck the Do you want to log BootP requests box after configuring instruments to avoid having the logfile use up excessive disk space Adding each instrument to the network using BootP 1 Follow Start gt All Programs gt Agilent BootP Service and select Edit BootP Settings The BootP Settings screen appears
88. er 5 m flow cell to waste Front Cover Leak funnel Leak funnel holder Tubing assembly i d 6 mm o d 9 mm 1 2 m to waste Leak downpipe Instant Pilot Instant Pilot G4208A requires firmware B 02 11 or above For cables refer to Cable Overview on page 230 226 Agilent 1200 Infinity Series DAD User Manual Parts and Materials for Maintenance 11 Overview of Maintenance Parts Agilent 1200 Infinity Series DAD User Manual 227 11 Parts and Materials for Maintenance Accessory Kits 228 Accessory kit p n G4212 68755 contains some specific accessories and tools needed for the installation of the detector p n 5062 2462 5063 6527 5042 9954 0100 1516 5067 4660 5181 1516 Description Teflon Tubing flexible i d 0 8 mm o d 1 6 mm 2 m re order 5 m flow cell to waste Tubing assembly i d 6 mm o d 9 mm 1 2 m to waste Tubing clip 2x re order 4 pk Fitting male PEEK 2 pk Inlet Capillary SST 0 12 mm I D 220 mm long CAN cable Agilent module to module 0 5 m Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 6 ee 12 e Identifying Cables J Cable Overview 230 Analog Cables 232 Remote Cables 234 BCD Cables 237 CAN LAN Cables 239 RS 232 Cable Kit 240 This chapter provides information on cables used with the Agilent 1260 Infinity 1290 Infinity LC modules ee Agilent Technologies 229 12 Identifying Cables Cable Ov
89. er Agilent modules Connect the LAN cable e g from an Agilent ChemStation as controller to the detector s LAN connector Connect the analog cable optional Connect the APG remote cable optional for non Agilent instruments 10 Turn on power by pushing the button at the lower left hand side of the module The status LED should be green Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 The module is turned on when the line power switch is pressed and the green indicator lamp is illuminated The module is turned off when the line power switch is protruding and the green light is off The module was shipped with default configuration settings To change these settings see chapter LAN Configuration After turn on of the detector it goes through a cycle of different states of heating up the optical unit and controlling the temperature This is described in Warm up of the Detector on page 149 Give the optical unit enough time to warm up and stabilize gt 60 minutes Agilent 1200 Infinity Series DAD User Manual 59 3 Installing the Module Flow Connections to the Detector Parts required Description 1 System 1 Max Light cartridge flow cell 1 Capillaries and tubing from Accessory Kit This procedure shows the detector outside of a system In an Agilent 1260 Infinity Liquid Chromatograph the detector is located below a G1316 TCC on the bench see Optimizing the Stack Configuration
90. er a TCP IP connection to the module is possible TCP IP parameters set by any method the parameters may be altered by opening a Telnet session 1 Open the system DOS prompt window by clicking on Windows START button and select Run Type cmd and press OK 2 Type the following at the system DOS prompt c gt telnet lt IP address gt or c gt telnet lt host name gt EV C WINDOWS system32 cmd exe Cz gt telnet 134 40 30 205 Figure 33 Telnet Starting a session where lt IP address gt may be the assigned address from a Bootp cycle a configuration session with the Handheld Controller or the default IP address see Configuration Switch on page 68 When the connection was established successfully the module responds with the following cv Telnet 134 40 30 205 3 Agilent Technolog 2A PROG1B8B15 Figure 34 A connection to the module is made 3 Type and press enter to see the available commands Agilent Technologies G4212A PRO81009015 gt command syntax escription isplay help info Figure 35 Telnet Commands Agilent 1200 Infinity Series DAD User Manual 85 4 86 LAN Configuration Table 19 Telnet Commands Value Description displays syntax and descriptions of commands displays current LAN settings ip lt X X X X gt sets new ip address SM lt X X X X gt sets new subnet mask gW lt X X X X gt sets new default gateway exit exits shell and saves all changes
91. erivatives after pre or post column derivatization Specifying a signal ratio that is typical for the sample class is one way of selectively plotting only those peaks that are of interest The signal output remains at zero so long as the ratio is out of the user specified ratio range When the ratio falls within the range the signal output corresponds to the normal absorbance giving single clear peaks on a flat baseline An example is shown in Figure 52 on page 140 and Figure 53 on page 141 Select 2 characteristic wavelengths 180 so Signal WL1 WL2 20 88 727 o Terphenyl i s n s Biphenyl aod BZ 304 S 207 N a A WL2 WL1 220 248 260 28a 3328 322 Wavelength nm Figure 52 Wavelength Selection for Ratio Qualifiers 140 Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Signals at 250 nm Biphenyl o Terphenyl No selectivity With ratio qualifier 250 222 nm 3 520 Time lini Figure 53 Selectivity by Ratio Qualifiers In a four component mixture only biphenyl was recorded The other three peaks were suppressed because they did not meet the ratio qualifier criterion and therefore the output was set to zero The characteristic wavelengths 249 nm A and 224 nm A were found from the spectra shown in Figure 52 on page 140 The ratio range was set at 2 2 4 2 2 10 Only when the ratio between 249 and 224 nm was within this range is the signal plotted Of al
92. ert LC2 left 25 25 255 0 0000 Figure 31 Edit BootP Adresses screen 4 In the Edit BootP Addresses screen press Add to create a new entry or select an existing line from the table and press Modify or Delete to change the IP address comment subnet mask for example in the Tab File If you change the IP address it will be necessary to power cycle the instrument for the changes to take effect 5 Leave Edit BootP Addresses by pressing Close 6 Exit BootP Settings by pressing OK Restarting the Agilent BootP Service 1 In the Windows control panel select Administrative Tools gt Services The Services screen appears see Figure 30 on page 82 2 Right click Agilent BootP Service and select Start 3 Close the Services and Administrative Tools screens Agilent 1200 Infinity Series DAD User Manual 83 4 LAN Configuration Manual Configuration Manual configuration only alters the set of parameters stored in the non volatile memory of the module It never affects the currently active parameters Therefore manual configuration can be done at any time A power cycle is mandatory to make the stored parameters become the active parameters given that the initialization mode selection switches are allowing it Non Volatile RAM Stored Parameter Ld Control Module Figure 32 Manual Configuration Principle 84 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 With Telnet Whenev
93. ervice gt EditBootPSettings 2 In BootP Settings check Do you want to log BootP requests to enable logging Logging V Do you want to log bootP requests BootP Log File ad a EEEE Figure 28 Enable BootP logging The log file is located in C Documents and Settings All Users Application Data Agilent BootP LogFile It contains a MAC address entry for each device that requests configuration information from BootP 3 Click OK to save the values or Cancel to discard them The editing ends 4 After each modification of the BootP settings i e EditBootPSettings a stop or start of the BootP service is required for the BootP service to accept changes See Stopping the Agilent BootP Service on page 82 or Restarting the Agilent BootP Service on page 83 5 Uncheck the Do you want to log BootP requests box after configuring instruments otherwise the log file will quickly fill up disk space 78 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Determining the MAC address directly from the LAN Interface card label 1 Turn off the instrument 2 Read the MAC address from the label and record it The MAC address is printed on a label on the rear of the module It is the number below the barcode and after the colon and usually begins with the letters AD See Figure 20 on page 66 and Figure 21 on page 66 3 Turn on the instrument Assigning IP Addresses Using the Agilent BootP Service The Agil
94. erview 230 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Analog cables p n Description 35900 60750 Agilent module to 3394 6 integrators 35900 60750 Agilent 35900A A D converter 01046 60105 Analog cable BNC to general purpose spade lugs Remote cables p n Description 03394 60600 Agilent module to 3396A Series integrators 3396 Series Il 3395A integrator see details in section Remote Cables on page 234 03396 61010 Agilent module to 3396 Series III 3395B integrators 5061 3378 Agilent module to Agilent 35900 A D converters or HP 1050 1046A 1049A 01046 60201 Agilent module to general purpose BCD cables p n Description 03396 60560 Agilent module to 3396 integrators G1351 81600 Agilent module to general purpose Agilent 1200 Infinity Series DAD User Manual CAN cables p n 5181 1516 5181 1519 LAN cables p n 5023 0203 5023 0202 RS 232 cables p n G1530 60600 RS232 61600 5181 1561 Identifying Cables 12 Description CAN cable Agilent module to module 0 5 m CAN cable Agilent module to module 1 m Description Cross over network cable shielded 3 m for point to point connection Twisted pair network cable shielded 7 m for point to point connection Description RS 232 cable 2 m RS 232 cable 2 5 m Instrument to PC 9 to 9 pin female This cable has special pin out an
95. es 166 Diode Current Leakage 166 UV Lamp Current 166 UV Lamp Voltage 167 UV Ignition Failed 167 UV Heater Current 168 Calibration Values Invalid 168 Wavelength Recalibration Lost 169 Illegal Value From Temperature Sensor 169 Illegal Value From Air Inlet Temperature Sensor 170 Heater Failed 170 Heater Power At Limit 171 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from error conditions aa Agilent Technologies 157 8 Error Information What Are Error Messages Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention before the analysis can be continued for example repair or exchange of consumables is necessary In the event of such a failure the red status indicator at the front of the module is switched on and an entry is written into the module logbook 158 Agilent 1200 Infinity Series DAD User Manual General Error Messages Error Information General error messages are generic to all Agilent series HPLC modules and may show up on other modules as well Timeout The timeout threshold was exceeded Probable cause 1 The analysis was completed successfully and the timeout function switched off the module as requested 2 Anot ready condition was present during a sequence or multiple injection run for a period longer than the timeout
96. ested actions 1 Not ready condition in one of the Ensure the instrument showing the not ready instruments connected to the remote line condition is installed correctly and is set up correctly for analysis 2 Defective remote cable Exchange the remote cable 3 Defective components in the instrument Check the instrument for defects refer to the showing the not ready condition instrument s documentation Agilent 1200 Infinity Series DAD User Manual Synchronization Lost Error Information 8 During an analysis the internal synchronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration If one or more of the modules is no longer recognized as being connected to the system the error message is generated Probable cause 1 CAN cable disconnected 2 Defective CAN cable 3 Defective main board in another module Leak Sensor Short Suggested actions Ensure all the CAN cables are connected correctly Ensure all CAN cables are installed correctly Exchange the CAN cable Switch off the system Restart the system and determine which module or modules are not recognized by the system The leak sensor in the module has failed short circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined
