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Agilent 1220 Infinity LC User Manual

1. p n 03396 61010 Pin 33XX Pin Agilent Signal Name Active module TTL 9 1 White Digital ground ae NC 2 Brown Prepare run Low o i 3 3 Gray Start Low z NC 4 Blue Shut down Low NC 5 Pink Not connected NC 6 Yellow Power on High E 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 Pin Agilent Signal Name Active A D 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 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low 355 14 Identifying Cables Agilent Module to General Purpose p n 01046 60201 Wire Color Pin Agilent Signal Name Active module TTL 7 White 1 Digital ground a Ol ou Brown 2 Prepare run Low 00 pes DE KEY Gray 3 Start Low oo o0 S iE Blue 4 Shut down Low og Pink 5 Not oa connected 5 5 15 Q Yellow 6 Power on High Red 7 Ready High Green 8 Stop Low Black 9 Start request Low 356 1220 Infinity LC BCD Cables 1220 Infinity LC Identifying Cables 14 One end of these cables provides a 15 pin BCD connector to be connected to the Agilent modules The
2. Agilent Technologies Notices Agilent Technologies Inc 2010 2014 2015 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 64280 90016 Rev D Edition 02 2015 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 thi
3. 1220 Infinity LC 1220 Infinity LC Test Functions and Calibration 9 Table 27 Pressure limit not reached but plateaus horizontal or positive Potential Cause Degasser and pump not flushed sufficiently air in the pump head Wrong solvent Corrective Action Purge the degasser and pump thoroughly with isopropanol under pressure use the restriction capillary Install isopropanol Purge the degasser and pump thoroughly Table 28 All plateaus negative Potential Cause Loose or leaky fittings Loose purge valve Contaminated purge valve Loose pump head screws Leaking seals or scratched plungers Leaking outlet valve Leaky damper Corrective Action Ensure all fittings are tight or exchange capillary Tighten the purge valve 14 mm wrench Open and close purge valve to flush out contamination Exchange the valve if still leaky Ensure the pump head screws are tight Exchange the pump seals Check the plungers for scratches Exchange if scratched Exchange the outlet valve Exchange damper 143 9 144 Test Functions and Calibration Table 29 First plateau positive second and third plateau negative Potential Cause Air in pump or new seals not yet seated Loose active inlet valve Loose pump head screws Loose outlet valve Leaking seal or scratched plunger Defective active inlet valve Corrective Action Flush pump thoroughly with isoprop
4. Agilent 1220 Infinity LC Power cable Flow cell User Manual on Documentation CD part of the shipment not module specific Installation guide Accessory kit see below 1 1 Installed 1 per order 1220 Infinity LC Installation 3 Accessory Kit Contents for G4286B p n Description G4286 68755 Accessory kit complete 0100 2562 Fitting onepiece fingertight 0890 1195 PTFE tubing 0 052 in i d 0890 1711 Flexible tubing to waste 3 m 5023 0203 Cross over network cable shielded 3 m for point to point connection 5062 8535 Waste accessory kit 5188 2758 PTFE silicone septa 16mm pre silt 100 pk delivered quantity is 0 010 5190 1501 Syringe 50 0 pL FN LC tip 9301 0411 Syringe Plastic 9301 1337 Syringe adapter 9301 1377 Screw Cap Vial clear 6 mL 100 PK delivered quantity is 0 010 9301 1379 Screw caps for 6 mL vials 100 PK delivered quantity is 0 010 9301 1420 Solvent bottle transparent G1311 60003 Bottle head assembly 1220 Infinity LC 31 3 Installation Accessory Kit Contents for G4288B C p n G4288 68755 0100 2562 0890 1195 0890 1711 5023 0203 5062 8535 5188 2758 5190 1501 9301 0411 9301 1337 9301 1377 9301 1379 9301 1420 9301 1450 G1311 60003 2x 32 Description Accessory kit complete Fitting onepiece fingertight PTFE tubing 0 052 in i d Flexible tubing to waste 3 m Cross over network cable shielded 3 m for point to point connection Was
5. Check external instruments for a shut down condition 199 10 Error Information 200 Lost CAN Partner Error ID 0071 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 Error ID 0062 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 threshold 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 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 1220 Infinity LC Error Information 10 Pump Error Messages
6. If the application requires a different type of flow cell or the flow cell needs maintenance 1 Press the release buttons and remove the lower front cover to gain access to the flow cell area 2 Disconnect the inlet and outlet capillaries 288 1220 Infinity LC Maintenance 11 Variable Wavelength Detector VWD 3 Unscrew the thumb screws in parallel and remove the flow cell 4 Insert the new flow cell and fix the thumb screws Next Steps 6 To check for leaks establish a flow and observe the flow cell outside of the cell compartment and all capillary connections 7 Replace the front cover 1220 Infinity LC 289 11 Maintenance Repairing the Flow Cell Parts required p n Description G1314 60086 Standard flow cell 10 mm 14 pL 40 bar G1314 65061 Cell Repair Kit includes 2x Gasket 1 2x Gasket 2 2x Window Quartz CAUTION Window surfaces scratched by tweezers Window surfaces can easily be scratched by using tweezers to remove the windows gt Do not use tweezers to remove the windows 1 1 Cell screw 2 Conical springs iy 3 Ring 2 IN Y 5 6 4 Gasket 2 IN 5 Quartz window 6 Gasket 1 OUT M AA a l Og 2 3x Oy 06 7 Ring 1 OUT Cc Figure 69 Standard Flow Cell 10 mm 14 pL 1 Press the release buttons and remove the lower front cover to gain access to the flow cell area 290 1220 Infinity LC Mainte
7. 352 1220 Infinity LC Identifying Cables 14 Agilent Module to BNC Connector p n 8120 1840 Pin BNC Pin Agilent Signal Name module yoo ted Shield Shield Analog ral AC heey Ne Center Center Analog Agilent Module to General Purpose p n 01046 60105 Pin Pin Agilent Signal Name module 1 Not connected 2 Black Analog _Se 3 Red Analog Oh 1220 Infinity LC 353 14 Identifying Cables Remote Cables 354 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 p n 03394 60600 Pin 3396A Pin Agilent Signal Name Active module TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 80 A 3 3 Gray Start Low z NC 4 Blue Shut down Low e oa NC 5 Pink Not Ls connected NC 6 Yellow Power on High 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 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready 1220 Infinity LC 1220 Infinity LC Identifying Cables 14 Agilent Module to 3396 Series III 3395B Integrators
8. Therefore flow cells with longer path lengths yield higher signals Although noise usually increases a little with increasing path length there is a gain in signal to noise ratio For example the noise increases by less than 10 but a 70 increase in signal intensity is achieved by increasing the path length from 6 mm to 10 mm When increasing the path length the cell volume usually increases in our example from 5 uL to 13 uL Typically this causes more peak dispersion As Figure 52 on page 132 demonstrates this does not affect the resolution in the gradient separation in our example As a rule of thumb the flow cell volume should be about 1 3 of the peak volume at half height To determine the volume of your peaks take the peak width as reported in the integration results multiply it by the flow rate and divide it by 3 Analysis of pesticide standard 6 mm optical path length i Absorbance 10 mm optical path length f j E A j la A fh Nl hf i AAU JUV APAT O _ 10 Time min Figure 52 Influence of cell path length on signal height Traditionally LC analysis with UV detectors is based on comparing measurements with internal or external standards To check photometric accuracy of the detector it is necessary to have more precise information on path lengths of the flow cells The correct response is expected response correction factor Details of t
9. These errors are specific to the pump Encoder Missing Error ID 2046 2050 2510 The optical encoder on the pump motor in the module is missing or defective The processor checks the presence of the pump encoder connector every 2 s If the connector is not detected by the processor the error message is generated Probable cause Suggested actions 1 Defective or disconnected pump encoder Please contact your Agilent service connector representative 2 Defective pump drive assembly Please contact your Agilent service representative Index Adjustment 1220 Infinity LC Error ID 2204 2214 The encoder index position in the module is out of adjustment During initialization the first piston is moved to the mechanical stop After reaching the mechanical stop the piston reverses direction until the encoder index position is reached If the time to reach the index position is too long the error message is generated Probable cause Suggested actions 1 Irregular or sticking drive movement Remove the pump head and examine the seals pistons and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Please contact your Agilent service representative 201 10 Error Information 202 Index Limit Error ID 2203 2213 The time required by the piston to reach the encoder index position was too short pump During initialization the first p
10. index adjustment 201 index limit 202 index missing 202 initialization failed 203 214 initialization with vial 214 invalid vial position 215 amp ignition failed 229 eak sensor open 197 eak sensor short 198 eak 197 ost CAN partner 200 MCGV fuse 211 metering home failed 215 missing pressure reading 203 missing vial 216 missing wash vial 216 motor failed 217 motor drive power 204 needle down failed 218 needle up failed 219 no run data available in device 234 pressure above upper limit 205 pressure below lower limit 205 pressure signal missing 206 pump configuration 206 pump head missing 207 remote timeout 198 safety flap missing 219 servo restart failed 208 shutdown 199 solvent zero counter 212 stroke length 209 temperature limit exceeded 209 temperature out of range 210 timeout 200 uv heater current 232 uv ignition failed 231 uv lamp current 224 uv lamp voltage 224 valve failed 210 valve to bypass failed 220 1220 Infinity LC valve to mainpass failed 220 vial in gripper 221 visible lamp current 230 visible lamp voltage 230 wait timeout 212 wavelength calibration failed 232 wavelength check failed 229 wavelength recalibration lost 233 exchange degasser 148 exchanging dual channel gradient valve DCGV 260 injection seal 264 passive inlet valve 246 purge valve frit 250 purge valve 250 export data 166 F fan failed 196 features GLP 25 safety and maintenace 25 filter motor 163
11. 2 Select G4281B pump module 3 Expand the pump function by clicking the small right arrow 4 In special commands you will find the tool 1220 Infinity LC Test Functions and Calibration 9 Autosampler Maintenance Positions Change Needle The Change Needle function moves the safety flap out of position and positions the needle for easy exchange and alignment Start moves the safety flap away from the needle and positions the needle approximately 15 mm above the needle seat Up moves the needle arm up stepwise Down moves the needle arm down stepwise The lowest position is used to align the needle at the correct position in the needle arm End repositions the safety flap around the needle Change Piston The Change Piston function draws the piston away from the home position relieving the tension on the spring In this position the analytical head assembly can be removed and reinstalled easily after maintenance Start draws the piston away from the home position relieving the tension on the spring End repositions the piston at the home position 1220 Infinity LC 149 9 Test Functions and Calibration Change Gripper The Change Gripper function moves the gripper to the front of the autosampler enabling easy access to the gripper release mechanism Start moves the gripper to the front of the sample tray area End repositions the gripper at the home position Arm Position Move Arm Home Moves the gripp
12. 7 Z i 4 Ter from wavelength 1 360 8 nm Leal am 0 P from wavelength 2 418 5 nm Tead nm 0 P from wavelength 3 536 4 nm Essl Bm 0 P 159 9 Test Functions and Calibration Evaluating the VWD Holmium Oxide Test The test is evaluated by the instrument and the measured maxima are displayed automatically The test fails if one or more of the maxima lies outside the limits Table 38 Limits Absorbance Maxima Limits 360 8 nm 1to 1 nm 418 5 nm 1to 1 nm 536 4 nm 1 to 1 nm Intensity Test VWD Intensity Test Description The Intensity Test measures the intensity of the UV lamp over the full VWD wavelength range 190 800 nm The test evaluates the results automatically and provides an intensity spectrum The test evaluates the highest intensity average intensity and lowest intensity across the full wavelength range The test is used to determine the performance of the lamp and optics see also VWD Cell Test Description on page 157 To eliminate effects due to absorbing solvents the test should be done with water in the flow cell The shape of the intensity spectrum is primarily dependent on the lamp and grating Therefore intensity spectra will differ slightly between instruments On completion of the test the intensity spectrum and intensity values are displayed The test should not be performed using the micro flow cell since the reduction in light intensity will cause the
13. An example of the reduction of baseline drifts is shown in Figure 42 on page 121 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 1pmol each PTH ASN PTH ALA PTH PHE PTH ARG PTH PRO 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 42 Gradient Analysis of PTH Amino Acids 1 pmol each with and without Reference 1220 Infinity LC 121 8 Detector Description Slit Width The detector has a variable slit at the entrance of the spectrograph This is an effective tool to adapt the detector to changing demand of different analytical problems 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 Figure 43 Benzene at 1 4 and 16 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 44 on page 123 122 1220 Infinity LC Detector Description 8 DAD1 A Sig 25
14. The Tables tab allows you to display the contents of all available diagnostic tables for the module You click the sign to open a table or the sign to close an open table Signals The Signals tab shows the plots of the available diagnostic signals from the module The signal plots that are available are module dependent where available both short term and long term plots are displayed for a signal State Info The State Info tool displays the current status of all Agilent 1220 Infinity LC modules the status is continuously updated Unless aborted the tool runs continuously for 60 min Click Stop Test to stop the tool 1220 Infinity LC Test Functions and Calibration 9 Solvent Delivery System Pump Leak Test Description 1220 Infinity LC The leak test is a built in troubleshooting test designed to verify the tightness of pump components The test should be used when problems with the pump are suspected The test involves monitoring the pressure increase at very low flow rates while different plungers are delivering solvent At these very low flow rates very small leaks can be detected by evaluating the pressure profile as the pump runs through a predefined pumping sequence The test requires blocking the pump with a blank nut then running the test with isopropanol IPA while monitoring the pressure profile Make absolutely sure that all parts of the flow path that are included in the test are very thoroughly flus
15. 10 00 0 02 mm 10 10 Nano flow cell kit 6 mm 80 nL 5 MPa G1315 68716 6 00 0 02 mm 6 6 Standard flow cell bio inert 10 mm 13 pL 120 bar 12 MPa 9 80 0 07 mm 10 9 8 for MWD DAD includes Capillary Kit Flow Cells BIO p n G5615 68755 G5615 60022 Be aware that there are additional tolerance of gasket thickness and its compression ratio which are considered to be very small in comparison with the machining tolerance 134 1220 Infinity LC 1220 Infinity LC 9 Test Functions and Calibration Agilent 1220 Infinity LC System Installation Check 137 Module Info 138 State Info 138 Solvent Delivery System 137 139 Pump Leak Test Description Running the Leak Test 141 Evaluating the Leak Test Results Pressure Too High Check 145 Pressure Too High Check Evaluation 147 Degasser Exchange 149 Maintenance Positions 150 Alignment Teaching 139 142 146 Purge Pump 148 Autosampler 149 Injector Steps 152 Gripper Verification 154 155 155 Oven Calibration Column Oven Oven Test 156 Variable Wavelength Detector VWD Cell Test 157 Dark Current Test Holmium Oxide Test Intensity Test 160 Filter Grating Motor Test 164 165 157 158 159 163 Detector Calibration Test Chromatogram ES Agilent Technologies 135 9 136 Test Functions and Calibration Spectral Scan 166 Diode Array Detector DAD 167 Self test 167 Filter Test 169 Slit Test 171 Dark Current Test 172 Intensity Te
16. 100 Pack Description Snap Cap clear polypropylene septum clear PTFE red rubber 100 Pack Snap Cap blue polypropylene septum clear PTFE red rubber 100 Pack Snap Cap green polypropylene septum clear PTFE red rubber 100 Pack Snap Cap red polypropylene septum clear PTFE red rubber 100 Pack Description Screw Cap blue polypropylene septum clear PTFE red rubber 100 Pack Screw Cap green polypropylene septum clear PTFE red rubber 100 Pack Screw Cap red polypropylene septum clear PTFE red rubber 100 Pack Screw Cap blue polypropylene septum clear PTFE silicone 100 Pack Screw Cap green polypropylene septum clear PTFE silicone 100 Pack Screw Cap red polypropylene septum clear PTFE silicone 100 Pack 1220 Infinity LC R 1220 Infinity LC e e a 090 ee 7 008 Column Oven Description amp s i amp Column Oven 110 This chapter provides an overview of the operational principles of the column oven Agilent Technologies 109 7 Column Oven Description Column Oven The column oven is based on a resistor heater matt with two thermal sensors to provide constant temperature in the whole column area A built in over temperature cut off fuse inhibits overheating The inner volume of the oven capillary is 6 uL Maximum column length is 25 cm 10 inch Operational range is 5 above ambient at least 10 C up to 60 C max specified flow rate is 5 mL min at 60 C
17. Bootp amp Store 57 Bootp 56 cable 359 initialization mode selection 56 link configuration selection 63 manual configuration with telnet 76 manual configuration 75 storing the settings permanently 74 TCP IP parameter configuration 54 375 Index using default 58 using stored 58 leak sensor open 197 leak sensor short 198 leak test 139 leakage current 158 leak correcting 314 ine frequency 19 ine voltage 19 inearrange 26 inearity 24 25 ink configuration selection 63 iquimeter 12 LMD 20 LOAD 94 95 ost CAN partner 200 M MAC address determine 69 mainpass 99 maintenance functions 268 step commands 150 maintenance exchanging lamps 286 overview 295 replacing firmware 318 318 using the cuvette holder 292 make before break 94 manual configuration of LAN 75 manual control 150 materials in contact with mobile phase 86 87 MCGV fuse 211 message ADC hardware error 225 calibration failed 225 376 calibration lost 229 diode current leakage 231 filter check failed 226 filter missing 226 grating missing 227 grating filter motor defective 227 heater current missing 228 heater failed 222 heater power at limit 222 holmium oxide test failed 228 233 illegal temperature value from sensor at air inlet 223 illegal value from sensor on main board 223 lamp ignition failed 229 no run data available in device 234 remote timeout 198 uv heater current 232 uv ignition failed 231 uv lamp current 22
18. Never operate the column oven with open front cover to ensure a correct column temperature always operate with closed front cover The counterpart of the oven isolation is fixed at the inner side of the front cover 110 1220 Infinity LC 1220 Infinity LC Detector Description Detector Types 112 Agilent 1220 Infinity LC Variable Wavelength Detector VWD 113 Detector 113 Agilent 1220 Infinity LC Diode Array Detector DAD 114 Introduction to the Detector 114 Optical System 115 Peak width response time 117 Sample and Reference Wavelength and Bandwidth 119 Slit Width 122 Optimizing Spectral Acquisition DAD only 124 Margin for Negative Absorbance 124 Optimizing Selectivity 125 Spectrum Settings DAD only 128 Match the Flow Cell to the Column 130 This chapter provides an overview of the operational principles of the detector ate Agilent Technologies 111 8 Detector Description Detector Types There are two different detector types available for the Agilent 1220 Infinity LC System e Variable Wavelength Detector VWD used in G4286B G4288B C G4290B C optical unit of the G1314F VWD e Diode Array Detector DAD used in G4294B optical unit of the G1315C DAD 112 1220 Infinity LC Detector Description 8 Agilent 1220 Infinity LC Variable Wavelength Detector VWD Detector The Agilent 1220 Infinity LC variable wavelength detector is designed for highest optical performance GLP compliance and easy
19. No valve adjustments are required after replacing internal components Table 21 Injection valve technical data Standard Motor type 4V 1 2 A stepper motor Seal material Vespel Tefzel available Number of ports 6 Switching time lt 150 ms 1220 Infinity LC 103 6 Injection System Description Autosampler Transport Assembly The transport unit comprises an X axis slide left right motion a Z axis arm up down motion and a gripper assembly rotation and vial gripping X motor Theta motor Gripper motor Gripper X axis Theta axis Z motor Flex board Figure 37 Transport Assembly The transport assembly uses four stepper motors driven in closed loop mode for accurate positioning of the gripper assembly for sample vial transport The rotational movement of the motors is converted to linear motion X and Z axes by toothed belts connected to the drive spindles The rotation theta axes of the gripper assembly is transferred from the motor by a toothed belt and series of gears The opening and closing of the gripper fingers are driven by a stepper motor linked by a toothed belt to the planetary gearing inside the gripper assembly 104 1220 Infinity LC Injection System Description 6 The stepper motor positions are determined by the optical encoders mounted onto the stepper motor housing The encoders monitor the position of the motors continually and correct for position errors automatically
20. 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 starts 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 12 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 57 4 58 LAN Configuration 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 13 Using Stored Principle Using Default
21. filter test 169 filter grating test 163 firmware 138 updates 318 318 upgade downgrade 318 upgrade downgrade 318 flow cell correction factors 132 specifications 26 standard parts 340 support windows 115 test 181 types and data 24 flow path blockage 145 flow precision 21 21 22 22 flowrange 21 22 1220 Infinity LC flow unstable 316 frequency range 19 G general error messages 195 gradient formation 21 22 gradient valve DCGV 260 grating motor 163 grating 116 116 gripper arm repair 283 gripper fingers 104 gripper verification 154 gripper change 150 half trays 105 holmium oxide declaration of conformity 371 filter 115 test 177 humidity 19 hydraulic path 82 hydraulic system 21 22 increased system pressure 317 index adjustment 201 index limit 202 index missing 202 information 138 on cuvette holder 292 onsolvents 365 on UV radiation 368 initialization failed 203 initialization mode selection 56 Index initialization pump 86 injecting sample 94 INJECT 94 96 injection seal 264 tefzel 95 vespel 95 injection sequence 99 injection valve 97 101 103 inlet valve 246 installation check 137 installation delivery checklist 30 site requirements 16 oO installing the autosampler sample trays 105 intensity test 160 174 Internet 372 introduction optical unit parts 115 L Lab Advisor 239 lamp intensity 160 lamp type 24 lamps 115 LAN automatic configuration with Bootp 64
22. for example ageing of the column To minimize this effect the pump provides a compressibility compensation feature that optimizes the flow stability according to the solvent type The compressibility compensation is set to a default value and can be changed through the user interface Without compressibility compensation the following happens during a stroke of the first plunger the pressure in the plunger chamber increases and the volume in the chamber is compressed depending on backpressure and solvent type The volume displaced into the system is reduced by the compressed volume When a compressibility value is set the processor calculates a compensation volume that is depending on the backpressure in the system and the selected compressibility This compensation volume is added to the normal stroke volume and compensates for the previously described loss of volume during the delivery stroke of the first plunger Optimizing the compressibility compensation setting The default compressibility compensation setting is 46 10 bar This setting represents an average value Under normal conditions the default setting reduces the pressure pulsation to values below 1 of system pressure that are sufficient for most applications and for all gradient analyses For applications using sensitive detectors the compressibility settings can be optimized by using the values for the various solvents If the solvent in use is not listed in the
23. old new 1220 Infinity LC 323 12 Parts for Maintenance Pump Head Assembly With Seal Wash Option Item p n G1312 60045 1 5063 6586 2 G1311 60002 3 01018 60027 4 0905 1175 OR 0905 1718 5065 9978 5 5062 2484 6 5042 8952 7 5063 6589 0905 1420 8 G1311 25200 9 G1312 60066 10 G1312 60067 11 5042 1303 12 G4280 60061 13 0515 2118 01018 23702 Description Pump head assembly with seal wash Sapphire piston Piston housing Support ring seal wash Wash seal PTFE Wash Seal PE Tubing 1 mm i d 3 mm o d silicone 5 m Gasket seal wash pack of 6 Seal holder Piston seal PTFE carbon filled black pack of 2 default PE seals pack of 2 Pump chamber housing Passive inlet valve 1220 1260 Outlet valve 1220 1260 Lock screw Purge valve Pump head screw M5 60 mm Insert tool The Pump head assembly with seal wash G1312 60045 includes items 1 8 11 and 13 Active seal wash is not supported for the 1220 Infinity LC only continuous seal wash 324 1220 Infinity LC Parts for Maintenance 12 Solvent Delivery System Figure 73 Pump Head with Seal Wash Option NOTE The design of the seal wash gasket has changed see below old new 1220 Infinity LC 325 12 Parts for Maintenance Outlet Ball Valve Assembly p n Description G1312 60067 Outlet valve 1220 1260 326 1220 Infinity LC Purge Valve Assembly Item p n G4280 60061 2 01018 22707 3 5067 4728 Parts for Mainten
24. p n Description 0101 1422 Injection valve 0100 1852 Isolation seal 1 0101 1416 Rotor seal PEEK 2 0101 1417 Stator head 3 1535 4857 Stator screws 338 1220 Infinity LC Parts for Maintenance 12 Column Oven p n Description G4280 60040 Complete column oven assembly G4280 60017 Heater door assembly 1220 Infinity LC 339 12 Parts for Maintenance Detector Variable Wavelength Detector VWD Standard Flow Cell 10 mm 14 pL Item p n G1314 60086 5062 8522 G1314 65061 1 G1314 65062 2 79853 29100 3 G1314 65066 4 G1314 65064 5 79853 68742 6 G1314 65063 7 G1314 65065 340 Description Standard flow cell 10 mm 14 uL 40 bar Capillary column detector PEEK 600 mm lg 0 17 mm i d 1 16 inch o d Cell Repair Kit includes 2x Gasket 1 2x Gasket 2 2x Window Quartz Cell screw kit Conical spring kit 10 pk Ring 2 kit IN small hole i d 1 mm PEEK 2 pk Gaskets 2 IN small hole i d 1 mm KAPTON 10 pk Window quartz kit 2 pk Gasket 1 kit OUT large hole i d 2 4 mm KAPTON 2 pk Ring 1 kit OUT large hole i d 2 4 mm PEEK 2 pk 1220 Infinity LC Parts for Maintenance 12 Detector 1 Cell screw 2 Conical springs 3 Ring 2 IN 4 Gasket 2 IN 5 Quartz window 6 Gasket 1 OUT 7 Ring 1 OUT Figure 74 Standard Flow Cell 10 mm 14 pL 1220 Infinity LC 341 12 Parts for Maintenance Detector Lamp p n Description G1314 60100 Deuterium lamp 342 1220 I
25. p n Description G1530 60600 RS 232 cable 2 m RS232 61601 RS 232 cable 2 5 m 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 8 m 360 1220 Infinity LC This chapter provides addition information on safety legal and web 1220 Infinity LC 15 Appendix General Safety Information 362 Solvent Information 365 Radio Interference 367 UV Radiation 368 Sound Emission 369 Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 370 Declaration of Conformity for HOX2 Filter 371 Agilent Technologies on Internet 372 Apg Agilent Technologies 361 15 Appendix General Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised
26. representative 4 Cable connector defective Please contact your Agilent service representative Grating Missing 1220 Infinity LC Error ID 7819 The grating motor is not detected Probable cause Suggested actions 1 Grating motor is not connected Please contact your Agilent service representative 2 Cable connector defective Please contact your Agilent service representative 227 10 Error Information 228 No heater current Error ID 7453 The lamp heater current in the detector is missing During lamp ignition the processor monitors the heater current If the current does not rise above the lower limit within 1 the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the lamp is connected 2 Ignition started without the top foam Please contact your Agilent service representative in place 3 Fan not running permitting lamp on Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 5 Defective or non Agilent lamp Exchange the lamp 6 Defective power supply Please contact your Agilent service representative Wavelength holmium check failed Error ID 7318 The holmium oxide test in the detector has failed During the holmium test the detector moves the holmium filter into the light path and compares the measured absorbance maxima of the holmium oxide filter with expected maxima If the measu
27. sits flat on the valve body 7 Install stator head Tighten the bolts alternately two turns at a time until the stator head is secure 1220 Infinity LC 277 11 Maintenance Next Steps 9 Slide the waste tube into the waste holder in the leak tray 10 On completion of this procedure Install the front cover 278 1220 Infinity LC Maintenance 11 Exchanging the Metering Seal When Poor injection volume reproducibility Leaking metering device Tools required p n Description Wrench 1 4 inch supplied in HPLC Tool Kit Hexagonal key 4 mm supplied in HPLC Tool Kit 8710 2411 Hexagonal key 3 mm supplied in HPLC Tool Kit Parts required p n Description 1 5063 6589 Metering seal pack of 2 for 100 uL analytical head 1 5063 6586 Sapphire piston Preparations Select Start in the Tools function in the LMD software Change piston Remove the upper front cover 1 Remove the two capillaries from the metering head 2 Remove the two fixing bolts and pull the head assembly assembly away from the sampler Notice that the closed side of the metering head faces upwards A i TOOT 5 wW lt E 1220 Infinity LC 279 11 Maintenance 3 Remove the two fixing bolts from the base of the metering head assembly 4 Disassemble the metering head assembly 5 Use a small screwdriver to carefully remov