97. et for sample and reference Limits Wavelength 190 0 to 640 0 nm in steps of 0 1 nm Bandwidth 1 0 to 400 0 nm in steps of 0 1 nm Setting an appropriate reference wavelength could improve the baseline behavior Alternatively use the 1 6 ul heat exchanger from the G1316C TCC or an optional DAD heat exchanger if available Peakwidth enables you to select the peak width response time for your analysis The peak width is defined as the width of a peak in minutes at half the peak height Set the peak width to the narrowest expected peak in your chromatogram The peak width sets the optimum response time for your detector The peak detector ignores any peaks that are considerably narrower or wider than the peak width setting The response time is the time between 10 and 90 of the output signal in response to an input step function When the All spectrum storage 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 which is the acquisition time Limits When you set the peak width in minutes the corresponding response time is set automatically and the appropriate data rate for signal and spectra acquisition is selected Do not use peak width shorter than necessary Do not use 0 025 seconds response
98. eter configuration To operate properly in a network environment the LAN interface must be configured with valid TCP IP network parameters These parameters are e IP address e Subnet Mask e Default Gateway The TCP IP parameters can be configured by the following methods e by automatically requesting the parameters from a network based BOOTP Server using the so called Bootstrap Protocol e by manually setting the parameters using Telnet e by manually setting the parameters using the Instant Pilot G4208A The LAN interface differentiates between several initialization modes The initialization mode short form init mode defines how to determine the active TCP IP parameters after power on The parameters may be derived from a Bootp cycle non volatile memory or initialized with known default values The initialization mode is selected by the configuration switch see Table 18 on page 73 Agilent 1200 Infinity Series DAD User Manual 67 4 LAN Configuration Configuration Switch The configuration switch can be accessed at the rear of the module Figure 22 Location of Configuration Switch The module is shipped with all switches set to OFF as shown above To perform any LAN configuration SW1 and SW2 must be set to OFF Table 15 Factory Default Settings Initialization Init Mode Bootp all switches down For details see Initialization mode selection on page 69 Link C
99. example The Tab File is located at C Documents and Settings All Users Application Data Agilent BootP TabFile Agilent 1200 Infinity Series DAD User Manual 81 4 82 LAN Configuration Changing the IP Address of an Instrument Using the Agilent BootP Service Agilent BootP Service starts automatically when your PC reboots To change Agilent BootP Service settings you must stop the service make the changes and then restart the service Stopping the Agilent BootP Service 1 From the Windows control panel select Administrative Tools gt Services The Services screen appears 13 Eje Aton yew Heb e s DPDGIQ gt s n Select an tem to view Rs description istes Beodgoind Intedg Boerwatch HCP chore Bdetrteted irk Tra Boceerdeted Transa apne pee Figure 30 Windows Services screen 2 Right click Agilent BootP Service 3 Select Stop 4 Close the Services and Administrative Tools screen Editing the IP address and other parameters in EditBootPSettings 1 Select Start gt All Programs gt Agilent BootP Service and select Edit BootP Settings The BootP Settings screen appears 2 When the BootP Settings screen is first opened it shows the default settings from installation Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 3 Press Edit BootP Addresses to edit the Tab File 006000111933 Agera CI 1011 10 Agiert LEI ngt 255 255 255 0 0000 005000222883 Aghera C2 101 1 1 102 Agl
100. f the profile of the Max Light Cartridge Cell differs in the low UV range then absorbing solvents are in the cell and should be flushed out See also Cleaning of Max Light Cartridge Cell on page 218 When using the Max Light Cartridge Cell for tests calibrations it should be run at 0 5 ml min constant flow with water This assures that the light path is always flushed Below table gives an idea on the signal height variation of the Max Light Cartridge Cells compared to Max Light Cartridge Test Cell Table 24 Max Light Cartridge Cells compared to Max Light Cartridge Test Cell Part Number Description Signal Height typical G4212 60011 Max Light Cartridge Test Cell 100 G4212 60008 Max Light Cartridge Cell 10 mm V o 1 pl 100 G4212 60007 Max Light Cartridge Cell 60 mm V O 4 pl 100 Agilent 1200 Infinity Series DAD User Manual 175 9 Test Functions and Calibration Conditions of Detector The test usually should be performed with a detector turned on for at least one hour so that the temperature regulation of the optical unit is working not active during the first 30 minutes after turn on If the detector is on tests can be performed usually 10 minutes after the UV lamp has been turned on 176 Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration Failing a Test If a test fails with the Max Light Cartridge Cell repeat the test with the Max Light Cartridge Test Cell and compare
101. fault settings Advanced Spectrum Store None z Rar f t nr Analog Output Output 1 Zero Offset S Attenuation 1000 v mdu Margin for negative Absorbance Siit 100 mAU 4 v nm Autobalance Lamps on required for aquisition V Prerun V UY Lamp Postrun Figure 42 Method Parameter Settings The 1260 Infinity DAD G4212B has a fixed slit width of 4 nm 110 Agilent 1200 Infinity Series DAD User Manual Spectrum Settings Store Spectrum Store e Iro nm Apex Baselines P Apex Slopes Thr Apex Slope Baselines Allin Peak Analog Output pad 2nd Spectrum Nutan 1 None Apex Apex Baselines Apex Slopes Apex Slopes Baselines All in Peak Every 2nd spectrum Range Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Defines at which points on signal A spectra will be taken and saved Signal A is used to control the peak controlled spectra acquisition the other signals have no influence on spectra acquisition Limits 190 0 to 640 0 nm in steps of 0 1 nm for both low and high values The high value must be greater than the low value by at least 0 1 nm No spectra are taken Spectra are taken at the apex of the peak Spectra are taken at the apex and baselines of the peak Spectra are taken at the apex upslope and down slope of the peak Spectra are taken at the apex baselines upslope and down slope of the peak All spectra within the peak are taken Spectra
102. figuration This procedure describes the change of the TCP IP settings on your PC to match the module s default parameters in a local configuration see Table 17 on page 72 1 Open the Local Area Connection Properties and select Internet Protocol TCP IP Then click on Properties _4_ Local Area Connection Properties General Advanced Connect using B Broadcom NetXtreme Gigabit Etheme Configure This connection uses the following items Client for Microsoft Networks v B File and Printer Sharing for Microsoft Networks M E QoS Packet Scheduler Internet Protocol TCP IP Install Uninstall Description Transmission Control Protocol Intemet Protocol The default wide area network protocol that provides communication across diverse interconnected networks Properties IV Show icon in notification area when connected IV Notify me when this connection has limited or no connectivity 90 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 PC and Agilent ChemStation Setup 2 You may enter here the fixed IP address of the module or use the Alternative Configuration Internet Protocol TCP IP Properties Agilent 1200 Infinity Series DAD User Manual 91 4 LAN Configuration PC and Agilent ChemStation Setup 3 We will use the direct LAN access via Cross over LAN cable with the module s IP address Internet Protocol TCP IP Properties 4 Click on
103. g lamp 5190 0917 and may be not achieved when other lamp types or aged lamps are used ASTM drift tests require a temperature change below 2 C hour 3 6 F hour over one hour period Our published drift specification is based on these conditions Larger ambient temperature changes will result in larger drift Better drift performance depends on better control of the temperature fluctuations To realize the highest performance minimize the frequency and the amplitude of the temperature changes to below 1 C hour 1 8 F hour Turbulences around one minute or less can be ignored Performance tests should be done with a completely warmed up optical unit gt two hours ASTM measurements require that the detector should be turned on at least 24 h before start of testing Time Constant versus Response Time According to ASTM E1657 98 Standard Practice of Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatography the time constant is converted to response time by multiplying by the factor 2 2 Agilent 1200 Infinity Series DAD User Manual 43 2 44 Site Requirements and Specifications Performance Specifications Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 3 Installing the Module Unpacking the Module 46 Damage tothe module 46 Delivery Checklist 47 Detector Accessory Kit Contents 47 Optimizing the Stack Configuration 48 One Stack Configuration 49 Two
104. g noise by averaging over a wavelength range compared to a 4 nm bandwidth the baseline noise is reduced by a factor of approximately 2 5 whereas the signal is about 75 of a 4 nm wide band The signal to noise ratio for a 30 nm bandwidth is twice that for a 4 nm bandwidth in our example Bandwidth 30 nm 12 nm 4nm Figure 46 Influence of Bandwidth on Signal and Noise Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Because the detector averages absorbance values that are calculated for each wavelength using a wide bandwidth does not negatively impact linearity The use of a reference wavelength is highly recommended to further reduce baseline drift and wander induced by room temperature fluctuations or refractive index changes during a gradient An example of the reduction of baseline drifts is shown in Figure 47 on page 133 for PTH amino acids Without a reference wavelength the chromatogram drifts downwards due to refractive index changes induced by the gradient This is almost completely eliminated by using a reference wavelength With this technique PTH amino acids can be quantified in the low picomole range even in a gradient analysis Z y lt q za T 1pmol each Eo 2 A TE a a Wavelength 267 nm Reference 380nm Wavelength 267nm No reference Time min Grad 0 02 m KH P0 ACN from 12 ACN to 45 ACN in 12 min Figure 47 Gradient Analysis of PTH Amino Acids 1 p