28. 112 303 306 2007 the holmium oxide glass filters are inherently stable with respect to the wavelength scale and need no recertification The expanded uncertainty of the certified wavelength values is 0 2 nm Agilent Technologies guarantees as required by NIST that the material of the filters is holmium oxide glass representing the inherently existent holmium oxide absorption bands Test wavelengths Where x can be any alphanumeric character Wavelength Accuracy Bandwidth G1315x G1365x 1100 1200 1260 1 nm 6nm G7115x G7165x 1260 G1600x G7100x CE G1314x 1100 1200 1260 1290 360 8um 418 5nm G7114x 1260 1290 36 4nm G4286x 94x 1120 1220 The variation in Measured Wavelength depends on the different Optical Bandwidth 28 Oct 2014 Sn Bogarta R amp D Manager Quality Manager P N 89550 90501 Revision G KX MTNA TON UME Effective by 28 Oct 2014 371 15 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 372 1220 Infinity LC Index GLP features 20 A absorbance Beer Lambert 131 achromat sourcelens 115 adapter 246 Agilent Technologies 372 algae growth 92 algea information 365 alignment teaching 152 alignment gripper 154 alpha and beta line 185 ambient non operating temperature 19 ambient o
29. 1535 4045 5068 0082 0101 1417 5067 1581 5068 0018 8710 0060 Description Manual injection valve 600 bar complete including loop and needle port Isolation seal Rotor seal PEEK Stator head Needle port Stator screws Hex key wrench 9 64 inch 331 12 Parts for Maintenance 332 Sample Loops Sample loops stainless steel p n Description 0101 1248 Sample loop 5 pL 0100 1923 Sample loop 10 pL 0100 1922 Sample loop 20 pL 0100 1924 Sample loop 50 pL 0100 1921 Sample loop 100 pL 0101 1247 Sample loop 200 pL 0101 1246 Sample loop 500 pL 0101 1245 Sample loop 1 mL 0101 1244 Sample loop 2 mL Sample loops PEEK p n Description 0101 1241 Sample loop 5 pL 0101 1240 Sample loop 10 pL 0101 1239 Sample loop 20 pL 0101 1238 Sample loop 50 pL 0101 1242 Sample loop 100 pL 0101 1227 Sample loop 200 pL 0101 1236 Sample loop 500 pL 0101 1235 Sample loop 1 mL 0101 1234 Sample loop 2 mL 1220 Infinity LC Autosampler 1220 Infinity LC Parts for Maintenance Autosampler Main Assemblies p n G4280 60230 G1329 60009 G4280 60027 01078 60003 0101 1422 G1313 44510 G1313 60010 G4280 87304 G4280 81615 G4280 81616 5067 1581 Description Autosampler complete Transport assembly Sampling unit assembly excluding injection valve and analytical head Analytical head assembly 100 pL Injection valve Vial tray Gripper assembly Waste capillary Cable sampling unit Cable sample transport Needle port 12
30. 2 mL clear glass write on spot 1000 Pack Snap Top Vial 2 mL clear glass write on spot 100 Pack silanized Snap Top Vial 2 mL amber glass write on spot 100 Pack Snap Top Vial 2 mL amber glass write on spot 1000 Pack Snap Top Vial 2 mL amber glass write on spot 100 Pack silanized Description Screw Cap Vials 2 mL clear glass 100 Pack Screw Top Vial 2 mL clear glass 1000 Pack Screw Top Vial 2 mL clear glass 100 Pack silanized Screw Top Vial 2 mL clear glass write on spot 100 Pack Screw Top Vial 2 mL clear glass write on spot 1000 Pack Screw Top Vial 2 mL clear glass write on spot 100 Pack silanized Screw Cap Vial 2 mL amber glass write on spot 100 pk Screw Top Vial 2 mL amber glass write on spot 1000 Pack Screw Top Vial 2 mL amber glass write on spot 100 Pack silanized 107 6 Injection System Description Crimp caps p n 5181 1210 5183 4498 5181 1215 5181 1216 5181 1217 Snap caps p n 5182 0550 5182 3458 5182 3457 5182 3459 Screw caps p n 5182 0717 5182 0718 5182 0719 5182 0720 5182 0721 5182 0722 108 Description Crimp Cap silver aluminum septum clear PTFE red rubber 100 Pack Crimp Cap silver aluminum septum clear PTFE red rubber 1000 Pack Crimp Cap blue aluminum septum clear PTFE red rubber 100 Pack Crimp Cap green aluminum septum clear PTFE red rubber 100 Pack Crimp Cap red aluminum septum clear PTFE red rubber
31. 200 bar 0 2950 psi up to 10 mL min lt 2 amplitude typically lt 1 at 1 mL min isopropanol at all pressures gt 1 MPa 10 bar User selectable based on mobile phase compressibility 1 0 12 5 solvents with pH lt 2 3 should not contain acids which attack stainless steel Low pressure dual mixing gradient capability using proprietary high speed proportioning valve Delay volume 800 1100 uL dependent on back pressure 0 95 or 5 100 user selectable lt 0 2 RSD at 0 2 and 1 mL min 1220 Infinity LC Site Requirements and Specifications 2 Performance Specifications Agilent 1220 Infinity LC Autosampler Table5 Performance Specifications Agilent 1220 Infinity LC Autosampler Type Specification Pressure Operating range 0 60 MPa 0 600 bar 0 8820 psi Injection range 0 1 100 uL in 0 1 pL increments Up to 1500 uL with multiple draw hardware modification required Replicate injections 1 99 from one vial Precision lt 0 25 RSD from 5 100 pL lt 1 RSD 1 5 pL variable volume Minimum sample volume 1 pL from 5 pL sample in 100 uL microvial or 1 pL from 10 pL sample in 300 uL microvial Carryover Typically lt 0 1 lt 0 05 with external needle cleaning Sample viscosity range 0 2 50 cp Sample capacity 100 x 2 mL vials in 1 tray 40 x 2 mL vials in tray 15 x 6 mL vials in tray Agilent vials only Injection cycle time Typically 50 s depending on dra
32. 3 6 Place the Solvent Inlet Filter end of the Bottle Head Assembly in the Solvent Bottle see picture below 3N 1 Ferrules with lock ring W 2 Tube screw 4 2 3 Wire marker E i1 4 Solvent tubing 5 m Ty 5 Frit adapter pack of 4 P 6 Sovent inlet fi eS Iter 20 um 15 i 6 Figure 4 Bottle Head Assembly and Solvent Bottle 7 Prime the tubing using the Syringe 9301 044 and Syringe adapter 9301 1337 part of the Accessory kit until the tubing is completely filled with water 8 Connect the Bottle Head Assembly connector see Figure 4 on page 39 Item 1 2 to the passive inlet valve isocratic pump or the degasser inlet Channel A gradient pump 9 Connect the waste tube with the fitting attached part of Accessory Kit to the flow cell outlet and the other end to an appropriate solvent waste container see Figure 5 on page 39 Flow cell inlet f 7 A Flow cell outlet Ze re Power push button Leak tray outlet Figure 5 Connections at the VWD Module 1220 Infinity LC 39 3 40 Installation 10 Attach the corrugated waste tube part of Accessory Kit to the VWD leak tray outlet adapter and guide it to a proper waste container see Figure 5 on page 39 11 Connect the waste tube part of Accessory Kit to the purge valve outlet adapter and the other end to the waste container 12 Connect the network connection between the Agilent 1220 Infinity LC and your PC More details a
33. 333 12 Parts for Maintenance 334 Analytical Head Assembly Item p n 01078 60003 5063 6586 0515 0850 01078 23202 5001 3739 5063 6589 01078 27710 0515 2118 Description Analytical head assembly 100 pL Sapphire piston Screw M4 40 mm long Adapter Support Seal assembly Metering seal pack of 2 for 100 uL analytical head Head body Screw M5 60 mm long for mounting assembly 1220 Infinity LC Parts for Maintenance 12 Injection System 1220 Infinity LC 335 12 Parts for Maintenance Sampling Unit Assembly Item 11 12 13 14 15 336 p n G4280 60027 G1313 66503 1500 0697 5062 8590 01078 87302 01078 60003 61313 87301 G1329 44115 0101 1422 61313 87300 G1313 87101 61313 43204 G1313 44106 G1313 68715 61313 87201 61313 68713 Description Sampling unit assembly excluding injection valve and analytical head SUD board Belt gear for metering unit and needle arm Stepper motor for metering unit and needle arm Loop capillary 100 pL Analytical head assembly 100 pL Capillary injection valve to analytical head 160 mm x 0 25 mm Safety cover Injection valve Waste tube injection valve assy 120 mm Needle seat assy 0 17 mm i d 2 3 uL Seat adapter Safety flap Flex board Needle assembly Clamp Kit includes needle clamp and 2 x clamp screw 1220 Infinity LC 1220 Infinity LC 337 12 Parts for Maintenance Injection System Injection Valve Assembly Item
34. 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 1220 Infinity LC LAN Configuration 4 3 Press Edit BootP Addresses to edit the Tab File Edit BootP Addresses 006000111893 Agrit 101 110 Agiert LEI night 255 255 2550 00 00 005000222803 Agler iC2 101 1 1 102 Agwat LCb 25525250 0000 Figure 21 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 20 on page 72 2 Right click Agilent BootP Service and select Start 3 Close the Services and Administrative Tools screens 1220 Infinity LC 73 4 LAN Configuration Storing the settings permanently with Bootp 74 If you want to change parameters of the module using the Bootp follow the instructions below 1 2 Turn off the module Change the module s settings
35. Default switches 7 and 8 set to ON Link Configuration Speed and duplex mode determined by auto negotiation For the G4294B the Configuration switches on the DAD main board must be used for configuring the LAN access of the instrument The switches on the 1220 Infinity LC main board must all be set to off 55 4 LAN Configuration Initialization mode selection The following initialization init modes are selectable Table 11 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 ON OFF OFF DHCP 1 Requires firmware B 06 40 or above Modules without LAN on board see G1369C LAN Interface Card 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 Server Figure 11 Bootp Principle 56 1220 Infinity LC 1220 Infinity LC LAN Configuration 4 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
36. Defective detector main board 5 Defective power supply Calibration Values Invalid Error ID 1036 Suggested actions Ensure the UV lamp is connected Please contact your Agilent service representative Exchange the 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 1220 Infinity LC Holmium Oxide Test Failed Wavelength Recalibration Lost 1220 Infinity LC Probable cause 1 Lamps switched off 2 Defective or dirty flow cell 3 Defective filter assembly 4 Defective achromat assembly 5 Defective PDA optical unit Error ID 1037 Error Information 10 Suggested actions Ensure the lamps are switched on Ensure the flow cell is inserted correctly and is free from contamination cell windows buffers etc Please contact your Agilent service representative Please contact your Agilent service representative Please co
37. Diode array Figure 38 Optical System of the Detector Lamps The light source for the UV wavelength range is a deuterium lamp with a shine through aperture As a result of plasma discharge in low pressure deuterium gas the lamp emits light over the 190 nm to approximately 800 nm wavelength range The light source for the visible and SWNIR wavelength range is a low noise tungsten lamp This lamp emits light over the wavelength range 470 950 nm 1220 Infinity LC 115 Detector Description Achromat Source Lens Holmium Oxide Filter Cell Support Window Flow Cell Compartment Spectrograph Variable Entrance 116 Slit System Grating Diode Array The achromat receives the light from both lamps and focuses it so that the beam passes through the flow cell The holmium oxide filter is electromechanically actuated During the holmium filter test it moves into the light path The cell support window assembly separates the holmium filter area from the flow cell area The optical unit has a flow cell compartment for easy access to flow cells A variety of optional flow cells can be inserted using the same quick simple mounting system The flow cell can be removed to check the optical and electronic performance of the detector without having influences from the flow cell The spectrograph material is ceramic to reduce thermal effects to a minimum The spectrograph consists of the spectrograph lens the variable en
38. Infinity LC 63 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 11 on page 56 Assure that the detector connected to the network is powered off 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 64 1220 Infinity LC 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
39. Missing 219 Valve to Bypass Failed 220 Valve to Mainpass Failed 220 Vial in Gripper 221 General Detector Error Messages 222 Heater at fan assembly failed 222 Heater Power At Limit 222 Illegal Temperature Value from Sensor on Main Board 223 Illegal Temperature Value from Sensor at Air Inlet 223 UV Lamp Current 224 UV Lamp Voltage 224 VWD Detector Error Messages 225 ADC Hardware Error 225 Wavelength calibration setting failed 225 Cutoff filter doesn t decrease the light intensity at 250nm 226 Filter Missing 226 Grating or Filter Motor Errors 227 Grating Missing 227 1220 Infinity LC 1220 Infinity LC Error Information 10 No heater current 228 Wavelength holmium check failed 228 Ignition Failed 229 Wavelength test failed 229 DAD Detector Error Messages 230 Visible Lamp Current 230 Visible Lamp Voltage 230 Diode Current Leakage 231 UV Ignition Failed 231 UV Heater Current 232 Calibration Values Invalid 232 Holmium Oxide Test Failed 233 Wavelength Recalibration Lost 233 DSP Not Running 234 No Run Data Available In Device 234 Instrument Logbook 235 This chapter provides information on the error messages that might be displayed and gives the possible causes and suggestions on their solutions 193 10 Error Information What are Error Messages 194 Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention
40. Select the Agilent BootP Service and click Start 1220 Infinity LC 67 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 Service gt EditBootPSettings 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 OS nd DS PE Figure 18 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 72 or Restarting the Agilent BootP Service on page 73 Uncheck the Do you want to log BootP requests box after configuring instruments otherwise the log file will quickly fill up disk space Determining the MAC address directly from the LAN Interface card label 68 Turn off the instrument Read the MAC address from the label and record it The MAC address
41. Sensor Open 1220 Infinity LC Error ID 0083 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 197 10 Error Information 198 Leak Sensor Short Error ID 0082 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 limits If the current increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective leak sensor Please contact your Agilent service representative 2 Leak sensor incorrectly routed being Please contact your Agilent service pinched by a metal component representative Remote Timeout Error ID 0070 A not ready condition is still present on the remote input When an analysis is started the sy
42. 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 12 on page 58 Default Active Parameter Parameter Figure 14 Using Default Principle Using the default address in your local area network may result in network problems Take care and change it to a valid address immediately Table 12 Using Default Parameters IP address 192 168 254 11 Subnet Mask 255 255 255 0 Default Gateway not specified 1220 Infinity LC 1220 Infinity LC LAN Configuration 4 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
43. actions Please contact your Agilent service representative Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Fan Failed Error ID 0068 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 Depending on the module assemblies e g the lamp in the detector are turned off to assure that the module does not overheat inside 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 1220 Infinity LC Leak Error Information 10 Error ID 0064 A leak was detected in the module The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the main board Probable cause Suggested actions 1 Loose fittings Ensure all fittings are tight 2 Broken capillary Exchange defective capillaries Leak
44. assembly 1 into the cell body Do not mix the gasket 6 and 7 different hole diameter 304 1220 Infinity LC Maintenance 11 Next Steps Using a 4 mm hex key tighten the window screw hand tight plus a quarter turn Reconnect the capillaries see Exchanging a Flow Cell on page 300 Perform a leak test Insert the flow cell Replace the front cover on own FS Q Perform a Wavelength Verification and Recalibration on page 185 or a Holmium Oxide Test on page 177 to check the correct positioning of the flow cell 1220 Infinity LC 305 11 Maintenance Replacing Capillaries on a Standard Flow Cell When If the capillary is blocked Tools required Description Wrench 1 4 inch for capillary connections Wrench 4mm for capillary connections Screwdriver Pozidriv 1 PT3 Parts required Description For parts see Standard Flow Cell on page 344 Preparations Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 300 All descriptions in this procedure are based on the default orientation of the cell as it is manufactured The heat exchanger capillary and the cell body can be fixed mirror symmetrically to have both capillaries routed to the bottom or to the top depending on the routing of the capillaries to the column The fittings at the flow cell body are special types for low dead volumes and not compatible
45. back to the mode Using Stored 59 4 LAN Configuration Dynamic Host Configuration Protocol DHCP 60 General Information DHCP The Dynamic Host Configuration Protocol DHCP is an auto configuration protocol used on IP networks The DHCP functionality is available on all Agilent HPLC modules with on board LAN Interface or LAN Interface Card and B firmware B 06 40 or above When the initialization mode DHCP is selected the card tries to download the parameters from a DHCP Server The parameters obtained become the active parameters immediately They are not stored to the non volatile memory of the card Besides requesting the network parameters the card also submits its hostname to the DHCP Server The hostname equals the MAC address of the card e g 0030d3177321 It is the DHCP server s responsibility to forward the hostname address information to the Domain Name Server The card does not offer any services for hostname resolution e g NetBIOS DHCP Active Server Parameter Figure 15 DHCP Principle 1 It may take some time until the DHCP server has updated the DNS server with the hostname information 2 It may be necessary to fully qualify the hostname with the DNS suffix e g 0030d3177321 country company com 3 The DHCP server may reject the hostname proposed by the card and assign a name following local naming conventions 1220 Infinity LC Setup DHCP Software required LAN Configu
46. cause 1 Lower pressure limit set too high 2 Leak 3 Defective main board Suggested actions Ensure the lower pressure limit is set to a value suitable for the analysis Inspect the pump head capillaries and fittings for signs of a leak Purge the module Run a pressure test to determine whether the seals or other module components are defective Please contact your Agilent service representative 205 10 Error Information Pressure Signal Missing Error ID 2016 The pressure signal of the damper is missing The pressure signal of the damper must be within a specific voltage range If the pressure signal is missing the processor detects a voltage of approximately 120 mV across the damper connector Probable cause Suggested actions 1 Damper disconnected Please contact your Agilent service representative 2 Defective damper Please contact your Agilent service representative Pump Configuration Error ID 2060 At switch on the gradient pump has recognized a new pump configuration The gradient pump is assigned its configuration at the factory If the gradient valve is disconnected and the gradient pump is rebooted the error message is generated However the pump will function as an isocratic pump in this configuration The error message reappears after each switch on Probable cause Suggested actions 1 Gradient valve disconnected Reconnect the gradient valve 206 1220 Infinity LC Erro
47. digital bandwidth is computed as average of absorbance there is no impact on linearity Use a wide 8 or 16 nm slit when your sample contains very small concentrations Always use signals with bandwidth at least as wide as the slit width 1220 Infinity LC 123 124 Detector Description Optimizing Spectral Acquisition DAD only Storage of all spectra consumes a lot of disk space It is very useful to have all spectra available during optimization of a method or when analyzing unique samples However when running many samples of the same type the large size of data files with all spectra may become a burden The detector provides functions to reduce the amount of data yet retaining the relevant spectral information For spectra options see Table 23 on page 129 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
48. holmium oxide filter The holmium oxide filter can be cleaned with alcohol and a lint free cloth 4 While releasing the holder with a screw driver carefully insert the holmium oxide filter 312 1220 Infinity LC Maintenance 11 5 Replace the flow cell cover and fix the six screws 4 W Ad 8 a e gt Next Steps Perform a holmium oxide test see Holmium Oxide f Test on page 177 to check the proper function of the holmium oxide filter 7 Insert the flow cell see Exchanging a Flow Cell on page 300 8 Replace the front cover Turn on the flow 1220 Infinity LC 313 11 Maintenance Correcting Leaks When If a leakage has occurred in the flow cell area or at the heat exchanger or at the capillary connections Tools required Description Tissue Wrench 1 4 inch for capillary connections Preparations Remove the front cover 1 Use tissue to dry the leak sensor area and the leak pan 2 Observe the capillary connections and the flow cell area for leaks and correct if required Leak pan Leak tubing Figure 70 Observing for Leaks 3 Replace the front cover 314 1220 Infinity LC Maintenance 11 Replacing Leak Handling System Parts When If the parts are corroded or broken Tools required None Parts required p n Description 1 5041 8388 Leak funnel 1 5041 8389 Leak funnel holder 1 5062 2463 Corrugated tubi
49. 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 9 on page 52 and Figure 10 on page 53 Turn on the instrument 1220 Infinity LC LAN Configuration 4 Assigning IP Addresses Using the Agilent BootP Service 1220 Infinity LC The Agilent 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 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
50. is selected Margin for Negative Absorbance The detector adjusts its gain during balance such that the baseline may drift slightly negative about 100 mAU In some special case for example when gradient with absorbing solvents are used the baseline may drift to more negative values Only for such cases increase the margin for negative absorbance to avoid overflow of the analog to digital converter 1220 Infinity LC Detector Description 8 Optimizing Selectivity Quantifying Coeluting Peaks by Peak Suppression In chromatography two compounds may often elute together A conventional dual signal detector can only detect and quantify both compounds independently from each other if their spectra do not overlap However in most cases this is highly unlikely 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 45 on page 125 shows hydrochlorothiazide is best detected at 222 nm where caffeine also shows significant absorbance It would therefore be impossible with a con
51. 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 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 1220 Infinity LC 65 4 66 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 Agi
52. of the Configuration Switch to Bootp amp Store mode see Table 11 on page 56 3 Start the Agilent Bootp Service and open its window 4 If required modify the parameters for the module according to your needs using the existing configuration Press OK to exit the Bootp Manager Now turn on the module and view the Bootp Server window After some time the Agilent Bootp Service will display the request from the LAN interface The parameters are now stored permanently in the non volatile memory of the module 7 Close the Agilent Bootp Service and turn off the module 8 Change the settings of the module s Configuration Switch to Using Stored mode see Table 11 on page 56 Power cycle the module The module can be accessed now via LAN without the Agilent Bootp Service 1220 Infinity LC LAN Configuration 4 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 22 Manual Configuration Principle 1220 Infinity LC 75 4 76 LAN Configuration With Telnet Whenever a TCP IP connection to the
53. of the damper Ensure the capillaries and frits between the pump head and damper inlet are free from blockage 2 Blocked outlet valve Exchange the outlet valve 3 High friction partial mechanical blockage Remove the pump head assembly Ensure there in the pump drive assembly is no mechanical blockage of the pump head assembly or pump drive assembly 4 Defective pump drive assembly Please contact your Agilent service representative 5 Defective main board Please contact your Agilent service representative 204 1220 Infinity LC Pressure Above Upper Limit Pressure Below Lower Limit 1220 Infinity LC Error ID 2014 2500 Error Information 10 The system pressure has exceeded the upper pressure limit Probable cause 1 Upper pressure limit set too low 2 Blockage in the flowpath after the damper 3 Defective damper 4 Defective main board Error ID 2015 2501 Suggested actions Ensure the upper pressure limit is set to a value suitable for the analysis Check for blockage in the flowpath The following components are particularly subject to blockage inline filter frit needle autosampler seat capillary autosampler sample loop autosampler column frits and capillaries with small internal diameters e g 50 um ID Please contact your Agilent service representative Please contact your Agilent service representative The system pressure has fallen below the lower pressure limit Probable
54. 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 pea Violet 2 BCD 7 80 AA Blue 3 BCD 6 40 a ee Yellow 4 BCD 4 10 Black 5 BCD 0 1 Ras 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 357 14 Identifying Cables Agilent Module to 3396 Integrators p n 03396 60560 Pin 3396 Pin Agilent Signal Name BCD Digit module an 1 1 BCD 5 20 2 2 BCD7 80 Se 15 oO Z 3 3 BCD 6 40 oO So 4 4 BCD 4 10 s je 2 5 5 BCDO 1 fie e9 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 358 1220 Infinity LC CAN LAN Cables 1220 Infinity LC Identifying Cables 14 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 359 14 Identifying Cables Agilent 1200 module to PC
55. plunger the second plunger delivers the drawn volume into the system For solvent compositions from the solvent bottles A and B the controller divides the length of the intake stroke into certain fractions in which the gradient valve connects the specified solvent channel to the pump input Table 17 Isocratic pump details Dead volume 800 1100 uL depending on back pressure Materials in contact with mobile phase Pump head SST gold sapphire ceramic Active inlet valve SST gold sapphire ruby ceramic PTFE Outlet valve SST gold sapphire ruby Adapter SST gold Purge valve SST gold PTFE ceramic PEEK Degasser chamber TFE PDD copolymer FEP PEEK PPS 1220 Infinity LC 1220 Infinity LC Solvent Delivery System Description 5 Table 18 Gradient pump details Delay volume 800 1100 uL dependent on back pressure Materials in contact with mobile phase MCGV Pump head Active inlet valve Outlet valve Adapter Purge valve Damping unit Degasser chamber PTFE SST gold sapphire ceramic SST gold sapphire ruby ceramic PTFE SST gold sapphire ruby SST gold SST gold PTFE ceramic PEEK Gold SST TFE PDD copolymer FEP PEEK PPS 87 5 Solvent Delivery System Description Compressibility Compensation 88 Principles of compressibility compensation The compressibility of the solvents in use affects retention time stability when the back pressure in the system changes
56. pump head on a flat surface Loosen the lock screw two revolutions and while holding the lower half of the assembly carefully pull the pump head away from the plunger housing Remove the support rings from the plunger housing and lift the housing away from the plungers I i j Pump head aE AA O ac L A Lock screw f Support rin A gt O ee r k STAS S5 Jo Plunger housing Su Plunger housing Plunger P CD Q 4 a CY 1220 Infinity LC 257 11 Maintenance 3 Check the plunger surface and remove any deposits The plunger surface can be cleaned with either alcohol or tooth paste If the plunger is scratched replace it Piston surface 4 Reassemble the pump head assembly Pump head Support ring Plunger housing 258 1220 Infinity LC Maintenance 11 Reinstalling the Pump Head Assembly When When reassembling the pump Tools required Description Hexagonal key 4 mm 1 Slide the pump head assembly onto the pump drive and use a 4 mm hexagonal key to tighten the pump head screws stepwise with increasing torque max 5 Nm Metering drive Pump head 5 AA ARSS D Pump head screws 2 Reconnect the capillaries and tubing 3 Reinstall the front cover 1220 Infinity LC 259 11 Maintenance Exchanging the Dual Channel Gradient Valve DCGV Tools required Parts required Preparations 260 p n Description 8710 089
57. reference Caffeine suppressed Hydrochlorothiazides uppressed Wavelength 204 nm Wavelength 222 nm Reference 260 nm Reference 282 nm 6 2 8 1 8 1 8 Lee 1 2 6 2 8 Time min Time min Figure 46 Peak Suppression Using Reference Wavelength Ratio Qualifiers for Selective Detection of Compound Classes Ratio qualifiers can be used where in a complex sample only one particular class needs to be analyzed a parent drug and its metabolites in a biological sample for example Another example is the selective analysis of derivatives after pre or 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 47 on page 127 and Figure 48 on page 127 126 1220 Infinity LC Detector Description 8 Select 2 characteristic jags wavelengths Signal WL1 WL2 20 38 8a 78 o Terphenyl 6a sa Biphenyl 40 384 2a Scaled w2 WLI 222 242 262 28a 322 322 Wavelength nm Figure 47 Wavelength Selection for Ratio Qualifiers Signals at 250 nm Biphenyl o Terphenyl No selectivity With ratio qualifie
58. 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 7 9 2009 3 06 30 PM Stop Time 7 9 2009 3 06 53 PM BERRGRRRSRRRR REE Test Procedure 7 1 Check Prerequisites 2 Switch on Analog Output amp 3 Switch off Analog Output Figure62 D A Converter DAC Test Results 1220 Infinity LC Test Functions and Calibration 9 ADC1 A ADC CHANNEL 76 49 76 468 76 555 02 04 os Figure 63 Running the Test with Instant Pilot i 12 1 4 16 18 D A Converter DAC 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 detect