105. ghest optical performance GLP compliance and easy maintenance It includes the following features Maximum of 160 Hz G4212A or 80 Hz G4212B data acquisition rate Higher sensitivity for conventional LC as well as ultra fast applications by using next generation optical design Increased sensitivity with 60 mm Max Light cartridge flow cell Optimized cell geometry for less peak dispersion for narrow bore applications More reliable and robust peak integration process automated due to less baseline noise drift refractive index and thermal effects especially under ultra fast gradient conditions RFID tracking technology is used for the UV lamp and the Max Light cartridge flow cells Multiple wavelength and full spectral detection at 160 Hz G4212A 80 Hz G4212B sampling rate keeping up with the analysis speed of ultra fast LC Programmable 1 8 nm slit G4212A or fixed 4 nm slit G4212B for rapid optimization of sensitivity linearity and spectral resolution provides optimum incident light conditions Improved Electronic temperature control ETC provides maximum baseline stability and practical sensitivity under fluctuating ambient temperature and humidity conditions Additional diagnostic signals for temperature and lamp voltage monitoring Easy exchange of flow cell by cartridge design For specifications see Specifications on page 41 10 Agilent 1200 Infinity Series DAD User Manual Introduction 1 O
106. ide it by 3 This may result in problems when the used peak width is set to large and all peaks are filtered accordingly Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards To check photometric accuracy of the Agilent detector it is necessary to have more precise information on path lengths of the detector flow cells Part Number Path Length Cell Volume C G4213 60008 1 0 cm 1 0 pL G4213 60007 6 0 cm 4 0 uL 128 Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Peak width response time Response time describes how fast the detector signal follows a sudden change of absorbance in the flow cell The detector uses digital filters to adapt response time to the width of the peaks in your chromatogram These filters do not affect peak area nor peak symmetry When set correctly such filters reduce baseline noise significantly Figure 44 on page 129 but reduce peak height only slightly In addition these filters reduce the data rate to allow optimum integration and display of your peaks and to minimize disk space required to store chromatograms and spectra DAD A Sign240 100 Refe360 100 042 12AINOIL_PW_100H 0 DADI A Sige280 100 Ram300 100 0 42 t2ANOI_PW_2EM D mau Response time 2 s PW gt 0 10 min 2 0 s response time 2 5 Hz PW lt 0 0016 min 0 016 s response time 160 Hz Response time 0 016 s Slit width 4 n
107. is another way of indicating how this filtering is set It is measured in seconds and is about one third of the peak width value which is measured in minutes It effectively shows how quickly the plotted signal responds to a step change in the input signal The full spectra is not available under all conditions Based on the data points the scan data rate is reduced see Table 21 on page 130 Agilent 1200 Infinity Series DAD User Manual 147 6 Optimizing the Detector Table 22 Peak Width Response Time Data Rate Peak width at half Response Signaldata Scan data rate Scan data rate Scan data rate Scan data rate height min s rate Hz HZ HZ HZ HZ 126 pts scan 251 pts scan 501 pts scan gt 501 pts scan lt 0 0016 0 016 1602 1602 80 40 20 gt 0 0016 0 03 1602 1602 80 40 20 gt 0 003 0 062 80 80 80 80 40 gt 0 006 0 12 40 40 40 40 40 gt 0 012 0 25 20 20 20 20 20 gt 0 025 0 5 10 10 10 10 10 gt 0 05 1 0 5 5 5 5 5 gt 0 10 2 0 2 5 2 5 2 5 2 5 2 5 gt 0 20 40 1 25 1 25 1 25 1 25 1 25 gt 0 40 8 0 0 625 0 62 0 625 0 625 0 625 gt 0 85 16 0 0 3125 0 31 0 3125 0 3125 0 3125 Values in the User Interface may be rounded 2 64212A only The maximum spectra scan rate depends on the data points per scan see Table 21 on page 130 Running at 160 Hz the spectra scan data rate is reduced automatically if the spectra scan data rate is more than 251 points scan 148 Agilent 1200 Infinity Series DAD User
108. ith or without data system Agilent Lab Advisor software helps to manage the lab for high quality chromatographic results and can monitor in real time a single Agilent LC or all the Agilent GCs and LCs configured on the lab intranet Agilent Lab Advisor software provides diagnostic capabilities for all Agilent 1200 Infinity Series modules This includes diagnostic capabilities calibration procedures and maintenance routines for all the maintenance routines The Agilent Lab Advisor software also allows users to monitor the status of their LC instruments The Early Maintenance Feedback EMF feature helps to carry out preventive maintenance In addition users can generate a status report for each individual LC instrument The tests and diagnostic features as provided by the Agilent Lab Advisor software may differ from the descriptions in this manual For details refer to the Agilent Lab Advisor software help files This manual provides lists with the names of Error Messages Not Ready messages and other common issues Agilent 1200 Infinity Series DAD User Manual Agilent 1200 Infinity Series DAD User Manual 8 Error Information What Are Error Messages 158 General Error Messages 159 Timeout 159 Shut Down 160 Remote Timeout 160 Synchronization Lost 161 Leak Sensor Short 161 Leak Sensor Open 162 Compensation Sensor Open 162 Compensation Sensor Short 163 Fan Failed 163 Leak 164 OpenCover 164 Cover Violation 165 Detector Error Messag
109. ith 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 WARNING Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual Safety Standards This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Agilent 1200 Infinity Series DAD User Manual 243 13 Appendix 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 de
110. k at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to access the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed Agilent 1200 Infinity Series DAD User Manual 57 3 Installing the Module ANALOG 1 Note the MAC address of the LAN interface rear of the module under the configuration switch see Figure 21 on page 66 It s required for LAN Configuration see Chapter LAN Configuration CONFIG CAN CAN Soe Dao Ack mP O 4e Made in Germany gt 2 2 fee Mehata garn PAIT irs m wv d h COMPACT FLASH S E A gt gt gt gt Product No G4212A PPLE 5 D gt LLL Ea gt gt gt gt gt CULL mame Tre gt gt 58 uy oO 1 A Rear View of Detector Electrical Connections and Label Figure 19 Set the Configuration Switch according the required initialization mode default fixed IP or Bootp see Chapter LAN Configuration Place the module in the stack see Optimizing the Stack Configuration on page 48 Ensure the line power switch at the front of the module is OFF Connect the power cable to the power connector at the rear of the module Connect the CAN cable to oth
111. l 209 10 Maintenance placing the Deuterium Lamp 3 Unscrew the 3 screws of the lamp housing cover and remove the cover 4 Locate the two screws that fix the lamp and unscrew ner Agilent Ga2z12 60008 Wm Wa A we Sr AN Re wrav a S 1 O G4212 60008 SO ren ie 1 0 ut Vax Wows OW Fal 210 Agilent 1200 Infinity Series DAD User Manual 10 Maintenance Replacing the Deuterium Lamp NOTE Do not touch the glass bulb with your fingers It may reduce the light output 7 Insert the lamp and reconnect the lamp connector 8 Locate the two screws and fix the lamp L Pe aaa r AIS Aaa ODE l ey N a b Am _A a a TA LE N at lt J G A NS Sy Ean J 7 o 2 0 d BEA 0 D D 9 Fit the lamp wires in the lamp house cover so that they are not scratched by the cover Agilent 1200 Infinity Series DAD User Manual 211 10 Maintenance 10 Replace the lamp housing cover and fix the 3 screws 11 Close the front cover 12 Perform a Wavelength Re calibration after lamp warm up 212 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Replacing the Max Light Cartridge Cell When If leaking or if intensity drops due to contaminated flow cell Tools required Hexagonal wrench Parts required p n Description
112. l four peaks only the third fulfilled the criterion Figure 53 on page 141 The others were not plotted Agilent 1200 Infinity Series DAD User Manual 141 6 Optimizing the Detector Optimizing the Detector Regarding to the System 142 Delay Volume and Extra Column Volume The delay volume is defined as the system volume between the point of mixing in the pump and the top of the column The extra column volume is defined as the volume between the injection point and the detection point excluding the volume in the column Extra Column Volume Extra column volume is a source of peak dispersion that will reduce the resolution of the separation and so should be minimized Smaller diameter columns require proportionally smaller extra column volumes to keep peak dispersion at a minimum In a liquid chromatograph the extra column volume will depend on the connection tubing between the autosampler column and detector and on the volume of the flow cell in the detector The extra column volume is minimized with the Agilent 1290 Infinity Agilent 1260 Infinity LC System due to the narrow bore 0 12 mm i d tubing the low volume heat exchangers in the column compartment and the Max Light cartridge cell in the detector How to Configure the Optimum Delay Volume To maintain resolution in the Agilent 1290 Infinity Agilent 1260 Infinity Diode array Detector the Max Light cartridge cell has a low dispersion volume o volume 1 0 ul and no f
113. lay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to 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 244 Agilent 1200 Infinity Series DAD User Manual Appendix 13 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 When working with solvents please observe appropriate safety procedures e g goggles safety gloves and protective clothing
114. lectronic fuses are implemented in the power supply WARNING Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to access the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed WARNING Incorrect line voltage at the module Shock hazard or damage of your instrument can result if the devices are connected to line voltage higher than specified gt Connect your module to the specified line voltage 36 Agilent 1200 Infinity Series DAD User Manual CAUTION Site Requirements and Specifications 2 Unaccessable power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear The male end of each power cord is different and designed to match the wall socket of a particular country o
115. lent ChemStation Setup 90 Agilent 1200 Infinity Series DAD User Manual Contents Using the Module 99 Preparing the Detector 100 Setting up the Detector with Agilent ChemStation 101 Main Screens of the Detector with Agilent Instant Pilot G4208A 119 Optimizing the Detector 123 Introduction 124 Optimization Overview 125 Optimizing for Sensitivity Selectivity Linearity and Dispersion 127 Optimizing Selectivity 138 Optimizing the Detector Regarding to the System 142 Warm up of the Detector 149 Troubleshooting and Diagnostics 151 Overview of the Module s Indicators and Test Functions 152 Status Indicators 153 Available Tests vs User Interfaces 155 Agilent Lab Advisor Software 156 Error Information 157 What Are Error Messages 158 General Error Messages 159 Detector Error Messages 166 Test Functions and Calibration 173 Introduction 174 Use of Max Light Cartridge Test Cell 175 Conditions of Detector 176 Failing a Test 177 Self Test 178 Intensity Test 180 Cell Test 183 Quick Noise Test 185 ASTM Drift and Noise Test 188 Slit Test G4212A 191 Wavelength Verification Test 193 Agilent 1200 Infinity Series DAD User Manual Contents Wavelength Calibration 195 D A Converter DAC Test 198 Dark Current Test 200 10 Maintenance 203 Warnings and Cautions 204 Introduction to Maintenance 206 Overview of Maintenance 207 Cleaning the Module 208 Replacing the Deuterium Lamp 209 Replacing the Max Light C