59. the injection valve returns to the mainpass position at the end of the sampling sequence The sampling sequence occurs in the following order 1 The injection valve switches to the bypass position 2 The plunger of the metering device moves to the initialization position 3 The gripper arm selects the vial At the same time the needle lifts out of the seat The gripper arm places the vial below the needle The needle lowers into the vial The metering device draws the defined sample volume The needle lifts out of the vial onion A If the automated needle wash is selected the gripper arm replaces the sample vial positions the wash vial below the needle lowers the needle into the vial then lifts the needle out of the wash vial 9 The gripper arm checks if the safety flap is in position 10 The gripper arm replaces the vial Simultaneously the needle lowers into the seat 11 The injection valve switches to the mainpass position 1220 Infinity LC Injection System Description 6 Autosampler Injection Sequence Before the start of the injection sequence and during an analysis the injection valve is in the mainpass position In this position the mobile phase flows through the autosamplers metering device sample loop and needle ensuring all parts in contact with sample are flushed during the run thus minimizing carry over Figure 33 Mainpass Position When the sample sequence begins the valve unit switche
60. the left and right channels are evaluated The test passes if both slopes are gt 4 C min 1220 Infinity LC 155 9 Test Functions and Calibration Oven Calibration Oven Calibration Description The oven calibration procedure enables the oven temperature to be measured against an external calibrated measuring device Normally temperature calibration is not required during the lifetime of the instrument however in order to comply with local regulatory requirements the 2 point calibration and verification procedure may be performed Running the Oven Calibration For the measurement and calibration procedure we recommend a measuring device that provides the necessary resolution and precision for example Hereaus Quat340 quartz surface temperature measurement sensor Contact your local Agilent Technologies support representative for ordering information Install the calibrated temperature measuring device Select the Oven Calibration in the user interface Wait for the oven to reach the first set point 40 C FP WwW N Measure the temperature of the heat exchanger and enter the value in the field Wait for the oven to reach the second set point 50 C co Measure the temperature of the heat exchanger and enter the value in the field 7 Click OK to save the calibration values to the oven or Cancel to abort the calibration process 156 1220 Infinity LC Test Functions and Calibration 9 Variable Wavele
61. to provide good precision The sample fills the loop and excess sample is expelled through the vent tube connected to port 2 from pump Figure 31 LOAD Position 95 6 Injection System Description INJECT Position In the INJECT position see Figure 32 on page 96 the pump is connected to the sample loop ports 5 and 6 connected All of the sample is washed out of the loop onto the column The needle port is connected to the vent tube port 2 Needle port a os Waste 2 1 from pump to column Sample loop Figure 32 INJECT Position Needles CAUTION Needle can damage valve gt Always use the correct needle size Use needles with 0 028 inch outer diameter 22 gauge x 2 inch long needle without electro taper and with 90 point style square tip 96 1220 Infinity LC Injection System Description 6 Autosampler 1220 Infinity LC Three sample rack sizes are available for the autosampler The standard full size rack holds 100 x 1 8 mL vials while the two half size racks provide space for 40 x 1 8 mL and 15 x 6 mL vials respectively Any two half size rack trays can be installed in the autosampler simultaneously The analytical head device provides injection volumes from 0 1 100 uL The autosamplers transport mechanism uses an X Z Theta movement to optimize vial pick up and return Vials are picked up by the gripper arm and positioned below the sampling unit The gripper transport
62. 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 Operation 362 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 1220 Infinity LC Appendix 15 impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided 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 avoid
63. unclip it Remove the cover 4 Place the new DCGV into position Make sure that the valve is positioned with the A channel at the bottom right position Tighten the two holding screws and connect the cable to its connector Channel A 1220 Infinity LC 261 11 Maintenance Solvent Delivery System 5 Replace the DCGV cover Reconnect the waste funnel 6 Reconnect the tube from the inlet valve to the middle with the waste tube holder in the top cover Insert waste position of the DCGV and then the solvent tubes at tube in the holder in the waste pan and clip tube to the channel A and B of the DCGV DCGV cover Solvent tubes x E Ors vi Q n 4 iis Ik JRL E Connecting tube DCGV to PIV 262 1220 Infinity LC Maintenance 11 Manual Injector Overview of Maintenance Procedures Table 45 Overview of maintenance procedures Procedure Typical frequency Time required Flushing the injector After using aqueous buffers or 5 min salt solutions Exchanging the injection valve After approximately 10000 to 10 min seal 20000 injections or when the valve performance shows indication of leakage or wear Flushing the Manual Injector CAUTION The use of aqueous buffers or salt solutions can lead to crystal formation Crystal formation may cause scratches on the injection seal gt Always rinse the valve with water after using aqueous buffers or salt
64. 00 lt 450000 Highest intensity in range 700mm 950nm lt 300000 Highest intensity for the D2 alpha line lt 1200000 Figure 56 Intensitiy Test Results report Specification ets cts cts cts cts cts cts Measured Result 68 08 h 18069 28464 16889 14665 89476 63598 169933 cts cts cts cts cts cts cts Passed Passed Passed Passed Passed Passed Passed In case of low counts in one or more ranges start the testing with the comparison of values with flow cell vs flow cell removed 175 9 176 Test Functions and Calibration Contaminations of the cell windows and or the lenses there are 3 between vis lamp and flow cell will reduce the light throughput If the detector fails in the range 501 nm 950 nm check e is the VIS lamp ON If not turn it on e is VIS lamp glass bulb blackended or broken If yes replace VIS lamp e does the UV lamp show a reflective coating towards the VIS lamp If yes replace UV lamp Example measured without flow cell VIS LAMP OFF or defect 110 counts VIS LAMP ON and OK 13613 counts Test Failed 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 Run the cell test see Cell Test on page 181 If the test fails exchange the flow cell windows 3 Dirty or contaminated optical components Clean optica
65. 1220 Infinity Oven kit then press Add Oven 3 Disconnect from the software and re boot your instrument 4 Re connect to the Instrument to the Instrument Utility Lab Advisor software 5 Now perform the Installation Check as described in Priming the System and Performing the Installation Check on page 48 6 When starting the Chromatographic Data System use Auto Configuration to have your new hardware configuration configured to the CDS 1220 Infinity LC 47 3 Installation Priming the System and Performing the Installation Check The steps described below are performed using the Instrument Utility Lab Advisor software 1 48 Connect all channels with HPLC grade water and use the Purge Pump for flushing the solvent channels Software Revision B 01 04 and below Tools gt Pump gt Purge Pump Software Revision B 02 01 and higher Service amp Diagnostics gt Pump Tools must be checked gt Purge Pump Prime all connected channels sufficiently until all channels are bubble free Use the Instrument Control functionality to prime your system with HPLC grade water to remove air out of the system Apply the following conditions Purge Valve closed Flow 2 mL min Time 5 min channel Set stroke 100 uL Perform the Installation Check from the Service and Diagnostics menu and print out the test result Create and print out a Status Report 1220 Infinity LC Installation 3 Performing a Check
66. 13 x Add Select signal Signal A RIU G13 7 Remove IV Autoscroll Generic plot RA 0000 STAT G13624 DE91600336 5 4 2010 3 19 20 PM RA 0000 STOP G13624 DE91600336 5 4 2010 3 24 11 PM Time min Figure 59 Test Chromatogram with Agilent Lab Advisor 7 To stop the test chromatogram enter in the command line STOP NOTE The test chromatogram is switched off automatically at the end of a run 184 1220 Infinity LC Test Functions and Calibration 9 Wavelength Verification and Recalibration 1220 Infinity LC 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 verification is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with bubble free degassed HPLC water in the flow cell If a deviation is found and displayed it can be recalibrated by pressing Adjust The deviations are tracked in the Calibration History diagnosis buffer in the detector DAD Wavelength Calibration G1315C x Calibration history Deviation D2 Alpha D2 Beta Time Date 0 01nm O 04mm 13 19 31 16 03 2005 D2 Alpha Heeg 1 2nm 656 1nm 1 2nm D2 Beta PEREL E TEL a A fa 1 2nm 486 0nm 1 2nm _Reset history D2 Alpha line deviation is 0 00nm D2 B
67. 16 Rev D EE Agilent Technologies
68. 2 The pump is based on a two channel dual plunger in series design that provides all essential functions that a solvent delivery system has to fulfill Metering of solvent and delivery to the high pressure side are performed by one pump assembly that can generate a pressure up to 600 bar The solvents are degassed by a vacuum degasser and solvent compositions are generated on the low pressure side by a high speed proportioning valve The dual channel gradient pump includes a built in dual channel online vacuum degasser The isocratic pump of the Agilent 1220 Infinity LC has no degasser The pump assembly includes a pump head with an inlet valve and an outlet valve A damping unit is connected between the two plunger chambers A purge valve including a PTFE frit is fitted at the pump outlet for convenient priming of the pump head 1220 Infinity LC Solvent Delivery System Description 5 Degasser The dual channel gradient pump comes with a built in online degasser The degasser is switched on automatically when the pump is switched on even if the flow is set to 0 mL min A constant vacuum of 75 Torr 100 mbar is created in the vacuum chamber of the two channels The solvent flows through a PTFE AF tube with an internal volume of 1 5 mL channel inside the vacuum chamber 1220 Infinity LC 83 5 Solvent Delivery System Description Principles of Operation 84 The liquid runs from the solvent reservoir through the degasser
69. 2 alpha line lt 1200000 cts 169947 cts 1 08 Holmiumtest_ in 30 nm Passed Figure 53 Self test Results report For details refer to the individual tests on the following pages 168 1220 Infinity LC Test Functions and Calibration 9 Filter Test The filter test checks the correct operation of the filter assembly When the test is started the holmium oxide filter is moved into position During filter movement the absorbance signal is monitored As the edge of the filter passes through the light path an absorbance maximum is seen Once the filter is in position the absorbance maximum of holmium oxide is determined Finally the filter is moved out of the light path During movement an additional absorbance maximum is expected as the edge of the filter passes through the light path The test passes successfully if the two maxima resulting from the edge of the filter assembly during filter movement are seen and the absorbance maximum of holmium oxide is within the limits g and evaluating filter test result 0 16 Figure 54 Filter Test Results report Filter Test Evaluation Filter Test Failed 1220 Infinity LC 169 9 Test Functions and Calibration Test Failed Probable cause Suggested actions 1 Filter assembly lever and filter not Install the filter assembly installed 2 Defective filter motor Please contact your Agilent service representative Holmium Oxide Maximum out of Limits Probable cause
70. 20 Infinity LC Instrument Logbook Method Instrument run started 09 1200 DAD 1 Power on 10 1200 DAD 1 UV lamp on 10 1200 DAD 1 Vis lamp on 10 1200 DAD 1 No Run data available in device 10 CP Macro Analyzing rawdata SHORT_02 D 10 Method Instrument Error Method Sequence stopped 10 Method Method aborted 1 0 Figure 64 Instrument Logbook Error Information 10 DAD Detector Error Messages 44 2 24 2 24 2 24 2 24 225 725 09 07 07 07 07 07 07 46 52 11 20 05 11 20 05 11 20 05 11 20 05 11 20 05 11 20 05 11 20 05 11 20 05 The logbook does not indicate a communication loss power fail It just shows the recovering Power on Lamps on 1220 Infinity LC 235 10 Error Information DAD Detector Error Messages 236 1220 Infinity LC 1220 Infinity LC 11 Maintenance PM Scope of Work and Checklist 239 Cautions and Warnings 240 Solvent Delivery System 242 Introduction 242 Checking and Cleaning the Solvent Filter 244 Exchanging the Passive Inlet Valve 246 Exchanging the Outlet Valve 248 Exchanging the Purge Valve Frit or the Purge Valve 250 Removing the Pump Head Assembly 253 Exchanging the Pump Seals and Seal Wear in Procedure 254 Exchanging the Plungers 257 Reinstalling the Pump Head Assembly 259 Exchanging the Dual Channel Gradient Valve DCGV 260 Manual Injector 263 Overview of Maintenance Procedures 263 Flushing the Manual Injector 263 Exchanging the Injection Valve Seal 264 Autosa
71. 220 Infinity LC 293 11 Maintenance Correcting Leaks When If a leakage has occurred in the flow cell area or at the capillary connections Tools required Description Tissue Wrench 1 4 inch for capillary connections Parts required Description None 1 Remove the lower front cover 2 Use tissue to dry the leak sensor area Observe the capillary connections and the flow cell area for leaks and correct if required 4 Replace the front cover Leak plane Waste outlet Leak sensor assembly 294 1220 Infinity LC Diode Array Detector DAD Overview of Maintenance Table 47 Overview of Maintenance Maintenance 11 The following pages describe maintenance simple repairs of the detector that can be carried out without opening the main cover Procedure Typical Frequency Notes Cleaning of module Deuterium lamp or tungsten lamp exchange Flow cell exchange Flow cell parts Cleaning or exchange Holmium oxide filter Cleaning or exchange Leak sensor drying Leak handling System replacement If required If noise and or drift exceeds your application limits or lamp does not ignite If application requires a different flow cell type If leaking or if intensity drops due to contaminated flow cell windows If contaminated If leak has occurred If broken or corroded An intensity test should be performed after replacement A holmium or wavelength calibration test shoul
72. 4 uv lamp voltage 224 visible lamp current 230 visible lamp voltage 230 wavelength calibration failed 232 wavelength check failed 229 metering device 101 missing pressure reading 203 module info 138 module options 138 motor drive power 204 move armhome 150 multi draw option 97 N needle drive 101 102 needle into sample 151 needle into seat 151 needle type 96 needle up 151 151 needle change 149 needles 96 negative absorbance 124 noise and drift ASTM 26 noise short term 24 non operating altitude 19 non operating temperature 19 numbering of vials 105 0 open gripper 152 operating Altitude 19 operating temperature 19 operational pressure range 21 22 optimization margins for negative absorbance 124 of selectivity 125 peak width 117 sample and reference wavelength 119 slit width 122 spectra acquisition 124 oven calibration 156 oventest 155 P park arm 150 parts for maintenance standard flow cell 340 parts identification cables 349 peak width response time 117 performance specifications 23 performance specifications 24 pHrange 21 22 photometric accuracy 132 physical specifications 19 19 1220 Infinity LC piston chamber 82 piston change 149 plateaus leak test 143 plungerhome 151 PM 239 power consumption 19 power considerations 16 cords 17 precision 95 pressure above upper limit 205 pressure below lower limit 205 pressure profile 139 pressure pulsation 21 22 88 90 pressure signal m
73. 4 4 Ref off NOISE NM1NM D mAU T T T T T T T o5 1 15 2 25 3 35 mir DAD1 A Sig 254 4 Ref off NOISE INM4NM D mAU F Slit width 4 nm ca AART aiaa iiaiai T T T T T T T 05 41 15 25 3 35 min DAD A Sig 254 4 Refzoff NOISEVINMTENM D mAU F Slit width 16 nm 2 Dannan anena AOOO 024 0 44 na aaaea repe eass 05 1 15 2 25 3 35 mii Figure 44 Influence of the Slit Width on Baseline Noise However with a wider slit the spectrograph s optical resolution its ability to distinguish between different wavelengths diminishes Any photodiode receives light within a range of wavelength determined by the slit width This explains why the fine spectral structure of benzene disappears when using a 16 nm wide slit 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 40 on page 120 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
74. 9 Screwdriver Pozidriv 1 p n Description 1 G4280 60004 Dual channel gradient valve Switch off the pump at the power switch Remove the upper front cover to gain access to the pump mechanics The lifetime of the dual channel gradient valve can be maintained by regularly flushing the valve especially when using buffer solutions If using buffer solutions flush all channels of the valve with water to prevent precipitation of the buffer Salt crystals can be forced into an unused channel and form plugs that may lead to leaks of that channel such leaks will interfere with the general performance of the valve When using buffer solutions and organic solvents in the Agilent 1220 Infinity LC Pump it is recommended to connect the buffer solution to the lower port of the gradient valve and the organic solvent to the upper port It is best to have the organic channel directly above the salt solution channel A salt solution B organic solvent 1220 Infinity LC 11 Maintenance Solvent Delivery System 1 Disconnect the connecting tube waste tube and the solvent tubes from the DCGV unclip them from the tube clips and place them into the solvent cabinet to avoid flow by hydrostatic pressure Solvent tubes z e N LL Connecting tube DCGV to PIV 3 Disconnect the DCGV cable unscrew the two holding screws and remove the valve 2 Press the lower sides of the cover to
75. AG838 stored TCP IP settings in non volatile memory sing Stored TCP IP Properties active i IP Address 134 40 27 95 connected to PC with controller software e g Agilent Subnet Mask 255 255 248 0 ChemStation here not connected Def Gateway 134 409 24 1 stored IP Address gt 134 40 27 99 z 255 255 248 0 Gateway 134 40 24 1 Controllers no connections Figure 27 Telnet Change IP settings 78 1220 Infinity LC LAN Configuration 4 7 When you have finished typing the configuration parameters type exit and press Enter to exit with storing parameters cx WINDOWS system32 cmd exe Agilent Technologies G4296A DEGHBHQH08 gt exit Connection to host lost C V a Figure 28 Closing the Telnet Session If the Initialization Mode Switch is changed now to Using Stored mode the instrument will take the stored settings when the module is re booted In the example above it would be 134 40 27 99 1220 Infinity LC 79 4 LAN Configuration Manual Configuration 80 1220 Infinity LC 1220 Infinity LC 5 Solvent Delivery System Description Overview 82 Degasser 83 Principles of Operation 84 Compressibility Compensation 88 Variable Stroke Volume 90 Using the Pump 91 This chapter provides an overview on the operational principles of the solvent delivery system pump and optional degasser ot Agilent Technologies 81 5 Solvent Delivery System Description Overview 8
76. Align the needle in the seat then tighten the screw firmly 2 7 Use Needle Up to lift the needle to a position approximately 2 mm above the seat 6 Reconnect the sample loop fitting to the needle fitting 1220 Infinity LC 271 11 Maintenance Next Steps 9 On completion of this procedure Install the front cover 10 Select End in the Tools function Change Needle 272 1220 Infinity LC Maintenance 11 Exchanging the Needle Seat Assembly When When the seat is visibly damaged When the seat capillary is blocked Tools required Description Wrench 1 4 inch supplied in HPLC Tool Kit Screwdriver flat head Parts required p n Description 1 G1313 87101 Needle seat assy 0 17 mm i d 2 3 uL Preparations Select Start in the Tools function in LMD Software Change Needle Remove the upper front cover Use the Needle Up command in the Change Needle function to lift the needle an additional 1 cm 1 Disconnect the seat capillary fitting from the injection 2 Use a small flat head screwdriver to ease out the needle valve port 5 seat 1220 Infinity LC 273 11 Maintenance 3 Insert the new needle seat assembly Press the seat firmly into position 4 Connect the seat capillary fitting to port 5 of the injection valve 5 Use Down to position the needle approximately 2 mm above the seat 6 Ensure the needle is
77. C The dimensions and weight of the Agilent 1220 Infinity LC allow it to be placed on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 in of space on either side and approximately 8 cm 3 1 in at the rear for air circulation and electric connections Make sure that the bench intended to carry the Agilent 1220 Infinity LC is designed to bear the weight of the instrument The Agilent 1220 Infinity LC should be operated upright 2 Site Requirements and Specifications Environment CAUTION Your Agilent 1220 Infinity LC will work within specifications at ambient temperatures and relative humidity as described in the following sections ASTM drift tests require a temperature change below 2 C hour 3 6 F hour measured 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 Condensation within the module Condensation can 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 i
78. Installing the Hardware Installation Paths Standard Installation Path No optional hardware upgrade is added to the module during installation 34 Installation Path Including the Installation of Upgrade Kits Oven upgrade kit Manual injector to ALS upgrade kit Isocratic to gradient upgrade kit The Installation of the gradient system upgrade kit and ALS upgrade kit must be done from Agilent trained service personnel only 1220 Infinity LC Standard Installation Path Hardware Installation Configure network access of Agilent 1220 Infinity LC Instrument configuration in CDS Flush the system and perform the installation check and perform a sample checkout run 1220 Infinity LC Installation 3 Installation Path Including the Installation of Upgrade Kits Hardware Installation Including installation of hardware upgrades kits Configure network access of Agilent 1220 Infinity LC Configure set new instrument type in the Instrument Utility Lab Advisor software Configure instrument in CDS and start CDS Flush the system and perform the installation check and perform a sample checkout run The installation of a Solvent Selection Valve SSV Option does not require the configuration of a new instrument type The SSV needs to be configured in the CDS only 35 3 Installation Installing the Hardware Installing the Agilent 1220 Infinity LC 1 Open the box and compare its content with the
79. Suggested actions 1 Holmium oxide filter not installed Install the holmium oxide filter 2 Dirty or contaminated filter Exchange the holmium oxide filter 170 1220 Infinity LC Test Functions and Calibration 9 Slit Test 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 Slit Test Evaluation Limit 0 7 1 3 Test Failed Probable cause Suggested actions 1 Flow cell still installed Remove the flow cell 2 Old or non Agilent lamp Run the Intensity Test on page 174 Exchange the lamp if old or defective 3 Defective slit assembly stray light Exchange the slit assembly 4 Defective detector main board Exchange the detector main board 5 Defective PDA optical unit Exchange the optical unit 1220 Infinity LC 171 172 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 leak
80. ade water remove all nitric acid some columns can be damaged by concentrated nitric acid check with pH indicator 3 Reinstall the filter 1220 Infinity LC 245 11 Maintenance Exchanging the Passive Inlet Valve When If leaking internally backflow Tools required Description Wrench 14mm Pair of tweezers Parts required p n Description G1312 60066 Passive inlet valve 1220 1260 Preparations Place the solvent bottles under the pump 1 Remove the upper front cover 2 Disconnect the solvent inlet tube from the inlet valve be aware that solvent may leak out of the tube due to hydrostatic flow 3 Unscrew the adapter from the inlet valve optional 246 1220 Infinity LC Maintenance 11 4 Using a 14 mm wrench loosen the inlet valve and remove the valve from pump head Figure 65 Passive inlet valve Insert the new valve into the pump head Using the 14 mm wrench turn the nut until it is hand tight Reconnect the adapter at the inlet valve optional Reconnect the solvent inlet tube to the adapter soo uN OS oI Reinstall the front cover 1220 Infinity LC 247 11 Maintenance Exchanging the Outlet Valve When If leaking internally Tools required Description Wrench 14mm Parts required p n Description G1312 60067 Outlet valve 1220 1260 Preparations Switch off pump at the main power switch Remove the upper front cover 1 Using a 1 4 inch wrench disconnect the valve capillary from the outlet
81. age current from each diode is measured and displayed graphically see Figure 55 on page 172 The leakage current represented in counts for each diode should fall within the limits red bands shown in the plot see Figure 55 on page 172 Dark Current Test Evaluation Limit 0 12000 counts Instrument al Number File C CHEM32 2 DIAGNOSE DAD DARK2 DGR Dark Current Plot Dark Current counts 10000 8000 6000 4000 2000 T T T T i T 200 400 600 800 Diode No Measured Result Dark current maximum value Dark current minimum value 0 U Gy aa Pec in Figure 55 Dark Currrent Test Results report 1220 Infinity LC Test Functions and Calibration 9 Test Failed Probable cause Suggested actions 1 Defective slit assembly stray light Run the Slit Test on page 171 part of the Self test on page 167 2 Defective detector main board Please contact your Agilent service representative 3 Defective PDA optical unit Please contact your Agilent service representative 1220 Infinity LC 173 9 Test Functions and Calibration Intensity Test The test is for the standard flow cells 10 mm and 6 mm pathlength only The nano flow cells 80 nL and 500 nL cannot be run with this test due to its low volume The intensity test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm Four spectral ranges are used
82. algae Always filter solvents small particles can permanently block the capillaries Avoid the use of the following steel corrosive solvents e Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on e High concentrations of inorganic acids like nitric acid sulfuric acid especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly O gt gt 2COCl 2HCl This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol 365 15 Appendix e Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides e Solutions of organic acids acetic acid formic acid and so on in organic solvents For example a 1 solution of acetic acid in methanol will attack steel e Solutions containing strong complexing agents for example EDTA ethylene diamine tetra acetic acid e Mixtures of carbon tetrachloride with 2 propanol or THF 366 1220 Infinity LC Appendix 15 Radio Interference Cables supplied by Agilent Technologies are screened to provide opt
83. aligned with the seat If required bend the needle slightly until the needle is aligned correctly Next Steps 7 On completion of this procedure Install the front cover 8 Select End in the Tools function Change Needle 274 1220 Infinity LC Maintenance Exchanging the Rotor Seal When Tools required Parts required Preparations CAUTION Poor injection volume reproducibility Leaking injection valve Description Wrench 1 4 inch Hex key 9 16 inch supplied in the tool kit p n Description 1 0101 1416 Rotor seal PEEK Remove upper front cover Remove the leak tubing if necessary Removing the stator head 11 The stator face is held in place by the stator head When you remove the stator head the stator face can fall out of the valve gt Carefully handle the valve to prevent damage to the stator face 1220 Infinity LC 275 11 Maintenance Autosampler 1 Remove all capillary fittings from the injection valve 2 Loosen each fixing bolt two turns at a time Remove the ports bolts from the head 276 1220 Infinity LC Maintenance 11 Autosampler 5 Install the new rotor seal and isolation seal Ensure the metal spring inside the isolation seal faces towards the valve body 0 6 Install the stator ring with the short of the two pins facing towards you at the 12 o clock position Ensure the ring
84. ample 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 1220 Infinity LC 119 120 Detector Description 437 30 Absorbance mAU sample wavelength 252 nm Anisic acid Reference bandwidth 100 nm 30 nm bandwidth Reference wavelength 360 E 220 248 260 280 300 320 340 360 380 480 Wavelength nm Figure 40 Optimization of Wavelength Setting A wide bandwidth has the advantage of reducing noise by averaging over a wavelength range compared to a 4 nm bandwidth the baseline noise is reduced by a factor of approximately 2 5 whereas the signal is about 75 of a 4 nm wide band The signal to noise ratio for a 30 nm bandwidth is twice that for a 4 nm bandwidth in our example Bandwidth 30 nm 12 nm Figure 41 Influence of Bandwidth on Signal and Noise 1220 Infinity LC Detector Description 8 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
85. ance 12 Solvent Delivery System Description Purge valve Valve body PTFE frits pack of 5 Seal Cap Assembly 1220 Infinity LC 327 12 Parts for Maintenance Passive Inlet Valve Assembly p n Description G1312 60066 Passive inlet valve 1220 1260 328 1220 Infinity LC Parts for Maintenance 12 Bottle Head Assembly Item p n Description G1311 60003 Bottle head assembly 1 5063 6598 Ferrules with lock ring 10 Pk 5063 6599 Tube screw 10 Pk 3 Wire marker 4 5062 2483 Tube PTFE 1 5mm x 5 m 3 mm od 5 5062 8517 Frit adapter pack of 4 6 5041 2168 Solvent inlet filter 20 um pore size 1220 Infinity LC 329 12 Parts for Maintenance Solvent Delivery System Hydraulic Path Item p n 1 G1312 67305 G1311 60003 2 G4280 60034 3 64280 81300 4 G4280 81301 5 5067 5378 5062 2461 G1311 60065 G1311 60001 G4280 60004 3160 1017 Description Outlet capillary pump to injector Bottle head assembly bottle to passive inlet valve or vacuum degasser Solvent tube vacuum degasser to DCGV Capillary plunger 1 to damper Capillary damper to plunger 2 Connecting tube DCGV to PIV Waste tube 5 m reorder pack Damper Isocratic Quaternary Pump 600 bar Pump drive Dual channel gradient valve Fan 330 1220 Infinity LC Injection System Manual Injector 1220 Infinity LC Parts for Maintenance 12 Injection Valve Assembly Item p n 5067 4202
86. anol under pressure use restriction capillary Tighten the active inlet valve 14 mm wrench Do not overtighten Ensure the pump head screws are tight Ensure the sieve in the outlet valve is installed correctly Tighten the outlet valve Exchange the pump seals Check the plungers for scratches Exchange if scratched Exchange the active inlet valve Table 30 First plateau negative second plateau positive Potential Cause Leaking outlet valve Loose pump head screws Leaking seals or scratched plungers Corrective Action Clean the outlet valve Ensure the sieve in the outlet valves are installed correctly Tighten the outlet valve Ensure the pump head screws are tight Exchange the pump seals Check the plunger for scratches Exchange if scratched Table 31 Ramp 3 does not reach limit Potential Cause Pump stopped due to error Large leaks visible at the pump seals Large leaks visible at active inlet valve outlet valve or purge valve Corrective Action Check the logbook for error messages Exchange the pump seals Ensure the leaky components are installed tightly Exchange the component if required 1220 Infinity LC Test Functions and Calibration 9 Table 32 Third plateau negative pressure drop gt 2 bar min Potential Cause Corrective Action Loose or leaky fittings Ensure all fittings are tight or exchange capillary Loose purge valve Tighten the purge valv
87. ard flow cell path length 10 nm flow 1 mL min LC grade methanol Noise lt t 0 5 10 AU at 254 nm TC 2 s ASTM RT 2 2 TC Linearity Linearity is measured with caffeine at 265 nm The specifications are based on the standard lamp G1314 60100 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 hours 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 27 2 Site Requirements and Specifications Performance Specifications 28 1220 Infinity LC 1220 Infinity LC 3 Installation Unpacking Your System 30 Delivery Che
88. ariable wavelength detector ADC Hardware Error Error ID 7830 7831 A D Converter hardware is defective Probable cause 1 A D Converter hardware is defective Suggested actions Please contact your Agilent service representative Wavelength calibration setting failed 1220 Infinity LC Error ID 7310 The intensity maximum was not found during wavelength calibration Calibration 0 Failed Calibration 1 Failed Probable cause 1 2 Lamp is OFF Incorrect flow cell installation Flow cell contamination or air bubbles Intensity too low Current step value too far from maximum Misaligned defective grating assembly Defective main board Zero order calibration failed 656 nm calibration failed Suggested actions Switch on the lamp Ensure the flow cell is installed correctly Clean replace flow cell windows or remove air bubbles Replace lamp Repeat the calibration Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 225 10 Error Information Cutoff filter doesn t decrease the light intensity at 250 nm Error ID 7813 The automatic filter check after lamp ignition has failed When the lamp is switched on the detector moves the cutoff filter into the light path If the filter is functioning correctly a decrease in lamp intensity is seen If the expected intensi
89. au 3 When the system pressure reaches 390 bar the flow is reduced to zero and the pressure stabilizes just below 400 bar One minute after reaching the maximum pressure the pressure drop should not exceed 2 bar min 1220 Infinity LC Test Functions and Calibration 9 Running the Leak Test When Tools required Parts required Preparations 1220 Infinity LC If problems with the pump are suspected Description Wrench 1 4 inch supplied in HPLC Tool Kit p n Description 1 G1313 87305 Restriction Capillary 1 01080 83202 Blank nut 1 500 mL Isopropanol Place a bottle of LC grade isopropyl alcohol in the solvent cabinet and connect its solvent tube to the active inlet valve of the pump Make absolutely sure that all parts of the flow path that are part of the test are very thoroughly flushed with IPA before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path will definitely cause the test to fail Running the test from the Agilent Lab Advisor 1 Select the Leak Test from the Test Selection menu 2 Start the test and follow the instructions Make sure to release the pressure by slowly opening the purge valve when the test has finished Evaluating the Leak Test Results on page 142 describes the evaluation and interpretation of the leak test results For detailed instructions refer to the Agilent Lab Advisor tool 141 Test Functions and Ca
90. 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 If an error occurs outside a method run other modules will not be informed about this error If it occurs within a method run all connected modules will get a notification all LEDs get red and the run will be stopped Depending on the module type this stop is implemented differently For example for a pump the flow will be stopped for safety reasons For a detector the lamp will stay on in order to avoid equilibration time Depending on the error type the next run can only be started if the error has been resolved for example liquid from a leak has been dried Errors for presumably single time events can be recovered by switching on the system in the user interface Special handling is done in case of a leak As a leak is a potential safety issue and may have occurred at a different module from where it has been observed a leak always causes a shutdown of all modules even outside a method run In all cases error propagation is done via the CAN bus or via an APG remote cable see documentation for the APG interface 1220 Infinity LC Error Information 10 General Error Messages General error messages are generic to all Agilent series HPLC modules and may show up on other modules as w
91. board e Please contact your Agilent service representative 2 Detector is exposed to illegal ambient Verify that the ambient conditions are within conditions the allowed range 1220 Infinity LC 223 10 Error Information 224 UV Lamp Current Error ID 7450 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 1 Lamp disconnected 2 Defective UV lamp or non Agilent lamp 3 Defective detector main board 4 Defective power supply UV Lamp Voltage Error ID 7451 Suggested actions Ensure the UV lamp connector is seated firmly Exchange the UV lamp Please contact your Agilent service representative Please contact your Agilent service representative The UV lamp anode voltage is missing The processor continually monitors the anode voltage across the lamp during operation If the anode voltage falls below the lower limit the error message is generated Probable cause 1 Defective UV lamp or non Agilent lamp 2 Defective detector main board 3 Defective power supply Suggested actions Exchange the UV lamp Please contact your Agilent service representative Please contact your Agilent service representative 1220 Infinity LC VWD Detector Error Messages Error Information 10 These errors are specific to the v
92. bout how to establish a network connection to the instrument can be found in Connecting the Agilent 1220 Infinity LC to the PC on page 44 or LAN Configuration on page 51 13 Verify that the power push button at the front of the module see Figure 5 on page 39 stands off Now connect the power cord to the Agilent 1220 Infinity LC and the power line 14 Before switching on the module check that all transport foams have been de installed see Figure 2 on page 37 Then switch on the module via the power push button 1220 Infinity LC Installation 3 Installing the Hardware Identifying the connections of the 1220 Infinity LC 1220 Infinity LC Agilent 1220 Infinity LC with VWD Figure 6 on page 41 shows an overview of the possible connections on the 1220 Infinity LC instrument with VWD MAC address label st e LAN connector RS232 serial and remote connectors CAN port Configuration dip switches for boot mode selection Power plug ED Figure 6 Connections of the Agilent 1220 Infinity LC with VWD 41 3 Installation Installing the Hardware Agilent 1220 Infinity LC with DAD Figure 7 on page 42 shows an overview of the possible connections on the 1220 Infinity LC instrument with DAD On the G4294B you must use the configuration dip switches on the DAD mainboard because this will be the communication host in this case The short CAN cable is the communication connection bet
93. ccurs is stored in the detector The wavelength verification calibration takes about 2 5 min and is disabled within the first 10 min after ignition of the lamp because initial drift may distort the measurement When the lamp is turned ON the 656 nm emission line position of the deuterium lamp is checked automatically When to Calibrate the Detector The detector is calibrated at the factory and under normal operating conditions should not require recalibration However it is advisable to recalibrate e after maintenance flow cell or lamp e after repair of components in the optical unit e after exchange of the optical unit or VWM board e at a regular interval at least once per year for example prior to an Operational Qualification Performance Verification procedure and e when chromatographic results indicate the detector may require recalibration 1220 Infinity LC Test Chromatogram Test Functions and Calibration 9 A built in pre defined test chromatogram on the VWM board is processed through ADC like normal signals from the diodes and can be used to check the ADC and the data handling system The signal is available at the analog output and on the GPIB The run time of the chromatogram is depending on the setting for response time peak width If no stop time is set the chromatogram will repeat continuously Response Time 0 06 sec 0 12 sec 0 25 sec 0 50 sec 1 00 sec 2 00 sec 4 00 sec 8 00 sec Stop Tim
94. ce on page 72 or Restarting the Agilent BootP Service on page 73 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 192 168 254 11 for example The Tab File is located at C Documents and Settings All Users Application Data Agilent BootP TabFile 1220 Infinity LC 71 4 LAN Configuration Changing the IP Address of an Instrument Using the Agilent BootP Service 72 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 RE Be aton yew teb s B iDRBI r gt r gt s n Select an tem to view ts description BoArtomatic Updates Rated Beadgound inteky DQ chlor coms Evert System S s Rated Rated f Provides th Rated Rated Manages n Rated Boderrtated ink Tra Maintains i Rated Byvetrdeted Transac Coordinate a P aesan a j Figure 20 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
95. ce needs to be scheduled 1220 Infinity LC 1220 Infinity LC ee 2 7 e Site Requirements and Specifications amp i Site Requirements 16 Power Considerations 16 Power Cord 17 Bench Space 17 Environment 18 Physical Specifications 19 Performance Specifications 20 Specification Conditions 27 This chapter provides information on environmental requirements physical and performance specifications ot Agilent Technologies 15 2 Site Requirements and Specifications Site Requirements A suitable environment is important to ensure optimal performance of the instrument Power Considerations The Agilent 1220 Infinity LC power supply has wide ranging capabilities Consequently there is no voltage selector at the instrument Instrument is partially energized when switched off The power supply still uses some power even when the power switch on the front panel is turned OFF Repair work at the detector can lead to personal injuries e g shock hazard when the detector cover is opened and the instrument is connected to power gt To disconnect the detector from the power line unplug the power cord Incorrect line voltage to the instrument Shock hazard or damage to your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument only to the specified line voltage CAUTION In case of an emergency it must be possible to
96. cklist 30 Installing the Hardware 34 Installation Paths 34 Installing the Agilent 1220 Infinity LC 36 Identifying the connections of the 1220 Infinity LC 41 Connecting and Configuring the Instrument to the Chromatographic Data System 43 Connecting the Agilent 1220 Infinity LC tothe PC 44 The Instrument Utility LabAdvisor Software 46 Configuration of the Instrument After an Upgrade Installation 47 Priming the System and Performing the Installation Check 48 Performing a Checkout Run 49 This chapter provides an overview on shipment content and installation To install the Agilent 1220 Infinity LC System it is highly recommended to follow the installation instructions step by step Apg Agilent Technologies 29 3 Installation Unpacking Your System CAUTION If the delivery packaging shows signs of external damage please call your Agilent Technologies sales and service office immediately Inform your service representative that the Agilent 1220 Infinity LC may have been damaged during shipment Signs of damage gt Do not attempt to install the Agilent 1220 Infinity LC Delivery Checklist 30 Delivery Checklist Ensure all parts and materials have been delivered with the Agilent 1220 Infinity LC The delivery checklist is shown below Please report missing or damaged parts to your local Agilent Technologies sales and service office Table9 Agilent 1220 Infinity Checklist Description Quantity
97. close as possible to a narrow peak of interest in your chromatogram Response time will the be approximately 1 3 of the peak width resulting in less than 5 peak height reduction and less than 5 additional peak dispersion Decreasing the peak width setting in the detector will result in less than 5 gain in peak height but baseline noise will increase by a factor of 1 4 for a factor of 2 response time reduction Increasing peak width response time by factor of two from the recommended setting over filtering will reduce peak height by about 20 and reduce baseline noise by a factor of 1 4 This gives you the best possible signal to noise ratio but may affect peak resolution 117 118 Detector Description Table 22 Peak Width Response Time Data Rate Peak Width minutes Response Time seconds Data Rate Hz lt 0 0025 0 025 80 gt 0 0025 0 05 80 gt 0 005 0 1 40 gt 0 01 0 2 20 gt 0 03 0 5 10 gt 0 05 1 0 5 gt 0 10 2 0 2 5 gt 0 20 4 0 1 25 gt 0 40 8 0 0 62 gt 0 85 16 0 0 31 1220 Infinity LC Detector Description 8 Sample and Reference Wavelength and Bandwidth The detector measures absorbance simultaneously at wavelengths from 190 to 950 nm Two lamps provide good sensitivity over the whole wavelength range The deuterium discharge lamp provides the energy for the UV range 190 to 400 nm and the tungsten lamp emits light from 400 to 950 nm for the visible and short wave near infrared If yo
98. compressibility tables when using isocratic mixtures of solvents and if the default settings are not sufficient for your application the following procedure can be used to optimize the compressibility settings 1220 Infinity LC 1220 Infinity LC Solvent Delivery System Description 5 When using mixtures of solvents it is not possible to calculate the compressibility of the mixture by interpolating the compressibility values of the pure solvents used in that mixture or by applying any other calculation In these cases the following empirical procedure has to be applied to optimize your compressibility setting 1 Start the pump with the required flow rate 2 Before starting the optimization procedure the flow must be stable Use degassed solvent only Check the tightness of the system with the pressure test 3 Your pump must be connected to control software with which the pressure and ripple can be monitored 4 The compressibility compensation setting that generates the smallest pressure ripple is the optimum value for your solvent composition Table 19 Solvent Compressibility Solvent pure Compressibility 1 10 bar Acetone Acetonitrile Benzene Carbon tetrachloride Chloroform Cyclohexane Ethanol Ethyl acetate Heptane Hexane Isobutanol lsopropanol Methanol 1 Propanol Toluene Water 126 115 95 110 100 118 114 104 120 150 100 100 120 100 87 46 89 5 Solvent Delivery Sy
99. d be performed after replacement A pressure tightness test should be done after repair A holmium or wavelength calibration test should be performed after replacement Check for leaks Check for leaks 1220 Infinity LC 295 11 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 allowing liquid to drip into the module WARNING Liquid dripping into the electronic compartment of your module 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 connections in the flow path 296 1220 Infinity LC Maintenance 11 Exchanging a Lamp When If noise or drift exceeds application limits or lamp does not ignite Tools required Description Screwdriver Pozidriv 1 PT3 Parts required p n Description 1 2140 0820 Longlife Deuterium lamp C with black cover and RFID tag OR 1 G1103 60001 Tungsten lamp WARNING Eye damage by detector light Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product gt Always turn the deuterium lamp off before removing it 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 d
100. delivery checklist for completeness 2 Place the Agilent 1220 Infinity LC on top of the bench 3 Remove both front covers top and lower by pressing the release buttons on both sides oe Figure 1 Front Cover Mechanism 36 1220 Infinity LC Installation 3 Installing the Hardware 4 Remove the two transport foams Figure 2 Remove the Transport Foam Figure 3 on page 38 shows the content of a fully equipped 1220 Infinity LC system with removed front covers Module type shown G4290B 1220 Infinity LC 37 3 Installation Installing the Hardware Solvent tray Gradient pump with degasser or isocratic pump not shown olvent selection valve optional not shown Autosampler or manual injector not shown Column oven optional Interface connectors LAN CAN power Variable Wavelength Detector VWD Power push button Figure 3 System Overview 1220 Infinity LC NOTE Additional options or upgrade kits should be installed prior to all solvent path installations Configuring your Agilent 1220 Infinity LC Module Information can be found in the Configuration of the Instrument After an Upgrade Installation on page 47 For further information about how to install the options and upgrade kits refer to Agilent 1220 Infinity LC Module manual 5 Place the Solvent Bottle filled with 0 5 L HPLC grade water in the Solvent Tray 38 1220 Infinity LC Installation
101. disconnect the instrument from the power line at any time Make sure that there is easy access to the power cable of the instrument so that the instrument can quickly and easily be disconnected from the line voltage gt Provide sufficient space next to the power socket of the instrument to allow the cable to be unplugged 16 1220 Infinity LC Site Requirements and Specifications 2 Power Cord Different power cords are offered as options with the system The female ends of all power cords are identical The female end plugs into the power input socket at the rear left side of the instrument The male end of each power cord is different and designed to match the wall socket of a particular country or 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 instrument 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 cables not supplied by Agilent Using cables that have not been 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 Bench Space 1220 Infinity L
102. e Instrument with DAD Instrument with VWD Figure 8 Location of the Configuration Dip Switches and LAN Port On the G4294B use the configuration dip switches of the DAD extension board to configure your LAN connection 44 1220 Infinity LC Installation 3 1 To connect the instrument with your PC using this default address configure the PC s network settings as followed IP 192 168 254 10 Subnet Mask 255 255 255 0 Default Gateway N A 2 Connect the crossover patch cable between the LAN Port of the Agilent 1220 Infinity LC Figure 8 on page 44 and the network connector of your PC The crossover cable is only for the direct connection between the module and the PC If you want to connect your Agilent 1220 Infinity LC via a hub to the network you should contact your local network administrator If you want to connect the instrument to a network we strongly recommend consulting your local network administrator to provide you with a valid network address For further details about LAN configuration of the Agilent 1220 Infinity LC please refer to the LAN Configuration section of the Installation chapter in the1220 Infinity LC User Manual Here you find details about TCP IP parameter configuration e Configuration Switches e Using a fixed IP address How to configure an individual IP address 1220 Infinity LC 45 3 The Instrument Utility LabAdvisor Software 46 During the installation process of the Agilent 1220 Infi
103. e 0 8 min 0 8 min 0 8 min 0 8 min 1 6 min 3 2 min Default settings 6 4 min 12 8 min The test chromatogram has four main peaks with the following absorbances Peak 1 2 3 1220 Infinity LC Absorbance approx 38 mAU 100 mAU 290 mAU 20 mAU 165 9 Test Functions and Calibration Spectral Scan The Spectral Scan tool is available for diode array and variable wavelength detectors DAD MWD and VWD It allows you to scan a spectrum over a specified wavelength range and export the data to a csv comma separated values file that can be used in other applications for example Microsoft Excel Scan Parameters UV Lamp On Switches on the UV lamp Blank Scan Scans a blank spectrum solvent only over the specified wavelength VWD only range at the specified resolution You specify the wavelength range in the from and to fields and the resolution in the step field Sample Scan Scans the sample spectrum over the specified wavelength range at the specified resolution You specify the wavelength range in the from and to fields and the resolution in the step field Export Data Exports the selected data in csv format for use in other applications 166 1220 Infinity LC Test Functions and Calibration 9 Diode Array Detector DAD This chapter describes the detector s built in test functions Self test 1220 Infinity LC The DAD self test see Figure 53 on page 168 runs a series of individual tes
104. e 14 mm wrench Contaminated purge valve Open and close purge valve to flush out contamination Exchange the valve if still leaky Loose pump head screws Ensure the pump head screws are tight Leaking seals or scratched plungers Exchange the pump seals Check the plungers for scratches Exchange if scratched Leaking outlet valve Exchange the outlet valve Leaky damper Exchange damper Pressure Too High Check This test checks the flow path for a blockage and tries to identify the module that is causing the blockage If the blockage is in the autosampler the test can identify whether the blockage occurs in the needle or needle seat The pump and autosampler are necessary to run the Pressure Too High Check 1220 Infinity LC 145 9 146 Test Functions and Calibration Pressure Too High Check Evaluation Start Conditions The pump and autosampler are brought to the READY state and an operating pressure of 200 bar is applied to the system The pump ripple is measured and the start of the test is delayed until the ripple is within the defined limits typically 1 of operating pressure Test Part 1 Part 1 of the test tries to determine in which part of the system the pressure problem lies After the system has achieved the start conditions the autosampler valve is switched from mainpass to bypass and the pressure slice is tested against a limit If the limit is exceeded the pressure problem lies in t
105. e To waste From solvent bottle Seal Plunger 1 Plunger 2 Ball screw drive Gear Motor with encoder Figure 29 Principle of the pump 1220 Infinity LC 85 5 86 Solvent Delivery System Description When turned on the pump runs through an initialization procedure to determine the upper dead center of the first plunger The first plunger moves slowly upwards into the mechanical stop of chamber and from there it moves back a predetermined distance The controller stores this plunger position in memory After this initialization the pump starts operation with the set parameters The inlet valve is opened and the down moving plunger draws solvent into the first chamber At the same time the second plunger moves upwards delivering into the system After a controller defined stroke length depending on the flow rate the drive motor is stopped and the inlet valve is closed The motor direction is reversed and moves the first plunger up until it reaches the stored upper limit and at the same time moves the second plunger downwards The sequence then starts again moving the plungers up and down between the two limits During the up movement of the first plunger the solvent in the chamber is pushed through the outlet ball valve into the second chamber The second plunger draws in half of the volume displaced by the first plunger and the remaining half volume is directly delivered into the system During the drawing stroke of the first
106. e microswitch does not close the error message is generated Probable cause Suggested actions 1 Defective injection valve Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative 220 1220 Infinity LC Error Information 10 Vial in Gripper 1220 Infinity LC Error ID 4033 The gripper arm attempted to move with a vial still in the gripper During specific stages of the sampling sequence no vial should be held by the gripper The autosampler checks if a sample vial is stuck in the gripper by closing and opening the gripper fingers while monitoring the motor encoder If the gripper fingers are unable to close the error message is generated Probable cause Suggested actions 1 Vial still in gripper Remove the vial using the Release Vial function in the user interface Reinitialize the autosampler 221 10 Error Information General Detector Error Messages 222 These errors are specific to both detector types VWD and DAD Heater at fan assembly failed Error ID 1073 Every time the deuterium lamp or the tungsten lamp DAD only 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 s
107. e g if the gripper is accidentally moved out of position when loading vials into the vial tray The initialization positions of the moving components are sensed by reflection sensors mounted on the flex board These positions are used by the processor to calculate the actual motor position An additional six reflection sensors for tray recognition are mounted on the flex board at the front of the assembly Supported Trays for the Autosampler 1220 Infinity LC p n Description G1313 44510 Tray for 100 x 2 mL vials G1313 44513 Halftray for 15 x 6 mL vials G1313 44512 Halftray for 40 x 2 mL vials Half tray combinations Half trays can be installed in any combination enabling both 2 mL and 6 mL vials to be used simultaneously Numbering of vial positions The standard 100 vial tray has vial positions 1 to 100 However when using two half trays the numbering convention is slightly different The vial positions of the right hand half tray begin at position 101 as follows Left hand 40 position tray 1 40 Left hand 15 position tray 1 15 Right hand 40 position tray 101 140 Right hand 15 position tray 101 115 105 6 Injection System Description Choice of Vials and Caps For reliable operation vials used with the Agilent 1220 Infinity LC autosampler must not have tapered shoulders or caps that are wider than the body of the vial The vials and caps shown with their part numbers in the tables below have been successful
108. e number of steps required to reach the reference positions are the same as the expected step number the test is passed If a motor fails to move or loses motor steps the test fails The test evaluates the results automatically VWD Filter Grating Test Results Probable causes of test failure Table 41 Filter Motor Test Cause Corrective action Defective filter motor assembly Exchange the filter motor assembly Defective VWM board Exchange the VWM board Table 42 Grating Motor Test Cause Corrective action Defective filter motor assembly Exchange the filter motor assembly Defective VWM board Exchange the VWM board 1220 Infinity LC 163 9 164 Test Functions and Calibration Detector Calibration Wavelength Verification Calibration Wavelength Calibration of the detector is done using the zero order position and 656 nm alpha emission line and beta emission line at 486 nm emission line positions of the deuterium lamp The calibration procedure involves three steps First the grating is calibrated on the zero order position The stepper motor step position where the zero order maximum is detected is stored in the detector Next the grating is calibrated against the deuterium emission line at 656 nm and the motor position at which the maximum occurs is stored in the detector Finally the grating is calibrated against the deuterium emission line at 486 nm and the motor position at which the maximum o
109. e the seal Clean the chamber with lint free cloth Ensure all particular matter is removed 6 Install the new seal Press the seal firmly into position 280 1220 Infinity LC Maintenance 11 7 Place the piston guide on top of the seal 8 Reassemble the metering head assembly Carefully insert the plunger into the base The closed side of the metering head must be on the same side as the lower one of the two capillary drillings 9 Install the fixing bolts Tighten the bolts securely 10 Install the metering head assembly in the autosampler Ensure the large hole in the metering head is facing downwards 1220 Infinity LC 281 11 Maintenance Autosampler 11 Reinstall the capillaries Next Steps 12 On completion of this procedure Install the front cover 13 Select End in the Tools function in the LMD software Change piston 282 1220 Infinity LC Maintenance 11 Autosampler Exchanging the Gripper Arm When Defective gripper arm Tools required Description Straightened paper clip Parts required p n Description 1 G1313 60010 Gripper assembly Preparations Select Start in the Tools function in the LMD software Change Gripper Turn off the power to the instrument Remove the upper front cover 1 Identify the slit below the gripper motor and the gripper 2 Rotate the arm approximately 2 5 cm 1 inch to the left arm release but