116. m o os 1 18 2 25 3 35 o a5 mis Figure 44 Influence of Response Time on Signal and Noise Table 21 on page 130 lists the filter choices of the detector To get optimum results set peak width as close as possible to a narrow peak of interest in your chromatogram Response time will the be approximately 1 3 of the peak width resulting in less than 5 peak height reduction and less than 5 additional peak dispersion Decreasing the peak width setting in the detector will result in less than 5 gain in peak height but baseline noise will increase by a factor of 1 4 for a factor of 2 response time reduction Increasing peak width response time by factor of two from the recommended setting over filtering will reduce peak height by about 20 and reduce baseline Agilent 1200 Infinity Series DAD User Manual 129 6 Optimizing the Detector noise by a factor of 1 4 This gives you the best possible signal to noise ratio but may affect peak resolution Table 21 Peak Width Response Time Data Rate Peak width at half Response Signal data Scan data rate Scan data rate Scan data rate Scan data rate height min s rate Hz HZ HZ HZ HZ 126 pts scan 251 pts scan 501 pts scan gt 501 pts scan lt 0 0016 0 016 1602 1602 80 40 20 gt 0 0016 0 03 1602 1602 80 40 20 gt 0 003 0 062 80 80 80 80 40 gt 0 006 0 12 40 40 40 40 40 gt 0 012 0 25 20 20 20 20 20 gt 0 025 0 5 10 10 10 10 10 gt 0 05 1 0 5 5 5 5 5 gt 0 10 2 0
117. mol each with and without Reference Agilent 1200 Infinity Series DAD User Manual 133 6 Optimizing the Detector Slit Width G4212A The 1290 Infinity DAD G4212A has a variable slit at the entrance of the spectrograph This is an effective tool to adapt the detector to changing demand of different analytical problems A narrow slit provides spectral resolution for analytes with very fine structures in the absorbance spectrum An example of such a spectrum is benzene The five main absorbance bands fingers are only 2 5 nm wide and just 6 nm apart from each other 240 245 250 255 Figure 48 Benzene at 1 and 4 nm slit width principle A wide slit uses more of the light shining through the flow cell This gives lower baseline noise as shown in Figure 49 on page 135 134 Agilent 1200 Infinity Series DAD User Manual Slit width 8 nm Slit width 1 nm Data Rate 160 Hz Optimizing the Detector 6 DADI A Sige240 100 Rete200 100 G42 1ZAINOL_SwW_1_D mau DADI A Sign280 100 Rem300 100 GAD 1ZAINOL_SW_S 0 o os 1 15 2 25 2 2s 4 as min mau Figure 49 Influence of the Slit Width on Baseline Noise However with a wider slit the spectrograph s optical resolution its ability to distinguish between different wavelengths diminishes Any photodiode receives light within a range of wavelength determined by the slit width This explains why the fine spectral structure of benzene disappears when using a 8
118. nal detector can only detect and quantify both compounds independently from each other if their spectra do not overlap However in most cases this is highly unlikely With a dual channel detector based on diode array technology quantifying two compounds is possible even when both compounds absorb over the whole wavelength range The procedure is called peak suppression or signal subtraction As an example the analysis of hydrochlorothiazide in the presence of caffeine is described If hydrochlorothiazide is analyzed in biological samples there is always a risk that caffeine is present which might interfere chromatographically with hydrochlorothiazide As the spectra in Figure 50 on page 138 shows hydrochlorothiazide is best detected at 222 nm where caffeine also shows significant absorbance It would therefore be impossible with a conventional variable wavelength detector to detect hydrochlorothiazide quantitatively when caffeine is present WL1 204 nm caffeine WL2 222 nm hydrochlorothiazide WL3 260 nm reference to suppress hydrochlorothiazide WL4 282 nm reference to suppress caffeine wa wa l WL1 WL2 Wavelength nm Figure 50 Wavelength Selection for Peak Suppression 138 Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 With a UV visible detector based on a diode array and the correct choice of a reference wavelength setting quantitative detection is possible To suppress caffei
119. ndicates the module has detected an internal problem which affects correct operation of the module Usually an error condition requires attention e g leak defective internal components An error condition always interrupts the analysis A red blinking modules with on board LAN or yellow blinking modules without on board LAN indicator indicates that the module is in resident mode e g during update of main firmware A fast red blinking modules with on board LAN or fast yellow blinking modules without on board LAN indicator indicates that the module is in boot loader mode e g during update of main firmware In such a case try to re boot the module or try a cold start 154 Agilent 1200 Infinity Series DAD User Manual Troubleshooting and Diagnostics 7 Available Tests vs User Interfaces e Depending on the user interface the available tests and the screens reports may vary see Chapter Test Functions and Calibrations e Preferred tool should be the Agilent Diagnostic Software see Agilent Lab Advisor Software on page 156 The Agilent ChemStation B 04 02 and above do not include any maintenance test functions e Screenshots used within these procedures are based on the Agilent Lab Advisor Software Agilent 1200 Infinity Series DAD User Manual 155 7 Troubleshooting and Diagnostics Agilent Lab Advisor Software 156 The Agilent Lab Advisor software is a standalone product that can be used w
120. ne the reference wavelength must be set to 282 nm At this wavelength caffeine shows exactly the same absorbance as at 222 nm When the absorbance values are subtracted from each another any indication of the presence of caffeine is eliminated In the same way hydrochlorothiazide can be suppressed if caffeine is to be quantified In this case the wavelength is set to 204 nm and the reference wavelength to 260 nm Figure 51 on page 139 shows the chromatographic results of the peak suppression technique The trade off for this procedure is a loss in sensitivity The sample signal decreases by the absorbance at the reference wavelength relative to the signal wavelength Sensitivity may be decreased by as much as 10 30 Hydrochlorothiazide Hydrochlorothiazide and caffeine and caffeine Wavelength 204 nm Wavelength 222 nm No reference No reference Hydrochlorothiazides Caffeine suppressed uppressed Wavelength 204 nm Wavelength 222 nm Reference 260 nm Reference 282 nm 6 2 8 112 1 2 6 2 8 1 2 1 2 Time min Time min Figure 51 Peak Suppression Using Reference Wavelength Agilent 1200 Infinity Series DAD User Manual 139 6 Optimizing the Detector Ratio Qualifiers for Selective Detection of Compound Classes Ratio qualifiers can be used where in a complex sample only one particular class needs to be analyzed a parent drug and its metabolites in a biological sample for example Another example is the selective analysis of d
121. nfinity 1290 Infinity LC System Manual Agilent 1200 Infinity Series DAD User Manual One Stack Configuration Installing the Module One Stack Configuration for Agilent 1260 Infinity LC Ensure optimum performance by installing the modules of the Agilent 1260 Infinity LC System in the following configuration See Figure 11 on page 49 and Figure 12 on page 50 This configuration optimizes the flow path for minimum delay volume and minimizes the bench space required Solvent cabinet Vacuum degasser Local User Interface Autosampler Column compartment Detector Figure 11 Recommended Stack Configuration for 1260 Front View Agilent 1200 Infinity Series DAD User Manual 3 49 3 Installing the Module Optimizing the Stack Configuration Remote cable CAN Bus cable to local user interface CAN Bus cable Analog detector signal 1 or 2 outputs per detector AC power LAN to LC ChemStation location depends on detector Figure 12 Recommended Stack Configuration for 1260 Rear View 50 Agilent 1200 Infinity Series DAD User Manual Installing the Module Optimizing the Stack Configuratio One Stack Configuration for Agilent 1290 Infinity LC Ensure optimum performance by installing the modules of the Agilent 1290 Infinity LC System in the following configuration See Figure 13 on page 51 and Figure 14 on page 52 This configuration optimizes the flow pa
122. nt Leakage When the detector is switched on the processor checks the leakage current of each of the optical diodes If the leakage current exceeds the upper limit the error message is generated Probable cause Suggested actions 1 Defective PDA optical unit Please contact your Agilent service representative 2 Defective connector or cable Please contact your Agilent service representative UV Lamp Current The UV lamp current is missing The processor continually monitors the anode current drawn by the lamp during operation If the anode current falls below the lower current limit the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the UV lamp connector is seated firmly 2 Defective UV lamp or non Agilent lamp Exchange the UV lamp 3 Defective detector main board Please contact your Agilent service representative 4 Defective power supply Please contact your Agilent service representative 166 Agilent 1200 Infinity Series DAD User Manual UV Lamp Voltage The UV lamp anode voltage is missing Error Information 8 The processor continually monitors the anode voltage across the lamp during operation If the anode voltage falls below the lower limit the error message is generated Probable cause 1 Defective UV lamp or non Agilent lamp 2 Defective detector main board 3 Defective power supply UV Ignition Failed The UV lamp failed to ignite Suggested actions
123. nt the configuration switch settings for the modules without on board LAN only 30 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Table5 8 bit Configuration Switch without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Parity Bits Reserved 1 0 Reserved TEST BOOT 1 1 rsvo sys rsvo rsvo Fc The LAN settings are done on the LAN Interface Card G1369A B Refer to the documentation provided with the card Communication Settings for RS 232C The communication protocol used in the column compartment supports only hardware handshake CTS RTR Switches 1 in down and 2 in up position define that the RS 232C parameters will be changed Once the change has been completed the column instrument must be powered up again in order to store the values in the non volatile memory Table6 Communication Settings for RS 232C Communication without on board LAN Mode Select 1 2 3 4 5 6 7 8 RS 232C 0 1 Baudrate Data Bits Parity Use the following tables for selecting the setting which you want to use for RS 232C communication The number 0 means that the switch is down and 1 means that the switch is up Agilent 1200 Infinity Series DAD User Manual 31 1 32 Introduction Table 7 Baudrate Settings without on board LAN Switches Baud Rate Switches Baud Rate 3 4 5 3 4 5 0 0 0 9600 1 0 0 9600 0 0 1 1200 1 0 1 14400 0 1 0 2400 1 1 0 19200 0 1 1 4800 1 1 1 3840
124. oint Set the peak width close to the width of a narrow peak of interest in your chromatogram 4 Setting wavelength and bandwidth Sample wavelength Never miss a peak by the use of a browser wavelength like 250 nm with 100 nm bandwidth Select specific wavelength with reduced optical bandwidth if you need selectivity e g 254 0 nm 4 nm and 360 0 nm 100 nm as reference wavelength Set the sample wavelength to a peak or valley to get best linearity in general select a valley to get best linearity for high concentrations Reference wavelength Select the reference wavelength with broad bandwidth 30 100 nm wavelength range where your analytes have little or no absorbance e g sample at 254 nm reference at 320 nm Select the reference wavelength as near as possible to the UV range 5 Setting the slit width G4212A only Use 4nm slit for normal applications Use narrow slit e g 1 nm if your analytes have narrow absorbance bands and for high concentrations Use a wide slit e g 8 nm to detect very low concentrations Optimizing spectral acquisition DAD only Select spectra acquisition mode according to your needs see Spectrum Settings on page 111 Set the spectral wavelength range for colorless samples 190 400 nm is sufficient Set step to 4 nm for normal use set small step and slit width if high resolution of spectra with fine structure is wanted peak resolution versus sensitivity