110. ecifications Agilent 1220 Infinity LC DAD Table8 Performance Specifications Type Specification Comments Detection type 1024 element diode array Light source Number of signals Maximum sampling rate Short term noise ASTM Single and Multi Wavelength Drift Linear absorbance range Wavelength range Wavelength accuracy Slit width Diode width Flow cell Time programmable Deuterium and tungsten lamps 8 80 Hz lt 0 7 10 AU at 254 4 nm and 750 nm TC 2s lt 0 9 10 3 AU h at 254 nm gt 2 AU 5 at 265 nm 190 950 nm 1nm 1 2 4 8 16 nm lt 1nm Standard 13 pL volume 10 mm cell path length and 120 bar 1740 psi pressure maximum Wavelength polarity peak width lamp bandwidth autobalance wavelength range threshold spectra storage mode The UV lamp is equipped with RFID tag that holds lamp typical information see Specification Conditions below see Specification Conditions below see Specification Conditions below Self calibration with deuterium lines verification with holmium oxide filter Programmable slit The flow cell is equipped with RFID tags that hold cell typical information pH range 1 0 9 5 1220 Infinity LC Site Requirements and Specifications 2 Specification Conditions 1220 Infinity LC ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions Stand
111. ector uses a Rheodyne 6 port sample injection valve 5067 4202 Sample is loaded into the external 20 uL sample loop through the injection port at the front of the valve The valve has a PEEK injection seal A make before break passage in the stator ensures flow is not interrupted when the valve is switched between the INJECT and LOAD positions and back again Load position Inject position Figure 30 Rheodyne 6 port sample injection valve 1220 Infinity LC Injection System Description 6 The Injection Seal The manual injector is supplied with a PEEK injection seal as standard Injecting Sample WARNING Ejection of mobile phase When using sample loops larger than 100 pL mobile phase may be ejected from the needle port as the mobile phase in the sample loop decompresses gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used Needle port Waste to column Sample loop 1220 Infinity LC LOAD Position In the LOAD position see Figure 31 on page 95 the pump is connected directly to the column ports 4 and 5 connected and the needle port is connected to the sample loop At least 2 to 3 sample loop volumes more if better precision is required of sample should be injected through the needle port
112. ects the light onto the photodiode array The diode array is a series of 1024 individual photodiodes and control circuits located on a ceramic carrier With a wavelength range from 190 950 nm the sampling interval is lt 1 nm 1220 Infinity LC Detector Description 8 Peak width response time Unfiltered Response time 0 05 min Response time 0 1 min 1220 Infinity LC 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 39 on page 117 but reduce peak height only slightly In addition these filters reduce the data rate to allow optimum integration and display of your peaks and to minimize disk space required to store chromatograms and spectra DAD1 A Sig 254 4 Ref off NOISE INM1NM D T s T T i T 7 T T k T l o5 1 15 2 25 3 35 min DADT A Sig 254 4 Refoff NOISEVINMOLS D maAU o 0 2 0 4 mAU o 0 2 0 4 T T T T T T T T o o5 4 15 2 25 3 36 mir DAD1 A Sig 254 4 Ref off NOISE NMO1 D mAU o i 05 4 15 2 25 3 35 mir Figure 39 Influence of Response Time on Signal and Noise Table 22 on page 118 lists the filter choices of the detector To get optimum results set peak width as
113. ed service personal only Safety flap flex board It is strongly recommended that the exchange of the safety flap and flex board is done by Agilent trained service personnel Transport assembly parts The adjustment of the motors and the tension on the drive belts are important for correct operation of the transport assembly It is strongly recommended that exchange of drive belts and the gripper assembly is done by Agilent trained service personnel There are no other field replaceable parts in the transport assembly If any other component is defective flex board spindles plastic parts the complete unit must be exchanged Cleaning the autosampler Electrical shock hazard Liquid dripping into the autosampler could cause shock hazard and damage to the autosampler gt Drain all solvent lines before opening any fittings 268 The autosampler covers should be kept clean Clean with a soft cloth slightly dampened with water or a solution of water and a mild detergent Do not use an excessively damp cloth that liquid can drip into the autosampler Maintenance Functions Certain maintenance procedures require the needle arm metering device and gripper assembly to be moved to specific positions to enable easy access to components The maintenance functions move these assemblies into the appropriate maintenance position 1220 Infinity LC Maintenance Exchanging the Needle Assembly When Tools required Part
114. ed 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 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 observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 1220 Infinity LC 363 15 Appendix Safety Symbols Table 48 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
115. educes the amount of data storage necessary Spectra are taken continuously depending on the setting of the Peakwidth Eight spectra are acquired per Peakwidth The acquisition time for one spectrum is slightly less than the Peakwidth divided by 8 that is greater than or equal to 0 01s and less than or equal to 2 55s If there are no peaks in Signal A there are no spectra You cannot process spectra present in other signals Range defines the wavelength range for spectral storage Limits 190 to 950 nm in steps of 1 nm for both low and high values The high value must be greater than the low value by at least 2 nm Step defines the wavelength resolution for spectral storage Limits 0 10 to 100 00 nm in steps of 0 1 nm The threshold is the height in mAU of the smallest expected peak The peak detector ignores any peaks which are lower than the threshold value and does not save spectra Limits 0 001 to 1000 00 mAU in steps of 0 001 mAU Usable for modes Apex Baselines Apex Slopes Baselines and All in Peak 1220 Infinity LC 129 8 Detector Description Match the Flow Cell to the Column Match the Flow Cell to the Column Figure 50 on page 130 shows recommendations for flow cells that match the column used If more than one selection is appropriate use the larger flow cell to get the best detection limit Use the smaller flow cell for best peak resolution Choosing a Flow Cell for the VWD Column le
116. ell Compensation Sensor Open Error ID 0081 The ambient compensation sensor NTC on the power switch board in the module has failed open circuit The resistance across the temperature compensation sensor NTC on the power switch board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable cause Suggested actions 1 Loose connection between the power Please contact your Agilent service switch board and the main board representative 2 Defective power switch board Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative Compensation Sensor Short Error ID 0080 The ambient compensation sensor NTC on the power switch board in the module has failed open circuit 1220 Infinity LC 195 10 Error Information 196 The resistance across the temperature compensation sensor NTC on the power switch 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 1 Defective power switch board 2 Loose connection between the power switch board and the main board Suggested
117. enting blockage of solvent filters Contaminated solvents or algae growth in the solvent bottle will reduce the lifetime of the solvent filter and will influence the performance of the pump This is especially true for aqueous solvents or phosphate buffers pH 4 7 The following suggestions will prolong the lifetime of the solvent filter and will maintain the performance of the pump e Use a sterile if possible amber solvent bottle to slow down algae growth Filter solvents through filters or membranes that remove algae Exchange solvents every two days or refilter e If the application permits add 0 0001 0 001 M sodium azide to the solvent Place a layer of argon on top of your solvent Avoid exposing the solvent bottle to direct sunlight Never use the system without a solvent filter installed 1220 Infinity LC 1220 Infinity LC 6 Injection System Description Manual Injector 94 The Injection Seal 95 Injecting Sample 95 Needles 96 Autosampler 97 Sampling Sequence 98 Injection Sequence 99 Sampling Unit 101 Needle Drive 102 Analytical head 102 Injection Valve 103 104 Supported Trays for the Autosampler Choice of Vials and Caps 106 Transport Assembly 105 This chapter provides an overview of the operational principles of the injection systems manual injector and autosampler Ee Agilent Technologies 93 Injection System Description Manual Injector 94 The Agilent 1220 Infinity LC manual inj
118. epair work at the module can lead to personal injuries e g shock hazard when the module cover is opened and the instrument is connected to power gt Never perform any adjustment maintenance or repair of the module with the top cover removed and with the power cord plugged in gt The security lever at the power input socket prevents that the module cover is taken off when line power is still connected Never plug the power line back in when cover is removed Sharp metal edges Sharp edged parts of the equipment may cause injuries gt To prevent personal injury be careful when getting in contact with sharp metal areas 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 volume of substances should be reduced to the minimum required for the analysis gt Do not operate the instrument in an explosive atmosphere 240 1220 Infinity LC Maintenance 11 CAUTION Electronic boards and components are sensitive to electrostatic discharge ESD ESD can damage electronic boards and components gt Be sure to hold the board by the edges and do not to
119. er arm to its home position for better access and exchange of trays Park Arm Secures the gripper arm to the park position behind the sampling unit Before parking the gripper arm ensure there is no vial in the gripper Injector Steps Each movement of the sampling sequence can be done under manual control This is useful during troubleshooting where close observation of each of the sampling steps is required to confirm a specific failure mode or verify successful completion of a repair Each injector step command actually consists of a series of individual commands that move the autosampler components to predefined positions enabling the specific step to be done 150 1220 Infinity LC 1220 Infinity LC Table 33 Step Valve Bypass Plunger Home Needle Up Vial to Seat Needle into Sample Draw Needle Up Vial to Tray Needle into Seat Valve Mainpass Reset Injector step commands Action Switches injection valve to the bypass position Moves the plunger to the home position Lifts the needle arm to the upper position Moves the selected vial to the seat position Lowers the needle into the sample Metering device draws the defined injection volume Lifts the needle out of the vial Returns the selected vial to the tray position Lowers the needle arm into the seat Switches the injection valve to the mainpass position Resets the injector Test Functions and Calibrat
120. ervice representative Heater Power At Limit Error ID 1074 The available power of the heater reached either the upper or lower limit This event is sent only once per run The parameter determines which limit has been hit 0 means upper power limit hit excessive ambient temperature drop 1 means lower power limit hit excessive ambient temperature increase Probable cause Suggested actions 1 Excessive ambient temperature change Wait until temperature control equilibrates 1220 Infinity LC Error Information 10 Illegal Temperature Value from Sensor on Main Board Error ID 1071 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 Defective sensor or main board Please contact your Agilent service representative 2 Detector is exposed to illegal ambient Verify that the ambient conditions are within conditions the allowed range Illegal Temperature Value from Sensor at Air Inlet Error ID 1072 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 The temperature sensor is defect e Replace the cable to the main
121. es gt 1 MPa 10 bar User selectable based on mobile phase compressibility 1 0 12 5 solvents with pH lt 2 3 should not contain acids which attack stainless steel Low pressure binary mixing gradient capability using proprietary high speed proportioning valve 600 900 uL dependent on back pressure measured with water at 1 mL min water caffeine tracer 0 95 or 5 100 user selectable lt 0 2 RSD or lt 0 4 min SD whatever is greater at 1 mL min based on retention time at constant room temperature 21 2 Site Requirements and Specifications Performance Specifications Agilent 1220 Infinity LC Pump VL Table 4 Performance Specifications Agilent 1220 Infinity LC Pump VL Type Specification Hydraulic system Settable flow range Flow range Flow precision Flow accuracy Pressure Pressure pulsation Compressibility compensation Recommended pH range Gradient formation optional Composition Range Composition Precision Dual plunger in series pump with proprietary servo controlled variable stroke drive floating plungers and passive inlet valve 0 001 10 mL min in 0 001 mL min increments 0 2 10 mL min lt 0 07 RSD or lt 0 02 min SD whatever is greater based on retention time at constant room temperature 1 or 10 pL min whatever is greater Operating range 0 40 MPa 0 400 bar 0 5880 psi up to 5 mL min Operating range 0 20 MPa 0
122. eta line deviation is 0 00nm OK Cancel Help real te Calibration settings equal to measured ones No calibration necessary Figure 60 Wavelength Verification and Recalibration Wavelength calibration should be done e after maintenance of the flow cell e lamp exchange or e after a major repair like processor board or optical unit exchange see also Replacing the Module s Firmware on page 318 After calibration the holmium oxide test see Figure 57 on page 178 provides verification of wavelength accuracy at three additional wavelengths 185 9 Test Functions and Calibration Diagnosis Information on Agilent ChemStation The Agilent ChemStation provides certain information on various assemblies in the detector 1 Open the Diagnosis and change to detailed view 2 Click on the assembly of interest and select Update Variables Display Figure on page 187 shows an example Table 43 on page 186 lists the assemblies which provide detailed information Table 43 Diagnosis detailed information Assembly Details General Product number firmware revision manufacturing date of intsrument or if replaced of main board serial number accumulated on time spectrometer serial number Vis lamp Accumulated on time actual on time lamp switch on accumulated on time switches switch on voltage current lamp current lamp voltage current UV lamp Accumulated on time actual on time lamp ignitio
123. finition of the maximum limits need to be determined based on the specific operating conditions of the instrument The detector module provides a EMF counter for the lamp The counter increments with lamp use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded The counter can be reset to zero after the lamp is exchanged The detector provides the following EMF counters Deuterium lamp on time This counter shows the total burn time of the deuterium lamp in hours EMF counters for the diode array detector 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 maintenan
124. flowcell is taken Theoretically the spectrum should be flat however in practice noise is superimposed on the spectrum The amplitude of the noise is a measure of the optical and electronic performance This test is part of the detector self test only see Self test on page 167 Spectral Flatness Evaluation Limit is lt 0 002 AU Test Failed Probable cause Suggested actions 1 Old or non Agilent lamp Run the Intensity Test Exchange the lamp if old or defective 2 Defective DAM board Exchange the DAM board 3 Defective PDA optical unit Exchange the optical unit 1220 Infinity LC 179 9 Test Functions and Calibration ASTM Noise Test The ASTM noise test determines the detector noise over a period of 20 minutes The test is done with the flowcell removed so the test results are not influenced by solvent or pump effects On completion of the test the noise result is displayed automatically This test is part of the detector self test only see Self test on page 167 ASTM Noise Test Evaluation Limit is 0 02 mAU Test Failed Probable cause Suggested actions 1 Insufficient lamp warm up time Allow lamp to warm up for at least 1 hour 2 Old or non Agilent lamp Exchange the lamp 180 1220 Infinity LC Test Functions and Calibration 9 Cell Test 1220 Infinity LC The cell test measures the intensity of the deuterium and tungsten lamps over the full wavelength range 190 950 nm once with t
125. g 1220 Infinity LC Error ID 4032 The safety flap was not detected Before the needle moves down into the needle seat to inject sample the safety flap locks into position Next the gripper checks the safety flap by trying to move the safety flap away from the needle If the gripper is able to move beyond the safety flap position safety flap not in position the error message is generated Probable cause Suggested actions 1 Safety flap missing or broken Please contact your Agilent service representative 219 10 Error Information Valve to Bypass Failed Error ID 4014 4701 The injection valve failed to switch to the bypass position The switching of the injection valve is monitored by two microswitches on the valve assembly The switches detect the successful completion of the valve movement If the valve fails to reach the bypass position or if the microswitch does not close the error message is generated Probable cause Suggested actions 1 Defective injection valve Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative Valve to Mainpass Failed Error ID 4015 The injection valve failed to switch to the mainpass position The switching of the injection valve is monitored by two microswitches on the valve assembly The switches detect the successful completion of the valve movement If the valve fails to reach the mainpass position or if th
126. ganic solvent to one of the upper gradient valve port It is best to have the organic channel directly above the salt solution channel Regular flushing with water of all DCGV channels is recommended to remove all possible salt deposits in the valve ports Before operating the pump flush the vacuum degasser optional with at least two volumes 3 mL especially when the pump has been turned off for some time for example overnight and volatile solvent mixtures are used in the channels Prevent blocking of solvent inlet filters never use the pump without solvent inlet filter Growth of algae should be avoided Check the purge valve frit and column frit regularly A blocked purge valve frit can be identified by black or yellow layers on its surface or by a pressure greater than 10 bar when pumping distilled water at a rate of 5 mL min with an open purge valve When using the pump at low flow rates for example 0 2 mL min check all 1 16 inch fittings for any signs of leaks When exchanging the pump seals also exchange the purge valve frit When using buffer solutions flush the system with water before switching it off Check the pump plungers for scratches when changing the plunger seals Scratched plungers will lead to micro leaks and will decrease the lifetime of the seal After changing the plunger seals pressurize the system according to the wear in procedure 91 5 92 Solvent Delivery System Description Prev
127. he autosampler otherwise it lies somewhere in the rest of the flow path Test Part 2 In Part 2 of the test an empty vial is driven to the needle and the valve is switched from bypass to mainpass so that the pressure should drop dramatically The pressure drop is checked against a limit If the autosampler is identified as the source of the problem and the limit is not reached the problem lies in the needle needle loop or metering drive otherwise the problem lise in the needle seat or needle seat capillary If the autosampler is not the source of the problem the problem lies either in the pump typically the filter or frit or after the autosampler heater capillary or column If the pressure drop limit is not achieved the problem lies in the pump otherwise the problem occurs after the autosampler 1220 Infinity LC Test Functions and Calibration 9 Purge Pump 1220 Infinity LC Purge Pump Description The Purge Pump tool enables you to purge the pump with solvent at a specified flow rate for a specified time For multi channel pumps and pumps with solvent selection valve SSV you select the channels to purge each channel can be purged with different conditions You can select a flow rate between 1 and 5 mL min in steps of 1 mL min You can select a time from 1 2 3 5 7 10 and 15 minutes The G1361A Prep Pump has an automatic purge cycle there are no user configurable options Purging the Pump To pu
128. he flow cell installed and once with the flow cell removed The resulting intensity ratio is a measure of the amount of light absorbed by the flow cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell This test should be performed inititially with a new detector flow cell The values should be kept for later reference comparison Cell Test Evaluation The Agilent ChemStation calculates the intensity ratio automatically The intensity ratio typically between 0 5 and 0 7 for new standard flow cells and 0 1 to 0 3 for new mico and high pressure cells is dependent on the degree of contamination of the flow cell windows and on the type of flow cell used Figure 58 Cell Test Results report with no flow cell inserted This test can be used for the standard flow cells only The nano flow cells will give very low values due to their design 181 9 Test Functions and Calibration Test Failed low ratio value 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 Exchange the flow cell windows 182 1220 Infinity LC Test Functions and Calibration 9 Using the B
129. he flow cells are shown in Table 24 on page 133 and Table 25 on page 134 1220 Infinity LC Detector Description 8 Correction factors for VWD flow cells Table 24 Correction factors for Agilent VWD flow cells Flow cell type Cell Part number Path length Path length Correction volume nominal actual factor Standard flow cell 14 uL Standard flow 10mm 10 15 0 19 mm 10 10 15 cell 10 mm 14 uL 40 bar G1314 60086 Semi micro flow cell 5 uL Semi micro flow 6mm 6 10 0 19 mm 6 6 10 cell 6 mm 5 pL 40 bar G1314 60083 Micro flow cell 2 uL Micro flow cell 3mm 2 80 0 19 mm 3 2 8 without I D tag 3 mm 2 uL 120 bar G1314 60087 High Pressure flow cell 14 uL High pressure 10mm 10 00 0 19 mm 6 5 75 flow cell 10 mm 14 uL 400 bar G1314 60082 Be aware that there are additional tolerance of gasket thickness and its compression ratio which are considered to be very small in comparison with the machining tolerance 1220 Infinity LC 133 8 Detector Description Correction factors for DAD flow cells Table 25 Correction factors for flow cells Flow cell Path length actual Correction factor Standard flow cell 10 mm 13 pL 120 bar 12 MPa 9 80 0 07 mm 10 9 8 G1315 60022 Semi micro flow cell 6 mm 5 pL 120 bar 12 MPa 5 80 0 07 mm 6 5 8 G1315 60025 Micro flow cell 3 mm 2 uL 120 bar 12 MPa G1315 60024 3 00 0 05 mm 0 07 3 3 mm Semi nano flow cell kit 10 mm 500 nL 5 MPa G1315 68724
130. he needle in vial position is determined by counting the motor steps from the upper needle sensor position Analytical head The analytical head is driven by the stepper motor connected to the drive shaft by a toothed belt The drive nut on the spindle converts the circular movement of the spindle to linear motion The drive nut pushes the sapphire plunger against the tension of the spring into the analytical head The base of the plunger sits on the large bearing of the drive nut which ensures the plunger is always centered A ceramic ring guides the movement of the plunger in the analytical head The home position of the plunger is sensed by an infra red sensor on the sampling unit flex board while the sample volume is determined by counting the number of steps from the home position The backward movement of the plunger driven by the spring draws sample from the vial Table 20 Analytical head technical data Standard 100 pL Number of steps 15000 Volume resolution 7 nL motor step Maximum stroke 100 uL Pressure limit 600 bar Plunger material Sapphire 1220 Infinity LC Injection System Description 6 Injection Valve The two position 6 port injection valve is driven by a stepper motor Only five of the six ports are used port 3 is not used A lever slider mechanism transfers the movement of the stepper motor to the injection valve Two microswitches monitor switching of the valve bypass and mainpass end positions
131. he sensor fails to recognize the needle arm movement the error message is generated Probable cause Suggested actions 1 Needle installed incorrectly or wrong Ensure the correct needle type is used and needle type too long installed correctly 2 Defective or dirty position sensor Please contact your Agilent service representative 3 Defective motor Please contact your Agilent service representative 4 Sticking spindle assembly Please contact your Agilent service representative 5 Defective main board Please contact your Agilent service representative 218 1220 Infinity LC Error Information 10 Needle Up Failed Error ID 4017 The needle arm failed to move successfully from the seat or out of the vial to the upper position The upper position of the needle arm is monitored by a position sensor on the sampling unit flex board The sensor detects the successful completion of the needle movement to the upper position If the needle fails to reach the end point or if the sensor fails to recognize the needle arm movement the error message is generated Probable cause Suggested actions 1 Defective or dirty position sensor Please contact your Agilent service representative 2 Defective motor Please contact your Agilent service representative 3 Sticking spindle assembly Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative Safety Flap Missin
132. hed with IPA before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path will definitely cause the test to fail Ramp 1 After initialization plunger 2 is at the top of its stroke The test begins with plunger 1 delivering with a stroke length of 100 uL and a flow of 153 uL min The plunger sequence during the pressure ramp is 1 2 1 2 The pressure increase during this phase should be linear Pressure disturbances during this phase indicate larger leaks or defective pump components Plateau 1 Plunger 2 continues to pump with a flow rate of 2 uL min for approximately one minute The pressure during the plateau should remain constant or increase slightly A falling pressure indicates a leak of gt 2 uL min 139 9 140 Test Functions and Calibration Ramp 2 The flow is changed to 153 uL min and plunger 2 continues to deliver for the rest of its stroke Then plunger 1 continues to pump to complete the second half of the ramp Plateau 2 The flow is reduced to 2 uL min for approximately one minute plunger 1 still delivering The pressure during the plateau should remain constant or increase slightly A falling pressure indicates a leak of gt 2 uL min Ramp 3 The flow increases to 220 uL min and the stroke is changed to 100 uL Plunger 1 completes its stroke Next the flow is changed to 510 uL min The ramp reaches 390 bar with the plunger sequence 2 1 2 1 Plate
133. his chapter describes the tests calibrations and tools that are available with the Instrument Utilities software or the Lab Advisor 10 Error Information This chapter provides information on the error messages that might be displayed and gives the possible causes and suggestions on their solutions 11 Maintenance This chapter provides general information on maintenance of the instrument 12 Parts for Maintenance This chapter provides information on parts for maintenance 13 Upgrading the Agilent 1220 Infinity LC This chapter provides information for upgrading the LC system 14 Identifying Cables This chapter provides information on cables used with the Agilent 1200 Infinity Series modules 15 Appendix This chapter provides addition information on safety legal and web 1220 Infinity LC Contents 1220 Infinity LC Contents Introduction 9 Agilent 1220 Infinity LC Configurations 10 Agilent 1220 Infinity LC VL Configurations 11 Early Maintenance Feedback 12 Site Requirements and Specifications 15 Site Requirements 16 Physical Specifications 19 Performance Specifications 20 Installation 29 Unpacking Your System 30 Installing the Hardware 34 Connecting and Configuring the Instrument to the Chromatographic Data System 43 Connecting the Agilent 1220 Infinity LC tothe PC 44 The Instrument Utility LabAdvisor Software 46 Configuration of the Instrument After an Upgrade Installation 47 Priming the Sys
134. hould be flow cell windows done after repair Drying the leak sensor If leak has occurred Check for leaks 1220 Infinity LC 285 11 Maintenance Exchanging the Deuterium Lamp When If noise or drift exceeds application limits or lamp does not ignite Tools required Description Screwdriver Pozidriv 1 PT3 Parts required p n Description 1 G1314 60100 Deuterium lamp 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 1 Press the release buttons and remove the lower front 2 Unscrew the heater assembly and remove it cover to have access to the lamp area 286 1220 Infinity LC Maintenance 11 Variable Wavelength Detector VWD 3 Unscrew disconnect and replace the lamp Insert fix and 4 Replace the heater assembly reconnect the lamp Next Steps 5 6 7 8 9 Replace the front cover Reset the lamp counter as described in the Utilities software documentation Turn the lamp ON Give the lamp more than 10 min to warm up Perform Wavelength Calibration to check the correct positioning of the lamp 1220 Infinity LC 287 11 Maintenance Variable W 4 annth Datactar VIVID Wavelen gth Detector VVVD Exchanging a Flow Cell When Tools required Description Wrench 1 4 inch for capillary connections Preparations Turn the lamp OFF
135. ials into the vial tray at the positions to be verified Select the first vial position in the vial position menu Select Go to selected position 4 If the fingers of the gripper arm are aligned centrally above the vial select the Pick vial button to verify the gripper arm lifts the vial out of the tray correctly If there is a misalignment the gripper must be realigned 5 Select the Putvial button to verify the gripper replaces the vial correctly If there is a misalignment the gripper must be realigned 6 Repeat the procedure for the next vial position 154 1220 Infinity LC Test Functions and Calibration 9 Column Oven Oven Test Oven Test Description The Oven Test is used to evaluate the heating performance of the two Peltier elements The heating rate over a 10 K interval from the start temperature is determined The start temperature must be between 30 C and 50 C and is determined as follows e If the current oven temperature is below 30 C the oven tries to attain a temperature of 30 C 30 C is used as the start temperature e If the current oven temperature is above 30 C but below 50 C the current oven temperature is used as the start temperature If the current oven temperature is above 50 C an error message is displayed The oven must then be allowed to cool to below 50 C before the test can be run Oven Test Evaluation At the end of the Oven Test the slope of the temperature rise of
136. ice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met 1220 Infinity LC In This Book 1220 Infinity LC In This Book This manual covers the Agilent 1220 Infinity LC System configurations e G4286B e G4288B C e G4290B C e G4294B Introduction This chapter provides an overview of the Agilent 1220 Infinity LC available configurations Site Requirements and Specifications This chapter provides information on environmental requirements physical and performance specifications Installation This chapter provides an overview on shipment content and installation LAN Configuration This chapter provides information on connecting the instrument to the Agilent ChemStation PC Solvent Delivery System Description This chapter provides an overview on the operational principles of the solvent delivery system pump and optional degasser Injection System Description This chapter provides an overview of the operational principles of the injection systems manual injector and autosampler In This Book 7 Column Oven Description This chapter provides an overview of the operational principles of the column oven 8 Detector Description This chapter provides an overview of the operational principles of the detector 9 Test Functions and Calibration T
137. imized 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 under operating conditions the radio interference limits are still met within the premises 1220 Infinity LC 367 15 Appendix UV Radiation 368 Emissions of ultraviolet radiation 200 315 nm from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs Threshold Limit Values according to the American Conference of Governmental Industrial Hygienists Table 49 UV radiation limits Exposure day Effective irradiance 8h 0 1 uW cm 2 10 min 5 0 W cm Typically the radiation values are much smaller than these limits Table 50 UV radiation typical values Position Effective irradiance Lamp installed 50 cm distance average 0 016 W cm Lamp installed 50 cm distance maximum 0 14 pW cm2 1220 Infinity LC Appendix 15 Sound Emission 1220 Infinity LC 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 N
138. ing in higher noise levels Since the detector is the last module in the flow path this problem is less common 316 1220 Infinity LC Maintenance 11 Symptoms observed with the Agilent 1220 Infinity LC In contrast to other HPLC systems such as HP 1090 and HP 1050 Series which use helium degassing algae have a better chance to grow in systems such as the Agilent 1220 Infinity LC where helium is not used for degassing most algae need oxygen and light for growth The presence of algae in the Agilent 1220 Infinity LC can cause the following to occur Blockage of PTFE frits pack of 5 01018 22707 purge valve assembly and column filter causing increased system pressure Algae appear as white or yellowish white deposits on filters Typically black particles from the normal wear of the piston seals do not cause the PTFE frits to block over short term use Short lifetime of solvent filters bottle head assembly A blocked solvent filter in the bottle especially when only partly blocked is more difficult to identify and may show up as problems with gradient performance intermittent pressure fluctuations etc Algae growth may also be the possible source of failures of the ball valves and other components in the flow path Preventing and or reducing the algae problem 1220 Infinity LC Always use freshly prepared solvents especially use demineralized water that has been filtered through about 0 2 um filters Never leave m
139. inity LC Configurations Available configurations of Agilent 1220 Infinity LC The Agilent 1220 Infinity LC is available in four different configurations Possible components include isocratic pump dual channel gradient pump with degasser manual injector autosampler column oven and detector Each configuration comes with at least one pump one injection system and one detector and includes Agilent Instrument Utilities Software Isocratic pump Gradient pump Gradient pump Manual injector Manual injector Autosampler Column oven Variable Variable Variable wavelength wavelength wavelength detector detector detector G4286B G4288B G4290B 10 Gradient pump Autosampler Column oven Diode array detector G4294B A Solvent Selection Valve SSV Upgrade Kit G4280 68708 is available 1220 Infinity LC Introduction 1 Agilent 1220 Infinity LC VL Configurations Available configurations of Agilent 1220 Infinity LC VL The Agilent 1220 Infinity LC VL is available in two different configurations Possible components include isocratic pump dual channel gradient pump with degasser manual injector autosampler column oven and detector Each configuration comes with at least one pump one injection system and one detector and includes Agilent Instrument Utilities Software Gradient Pump Gradient Pump Manual Injector Autosampler Column Oven Variable Variable Wavelength Wavelength Detec
140. intenance 12 Detector Figure 75 Standard Flow Cell Parts NOTE Gaskets 6 and 7 have different hole diameters window screw spring washers compression washer window holder quartz window Gasket OoOPwnN 1 2 3 4 56 Figure 76 Orientation of Spring Washers 1220 Infinity LC 345 12 Parts for Maintenance Detector Lamps p n Description 2140 0820 Longlife Deuterium lamp C with black cover and RFID tag G1103 60001 Tungsten lamp 346 1220 Infinity LC a 1220 Infinity LC amp a e ee 13 7 e Upgrading the Agilent 1220 Infinity LC amp J Oven Upgrade 348 This chapter provides information for upgrading the LC system ea Agilent Technologies 347 13 Upgrading the Agilent 1220 Infinity LC Oven Upgrade Parts required Software required 348 p n Description G4297A 1220 Infinity Oven Kit LabAdvisor Software a A O N Switch off the instrument Remove the lower front cover Disconnect the column and remove it Remove the leak tube Press the knurled portion at either side of the column tray inwards and remove the column tray 6 Unpack the oven upgrade kit and separate the two parts Click the oven into position in place of the column tray The electrical connection to the oven is made automatically 8 Replace the leak tube Click the oven insulation into place in the lower front cover with the cutout in the oven insulat
141. ion 9 Comments Command also switches the valve to bypass if it is not already in that position Command also lifts the needle to the upper position Command also positions the vial at the seat and lifts the needle to the upper position Command also positions the vial at the seat lifts the needle and lowers the needle into vial Command can be done more than once maximum draw volume of 100 uL cannot be exceeded Use Plunger Home to reset the metering device Command also switches the valve to bypass if it is not already in that position Command also lifts the needle to the upper position Command also returns the vial to the tray position 151 9 152 Test Functions and Calibration Alignment Teaching ALS Alignment Teaching Description The Alignment Teaching tool is required to compensate for small deviations in positioning of the autosampler gripper that may occur after the module has been disassembled for repair It requires that a 100 vial tray be inserted into the autosampler The alignment procedure uses two tray positions as reference points because the tray is rectangular a two point alignment is sufficient to correct all other vial positions on the tray When the correction calculation is complete the values for both X and theta are rounded to one decimal place On completion of the alignment procedure the corrected gripper positions are stored in the module s firmware To ensure correct ope
142. ion support at the bottom 10 Replace the column and reconnect the capillaries 11 Replace the lower front cover 12 Start the LabAdvisor Software and connect your Instrument open Instrument Controls and then open Conversions on any of the sub modules and click Add Oven The hardware configuration change will be finalized with the next power cycle 13 Power cycle the instrument and start your Chromatographic Data System Use Auto configure and the instrument now should be registered under its new main assembly number 1220 Infinity LC 1220 Infinity LC 14 Identifying Cables Cable Overview 350 352 Remote Cables 354 BCD Cables 357 CAN LAN Cables 359 Agilent 1200 module to PC 360 Analog Cables This chapter provides information on cables used with the Agilent 1200 Infinity Series modules Apg Agilent Technologies 349 14 Identifying Cables Cable Overview 350 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 35900 60750 35900 60750 01046 60105 Remote cables p n 03394 60600 03396 61010 5061 3378 01046 60201 BCD cables p n 03396 60560 G1351 81600 Description Agilent module to 3394 6 integrators Agilent 35900A A D converter Analog cable BNC to general purpose spade lugs Description Agilent module to 3396A Series integrators 3396 Series II 3395A i
143. issing 206 pressure too high check 145 pressure operatingrange 21 22 pressure 82 preventive maintenance 239 programmable slit width 26 proportioning valve high speed 82 PTFE frit 250 pump configuration 206 pump failure 316 pump head missing 207 pump head reinstalling 259 pump piston 91 pump overview 82 pump functional principle 84 hints for successful use 91 urge pump 147 urge valve frit 91 o SS purge valve 250 1220 Infinity LC radio interference 367 reassembling the pump head 259 recommended pH range 21 22 reference conditions 25 remote cable 354 repair procedures injection seal 264 repairs cleaning the instrument 296 correction leaks 314 metering plunger 2 9 metering seal 279 needle assembly 269 needle seat assembly 273 overview of simple repairs 285 replacing firmware 318 318 replacing leak handling system 315 rotorseal 275 reset 101 response time peak width 117 restart without cover 207 RFIDtag 114 rotor seal exchange 2 5 RS 232C cable 360 run recovery no run data available in 234 running the leak test 141 S safety class 362 safety features system 20 safety general information 362 standards 19 Index symbols 364 sample and reference wavelength 119 sample loops 94 sample scan 166 sample trays 105 numbering of vial positions 105 sample volume 95 sampling sequence 98 sampling unit 101 sapphire piston 84 84 scan 166 seal wear counters 12 selectivity
144. iston is moved to the mechanical stop After reaching the mechanical stop the piston reverses direction until the encoder index position is reached If the index position is reached too fast the error message is generated Probable cause Suggested actions 1 Irregular or sticking drive movement Remove the pump head and examine the seals pistons and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Please contact your Agilent service representative Index Missing Error ID 2205 2215 2505 The encoder index position in the module was not found during initialization During initialization the first piston is moved to the mechanical stop After reaching the mechanical stop the piston reverses direction until the encoder index position is reached If the index position is not recognized within a defined time the error message is generated Probable cause Suggested actions 1 Disconnected or defective encoder cable Please contact your Agilent service representative 2 Defective pump drive assembly Please contact your Agilent service representative 1220 Infinity LC Error Information 10 Initialization Failed Error ID 2207 2217 The module failed to initialize successfully within the maximum time window A maximum time is assigned for the complete pump initialization cycle If the time is exceeded before initialization is complete
145. klist 239 Cautions and Warnings 240 Solvent Delivery System 242 Manual Injector 263 Autosampler 267 Variable Wavelength Detector VWD 285 Diode Array Detector DAD 295 Algae Growth in HPLC Systems 316 Replacing the Module s Firmware 318 12 Parts for Maintenance 319 1220 Infinity LC System 320 Solvent Delivery System 322 Injection System 331 Column Oven 339 Detector 340 13 Upgrading the Agilent 1220 Infinity LC 347 Oven Upgrade 348 1220 Infinity LC Contents 14 Identifying Cables 349 Cable Overview 350 Analog Cables 352 Remote Cables 354 BCD Cables 357 CAN LAN Cables 359 Agilent 1200 module to PC 360 15 Appendix 361 General Safety Information 362 Solvent Information 365 Radio Interference 367 UV Radiation 368 Sound Emission 369 Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC 370 Declaration of Conformity for HOX2 Filter 371 Agilent Technologies on Internet 372 8 1220 Infinity LC 1220 Infinity LC e ee 1 r Introduction Agilent 1220 Infinity LC Configurations 10 Agilent 1220 Infinity LC VL Configurations 11 Early Maintenance Feedback 12 EMF counters for the pump 12 EMF counters for the autosampler 13 EMF counters for the variable wavelength detector 14 EMF counters for the diode array detector 14 This chapter provides an overview of the Agilent 1220 Infinity LC available configurations Apg Agilent Technologies 1 introduction Agilent 1220 Inf
146. l components with alcohol and achromat windows lint free cloth or replace the parts 4 Old or non Agilent lamp Exchange the lamp If the lamp fails in a single range there might be no reason to change the lamp if the application is not run in that specific range Redo the test with removed flow cell If the counts increase drastically more than a factor of 2 then flow cell components are contaminated and may require maintenance service If the intervals of lamp replacements are getting shorter the Agilent service should check the optical unit for contaminated components in the light path coupling lens source lens cell support assembly and flow cell windows 1220 Infinity LC Test Functions and Calibration 9 Holmium Oxide Test The holmium oxide test uses three characteristic absorbance maxima of the built in holmium oxide filter to verify wavelength accuracy see also Wavelength Verification and Recalibration on page 185 When the test is started the 1 nm slit is moved into the light path automatically To eliminate effects due to absorbing solvents the test should be done with water in the flow cell See also Declaration of Conformity for HOX2 Filter on page 371 Holmium Oxide Test Evaluation Limits 361 0 nm 360 0 362 0 nm 1nm 453 7 nm 452 7 454 7 nm 1nm 536 7 nm 535 7 537 7 nm Inm The test is evaluated by the instrument and the measured maxima are displayed automatically The te
147. lays current LAN settings ip lt X X X xX gt sets new ip address sm lt X X X X gt sets new subnet mask gw lt X X X x gt sets new default gateway exit exits shell and saves all changes 4 To change a parameter follows the style parameter value for example ip 134 40 27 230 Then press Enter where parameter refers to the configuration parameter you are defining and value refers to the definitions you are assigning to that parameter Each parameter entry is followed by a carriage return 1220 Infinity LC 77 4 LAN Configuration 5 Use the and press Enter to list the current settings SACL EE eee information about the LAN interface 7 MAC address initialization mode LAN Status Page Initialization mode is Using Stored active TCP IP settings TCP IP status here ready Init Mode Using Stored connected to PC with controller software e g Agilent ChemStation here not connected MAC Addre 6636D36AG838 TCP IP Properties active IP Address gt 134 40 27 95 Subnet Mask gt 255 255 248 0 Gateway 134 40 24 1 Controllers no connections Figure 26 Telnet Current settings in Using Stored mode 6 Change the IP address in this example 134 40 27 99 and type to list current settings AWINDOWS system32 cmd_exe telnet 134 40 27 95 STEER CLT change of IP setting to gt 4 Initialization mode is Using Stored LAN Status Page active TCP IP settings MAC Addre 838D38
148. length Verification Calibration on page 164 11 Replace the lower front cover 1220 Infinity LC 291 11 Maintenance Using the Cuvette Holder This cuvette holder can be placed instead of a flow cell in the variable wavelength detector Standard cuvettes with standards in it for example National Institute of Standards amp Technology NIST holmium oxide solution standard can be fixed in it This can be used for wavelength verifications When Tools required Description None Parts required p n Description G1314 60200 Cuvette Holder Cuvette with the Preparations Remove the normal flow cell Have cuvette with standard available If your own standard should be used to checkout the instrument standard e g NIST certified holmium oxide sample 1 Locate the cuvette holder on the desk 2 Unscrew the bracket 292 1220 Infinity LC 11 Maintenance 3 Insert the cuvette with the sample into the holder The clear side of the cuvette must be visible Light path Clear side 8 Replace the bracket and fix the cuvette 4 Reset the lamp counter as described in the user interface 5 Turn the lamp ON 7 Perform Wavelength Verification Calibration to check documentation Give the lamp more than 10 min to warm up the correct positioning of the lamp Next Steps 9 Install the cuvette holder in the instrument 10 Perform your verification 1
149. length calibration 164 theta axis 104 timeout 200 transport assembly 104 transport mechanism 97 troubleshooting error messages 194 U URL 372 using the cuvette holder 292 UVlampon 166 UV radiation 368 V vacuum degasser 91 valve bypass 151 valve failed 210 valve frit 250 valve mainpass 151 valve proportioning 82 variable entrance slit 116 variable reluctance motor 84 variable stroke volume 90 verification and recalibration of wavelength 185 vial contents temperature 23 vial numbering 105 vial racks 97 vialto seat 151 vial to tray 151 vials 97 106 voltage range 19 VWD EMF counters 14 Ww wait timeout 212 waste electrical and electronic equipment 370 wavelength recalibration lost 233 wavelength accuracy 24 26 calibration 164 range 190 600nm 24 range 26 verification and recalibration 185 WEEE directive 370 weight 19 X X axis 104 Z Z axis 104 1220 Infinity LC Index 1220 Infinity LC 379 www agilent com In This Book This manual contains information on how to use maintain repair and upgrade the Agilent 1220 Compact LC System The manual contains the following chapters e Introduction e Installation Agilent 1220 Infinity LC Description e Test Functions and Calibration e Error Information Maintenance and Repair e Parts for Maintenance and Repair e Upgrading the Agilent 1220 Infinity LC Appendix Agilent Technologies 2010 2014 2015 Printed in Germany 02 2015 G4280 900
150. lent 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 Next The default location for installation is C Program Files Agilent BootPService 10 Click Install to begin installation 1220 Infinity LC LAN Configuration 4 11 Files load when finished the BootP Settings screen appears BootP Settings a BootP Tab File Create Tab File Edit BootP Addresses Logging BootP Log File E Default Settings Subnet mask GO 0 00 Gateway GO 0 0 0 Cancel Help Figure 17 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 192 168 254 11 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 BootP Service in the Windows services On the Windows desktop click right on Computer icon select Manage gt Services and Applications gt Services
151. lex board Please contact your Agilent service representative 3 Defective transport assembly flex board Please contact your Agilent service representative 4 Defective sampling unit motor Please contact your Agilent service representative 5 Defective main board Please contact your Agilent service representative Initialization with Vial Error ID 4028 The autosampler attempted to initialize with a vial still in the gripper During initialization the autosampler checks correct operation of the gripper by closing and opening the gripper fingers while monitoring the motor encoder If a vial is still in the gripper when initialization is started the gripper fingers cannot close causing the error message to be generated Probable cause Suggested actions 1 Vial still in gripper Remove the vial using the Release Vial function in the user interface Reinitialize the autosampler 1220 Infinity LC Error Information 10 Invalid Vial Position Error ID 4042 The vial position defined in the method or sequence does not exist The reflection sensors on the transport assembly flex board are used to automatically check which sample trays are installed coding on tray If the vial position does not exist in the current sample tray configuration the error message is generated Probable cause Suggested actions 1 Incorrect tray or trays installed Install the correct trays or edit the method or sequence accordingly 2 Incorrec
152. libration Evaluating the Leak Test Results Defective or leaky components in the pump head lead to changes in the leak test pressure plot Typical failure modes are described below Please notice the difference between an error in the test and a failure of the test An error means that during the operation of the test there was an abnormal termination If a test failed this means that the results of the test were not within the specified limits Often it is only a damaged blank nut itself poorly shaped from overtightening that causes a failure of the test Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly tightened Table 26 No Pressure increase at Ramp 1 Potential Cause Pump not running Purge valve open Loose or leaky fittings Wrong solvent line connections Contaminated purge valve Large leaks visible at the pump seals Large leaks visible at active inlet valve outlet valve or purge valve Corrective Action Check the logbook for error messages Close the purge valve and restart the test Ensure all fittings are tight or exchange capillary Ensure the solvent lines from the degasser are connected correctly Open and close purge valve to flush out contamination Exchange the valve if still leaky Exchange the pump seals Ensure the leaky components are installed tightly Exchange the component if required
153. limit is exceeded the EMF flag in the user interface is displayed 1220 Infinity LC Introduction 1 EMF counters for the autosampler 1220 Infinity LC The user settable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements The wear of autosampler components is dependent on the analytical conditions Therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument The autosampler provides two EMF counters Each counter increments with autosampler use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded Each counter can be reset to zero after maintenance has been done The autosampler provides the following EMF counters Injection valve counter This counter display the total number of switches of the injection valve since the last reset of the counter Needle movements counter This counter displays the total number of movements of the needle into the seat since the last reset of the counter 13 1 14 EMF counters for the variable wavelength detector The user settable EMF limits for the EMF counter enables the early maintenance feedback to be adapted to specific user requirements The useful lamp burn time is dependent on the requirements for the analysis high or low sensitivity analysis wavelength and so on Therefore the de
154. 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 2 Uncheck the Do you want to log BootP requests once all instruments have been added 69 4 70 LAN Configuration 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 Add BootP Entry Se xj Mac Address Host Name IP Address Figure 19 Enable BootP logging 5 Make these entries for the instrument MAC address Host name Enter a Hostname of your choice The Host Name must begin with alpha characters i e LC1260 IP address Comment optional Subnet mask Gateway address optional The configuration information entered is saved in the Tab File 6 Click OK 1220 Infinity LC LAN Configuration 4 7 Leave Edit BootP Addresses by pressing Close 8 Exit BootP Settings by pressing OK 9 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 Servi
155. ly tested using a minimum of 15000 injections with the Agilent 1220 Infinity LC autosampler Crimp top vials p n Description 5181 3375 Crimp Top Vial 2 mL clear glass 100 Pack 5183 4491 Crimp Top Vial 2 mL clear glass 1000 Pack 5182 0543 Crimp Top Vial 2 mL clear glass write on spot 100 Pack 5183 4492 Crimp Top Vial 2 mL clear glass write on spot 1000 Pack 5183 4494 Crimp Top Vial 2 mL clear glass write on spot 100 Pack silanized 5181 3376 Crimp Top Vial 2 mL amber glass write on spot 100 Pack 5183 4493 Crimp Top Vial 2 mL amber glass write on spot 1000 Pack 5183 4495 Crimp Top Vial 2 mL amber glass write on spot 100 Pack silanized 5182 0567 Crimp Top Vial 1 mL polypropylene wide opening 100 Pack 5183 4496 Crimp Top Vial 1 mL polypropylene wide opening 100 Pack silanized 9301 0978 crimp top vial 0 3 mL polypropylene wide opening 1000 pack 106 1220 Infinity LC Snap top vials p n 5182 0544 5183 4504 5183 4507 5182 0546 5183 4505 5183 4508 5182 0545 5183 4506 5183 4509 Screw top vials p n 5182 0714 5183 2067 5183 2070 5182 0715 5183 2068 5183 2071 5182 0716 5183 2069 5183 2072 1220 Infinity LC Injection System Description 6 Description Snap Top Vial 2 mL clear glass 100 Pack Snap Top Vial 2 mL clear glass 1000 Pack Snap Top Vial 2 mL clear glass 100 Pack silanized Snap Top Vial 2 mL clear glass write on spot 100 Pack Snap Top Vial
156. m eek DAD Signals System 2 s f fpo fero fe fo 230 fie foso w Ea DEC fis fso An m fs fs o fie faso fo fm 3 a Every 2nd spectrum ER feo Threshold mal 1220 Infinity LC Detector Description 8 Table 23 Spectrum Settings Store None Apex Baselines Apex Slopes Baselines All in Peak Every 2nd spectrum All Range Step Threshold Defines at which points on signal A spectra will be taken and saved Signal A is used to control the peak controlled spectra acquisition the other signals have no influence on spectra acquisition No spectra are taken Spectra are taken at the apex and baselines of the peak Spectra are taken at the apex baselines upslope and downslope of the peak All spectra within the peak are taken The three spectra acquisition types mentioned above are also referred to as peak controlled spectra acquisition The peak detection is done by the detector firmware based on the threshold and peakwidth parameters you set for the DAD If you want to use peak controlled spectra storage make sure that you set these parameters to recognize all the peaks of interest The integration algorithm also includes peak detection based on the threshold and peakwidth parameters set in the integration events Spectra are taken continuously as for All but only every second spectrum is stored other spectra are discarded This r
157. maintenance with e Deuterium lamp for highest intensity and lowest detection limit over a wavelength range of 190 600 nm Optional flow cell cartridges standard 10 mm14 uL high pressure 10 mm14 uL micro 3 mm2 uL semi micro 6 mm5 uL are available and can be used depending on the application needs Easy front access to lamp and flow cell for fast replacement and e Built in holmium oxide filter for fast wavelength accuracy verification 1220 Infinity LC 113 8 Detector Description Agilent 1220 Infinity LC Diode Array Detector DAD Introduction to the Detector The detector is designed for highest optical performance GLP compliance and easy maintenance It includes the following features 80 Hz data acquisition rate for ultra fast LC applications RFID tags for all flow cells and UV lamps provides traceable information about these assemblies Long life deuterium with RFID tag and tungsten lamps for highest intensity and lowest detection limit over a wavelength range of 190 950 nm No loss in sensitivity for up to eight wavelengths simultaneous Programmable slit from 1 16 nm for complete optimization of sensitivity linearity and spectral resolution Optional flow cell cartridges with RFID tag standard 10 mm13 uL semi micro 6 mm5 uL micro 3 mm2 uL 80 nL 500 nL 10 mm high pressure 10 mm1 7 uL and prep cells are available and can be used depending on the application needs Easy front access to la
158. mechanism and sampling unit are driven by motors Movement is monitored by optical sensors and optical encoders to ensure correct operation The metering device is always flushed after injection to ensure minimum carry over The six port injection valve unit only 5 ports are used is driven by a high speed hybrid stepper motor During the sampling sequence the valve unit bypasses the autosampler and directly connects the flow from the pump to the column During injection and analysis the valve unit directs the flow through the autosamplers which ensures that the sample is injected completely into the column and that any sample residue is removed from the metering unit and needle from before the next sampling sequence begins 97 98 Injection System Description Sampling Sequence The movements of the autosampler components during the sampling sequence are monitored continuously by the processor The processor defines specific time windows and mechanical ranges for each movement If a specific step of the sampling sequence can t be completed successfully an error message is generated Solvent is bypassed from the autosamplers by the injection valve during the sampling sequence The sample vial is selected by a gripper arm from a static sample rack The gripper arm places the sample vial below the injection needle The required volume of sample is drawn into the sample loop by the metering device Sample is applied to the column when
159. module is possible TCP IP parameters set by any method the parameters may be altered by opening a Telnet session 1 2 Open the system DOS prompt window by clicking on Windows START button and select Run Type cmd and press OK Type the following at the system DOS prompt c gt telnet lt IP address gt or c gt telnet lt host name gt E C AWINDOWS system32 cmd exe C gt telnet 134 46 27 95 Figure 23 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 Switches on page 55 When the connection was established successfully the module responds with the following ET C AWINDOWS system32 cmd exe telnet 134 40 27 95 Agilent Technologies G1i315C PP 8000624 Figure 24 A connection to the module is made 1220 Infinity LC LAN Configuration 4 3 Type and press enter to see the available commands WINDOWS system32 cmd_exe telnet 134 40 27 95 Agilent Technologies G1315C PP 8880624 gt command syntax description display help info display current LAN settings ip lt x x x x gt set IP Address sm X X X X gt set Subnet Mask gu lt x x x x gt set Default Gateway exit exit shell gt Figure 25 Telnet Commands Table 16 Telnet Commands Value Description displays syntax and descriptions of commands disp