125. ole or in part by improper use of the products unauthorized alterations adjustments or modifications to the products failure to comply with procedures in Agilent product user guides or use of the products in violation of applicable laws rules or regulations gt Use your Agilent products only in the manner described in the Agilent product user guides CAUTION Safety standards for external equipment gt If you connect external equipment to the instrument make sure that you only use accessory units tested and approved according to the safety standards appropriate for the type of external equipment Agilent 1200 Infinity Series DAD User Manual 205 10 Maintenance Introduction to Maintenance The module is designed for easy maintenance Maintenance can be done from the front with module in place in the system stack There are no serviceable parts inside Do not open the module 206 Agilent 1200 Infinity Series DAD User Manual Overview of Maintenance Maintenance 10 The following pages describe maintenance simple repairs of the detector that can be carried out without opening the main cover Table 25 Overview of Maintenance Procedure Typical Frequency Notes Cleaning of module If required Deuterium lamp If noise and or drift exceeds your application limits or A wavelength calibration test and an exchange lamp does not ignite intensity test should be performed after replacement Flow cell exchange If
126. on switch e The power input socket accepts a line voltage of 100 240 VAC 10 witha line frequency of 50 or 60 Hz Maximum power consumption varies by module 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 Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Agilent 1200 Infinity Series DAD User Manual 19 1 introduction Electrical Connections Rear view of the module REMOTE oto uss a LAN A 4 iB p Sk amu amo unm Tamsa gt COMPACT FLASH Se ata G Como Product No 64212A SETETE 7 Loren vee cs on Dhont vial No 10 mM Ag tow webamtegan MLD Morsan Made in Germany Figure 7 Rear View of Detector Electrical Connections and Label NOTE The CompactFlash Card Slot is not active yet It may be used for future enhancements 20 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Information on Instrument Serial Number Serial Number Information 1200 Series and 1290 Infinity The serial number information on the instrument labels provide the following information CCYWW
127. onfiguration speed and duplex mode determined by auto negotiation for details see Link configuration selection on page 73 68 Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Initialization mode selection The following initialization init modes are selectable Table 16 Initialization Mode Switches SW6 SW7 SW8 Init Mode OFF OFF OFF Bootp OFF OFF ON Bootp amp Store OFF ON OFF Using Stored OFF ON ON Using Default Bootp When the initialization mode Bootp is selected the module tries to download the parameters from a Bootp Server The parameters obtained become the active parameters immediately They are not stored to the non volatile memory of the module Therefore the parameters are lost with the next power cycle of the module Bootp gt Active Server Parameter Figure 23 Bootp Principle Agilent 1200 Infinity Series DAD User Manual 69 4 70 LAN Configuration Bootp amp Store When Bootp amp Store is selected the parameters obtained from a Bootp Server become the active parameters immediately In addition they are stored to the non volatile memory of the module Thus after a power cycle they are still available This enables a kind of bootp once configuration of the module Example The user may not want to have a Bootp Server be active in his network all the time But on the other side he may not have any other configuration method than Bootp In this case he sta
128. or and UV lamp must be on for at least 2 hours ASTM measurements based on specifications may require longer stabilization times When using a Max Light Cartridge Cell a flow rate of 0 5 ml min with water is required Agilent 1200 Infinity Series DAD User Manual 185 9 Test Functions and Calibration Quick Noise Test 1 Run the Quick Noise Test with the recommended user interface for further information see Online Help of user interface Quick Noise Test Description The test performs a quick Noise Evaluation without reference G4212A PR00100015 Passed 749 2009 2 03 53 PM 7 9 2009 2 09 10 PM EO ___ _ aooema _ _ Figure 63 Quick Noise Test Results Figure 64 Quick Noise Test Signals 186 Agilent 1200 Infinity Series DAD User Manual Test Failed Quick Noise Test Evaluation Probable cause 1 Insufficient lamp warm up time 2 Absorbing solvent or air bubble in flow cell 3 Dirty or contaminated flow cell 4 Old UV lamp Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration Suggested actions Allow detector and UV lamp turned on for at least 2 hours Ensure the flow cell is filled with water and free from air bubbles Flush flow cell Clean the flow cell as described in Cleaning of Max Light Cartridge Cell on page 218 Exchange the UV lamp 187 9 9 Test Functions and Calibration ASTM Drift and Noise Test When Parts required
129. over 164 164 illegal value from air inlet senso 170 illegal value from heater sensor 169 remote timeout 160 uv heater current 168 uv ignition failed 167 uvlamp current 166 uvlamp voltage 167 wavelength calibration failed 168 method parameter settings using 107 negative absorbance 137 noise and drift ASTM 41 Noise and Linearity specifications 43 noise 188 non operating altitude 40 non operating temperature 40 0 operating Altitude 40 operating temperature 40 optical 11 Agilent 1200 Infinity Series DAD User Manual optimization detector performance 124 detector sensitivity 143 for sensitivity selectivity linearity dispersion 127 how to get the best performance 124 margins for negative absorbance 137 of selectivity 138 overview 125 peak width 129 performance 123 sample and reference wavelength 131 slit width 134 spectra acquisition 136 stack configuration 48 wavelength and bandwidth 144 optimizing 1260 System 142 flow cell 126 other advanced method parameter using 113 overview for maintenance 226 P packaging damaged 46 parts identification accessory kit 228 PC and Agilent ChemStation Setup 90 PC setup local configuration 90 peak width response time 129 peak width 147 performance optimization 124 specifications 41 photometric accuracy 128 253 Index physical specifications 40 power supply indicator 153 power considerations 36 power consumption 40 power cords 37 prog
130. ovides visual feedback in the user interface when the limit is exceeded Some counters can be reset to zero after the required maintenance procedure Using the EMF Counters The user settable EMF limits for the EMF Counters enable the early maintenance feedback to be adapted to specific user requirements The useful maintenance cycle is dependent on the requirements for use Therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially the default EMF limits should be set When instrument performance indicates maintenance is necessary take note of the values displayed by the EMF 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 Agilent 1200 Infinity Series DAD User Manual 17 1 Introduction 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 of foam plastic spacers in which the mechanical and electronic boards com
131. page 72 Default Active Parameter Parameter Figure 26 Using Default Principle Using the default address in your local area network may result in network problems Take care and change it to a valid address immediately Agilent 1200 Infinity Series DAD User Manual 71 4 72 LAN Configuration Table 17 Using Default Parameters IP address 192 168 254 11 Subnet Mask 255 255 255 0 Default Gateway not specified Since the default IP address is a so called local address it will not be routed by any network device Thus the PC and the module must reside in the same subnet The user may open a Telnet session using the default IP address and change the parameters stored in the non volatile memory of the module He may then close the session select the initialization mode Using Stored power on again and establish the TCP IP connection using the new parameters When the module is wired to the PC directly e g using a cross over cable or a local hub separated from the local area network the user may simply keep the default parameters to establish the TCP IP connection In the Using Default mode the parameters stored in the memory of the module are not cleared automatically If not changed by the user they are still available when switching back to the mode Using Stored Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Link configuration selection The LAN interface supports 10 or 100 Mbp
132. ponents 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 e virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly e the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations e the plastic layers help cushion the electronic and mechanical parts from physical shock and e the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself 18 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Electrical Connections e The CAN bus is a serial bus with high speed data transfer The two connectors for the CAN bus are used for internal module data transfer and synchronization e One analog output provides signals for integrators or data handling systems 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 the module from a computer through a RS 232C connection This connector is activated and can be configured with the configurati
133. ptical System Optical System The optical system of the detector is shown in Figure 1 on page 11 Figure 1 Optical System of the Detector 1 UV lamp 2 Lamp mirror 3 Flow cell 4 Fold mirror 5 Programmable G4212A or Fixed G4212B slit 6 Grating 7 Array The illumination source is a deuterium arc discharge lamp 1 for the ultraviolet UV wavelength range Its light is focused by a lamp mirror 2 onto the entrance of the Max light cartridge flow cell 3 with optofluidic waveguides The light leaves the Max light cartridge flow cell at the other side and is focused by the fold mirror 4 through the slit assembly 5 onto a holographic grating 6 light being dispersed onto the diode array 7 This allows simultaneous access to all wavelength information Agilent 1200 Infinity Series DAD User Manual 11 1 Introduction Lamp The light source for the UV wavelength range is a long life UV lamp with RFID tag As a result of plasma discharge in low pressure deuterium gas the lamp emits light over the 190 nm to approximately 800 nm wavelength range Figure 2 UV Lamp 12 Agilent 1200 Infinity Series DAD User Manual Introduction 1 Max Light Cartridge Flow Cell The detector allows easy access to flow cells via a cartridge A variety of optional flow cells can be inserted using the same quick simple mounting system A Max Light Cartridge Cell 10 mm V o 1 0 ul and a Max Light Cartridge Cell 60 mm V o 4 uL