160. mple or reference diodes or ADC circuits which may cause non linearity or excessive baseline noise During the test the lamp is switched off Next the leakage current from both diodes is measured The test evaluates the results automatically Evaluating the VWD Dark Current Test Table 35 Limits Sample circuit lt 7900 counts Reference circuit lt 7900 counts Probable causes of test failure Table 36 Sample circuit noise exceeds limit Cause Corrective action Defective sample diode Exchange the sample diode Defective sample ADC board Exchange the sample ADC board Table 37 Reference circuit noise exceeds limit Cause Corrective action Defective reference diode Exchange the reference diode Defective reference ADC board Exchange the reference ADC board 158 1220 Infinity LC Test Functions and Calibration Holmium Oxide Test 1220 Infinity LC VWD Holmium Oxide Test Description The Holmium Oxide Test uses three characteristic absorbance maxima of the built in holmium oxide filter to verify wavelength accuracy see also Wavelength Calibration The test evaluates the results automatically and provides a spectrum of the holmium oxide filter To eliminate effects due to absorbing solvents the test should be done with water in the flow cell On completion of the test the results are displayed automatically Holmium Oxide Test Report VWD Holmium Spectrum Absorbance AU I M lin
161. mpler 267 Introduction 267 Exchanging the Needle Assembly 269 Exchanging the Needle Seat Assembly 273 Exchanging the Rotor Seal 275 Exchanging the Metering Seal 279 Exchanging the Gripper Arm 283 Variable Wavelength Detector VWD 285 Introduction 285 Exchanging the Deuterium Lamp 286 Exchanging a Flow Cell 288 oh Agilent Technologies 237 11 Maintenance Repairing the Flow Cell 290 Using the Cuvette Holder 292 Correcting Leaks 294 Diode Array Detector DAD 295 Overview of Maintenance 295 Cleaning the Module 296 Exchanging a Lamp 297 Exchanging a Flow Cell 300 Maintenance of the Flow Cell 303 Replacing Capillaries on a Standard Flow Cell 306 Cleaning or Exchanging the Holmium Oxide Filter 311 Correcting Leaks 314 Replacing Leak Handling System Parts 315 Algae Growth in HPLC Systems 316 Replacing the Module s Firmware 318 This chapter provides general information on maintenance of the instrument 238 1220 Infinity LC Maintenance 11 PM Scope of Work and Checklist Preventive Maintenance Scope of Work and Checklist To perform a preventive maintenance PM follow the PM Scope of Work and PM Checklist step by step The PM Scope of Work and PM Checklist documents can be found in the on the DVD for the Lab Advisor Software 1220 Infinity LC 239 11 Maintenance Cautions and Warnings Module is partially energized when switched off as long as the power cord is plugged in Risk of stroke and other personal injury R
162. mps and flow cell for fast replacement Built in holmium oxide filter for fast wavelength accuracy verification Built in temperature control for improved baseline stability Additional diagnostic signals for temperature and lamp voltage monitoring For specifications see Performance Specifications Agilent 1220 Infinity LC DAD on page 26 114 1220 Infinity LC Detector Description 8 Optical System The optical system of the detector is shown in Figure below Its illumination source is a combination of a deuterium arc discharge lamp for the ultraviolet UV wavelength range and a tungsten lamp for the visible VIS and short wave near infrared SWNIR wavelength range The image of the filament of the tungsten lamp is focused on the discharge aperture of the deuterium lamp by means of a special rear access lamp design which allows both light sources to be optically combined and share a common axis to the source lens The achromat source lens forms a single focused beam of light through the flow cell Each cell room and lamp are separated by a quartz window which can be cleaned or replaced In the spectrograph light is being dispersed onto the diode array by a holographic grating This allows simultaneous access to all wavelength information Cell support window Tungsten lamp Coupling lens Deuterium lamp Achromat source lens Holmium oxide filter Flow cell Spectro lens Slit Grating
163. n its box and allow it to warm slowly to room temperature to avoid condensation 18 1220 Infinity LC Site Requirements and Specifications 2 Physical Specifications Table 1 Physical Specifications Type Specification Comments Weight 30 kg 66 Ibs G4294B 43 kg 94 Ibs Dimensions height x width 640 x 370 x 420 mm 25 2 x 14 6 x 16 5 x depth inches G4294B 640x370x485 mm 25 2x14 6x19 1 inches Line voltage 100 240 V 10 Wide ranging capability Line frequency 50 or 60 Hz 5 Power consumption 240 VA 210 W 717 BTU Maximum Ambient operating 4 55 C 39 131 F temperature Ambient non operating 40 70 C 40 158 F temperature Humidity lt 95 r h at 40 C 104 F Non condensing Operating altitude Up to 2000 m 6562 ft Non operating altitude Up to 4600 m 15092 ft For storing the module Safety standards IEC CSA Installation category Il Pollution degree2 For indoor use only UL 1220 Infinity LC 19 2 Performance Specifications 20 Site Requirements and Specifications Performance Specifications Agilent 1220 Infinity LC Table 2 Performance Specifications Agilent 1220 Infinity LC Type Specification Safety features Control and data evaluation Communications GLP features Extensive diagnostics error detection and display leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintena
164. n the documentation Module Specific Information There is no specific information for this module 1220 Infinity LC R 1220 Infinity LC e a e r a ee 12 90 e Parts for Maintenance amp o 1220 Infinity LC System 320 System Parts 320 Fuses 321 Solvent Delivery System 322 Injection System 331 Manual Injector 331 Autosampler 333 Column Oven 339 Detector 340 Variable Wavelength Detector VWD 340 Diode Array Detector DAD 344 This chapter provides information on parts for maintenance ea Agilent Technologies 319 12 Parts for Maintenance 1220 Infinity LC System System Parts System part numbers p n 0950 4997 G4280 65050 G4280 68723 G4280 60102 G4280 60001 G4280 65001 G4280 65802 5067 5378 G4280 68708 G4280 80004 8121 1833 G4280 81602 G4280 81620 G4280 40007 G4280 40016 G4280 44013 G4280 44500 G4280 44501 G4280 44502 G4280 44016 5061 3356 320 Description Power supply Agilent 1220 Infinity LC main board Cabinet kit Front door top Front door bottom Power switch board FSL board Status LED board Connecting tube DCGV to PIV SSV Fan Power Switch Cable Cable status LED Temp Sensor Cable Light pipe status Power Switch Coupler ZL Leak plane man inj Leak panel bottom Leak plane pump Leak plane ALS Holder temp sensor Leak sensor 1220 Infinity LC Fuses 1220 Infinity LC Parts for Maintenance 12 5 mainboard fu
165. nance 11 2 Disconnect the inlet and outlet capillaries 3 Unscrew the thumb screws in parallel and remove the flow cell 4 Disassembling the flow cell a Unscrew the cell screw using a 4 mm hexagonal wrench b Remove the SST rings using a pair of tweezers c Use adhesive tape to remove the PEEK ring the window and the gasket d Repeat step 1 on page 290 through step 3 on page 291 for the other window Keep the parts separate otherwise they could get mixed up 5 Cleaning the flow cell parts a Pour isopropanol into the cell hole and wipe clean with a piece of lint free cloth b Clean the windows with ethanol or methanol Dry with a piece of lint free cloth 6 Reassembling the flow cell a Hold the flow cell cassette horizontal and place the gasket in position Ensure that both cell holes can be seen through the holes of gasket Always use new gaskets b Place the the window on gasket c Place the PEEK ring on the window d Insert the conical springs Make sure that the conical springs point towards the window otherwise the window might break when the cell screw is tightened e Screw the cell screw into the flow cell and tighten it 7 Repeat the procedure for the other side of the cell 8 Reconnect the inlet and outlet capillaries 9 Test the flow cell for leaks If there are no leaks insert the flow cell into the detector 10 Perform Wavelength Calibration to check the correct positioning of the flow cell Wave
166. nce areas Agilent EZChrom Compact Agilent ChemStation Agilent Instrument Utilities Agilent Lab Advisor Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN Early maintenance feedback EMF electronic records of maintenance and errors 1220 Infinity LC 1220 Infinity LC Table 3 Site Requirements and Specifications 2 Performance Specifications Agilent 1220 Infinity LC Pump Performance Specifications Agilent 1220 Infinity LC Pump Type Specification Hydraulic system Settable flow range Flow range Flow precision Flow accuracy Pressure Pressure pulsation Compressibility compensation Recommended pH range Gradient formation optional Delay volume Composition range Composition precision Dual plunger in series pump with proprietary servo controlled variable stroke drive floating plungers and passive inlet valve 0 001 10 mL min in 0 001 mL min increments 0 2 10 0 mL min lt 0 07 RSD or lt 0 02 min SD whatever is greater based on retention time at constant room temperature 1 or 10 pL min whatever is greater degassed H30 80 100 bar 1 mL min at constant ambient temperature Operating range 0 60 MPa 0 600 bar 0 8820 psi up to 5 mL min Operating range 0 20 MPa 0 200 bar 0 2950 psi up to 10 mL min lt 2 amplitude typically lt 1 3 at 1 mL min isopropanol at all pressur
167. nfinity LC Parts for Maintenance 12 Detector Optical Unit and Fan Assembly p n Description G1314 60061 Complete optical unit assembly G4280 80004 Fan G1314 60113 Heater Assembly G1314 67000 Heater Interface Board Kit includes 4 rivets G1314 65802 VWD temp sensor board NOTE Repairs to the optical unit require specialist knowledge 1220 Infinity LC 343 12 Parts for Maintenance Diode Array Detector DAD Standard Flow Cell Item p n G1315 60022 1 79883 22402 5062 8553 3 79883 28801 4 79883 22301 5 1000 0488 6 G1315 68711 7 G1315 68710 8 G1315 87321 10 G1315 87302 11 G1315 84910 0515 1056 5022 2184 G1315 68712 79883 68703 344 Description Standard flow cell 10 mm 13 pL 120 bar 12 MPa Window screw Washer kit 10 pk Compression washer Window holder Quartz window Gasket BACK PTFE 2 3 mm hole outlet side 12 pk Gasket FRONT PTFE 1 3 mm hole inlet side 12 pk Window assembly comprises window screw spring washers compression washer window holder and quartz window Capillary IN 0 17 mm 590 mm lg including heat exchanger Capillary OUT 0 17 mm 200 mm lg Clamp unit Screw M 2 5 4 mm lg for cell body clamp Union ZDV Cell repair kit STD includes window screw kit 4 mm hexagonal wrench and seal kit Window screw kit includes 2 quartz windows 2 compression washers 2 window holders 2 window screws and 10 washers 1220 Infinity LC Parts for Ma
168. ng PP 6 5 mm id 5 m Preparations Remove the front cover 1 Pull the leak funnel out of the leak funnel holder 2 Pull out the leak funnel with the tubing 3 Insert the leak funnel with the tubing in its position 4 Insert the leak funnel into the leak funnel holder Leak funnel and holder Leak tubing Figure 71 Replacing Leak Handling System Parts 5 Replace the front cover 1220 Infinity LC 315 11 Maintenance Algae Growth in HPLC Systems The presence of algae in HPLC systems can cause a variety of problems that may be incorrectly diagnosed as instrument or application problems Algae grow in aqueous media preferably in a pH range of 4 8 Their growth is accelerated by buffers for example phosphate or acetate Since algae grow through photosynthesis light also stimulates their growth Small algae growth is seen even in distilled water after some time Instrumental problems associated with algae Algae deposit and grow everywhere within the HPLC system causing e deposits on ball valves inlet or outlet resulting in unstable flow or total failure of the pump e small pore solvent inlet filters to plug resulting in unstable flow or total failure of the pump small pore high pressure solvent filters usually placed before the injector to plug resulting in high system pressure e column filters to plug resulting in high system pressure e flow cell windows of detectors to become dirty result
169. ngth Detector VWD Cell Test VWD Cell Test Description The Cell Test compares the intensity of the deuterium lamp measured by the sample and reference diodes unfiltered and not logarithmized when the grating is in the zero order position The resulting intensity ratio sample reference is a measure of the amount of light absorbed by the flow cell The test can be used to check for dirty or contaminated flow cell windows When the test is started the gain is set to 1 To eliminate effects due to absorbing solvents the test should be done with water in the flow cell The test should not be performed using the micro flow cell since the reduction in light intensity will cause the test to fail Evaluating the VWD Cell Test Results The intensity ratio is dependent on the degree of contamination of the flow cell windows and on the type of flow cell used The lower the ratio the more light is absorbed by the flowcell Table 34 Probable causes of excessive flowcell absorbance Cause Corrective action Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles Dirty or contaminated flow cell Exchange the flow cell windows 1220 Infinity LC 157 9 Test Functions and Calibration Dark Current Test VWD Dark Current Test Description The dark current test measures the leakage current from the sample and reference circuits The test is used to check for defective sa
170. ngth Typical peak Recommended flow cell width lt 5cm 0 025 min 10 cm 0 05 min 20 cm 0 1 min Standard flow cell gt 40 cm 0 2 min Typical flow 0 2 ml min 0 2 0 4 ml min 0 4 0 8 ml min 1 5 ml min rate Internal column diameter 4 6mm Figure 50 Choosing a flow cell 130 1220 Infinity LC Detector Description 8 Match the Flow Cell to the Column Choosing a Flow Cell for the DAD Typical column Typical peak Recommended flow cell length width 10 cm 0 05 min Semi micro flow cell High pressure flow cell for Standard pressures Typical flow 0 01 0 2 0 2 0 4 0 4 0 4 1 5 0 01 5 rate ml min ml min ml min ml min ml min Internal column diameter 0 5 1mm 2 1 mm 3 0 mm 4 6 mm 1220 Infinity LC Figure 51 Choosing a Flow Cell in HPLC Flow Cell Path Length Lambert Beer s law shows a linear relationship between the flow cell path length and absorbance Absorbance log T log _e C d where is the transmission defined as the quotient of the intensity of the transmitted light I divided by the intensity of the incident light Io is the extinction coefficient which is a characteristic of a given substance under a precisely defined set of conditions of wavelength solvent temperature and other parameters is the concentration of the absorbing species usually in g l or mg l and is the path length of the cell used for the measurement 131 132 Detector Description
171. nity LC this software is used for flushing the system and performing the System Installation check see Priming the System and Performing the Installation Check on page 48 1 Install the Instrument Utility or Lab Advisor software according to the Installation Procedure on the software CD 2 Setup your Instrument to the software and Connect it Whenever a hardware upgrade Isocratic to Gradient Column Oven Autosampler upgrade has been installed it is necessary to re configure your instrument in the Instrument Utility Lab Advisor software Therefore please follow the steps that are described in Configuration of the Instrument After an Upgrade Installation on page 47 before you proceed 1220 Infinity LC Installation 3 Configuration of the Instrument After an Upgrade Installation This step is only necessary if any of the following hardware upgrade kits has been installed to the instrument e G4297A 1220 Infinity Oven kit e G4298A 1220 Infinity upgrade manual injector to ALS G4299A 1220 Infinity upgrade isocratic to gradient pump 1 Connect the Instrument to the Instrument Utility Lab Advisor software 2 Configure your Instrument according to the applied hardware changes Software Revision B 01 04 and below Tools gt Module Service Center any module Software Revision B 02 01 and higher Instrument Control gt Controls any module gt Convert Device Type For example if you installed a G4297A
172. ns ee i inlet P Qa outlet thumbscrew waste Next Steps 8 Perform a Wavelength Verification and Recalibration on page 185 or a Holmium Oxide Test on page 177to check the correct positioning of the flow cell 9 Close the front cover 302 1220 Infinity LC Maintenance 11 Maintenance of the Flow Cell When If the flow cell needs repair due to leaks or contaminations reduced light throughput Tools required Description Wrench 1 4 inch for capillary connections Hexagonal key 4 mm Toothpick Parts required Description For parts see Standard Flow Cell on page 344 Preparations Turn the flow off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 300 1220 Infinity LC 303 11 Maintenance 1 Use a4 mm hex key to unscrew the window assembly 1 and remove the gasket 2 from the cell body Do not mix the gasket 6 and 7 different hole diameter Carefully take one of the gaskets 6 back or 7 front and insert it into the cell body Do not mix the gasket 6 and 7 Gasket 7 has the smaller hole and must be on the light entrance side Verify that the gasket is positioned flat on the bottom and the light path is not blocked If you removed all individual parts from the window assembly refer to the figures in Standard Flow Cell on page 344 for the correct orientation of the parts 2 Insert the window
173. ns accumulated on time reset ignition voltage current lamp voltage lamp voltage current Available with ID tag lamp only product number serial number production date last intensity test Holmium Filter Filter movements filter moves reset log Flow Cell Available with ID tag flow cells only Product number production date pathlength max pressure serial number volume last cell test Micro Slit Slit movements filter moves reset log 186 1220 Infinity LC Test Functions and Calibration 9 Diode Array Detector DAD Details of UV lamp with RFID tag Details of flow cell with RFID tag ease ee ea Figure 61 Diagnosis screen in Agilent ChemStation detailed view 1220 Infinity LC 187 9 Test Functions and Calibration D A Converter DAC Test When Preparations 188 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 by 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 and a frequency of approximately 1 cycle 24 seconds is applied to the
174. nt BootP Service 69 Changing the IP Address of an Instrument Using the Agilent BootP Service 72 Storing the settings permanently with Bootp 74 Manual Configuration 75 With Telnet 76 This chapter provides information on connecting the instrument to the Agilent ChemStation PC ah Agilent Technologies 51 4 LAN Configuration To do first 52 The Agilent 1220 Infinity LC 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 left side of the instrument next to the configuration switch Part number of the detector G4280 61000 main board Revision Code 2B ZZ 747 4 Vendor Year and Week MAC 0030D31210A0 of assembly MAC address Made in Germany Country of Origin Figure 9 MAC label 1220 Infinity LC LAN Configuration 4 To do first 2 Connect the instrument s LAN interface to the PC network card using a crossover network cable point to point or a hub or switch using a standard LAN cable MAC label LAN port a Instrument with DAD Instrument with VWD Figure 10 Location of LAN interface and MAC label 1220 Infinity LC 53 4 LAN Configuration TCP IP parameter configuration To operate properly in a network environment the LAN interface mus
175. ntact your Agilent service representative 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 1 The detector is new 2 The detector has been repaired Suggested actions Recalibrate the detector Please contact your Agilent service representative 233 10 Error Information DSP Not Running This error message comes up when the communication between the optical unit and the main board has a problem Probable cause Suggested actions 1 Random communication error e Switch the detector off and on again at the power switch If the error reoccurs e Please contact your Agilent service representative 2 Defective detector main board Please contact your Agilent service representative 3 Defective PDA optical unit Please contact your Agilent service representative No Run Data Available In Device In a very rare case the capacity of the CompactFlash Card is not sufficient This could happen for example when the interrupt of LAN communication takes longer and the detector uses special settings e g full data rate at 80 Hz plus full spectra plus all signals during data buffering Probable cause Suggested actions 1 CompactFlash Card is full Correct communication problem Reduce data rate 234 12
176. ntegrator see details in section Remote Cables on page 354 Agilent module to 3396 Series III 3395B integrators Remote Cable Agilent module to general purpose Description Agilent module to 3396 integrators Agilent module to general purpose 1220 Infinity LC 1220 Infinity LC CAN cables p n 5181 1516 5181 1519 LAN cables p n 5023 0203 5023 0202 RS 232 cables p n G1530 60600 RS232 61601 5181 1561 Identifying Cables 14 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 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 RS 232 cable 8 m 351 14 Identifying Cables Analog Cables T O 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
177. obable cause Suggested actions 1 Gradient valve disconnected Ensure the gradient valve is connected correctly 2 Connection cable inside instrument not Please contact your Agilent service connected representative 3 Connection cable inside instrument Please contact your Agilent service defective representative 4 Gradient valve defective Exchange the gradient valve 1220 Infinity LC Error Information 10 MCGV Fuse 1220 Infinity LC Error ID 2043 Valve Fuse 0 Channels A and B Valve Fuse 1 Channels C and D The gradient valve in the quaternary pump has drawn excessive current causing the electronic fuse to open Probable cause Suggested actions 1 Defective gradient valve Restart the quaternary pump If the error message appears again exchange the gradient valve 2 Defective connection cable front panel to Please contact your Agilent service main board representative 3 Defective main board Please contact your Agilent service representative 211 10 Error Information 212 Wait Timeout Error ID 2053 When running certain tests in the diagnostics mode or other special applications the pump must wait for the pistons to reach a specific position or must wait for a certain pressure or flow to be reached Each action or state must be completed within the timeout period otherwise the error message is generated Possible Reasons for a Wait Timeout Pressure not reached Pump channel A did not
178. obile phase in the instrument for several days without flow Always discard old mobile phase Use the Solvent bottle amber 9301 1450 supplied with the instrument for your aqueous mobile phase If possible add a few mg l sodium azide or a few percent organic solvent to the aqueous mobile phase 317 11 Maintenance Replacing the Module s Firmware When Tools required OR OR Parts required Preparations 318 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 anew module with newer firmware is added to a system or if third party control software requires a special version Description LAN RS 232 Firmware Update Tool Agilent Lab Advisor software Instant Pilot G4208A only if supported by module Description 1 Firmware tools and documentation from Agilent web site Read update documentation provided 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 _layouts agilent downloadFirmware aspx whid 69761 2 For loading the firmware into the module follow the instructions i
179. optimization 125 servo restart failed 208 setable flowrange 21 22 shutdown 199 signal plots 138 simple repairs autosampler 267 site requirements bench space 17 environment 18 power considerations 16 power cords 17 slittest 171 slitwidth 26 122 solvent delivery system 82 solvent filters checking 244 cleaning 245 prevent blockage 92 solvent information 365 solvent inlet filters 91 Solvent Selection Valve 10 11 solvent zero counter 212 specification physical 19 specifications diode width 26 377 Index flow cell 26 linear range 26 noise and drift ASTM 26 performance 24 physical 19 programmable slit width 26 wavelength accuracy 26 wavelength range 26 spectral flatness test 179 spectralscan 166 spectra acquisition 124 spectrograph diodes pernm 116 SSV 10 11 state info 138 stator 103 step commands 150 stepper motor 102 storing the settings permanently 74 stroke length 209 stroke volume 84 90 suppression quantifying 125 system configurations 10 T TCP IP parameter configuration 54 telnet configuration 76 temperature limit exceeded 209 temperature out of range 210 temperature sensor 197 temperature 23 test chromatogram 165 183 test function D A converter 188 DAC 188 tests 378 ASTM noise ChemStation only 180 dark current 172 filter 169 flow cell ChemStation only 181 holmium oxide 177 intensity 174 slit 171 spectral flatness ChemStation only 179 test chromatogram 183 wave
180. or and external device 2 Defective detector main board 1220 Infinity LC Suggested actions Check or replace the cable Please contact your Agilent service representative 189 9 Test Functions and Calibration Diode Array Detector DAD 190 1220 Infinity LC 1220 Infinity LC 10 Error Information What are Error Messages 194 General Error Messages 195 Compensation Sensor Open 195 Compensation Sensor Short 195 Fan Failed 196 Leak 197 Leak Sensor Open 197 Leak Sensor Short 198 Remote Timeout 198 Shutdown 199 Lost CAN Partner 200 Timeout 200 Pump Error Messages 201 Encoder Missing 201 Index Adjustment 201 Index Limit 202 Index Missing 202 Initialization Failed 203 Missing Pressure Reading 203 Motor Drive Power 204 Pressure Above Upper Limit 205 Pressure Below Lower Limit 205 Pressure Signal Missing 206 Pump Configuration 206 Pump Head Missing 207 Restart Without Cover 207 Servo Restart Failed 208 Stroke Length 209 ote Agilent Technologies 191 10 Error Information 192 Temperature Limit Exceeded 209 Temperature Out of Range 210 Valve Failed MCGV 210 MCGV Fuse 211 Wait Timeout 212 Solvent Zero Counter 212 Autosampler Error Messages 213 Arm Movement Failed 213 Initialization Failed 214 Initialization with Vial 214 Invalid Vial Position 215 Metering Home Failed 215 Missing Vial 216 Missing Wash Vial 216 Motor Temperature 217 Needle Down Failed 218 Needle Up Failed 219 Safety Flap
181. ormal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 369 15 Appendix Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all electric and electronic appliances 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 of in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information 370 1220 Infinity LC Appendix 15 Declaration of Conformity for HOX2 Filter Declaration of Conformity for HOX2 Filter 1220 Infinity LC Declaration of Conformity We herewith inform you that the Holmium Oxide Glass Filter used in Agilents absorbance detectors listed in the table below meets the requirements of National Institute of Standards and Technology NIST to be applied as certified wavelength standard According to the publication of NIST in J Res Natl Inst Stand Technol
182. out Run 1 Start the Chromatographic Data System 2 Create a checkout method with the following parameters Flow 1 mL min Inj Volume 20 uL Autosampler Oven temp not controlled VWD Wavelength 254 nm Runtime 1 min This checkout run is done with the factory installed restriction capillary in place 3 Prepare 1ml of a checkout sample acetone for example and put it on vial position 1 in the autosampler tray For Manual Injector configurations load 20 uL of checkout sample in the loop Overfill the injection loop at least 3 times e g inject at least 60 uL at a 20 uL sample loop 4 Start a single run As result a single peak should be visible 5 Print out the report Store all created and printed out reports in a binder Now you are finished with the installation of the Agilent 1220 Infinity LC 1220 Infinity LC 49 3 Installation Performing a Checkout Run 50 1220 Infinity LC 1220 Infinity LC 4 LAN Configuration Todofirst 52 TCP IP parameter configuration 54 Configuration Switches 55 Initialization mode selection 56 Dynamic Host Configuration Protocol DHCP 60 General Information DHCP 60 Setup DHCP 61 Link configuration selection 63 Automatic Configuration with BootP 64 About Agilent BootP Service 64 How BootP Service Works 65 Situation Cannot Establish LAN Communication 65 Installation of BootP Service 66 Two Methods to Determine the MAC Address 68 Assigning IP Addresses Using the Agile
183. own 1220 Infinity LC 297 11 Maintenance Diode Array Detector DAD 1 Open the front cover to gain access to the flow cell area 2 Disconnect lamp from the connector unscrew the Vis lamp left and or UV lamp right and remove the lamp Do not touch the glass bulb with your fingers Paras 3 When replacing the Vis lamp assure that the Vis lamp is inserted as shown flat edge towards the deuterium lamp 4 Insert the lamp Fix the screws and reconnect the lamp to connector a ia 298 1220 Infinity LC Maintenance 11 Next Steps Close the font cover Reset the lamp counter as described in the user interface documentation lamps with I D tag cannot be reset Turn the lamp on and give the lamp 10 minutes to warm up on oOo ol Perform a Wavelength Verification and Recalibration on page 185or a Holmium Oxide Test on page 177 to check the correct positioning of the UV lamp 9 Perform an Intensity Test on page 174 1220 Infinity LC 299 11 Maintenance Exchanging a Flow Cell When Tools required Parts required OR OR OR OR Preparations If an application needs a different type of flow cell or the flow cell needs repair Description Wrench 1 4 inch for capillary connections p n Description 1 G1315 60022 Standard flow cell 10 mm 13 pL 120 bar 12 MPa 1 G1315 60025 Semi micro flo
184. perating temperature 19 analog cable 352 analytical head 102 armdown 152 armup 152 array 116 ASTM environmental conditions 18 noise test ChemStation only 180 reference and conditions 25 AUTO mode 90 automatic configuration with Bootp 64 autosampler EMF counters 13 introduction 97 simple repairs 267 1220 Infinity LC transprot assembly parts 268 ball screw drive 84 band width 6 5nm 24 BCD cable 35 7 Beer Lambert law 131 bench space 17 beta and alpha line 185 blank scan 166 blockage 145 204 BootP service installation 66 restart 73 settings 72 stop 72 Bootp amp Store 57 automatic configuration 64 initialization modes 56 storing the settings permanently 74 using default 58 using stored 58 buffer application 91 buffer solution 260 bypass 99 C cable analog 352 BCD 357 CAN 359 LAN 359 Index remote 354 RS 232 360 cables analog 350 BCD 350 CAN 351 LAN 351 overview 350 remote 350 RS 232 351 calibration oven 156 CAN cable 359 caps 106 cell 15 7 change gripper 150 needle 149 piston 149 cleaning the autosampler 268 cleaning the module 296 close gripper 152 column oven 110 communications 20 compensation sensor open 195 compensation sensor short 195 21 22 pA ae as compressibility compensation 88 condensation 18 configurations 10 control system 20 composition precision composition range 21 22 373 Index correction factors for flow cells 132 co