134. r increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative 162 Agilent 1200 Infinity Series DAD User Manual Error Information 8 Compensation Sensor Short The ambient compensation sensor NTC on the main board in the module has failed short circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor falls below the lower limit the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Fan Failed The cooling fan in the module has failed The hall sensor on the fan shaft is used by the main board to monitor the fan speed If the fan speed falls below a certain limit for a certain length of time the error message is generated Probable cause Suggested actions 1 Fan cable disconnected Please contact your Agilent service representative 2 Defective fan Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Agilent 1200 Infinity Series DAD User Manual 163 8 Error Information Leak A leak was detected in the module The signals from the two
135. r region Absence of ground connection or use of unspecified power cord The absence of ground connection or the use of unspecified power cord can lead to electric shock or short circuit gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Agilent 1200 Infinity Series DAD User Manual 37 2 Site Requirements and Specifications WARNING Unintended use of supplied power cords Using power cords for unintended purposes can lead to personal injury or damage of electronic equipment gt Never use the power cords that Agilent Technologies supplies with this instrument for any other equipment Bench Space The module dimensions and weight see Table 12 on page 40 allow you to place the module on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 8 1 inches in the rear for air circulation and electric connections If the bench should carry an Agilent system make sure that the bench is designed to bear the weight of
136. rammable slit width 41 Q quick noise test 185 radio interference 247 recalibration initial 64 recyclable material 42 remote cable 234 repairs cautions and warnings 204 replacing firmware 223 response time peak width 129 response time versus time constant 43 response time 147 RS 232C cable 240 communication settings 31 S safety class 243 safety general information 243 standards 40 symbols 242 sample and reference wavelength 131 selectivity optimization 138 self test 178 serial number information 21 21 254 setup ChemStation 93 detector 101 shut down 160 signal wavelength 145 site requirements power cords 37 slittest 191 slitwidth 41 134 slit fix 15 programmable 14 solvents 249 sound emission 248 special interfaces 27 special settings boot resident 33 forced cold start 34 specification physical 40 specifications analog signal output 42 communications 42 control and data evaluation 42 diode width 41 flow cell 41 GLP features 42 linear range 41 noise and drift ASTM 41 noise and linearity 43 programmable slit width 41 safety and maintenance 42 signal data rate 41 spectra data rate 41 wavelength accuracy 41 wavelength bunching 41 wavelength range 41 spectra acquisition 136 spectrum settings using 111 stack configuration 54 rearview 54 suppression quantifying 138 synchronization lost 161 system setup and installation optimizing stack configuration 48 system 11
137. rference 247 Sound Emission 248 Flow Cell 249 Agilent Technologies on Internet 250 This chapter provides addition information on safety legal and web ee Agilent Technologies 241 13 Appendix Safety Safety Symbols Table 28 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available A and the user should not touch it when heated up WARNING es alerts you to situations that could cause physical injury or death gt 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 loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 242 Agilent 1200 Infinity Series DAD User Manual Appendix 13 General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or w
138. rts the Bootp Server temporarily powers on the module using the initialization mode Bootp amp Store waits for the Bootp cycle to be completed closes the Bootp Server and powers off the module Then he selects the initialization mode Using Stored and powers on the module again From now on he is able to establish the TCP IP connection to the module with the parameters obtained in that single Bootp cycle Bootp Active Server Parameter Non Volatile RAM Stored Parameter Figure 24 Bootp amp Store Principle Use the initialization mode Bootp amp Store carefully because writing to the non volatile memory takes time Therefore when the module shall obtain its parameters from a Bootp Server every time it is powered on the recommended initialization mode is Bootp Agilent 1200 Infinity Series DAD User Manual LAN Configuration 4 Using Stored When initialization mode Using Stored is selected the parameters are taken from the non volatile memory of the module The TCP IP connection will be established using these parameters The parameters were configured previously by one of the described methods Non Volatile RAM Active Parameter Stored Parameter Figure 25 Using Stored Principle Using Default When Using Default is selected the factory default parameters are taken instead These parameters enable a TCP IP connection to the LAN interface without further configuration see Table 17 on
139. s voltages and currents of lamps that can be used for diagnosing baseline problems see Diagnostic Signals 152 Agilent 1200 Infinity Series DAD User Manual Troubleshooting and Diagnostics 7 Status Indicators Status Indicators Two status indicators are located on the front of the module The lower left indicates the power supply status the upper right indicates the module status Status indicator a a si i _ ower supply indicator Figure 57 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 Agilent 1200 Infinity Series DAD User Manual 153 7 Troubleshooting and Diagnostics Module Status Indicator The module status indicator indicates one of six possible module conditions e When the status indicator is OFF and power switch light is on the module is in a prerun condition and is ready to begin an analysis e A green status indicator indicates the module is performing an analysis run mode A yellow indicator indicates a not ready condition The module is ina 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 e An error condition is indicated when the status indicator is red An error condition i
140. s operation in full or half duplex modes In most cases full duplex is supported when the connecting network device such as a network switch or hub supports IEEE 802 3u auto negotiation specifications When connecting to network devices that do not support auto negotiation the LAN interface will configure itself for 10 or 100 Mbps half duplex operation For example when connected to a non negotiating 10 Mbps hub the LAN interface will be automatically set to operate at 10 Mbps half duplex If the module is not able to connect to the network through auto negotiation you can manually set the link operating mode using link configuration switches on the module Table 18 Link Configuration Switches SW3 SW4 SW5 Link Configuration OFF speed and duplex mode determined by auto negotiation ON OFF OFF manually set to 10 Mbps half duplex ON OFF ON manually set to 10 Mbps full duplex ON ON OFF manually set to 100 Mbps half duplex ON ON ON manually set to 100 Mbps full duplex Agilent 1200 Infinity Series DAD User Manual 73 4 LAN Configuration Automatic Configuration with BootP All examples shown in this chapter will not work in your environment You need your own IP Subnet Mask and Gateway addresses Assure that the detector configuration switch is set properly The setting should be either BootP or BootP amp Store see Table 16 on page 69 Assure that the detector connected to the network is powered off
141. s set to high temperatures the up streaming air could influence the stability of the detector baseline Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Setting up the Detector with Agilent ChemStation The setup of the detector is shown with the Agilent ChemStation B 04 02 based on the 1290 Infinity DAD G4212A Depending on the controller e g Agilent Instant Pilot EZChrom Elite MassHunter the screens look different For the Instant Pilot refer to Main Screens of the Detector with Agilent Instant Pilot G4208A on page 119 This section describes the detector settings only For information of the Agilent ChemStation or other Agilent 1260 Infinity 1290 Infinity Series modules refer to the corresponding documentation or system manual After successful load of the ChemStation you should see the module as an active item in the graphical user interface GUI Agilent 1200 Infinity Series DAD User Manual 101 5 Using the Module Setting up the Detector with Agilent ChemStation nil D NotReady Instrument 0 00 0 00 Not Ready Figure 41 ChemStation Method amp Run 102 Agilent 1200 Infinity Series DAD User Manual The Detector GUI 1290 Infinity DAD O Not Ready WL BWRefWL RefBW mAU 254 0 4 210 0 4 214 0 4 230 0 4 260 0 4 360 0 360 0 360 0 360 0 360 0 100 100 100 100 100 17 14 1 13 8 1 1 1 2 Agilent 1200 Infinity Series DAD U
142. ser Manual Using the Module 5 Setting up the Detector with Agilent ChemStation Within the detector GUI there are active areas If you move the mouse cursor across the icons the cursor will change and you may click on the button 1 to Make Device Ready Turn device off standby turn on off the lamp Signal Information activated by button 1 shows actual values of all selected signals Signal name A B C Sample wavelength bandwidth Reference wavelength bandwidth Absorbance If more signals are activated the size of the detector GUI will change accordingly 103 5 Using the Module Setting up the Detector with Agilent ChemStation S 1290 Infinity DAD Idle M WL BW RefWL RefBW mAU A 250 0 100 off off 1 1 104 A right click into the Active Area will open a menu to Show the Control Interface special module settings Show the Method interface similar as via menu Instrument Setup Instrument Method Set Error Method Identify Module Status LED will blink Perform a Balance Switch the UV lamp on off same as click on button Make Device Ready Turn device off standby Module Status shows Run Ready Error state and Not Ready text or Error text Error Red Not ready yellow Ready green Pre run Post run purple Run blue Idle green Offline dark gray Standby light gray Agilent 1200 Infinity Series DAD User Manual Idle Mh 129
143. stalling the Module 3 Ensure all parts and materials have been delivered with the module The delivery checklist is shown below Please report missing or damaged parts to your local Agilent Technologies sales and service office Table 14 Detector Checklist Description Quantity Detector 1 Power cable 1 Cross over network cable 1 Twisted pair network cable 1 Max Light Cartridge Cell 1 10 mm V 1 0 uL or 60 mm V o 4 0 pL User Manual on Documentation CD part of the Accessory kit shipment not module specific 1 Detector Accessory Kit Contents Detector Accessory Kit Contents p n G4212 68755 p n 5062 2462 5063 6527 5042 9954 0100 1516 5067 4660 5181 1516 Description Teflon Tubing flexible i d 0 8 mm o d 1 6 mm 2 m re order 5 m flow cell to waste Tubing assembly i d 6 mm o d 9 mm 1 2 m to waste Tubing clip 2x re order 4 pk Fitting male PEEK 2 pk Inlet Capillary SST 0 12 mm I D 220 mm long CAN cable Agilent module to module 0 5 m Agilent 1200 Infinity Series DAD User Manual 47 3 Installing the Module Optimizing the Stack Configuration 48 If your module is part of a complete Agilent 1260 Infinity 1290 Infinity LC System you can ensure optimum performance by installing the following configurations These configurations optimize the system flow path ensuring minimum delay volume For other possible configurations please refer to the Agilent 1260 I
144. system Part of the processing reduces the data to an appropriate data rate which allows the chromatographic peaks to be accurately drawn As with most analytical determinations groups of readings are effectively averaged to reduce error in the result The detector bunches raw data points and produces the output signal data at the required data collection rate by an electronic filtering process If the resulting data rate is too slow over filtering the peak heights will be reduced and the resolution between them reduced too fast and the data is noisier than it need be to accurately profile narrow peaks The peak width setting in the detector allows the user to correctly set these parameters without needing any knowledge other than sight of the chromatogram integration results to see how wide the peaks are The peak width setting should be set for the narrowest peak width observed in the chromatogram If it is set too wide it will make the peaks appear lower in height and wider and potentially less resolved and if it is set too narrow it will increase the baseline noise unnecessarily Essentially the software uses this value to set the data collection rate such that it collects enough data points over the narrowest peaks and it is aiming for 15 to 25 points across a peak The 1290 Infinity DAD can collect at a maximum 160 Hz if required which would allow enough data points to be collected over a peak that is only 0 1 s wide The response time setting
145. t 39 flow connections 60 60 of the detector 57 power considerations 36 Instant Pilot using 119 instrument configuration using 117 instrument curves using 116 instrument layout 18 intensity test 180 interfaces 22 internet 250 L lamp uv 12 LAN configuration ChemStation 93 PC setup 90 LAN Agilent 1200 Infinity Series DAD User Manual Index automatic configuration with Bootp 74 Bootp amp Store 70 Bootp 69 cable 239 configuration switche 68 first steps 66 initialization mode selection 69 link configuration selection 73 manual configuration with telnet 85 manual configuration 84 PC and Agilent ChemStation Setup 90 TCP IP parameter configuration 67 using default 71 using stored 71 what you have to do first 66 eak sensor open 162 eak sensor short 161 eak 164 ine frequency 40 ine voltage 40 inearrange 41 inearity specifications 43 ink configuration selection 73 ocal configuration 90 M MAC address determine 79 MAC address 66 maintenance definition of 206 drying the leak sensor 220 feedback 17 lamp and flow cell RFID tag 224 overview 207 replacing firmware 223 replacing leak handling system 221 replacing the deuterium lamp 209 replacing the flow cell 213 serial number and firmware revision 224 manual configuration of LAN 84 max light cartridge flow cell 13 message cover violation 165 diode current leakage 166 heater failed 170 heater power at limit 171 ignition without c
146. tain parameter can be selected Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Setting up the Detector with Agilent ChemStation Time Table Graph In this view the activated signals are shown how they change according the time table 7 40 lzs00 1000 Fi 2200 lt 40 gt ano 1000 Wi 2500 1000 jao 1000 v s a T a a a T 7 Si Agilent 1200 Infinity Series DAD User Manual 115 5 Using the Module Setting up the Detector with Agilent ChemStation Instrument Curves The detector has several signals internal temperatures voltages of lamps that can be used for diagnosing problems These can be baseline problems deriving from deuterium lamps wander drift problems due to temperature changes These signals can be used in addition to the normal baseline signal to determine whether correlation to temperature or voltage current of the lamp These signals are available via the Agilent ChemStation Online Plot Data Signal and or Agilent Lab Advisor Software 116 Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Setting up the Detector with Agilent ChemStation Instrument Configuration These settings are available via menu Instrument Instrument Configuration instrument Configuration Y xl EET S Ie a peng eae Qs g SH 040 1642124 PROMS D rors te GG auspo Of ameco Figure 43 Menu Instr
147. temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the main board Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries Open Cover The top foam has been removed Probable cause Suggested actions 1 Foam not activating the sensor Please contact your Agilent service representative 2 Dirty or defective sensor Please contact your Agilent service representative 164 Agilent 1200 Infinity Series DAD User Manual Error Information 8 Cover Violation The top foam has been removed The sensor on the main board detects when the top foam is in place If the foam is removed while the lamp is on or if an attempt is made to switch on for example the lamp with the foam removed the lamp is switched off and the error message is generated Probable cause Suggested actions 1 The top foam was removed during operation Please contact your Agilent service representative 2 Foam not activating the sensor Please contact your Agilent service representative Agilent 1200 Infinity Series DAD User Manual 165 8 Error Information Detector Error Messages These errors are detector specific Diode Curre
148. terminations It is important that the reference bandwidth does not extend to a part of the spectrum that has some absorbance as this would then reduce the resulting signal and sensitivity would be reduced The use of a reference wavelength can help to reduce drift or wander in the chromatogram caused by refractive index changes due to room temperature fluctuation or gradient operation The effect of a reference signal can be easily tested by setting two otherwise identical signals one with and one without a reference signal If there is no part of the spectrum with zero absorbance then it will be better to have the reference signal turned off Agilent 1200 Infinity Series DAD User Manual 145 6 Optimizing the Detector signal Pa wavelength Anisic Acid reference bandwidth 100 nm reference 30 nm bandwidth wavelength 350 nm 220 240 260 288 3808 Wavelength Figure 54 Spectrum of Anisic Acid 146 Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 Peak Width Response Time and Data Collection Rate The peak width setting response time and data rate in the detector are all linked The available settings are shown in Table 21 on page 130 It is important to set this correctly for optimum sensitivity and to preserve the resolution achieved in the separation The detector internally acquires data points faster than is needed for a chromatogram and processes them to produce the signal seen by the data
149. th 145 BCD cable 237 Beer Lambert law 127 bench space 38 BootP service installation 76 restart 83 settings 82 stop 82 Bootp amp Store 70 automatic configuration 74 initialization modes 69 using default 71 using stored 71 C cable analog 232 BCD 237 CAN 239 connecting APG remote 54 connecting CAN 54 connecting GPIB 54 connecting LAN 54 connecting the ChemStation 54 connecting the power 54 LAN 239 remote 234 RS 232 240 cables analog 230 BCD 230 CAN 231 LAN 231 Agilent 1200 Infinity Series DAD User Manual overview 230 remote 230 RS 232 231 CAN cable 239 cartridge cleaning 218 max light 218 storage 219 cautions and warnings 204 celltest 183 ChemStation setup 93 cleaning flow cell 218 Communication settings RS 232C 31 compensation sensor open 162 compensation sensor short 163 condensation 39 46 configuration switche 68 configuration one stack 49 49 51 stack 48 two stack front 55 two stack rear 56 two stack 53 55 control and data evaluation 42 control settings using 106 correction factors for flow cells 128 D D A converter 198 251 Index DAC Agilent LabAdvisor 198 Instant Pilot 199 dark current 200 data collection rate 147 data evaluation and control 42 defect on arrival 46 delay volume 142 delivery checklist 47 detection compound classes 140 detector warmup 149 detector achieving higher sensitivity 143 installation 57 preparation 100 setup with ChemSt
150. th for minimum delay volume and minimizes the bench space required The Agilent 1290 Infinity Binary Pump should always be installed at the bottom of the stack Instant Pilot Solvent cabinet Detector Column compartment Autosampler Pump S sr yr Figure 13 Recommended Stack Configuration for 1290 Front View Agilent 1200 Infinity Series DAD User Manual 51 3 3 Installing the Module Optimizing the Stack Configuration LAN to LC ChemStation INAV WINN CAN Bus cable to Instant Pilot Analog detector signal optional AC Power CAN Bus cable Figure 14 Recommended Stack Configuration Rear View 52 Agilent 1200 Infinity Series DAD User Manual Installing the Module 3 Two Stack Configuration Two Stack Configuration for Agilent 1260 Infinity LC To avoid excessive height of the stack when the autosampler thermostat is added to the system it is recommended to form two stacks Some users prefer the lower height of this arrangement even without the autosampler thermostat A slightly longer capillary is required between the pump and autosampler See Figure 15 on page 53 and Figure 16 on page 54 Instant Pilot Detector Column compartment
151. time no filtering high noise and no need actually ultra fast LC doesn t deliver peaks lt 0 0025 min lt 0 15 sec The 1260 Infinity DAD G4212B has a data rate of up to 80 Hz Agilent 1200 Infinity Series DAD User Manual Peakwidth time programmed Peakwidth same as Peakwidth v 2 times greater than Peakwidth 4 times greater than Peakwidth 8 times greater than Peakwidth Stoptime Posttime Stoptime Posttime As Pump Injector Off min min Agilent 1200 Infinity Series DAD User Manual Using the Module 5 These selections can be made during time programmed operation When used in a timetable Peakwidth changes the filters used for peak controlled spectra acquisition but not the data rate of a chromatographic signal This setting makes sense only with peak controlled spectra it allows you to change the peakwidth setting to account for broadening peaks at the end of the run The stoptime is the time where either the complete system stops As Pump Injector or the module if different from system stop time The data collection is stopped at this time A posttime period can be used to allow module s items to equilibrate e g after gradient change or temperature change 109 5 Using the Module Advanced Method Parameter Settings These settings are available via a click on the Advanced link of the Method Parameter Settings in case the Time Table Settings are open This screen shows the de
152. tly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met For Research Use Only Agilent 1200 Infinity Series DAD User Manual In This Book In This Book This manual covers the Agilent 1290 Infinity Diode Array Detector G4212A and the Agilent 1260 Infinity Diode Array Detector G4212B Find information on other Agilent Diode Array Detectors in separate manuals 1 Introduction This chapter gives an introduction to the detector instrument overview and internal connectors 2 Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications 3 Installing the Module This chapter provides information on unpacking checking on completeness stack considerations and installation of the module 4 LAN Configuration This chapter provides information on connecting the module to the Agilent ChemStation PC 5 Using the Module This chapter provides information on how to set up the module for an analysis and explains the basic settings 6 Optimizing the Detector This chapter provides information on how to optimize the detector 7 Troubleshooting and Diagnostics Overview about the troubleshooting and diagnostic features Agilent 1200 Infinity Series DAD User Manual 3 In This Book 8 Error Information This chapter des
153. to Achieve Higher Sensitivity 143 Warm up of the Detector 149 This chapter provides information on how to optimize the detector ait Agilent Technologies 123 6 Optimizing the Detector Introduction The detector has a variety of parameters that can be used to optimize performance Depending on whether signal or spectral data need to be optimized different settings are recommended The following sections describe optimization for e signal sensitivity selectivity and linearity e spectral sensitivity and resolution DAD only and e disk space required for storing data The information in this chapter should be seen as a basic introduction to diode array detector techniques Some of these techniques may not be available in the instrument software controlling the detector How to Get the Best Detector Performance The information below will guide you on how to get the best detector performance Follow these rules as a start for new applications It gives rules of thumb for optimizing detector parameters 124 Agilent 1200 Infinity Series DAD User Manual Optimization Overview Table 20 Optimization Overview Optimizing the Detector 6 Parameter Impact 1 Selection of flow cell Choose flow cell according to used column Choosing a Flow Cell on page 126 2 Connection of flow cell 3 Setting the peak width response time Use peak width according Choosing a Flow Cell on page 126 as starting p
154. ts and Specifications Physical Specifications 40 Table 12 Physical Specifications Type Weight Dimensions height x width x depth Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating Altitude Non operating altitude Safety standards IEC CSA UL Specification 11 5 kg 26 Ibs 140 x 345 x 435 mm 5 5 x 13 5 x 17 inches 100 240 VAC 10 50 or 60 Hz 5 160 VA 130 W 444 BTU 4 40 C 39 104 F 40 70 C 4 158 F Operating lt 80 Non Operating lt 95 Up to 2000 m 6562 ft Up to 4600 m 15091 ft Comments Wide ranging capability Maximum Non condensing For storing the module Installation Category Il Pollution Degree 2 For indoor use only Agilent 1200 Infinity Series DAD User Manual Site Requirements and Specifications Performance Specifications Specifications Table 13 Performance Specifications G4212A B 2 Type Specification Comments Detection type Light source Wavelength range Short term noise ASTM Single and Multi Wavelength Drift Linear absorbance range Wavelength accuracy Wavelength bunching Slit width Diode width Signal data rate Spectra Data rate Flow cells 1024 element photodiode array Deuterium lamp 190 640 nm lt 3x 10 AU at 230 nm 4 nm lt 0 5 x 10 AU hr at 230 nm gt 2 0 AU 5
155. ue Parts required p n Description 1 5061 3388 Leak funnel 1 5041 8389 Leak funnel holder 1 5062 2463 Tubing Flex 5 m 1 G4212 40027 Leak downpipe Preparations Turn the pump off 1 Remove the front cover 2 Locate the leak interface area Agilent 1200 Infinity Series DAD User Manual 221 10 Maintenance Replacing Leak Handling System Parts 3 Pull the leak funnel out of the leak funnel holder and slide 4 Insert the leak interface system parts Ensure the tubing the Leak downpipe up for removal is fitted correctly in the bottom N BLM 4 SUES ARAANARAARRARAN 5 Close the front cover 222 Agilent 1200 Infinity Series DAD User Manual Maintenance 10 Replacing Module Firmware When The installation of newer firmware might be necessary if a newer version solves problems of older versions or to keep all systems on the same validated revision The installation of older firmware might be necessary to keep all systems on the same validated revision or if a new module with newer firmware is added to a system or if third part control software requires a special version Tools required LAN RS 232 Firmware Update Tool or Agilent Lab Advisor software e Instant Pilot G4208A only if supported by module Parts required Description 1 Firmware tools and documentation from Agilent web site Preparations Read update documentation provide
156. ument Configuration Via the Instrument Configuration screen additional modules can be added to a system Agilent 1200 Infinity Series DAD User Manual 117 5 Using the Module Setting up the Detector with Agilent ChemStation Use the Auto Configuration to define the LAN communication between the Agilent ChemStation and the host module usually the Agilent detector Changing parameters become active after reboot of the P address 192 168 254 11 ChemStation Hostname Agilent 1100 1200 1290 Series LE Auto Ce Device name based on the module Type ID based on the module product number Some modules may allow changing the type based on Device name EENET hardware firmware This results in a change of features Type ID 1642124 and functions Serial number based on the module Serial number RROTIOODIS Firmware revision based on the module Firmware revision B 06 23 0003 Options lists installed options Connection settings 118 Agilent 1200 Infinity Series DAD User Manual Using the Module 5 Main Screens of the Detector with Agilent Instant Pilot G4208A Below the main screens for the use of the detector are shown The Welcome screen shows all modules of the system errs F TAO ty 642124 pRoo100015 1 Configure 2Maintenance 3Diagnosis Sequence status J Logbook Morea Welcome The Control screen allows Lamp On Off 1 System On
157. urther volume optimization is required In situations where the alternative Agilent Max Light high sensitivity cell is used to get higher sensitivity the cell volume is optimized for the use with 3 mm and 4 6 mm inner diameter columns Agilent 1200 Infinity Series DAD User Manual Optimizing the Detector 6 How to Achieve Higher Sensitivity The detector has a number of parameters that are used to optimize performance The following sections describe how the detector parameters affect performance characteristics e Flow cell affects sensitivity e Wavelength and bandwidth affect sensitivity selectivity and linearity e Slit Width affects sensitivity spectral resolution and linearity e Peak Width affects sensitivity and resolution Flow Cell The Max Light cartridge flow cell has a standard 10 mm path length and is optimized for minimal volume and dispersion 6 volume 1 0 ul It has high light transmission minimizing noise to reduce noise due to the optofluidic waveguide It is suitable for use with a wide range of analytical columns from short narrow bore columns to long standard diameter 4 6 mm columns Generally the peak dispersion volume calculated from peak width x flow rate should be greater than about 2 ul for this cell for example 0 02 min x 200 ul min 4 ul The Max Light high sensitivity cell has a path length of 60 mm and this will give between three and five times increase in signal to noise values depending on th
158. utter ina simple and compact component The slit width is directly controlled by the micro processor of the instrument and is fixed to 4 nm Agilent 1200 Infinity Series DAD User Manual 15 1 16 Introduction Optical System Grating and Diode Array The combination of dispersion and spectral imaging is accomplished by using a concave holographic grating The grating separates the light beam into all its component wavelengths and reflects the light onto the photodiode array The diode array is a series of 1024 individual photodiodes and control circuits located on a ceramic carrier It has a wavelength range from 190 640 nm and the sampling interval is 0 5 nm Figure 6 Grating and diode array Agilent 1200 Infinity Series DAD User Manual Introduction 1 Early Maintenance Feedback 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 module and the analytical conditions and not on a predefined time interval The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user selectable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters EMF counters increment with use and can be assigned a maximum limit which pr
159. vity to that molecule The detector is linear up to 2 AU and beyond for many applications This offers a wide linear range for concentration For high concentration analysis the concentration linear range can be extended by setting the wavelength to one with a lower absorbance such as a wavelength minimum or by taking a wider bandwidth which usually includes lower absorbance values The use of wavelength maxima and minima for quantitation dates back to conventional UV detectors which because of mechanical tolerances in moving gratings needed to avoid steeply sloping parts of the spectrum Diode array based detectors do not have this limitation but for reasons of convention maxima and minima are chosen in preference to other parts of the spectrum The reference bandwidth is normally set on a region of the UV spectrum in which the analyte has no absorbance This is shown in the spectrum for anisic acid in Figure 54 on page 146 This spectrum is typical of many small molecules containing a UV chromophore For best results the reference has been set so that it is a wide band as close to the signal wavelength as possible but on a zero absorbance region Reference bandwidths of 60 nm to 100 nm are commonly used The default reference is 360 nm with a bandwidth of 100 nm A wide bandwidth is used because this reduces the noise in the reference signal from statistical theory the error i e noise in this case is reduced by the square root of the number of de
160. y through control module and ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user setable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with the emission lines of the deuterium lamp All materials recyclable For G4212A 1 B 04 02 or above 2 3 3 2 SP1 or above 3 B 02 01 SP1 or above For G4212B 1 B 04 02 DSP3 or above 2 3 3 2 SP2 or above 3 B 04 00 and B 03 01 SP2 or above B 02 11 or above B 01 03 SP4 or above 42 Agilent 1200 Infinity Series DAD User Manual Site Requirements and Specifications 2 Specification Conditions ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions e Wavelength 230 nm 4 nm with Reference Wavelength 360 nm 100 nm Slitwidth 4 nm TC 2 s or with RT 2 2 TC ASTM e Max Light Cartridge Cell 10 mm V o 1 0 ul with flow of 0 5 ml min LC grade water or Max Light Cartridge Test Cell Linearity Linearity is measured with caffeine at 265 nm 4 nm with slit width 4 nm and TC 1 s or with RT 2 s with Max Light Cartridge Cell 10 mm V o 1 ul gt 2 0 AU 5 typical 2 5 AU 5 The specifications are based on the standard RFID ta
161. y applying a digital test signal to the DAC The DAC outputs an analog signal of approximately 50 mV if the zero offset of the analog output is set to the default value of 5 which can be plotted on an integrator A continuous square wave with an amplitude of 10 uV anda frequency of approximately 1 cycle 24 seconds is applied to the signal The amplitude of the square wave and the peak to peak noise are used to evaluate the DAC test If the analog detector signal is noisy or missing Lamp must be on for at least 10 minutes Connect integrator chart recorder or data system to the detector analog output Running the test with Agilent LabAdvisor 1 Run the D A Converter DAC Test for further information see Online Help of user interface Test Name DJA Converter Test Description The test switches a test signal to the analog output that can be measured using an integrator or strip chart recorder Module G4212A PRO0100015 Status Passed Start Time 719 2009 3 06 30 PM Stop Time 7 9 2009 3 06 53 PM HERRGRRRRRERRR REE Test Procedure Y 1 Check Prerequisites 4 2 Switch on Analog Output 6 3 Switch off Analog Output Figure 71 D A Converter DAC Test Results Agilent 1200 Infinity Series DAD User Manual Test Functions and Calibration 9 ADCT A ADC CHANNEL mAu 76 504 76 522 76 49 76588 7065 o2 os os Figure 72 Running the Test with Instant Pilot i 12 14 16 18 D A Converter DAC

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