185. protected ground terminal CAN Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product e The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up gt WARNING aia 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 364 1220 Infinity LC Appendix 15 Solvent Information 1220 Infinity LC Observe the following recommendations on the use of solvents Flow Cell Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell Prevent any crystallization of buffer solutions This will lead into a blockage damage of the flow cell If the flow cell is transported while temperatures are below 5 C it must be assured that the cell is filled with alcohol Aqueous solvents in the flow cell can built up algae Therefore do not leave aqueous solvents sitting in the flow cell Add small of organic solvents for example acetonitrile or methanol 5 Solvents Brown glass ware can avoid growth of
186. r 249 224 nm 3 520 Time min Figure 48 Selectivity by Ratio Qualifiers In a four component mixture only biphenyl was recorded The other three peaks were suppressed because they did not meet the ratio qualifier criterion and therefore the output was set to zero The characteristic wavelengths 249 nm A and 224 nm Ag were found from the spectra shown in Figure 47 on page 127 The ratio range was set at 2 2 4 2 2 10 Only when the ratio between 249 and 224 nm was within this range is the signal plotted Of all four peaks only the third fulfilled the criterion Figure 48 on page 127 The others were not plotted 1220 Infinity LC 127 8 Detector Description Agilent 1220 Infinity LC Diode Array Detector DAD Spectrum Settings DAD only Not Ready Information 128 To change the Spectra settings open 1 To change the Spectra settings select Setup Detector Signals 2 In the section Spectrum click on the drop down list and chose a parameter Table 23 on page 129 shows the possible parameters 3 Change the Range Step width and Threshold according to your needs DAD Signals System 2 fs fie fo fo g 20 fie feo fo g fie fso fog fis feo fo g feso fie fso fo g a si D A z n Every 2nd spectrum 7 None Apex Baselines Apex Slopes Baselines Allin peak Every 2nd spectrum Threshold Sree oreo Figure 49 Spectra Settings fie f fo g fao fe fso fo gon see
187. r 5800 psi pressure maximum Micro 1 pL volume 5 mm cell path length and 40 bar 580 psi pressure maximum Semi micro 5 pL volume 6 mm cell path length and 40 bar 580 psi pressure maximum Recorder integrator 100 mV or 1 V output range 0 001 to 2 AU one output 1220 Infinity LC Site Requirements and Specifications 2 Table 7 Performance Specifications Agilent 1220 Infinity LC VWD Type Specification Comments Communications Controller area network CAN RS 232C APG Remote ready start stop and shut down signals LAN optional Safety and maintenance Extensive diagnostics error detection and display through Agilent ChemStation leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features Early maintenance feedback EMF for continuous tracking of instrument usage in terms of lamp burn time with user settable limits and feedback messages Electronic records of maintenance and errors Verification of wavelength accuracy with built in holmium oxide filter Housing All materials recyclable ASTM Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid Chromatography Reference conditions cell path length 10 mm response time 2 s flow 1 mL min LC grade methanol Linearity measured with caffeine at 272 nm 1220 Infinity LC 25 Site Requirements and Specifications Performance Sp
188. r Information 10 Pump Head Missing Error ID 2202 2212 The pump head end stop in the pump was not found When the pump restarts the metering drive moves forward to the mechanical end stop Normally the end stop is reached within 20 s indicated by an increase in motor current If the end point is not found within 20 s the error message is generated Probable cause Suggested actions 1 Pump head not installed correctly screws Install the pump head correctly Ensure nothing not secured or pump head not seated e g capillary is trapped between the pump correctly head and body 2 Broken piston Exchange the piston Restart Without Cover Error ID 2502 The module was restarted with the top cover and foam open The sensor on the main board detects when the top foam is in place If the module is restarted with the foam removed the module switches off within 30 s and the error message is generated Probable cause Suggested actions 1 The module started with the top cover and Please contact your Agilent service foam removed representative 1220 Infinity LC 207 10 Error Information Servo Restart Failed Error ID 2201 2211 The pump motor in the module was unable to move into the correct position for restarting When the module is switched on the first step is to switch on the C phase of the variable reluctance motor The rotor should move to one of the C positions The C position is required for the servo to be able
189. r fingers close too far This is sensed by the processor encoder position causing the error message to be generated Probable cause Suggested actions 1 Novialin the position defined inthe method Install the sample vial in the correct position or or sequence edit the method or sequence accordingly 2 Incorrect gripper alignment Align gripper 3 Defective gripper assembly defective Exchange the gripper assembly gripper fingers or belt 4 Defective transport assembly flex board Please contact your Agilent service representative Missing Wash Vial Error ID 4035 4542 4707 The wash vial programmed in the method was not found When the gripper arm picks a vial out of the sample tray the processor monitors the gripper motor encoder If a vial is present the closing of the gripper fingers is limited by the vial However if no vial is present the gripper fingers close too far This is sensed by the processor encoder position causing the error message to be generated Probable cause Suggested actions 1 No wash vial in the position defined in the Install the wash vial in the correct position or method edit the method accordingly 1220 Infinity LC Error Information 10 Motor Temperature Error ID 4027 4040 4261 4451 One of the motors of the transport assembly has drawn excessive current causing the motor to become too hot The processor has switched OFF the motor to prevent damage to the motor See figure Fig
190. r is blocked If internally leaking If internally leaking If internally leaking If the frit shows indication of contamination or blockage If pump performance indicates seal wear After exchanging the pump seals Before exchanging the seals or plungers If scratched Gradient performance problems intermittent pressure fluctuations Pressure ripple unstable run Leak Test for verification Pressure ripple unstable run Leak Test for verification Solvent dripping out of waste outlet when valve closed A pressure drop of gt 10 bar across the frit 5 mL min H 30 with purge open indicates blockage Leaks at lower pump head side unstable retention times pressure ripple unstable run Leak Test for verification Seal life time shorter than normally expected check plungers while changing the seals 1220 Infinity LC Maintenance 11 Instrument is partially energized when switched off The power supply still uses some power even if the switch on the front panel is turned off gt To disconnect the Agilent 1220 Infinity LC pump from line unplug the power cord Sharp metal edges Sharp edged parts of the equipment may cause injuries gt To prevent personal injury be careful when getting in contact with sharp metal areas When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can carry health risks gt Obser
191. ration 4 tio toco The modules in the stack must have at least firmware from set A 06 34 and the above mentioned modules B 06 40 or above must from the same firmware set 1 Note the MAC address of the LAN interface provided with G1369C LAN Interface Card or Main Board This MAC address is on a label on the card or at the rear of the main board e g 0030d3177321 On the Instant Pilot the MAC address can be found under Details in the LAN section System Info Controller DE12345678 G4208A Main Revision EX RPA Cn DAD DE64260019 G1315D Main Revision Resident Revison B 06 41 0002 B 06 40 0007 On time 3d 01 33h Installed Options Dhcp LAN TCP IP Mode DHCP LAN TCP IP Address 130 168 132 219 0030D314F89E TYPE G61315 66565 SER MAC REV AC MFG 2140 0820 848728 no info v information on each module S 10 08 Figure 16 1220 Infinity LC LAN Setting on Instant Pilot 61 4 62 LAN Configuration 2 Set the Configuration Switch to DHCP either on the G1369C LAN Interface Card or the main board of above mentioned modules Table 13 SW 4 ON G1369C LAN Interface Card configuration switch on the card SW5 SW 6 SW7 SW 8 Initialization Mode OFF OFF OFF OFF DHCP Table 14 SW 6 ON LC Modules inclusive 1120 1220 configuration switch at rear of the instru ment SW7 SW 8 Initialization Mode OFF OFF DHCP 3 Turn on
192. ration of the autosampler the alignment procedure must be carried out in the correct sequence and in full that is without skipping any part ALS Alignment Controls Button Description Keyboard Shortcut A Rotate the gripper by Cursor Up increasing theta lt q Move the gripper horizontally Cursor Left to the left gt Move the gripper horizontally Cursor Right to the right hA Rotate the gripper by Cursor Down decreasing theta Arm Up Lifts the gripper arm Page Up Arm Down Lowers the gripper arm Page Down Open Gripper Opens the gripper Close Gripper Closes the gripper 1220 Infinity LC 1220 Infinity LC Test Functions and Calibration 9 Button Description Keyboard Shortcut Start gt gt Starts the execution of the Enter procedure Shown only at the start Continue gt gt Jumps to the next step of the Enter procedure Shown only during alignment Restart Restarts the execution of the step Running the ALS Alignment Teaching To ensure correct operation of the autosampler the alignment procedure must be carried out in the correct sequence and in full that is without skipping any part To align the ALS 1 2 3 7 U U Insert a 100 vial tray into the autosampler Place capped vials into positions 15 and 95 Click Start gt gt The gripper arm moves to a position above vial 15 Answer Yesto reset the correction values to their factory defaults or No to leave them a
193. re This procedure is required for Standard seals pack of 2 5063 6589 only It will damage the PE seals pack of 2 0905 1420 gt Never perform the seal wear in procedure with normal phase application seals 256 1 Place a bottle with 100 mL of isopropanol in the solvent cabinet and attach a bottle head assembly including tubing to the bottle 2 Connect the inlet tube from the bottle head directly to the inlet valve 3 Connect one end of the Restriction capillary 5022 2159 to the purge valve Insert the other end into a waste container 4 Open the purge valve and purge the system for 5 min with isopropanol at a flow rate of 2 mL min 5 Close the purge valve and set the flow to a rate adequate to achieve a pressure of 350 bar 6 Pump for 15 min at this pressure to wear in the seals 7 Turn off the pump and slowly open the purge valve to release the pressure from the system 8 Disconnect the restriction capillary and reinstall the bottle containing the solvent for your application 9 Rinse your system with the solvent used for your application 1220 Infinity LC Exchanging the Plungers Maintenance 11 When When scratched Tools required p n Description 8710 0510 Wrench open 1 4 5 16 inch 8710 2392 Hexagonal key 4 0 mm 15 cm long T handle Parts required p n Description 5067 4695 Sapphire piston Preparations Switch off the pump at the main power switch Remove the upper front cover 1 Place the
194. reach the delivery phase Pump channel B did not reach the delivery phase Pump channel A did not reach the take in phase Pump channel B did not reach the take in phase Solvent volume not delivered within the specified time Probable cause Suggested actions 1 Flow changed after starting test Ensure correct operating condition for the special application in use 2 Defective pump drive assembly Please contact your Agilent service representative Solvent Zero Counter Error ID 2055 2524 Pump firmware version A 02 32 and higher allow to set solvent bottle fillings in the data system If the volume level in the bottle falls below the specified value the error message appears when the feature is configured accordingly Probable cause Suggested actions 1 Volume in bottle below specified volume Refill bottles and reset solvent counters 2 Incorrect setting Make sure the limits are set correctly 1220 Infinity LC Autosampler Error Messages Error Information 10 These errors are specific to the autosampler Arm Movement Failed 1220 Infinity LC Error ID 4002 The transport assembly was unable to complete a movement in one of the axes The processor defines a certain time window for the successful completion of a movement in any particular axis The movement and position of the transport assembly is monitored by the encoders on the stepper motors If the processor does not receive the correct position info
195. red maxima are outside the limits the error message is generated Probable cause Suggested actions 1 Misaligned defective grating assembly Ensure the flow cell is inserted correctly and is free from contamination cell windows buffers and so on Run the filter motor test to determine if the filter motor assembly is defective If defective please contact your Agilent service representative Run the grating motor test to determine if the grating assembly is defective If defective please contact your Agilent service representative 1220 Infinity LC Error Information 10 Ignition Failed Error ID 7452 The lamp failed to ignite The processor monitors the lamp current during the ignition cycle If the lamp current does not rise above the lower limit within 2 5 s the error message is generated Probable cause Suggested actions 1 Lamp disconnected Ensure the lamp is connected 2 Defective or non Agilent lamp Exchange the lamp 3 Defective power supply Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative Wavelength test failed Error ID 7890 The automatic wavelength check after lamp ignition has failed When the lamp is switched on the detector waits 1 min to warm up the lamp Then a check of the deuterium emission line 656 nm via the reference diode is performed If the emission line is more than 3 nm away from 656 nm the er
196. remove the pump head from the pump drive Metering drive Pump head Pump head screws 253 11 Maintenance Exchanging the Pump Seals and Seal Wear in Procedure Exchanging the Pump Seals Piston seal PTFE carbon filled black pack of 2 default When Seal leaking if indicated by the results of the leak test Tools required p n Description 8710 0510 Wrench open 1 4 5 16 inch 8710 2392 Hexagonal key 4 0 mm 15 cm long T handle Parts required p n Description 5063 6589 0905 1420 PE seals pack of 2 5022 2159 Restriction capillary Preparations Remove the upper front cover Switch off the pump at the main power switch Place the pump head on a flat surface Loosen the lock screw two revolutions and while holding the lower half of the assembly carefully pull the pump head away from the plunger housing Pump head Plunger housing Remove the support rings from the plunger housing and lift the housing away from the plungers Support ring gt gt Plunger housing A Plunger 254 1220 Infinity LC 3 Using one of the plungers carefully remove the seal from the pump head be careful not to break the plunger Remove wear retainers if still present Seal 4 Insert new seals into the pump head Seals Te Pump head Support ring Plunger housing 1220 Infinity LC 255 11 Maintenance CAUTION Seal Wear in Procedu
197. rge the pump 1 2 3 Prepare each channel with the appropriate purge solvents Select Purge Pump from the Tool Selection screen In the Purge Configuration dialog box a If necessary select the channel s that you want to purge b For each selected channel select a Flow and a purge Time c Click OK to close the Purge Configuration dialog box When the request to open the purge valve appears open the purge valve on the pump then click OK to close the message box During purging the General tab shows the current channel that is being purged and the remaining purge time The Signals tab shows a plot of pressure against time for the complete purge cycle When the purge time has elapsed and the request to close the purge valve appears close the purge valve on the pump then click OK to close the message box The pump purge process is complete 147 9 148 Test Functions and Calibration Degasser Exchange The Degasser Exchange Tool allows you to set a new calibration value after exchanging the degasser unit When you start the Degasser Exchange Tool a dialog box is displayed asking you to enter the calibration value written on the degasser label Type the calibration value in the field and click OK to upload it to the degasser With the introduction of Lab Advisor B 02 04 093 the Degasser Exchange Tool function has been moved to Instrument Control tab To use the tool do as follows 1 Go to Instrument Control tab
198. rmation from the encoders within the time window the error message is generated See figure Figure 37 on page 104 for axes identification Arm Movement 0 Failed X axis Arm Movement 1 Failed Z axis Arm Movement 2 Failed Theta gripper rotation Arm Movement 3 Failed Gripper gripper fingers open close Probable cause 1 Mechanical obstruction 2 High friction in the transport assembly 3 Defective motor assembly 4 Defective sample transport assembly flex board 5 Defective main board Suggested actions Ensure unobstructed movement of the transport assembly Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative 213 10 Error Information 214 Initialization Failed Error ID 4020 The autosampler failed to complete initialization correctly The autosampler initialization procedure moves the needle arm and transport assembly to their home positions in a predefined sequence During initialization the processor monitors the position sensors and motor encoders to check for correct movement If one or more of the movements is not successful or is not detected the error message is generated Probable cause Suggested actions 1 Mechanical obstruction Ensure unobstructed movement of the transport assembly 2 Defective sampling unit f
199. ront of the instrument with the instrument in place in the Agilent 1220 Infinity LC These repairs are described in following sections Overview of procedures Procedure Typical frequency Time required Exchanging the needle When needle shows indication of damage 15min assembly or blockage Exchanging the seat assembly When the seat shows indication of 10 min damage or blockage Exchanging the rotor seal After approximately 30000to 30 min 40000injections or when the valve performance shows indication of leakage or wear Exchanging the metering seal When autosampler reproducibility 30 min indicates seal wear Exchanging the gripper arm When the gripper arm is defective 10 min The power supplies still use some power even if the power switch on the front panel is turned off Repair work at the autosampler can lead to personal injuries e g shock hazard when the autosampler cover is opened and the instrument 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 1220 Infinity LC 267 11 Maintenance Exchanging Internal Parts Some repairs may require exchange of defective internal parts Exchange of these parts requires removing the autosampler unit from the Agilent 1220 Infinity LC these repairs have to be done by train
200. ror message is generated Probable cause Suggested actions 1 Calibration incorrect Recalibrate the detector 1220 Infinity LC 229 10 Error Information DAD Detector Error Messages 230 These errors are specific to the diode array detector Visible Lamp Current The visible lamp current is missing The processor continually monitors the lamp current during operation If the current falls below the lower current limit the error message is generated Probable cause 1 Lamp disconnected 2 Defective visible lamp 3 Defective connector or cable 4 Defective power supply Visible Lamp Voltage The visible lamp voltage is missing Suggested actions Ensure the visible lamp connector is seated firmly Exchange the visible lamp Please contact your Agilent service representative Please contact your Agilent service representative The processor continually monitors the voltage across the lamp during operation If the lamp voltage falls below the lower limit the error message is generated Probable cause 1 Defective connector or cable 2 Defective power supply Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative 1220 Infinity LC Diode Current Leakage Error ID 1041 Error Information 10 When the detector is switched on the processor checks the leakage current of each of the optical diodes If the leakage c
201. s being drawn for long periods the temperature of the circuits increases If the temperature exceeds the upper limit the error message is generated Probable cause Suggested actions 1 High friction partial mechanical blockage Remove the pump head assembly Ensure there in the pump drive assembly is no mechanical blockage of the pump head assembly or pump drive assembly 2 Partial blockage of the flowpath in front of Ensure the outlet valve is not blocked the damper 3 Defective pump drive assembly Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 209 10 Error Information 210 Temperature Out of Range Error ID 2517 The temperature sensor readings in the motor drive circuit are out of range The values supplied to the ADC by the hybrid sensors must be between 0 5 V and 4 3 V If the values are outside this range the error message is generated Probable cause Suggested actions 1 Defective main board Please contact your Agilent service representative Valve Failed MCGV Error ID 2040 Valve 0 Failed valve A Valve 1 Failed valve B Valve 2 Failed valve C Valve 3 Failed valve D One of the valves of the multi channel gradient valve has failed to switch correctly The processor monitors the valve voltage before and after each switching cycle If the voltages are outside expected limits the error message is generated Pr
202. s document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend 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 pract
203. s required Preparations When the needle is visibly damaged When the needle is blocked Description Wrench 1 4 inch supplied in HPLC Tool Kit Hexagonal key 2 5 mm supplied in HPLC Tool Kit Pair of pliers p n Description 1 G1313 87201 Needle assembly 11 Select Change Needle in the Tools function in the Instrument Utilities or Lab Advisor Software and select Start When the needle is positioned approximately 15 mm above the needle seat remove the upper front cover Personal injury To avoid personal injury keep fingers away from the needle area during autosampler operation gt Do not bend the safety flap away from its position or attempt to remove the safety cover gt Do not attempt to insert or remove a vial from the gripper when the gripper is positioned below the needle 1220 Infinity LC 269 11 Maintenance Autosampler 1 Select Needle Down until the needle screw is aligned 2 Remove the sample loop fitting from the needle fitting with the hole in the safety cover 3 Loosen the fixing screw 1 and lift out the needle 2 4 Select Needle Down to move the needle arm to its lowest position The needle arm must be in its lowest position before installing the new needle otherwise leaks at the needle seat will occur due to incorrect needle installation 270 1220 Infinity LC Maintenance 11 Autosampler 5 Insert the new needle 1
204. s they are Use Arm Down to move the fingers of the gripper as close as possible to he top of the vial without touching ct Use A and Yy for rotation and lt and gt for movement left and ight to adjust the gripper position in the horizontal plane se Open Gripper to open the gripper fingers se Arm Down to move the gripper arm down a further 5 mm until the vial cap and the rubber of the gripper fingers are the same height Check that the vial is in the center of the gripper fingers and readjust the position if necessary step 6 10 When you are satisfied that the gripper position is correct click Continue The gripper arm moves to a position above vial 95 153 9 Test Functions and Calibration 11 Repeat steps 6 to 9 to align the gripper at position 95 12 Click Continue On completion of the calculation the values for both X and theta are rounded to one decimal place The correction values are stored permanently in the non volatile memory of the sampler and the sampler is initialized Gripper Verification ALS Gripper Verification Description The verification procedure uses several vial positions as reference points to verify the gripper alignment is correct If verification indicates one or more positions are out of alignment the alignment procedure should be done Verifying the Gripper Positions Vial positions 1 10 55 81 and 100 can be used for position verification 1 Insert empty capped v
205. s to the bypass position Solvent from the pump enters the valve unit at port 1 and flows directly to the column through port 6 1220 Infinity LC 99 6 Injection System Description Autosampler Figure 34 Bypass Position Next the needle is raised and the vial is positioned below the needle The needle moves down into the vial and the metering unit draws the sample into the sample loop Figure 35 Drawing the Sample 100 1220 Infinity LC Injection System Description 6 Autosampler When the metering unit has drawn the required volume of sample into the sample loop the needle is raised and the vial is replaced in the sample tray The needle is lowered into the needle seat and the injection valve switches back to the mainpass position flushing the sample onto the column Figure 36 Mainpass Position Sample Injection Sampling Unit The sampling unit comprises three main assemblies needle drive metering device and injection valve NOTE The replacement sampling unit excludes the injection valve and metering head assemblies 1220 Infinity LC 101 102 Injection System Description Needle Drive The needle movement is driven by a stepper motor connected to the spindle assembly by a toothed belt The circular motion of the motor is converted to linear motion by the drive nut on the spindle assembly The upper and lower needle positions are detected by reflection sensors on the sampling unit flex board while t
206. ses p n Description 2110 1417 Fuse 3 15 A250 V Next to each fuse is an LED Red LED indicates the fuse is blown If one of the fuses is blown the green LED of the power switch flashes e Fuse F1 degasser pump injector motors Fuse F2 injector sensors column oven ext 24 V connector Fuse F3 processor core 5 V 15 V 15 V supply on mainboard e Fuse F4 VWD incl D2 lamp Fuse F5 VWD heater fan 1 fuse netfilter p n Description 2110 1004 Fuse 10At 321 12 Parts for Maintenance Solvent Delivery System Pump Head Assembly Without Seal Wash Item p n G1312 60056 1 5063 6586 G1311 60002 3 5067 1560 4 5062 2484 5 5042 8952 6 5063 6589 OR 0905 1420 7 G1311 25200 8 G1312 60066 9 G1312 60067 10 5042 1303 11 G4280 60061 12 0515 2118 Description Pump Head 1200 SL without Seal Wash Sapphire piston Piston housing Support Ring SL no seal wash Gasket seal wash pack of 6 Seal holder Piston seal PTFE carbon filled black pack of 2 default PE seals pack of 2 Pump chamber housing Passive inlet valve 1220 1260 Outlet valve 1220 1260 Lock screw Purge valve Pump head screw M5 60 mm The Pump Head 1200 SL without Seal Wash G1312 60056 includes items 1 7 10 and 12 322 1220 Infinity LC Parts for Maintenance 12 Solvent Delivery System Figure 72 Pump head assembly without seal wash option NOTE The design of the seal wash gasket has changed see below
207. solutions 1 Switch the valve to the INJECT position 2 Use the pump to flush the sample loop and seal grooves 3 Use the needle port cleaner supplied with the valve and syringe to flush the needle port and vent capillary 1220 Infinity LC 263 11 Maintenance Exchanging the Injection Valve Seal When Poor injection volume reproducibility Leaking injection valve Tools required Description Hex key 9 64 inch supplied in the tool kit Parts required p n Description 5068 0082 Rotor seal PEEK 1 Loosen the three stator screws Remove the stator head 2 Remove the stator ring Zz S A A amp Wy f eae le fs NI X Pa NG 264 1220 Infinity LC Maintenance 11 3 Remove the rotor seal A A j 5S tp KA Y N SA y 5 S JA lt ie y A a J I f Y ij A tO y j j 4 Install the new rotor seal 5 Install the stator ring Ensure the pin in the stator ring is aligned with the hole in the valve body 6 Install the stator head onto the valve 1220 Infinity LC 265 11 Maintenance 7 Secure stator head in place with the stator screws Tighten each screw alternately 4 turn until the stator head is secure 266 1220 Infinity LC Maintenance 11 Autosampler Introduction The autosampler is designed for easy repair The most frequent repairs can be done from the f
208. st 174 Holmium Oxide Test 177 Spectral flatness test 179 ASTM Noise Test 180 Cell Test 181 Using the Built in Test Chromatogram 183 Wavelength Verification and Recalibration 185 Diagnosis Information on Agilent ChemStation 186 D A Converter DAC Test 188 This chapter describes the tests calibrations and tools that are available with the Instrument Utilities software or the Lab Advisor 1220 Infinity LC Test Functions and Calibration 9 Agilent 1220 Infinity LC System Installation Check The Installation Check switches on all available modules purges the system for five minutes at 1 mL min tests the flow path by applying a pressure up to 200 bar and switches on the oven if available and detector The pump and detector are mandatory for this check the oven and autosampler are optional The Installation Check passes if the following conditions are met e All modules switch on successfully within the timeout period 120 s The pump achieves 200 bar after 5 min The oven reaches 2 K above its actual temperature The detector lamp ignites and the detector reaches a Ready state 1220 Infinity LC 137 9 138 Test Functions and Calibration Module Info The Module Info tool collects diagnostic information from a module and writes the results to a file You can view the results in three tabs General The General tab shows information about the module s firmware and options in a two column table Tables
209. st fails if one or more of the maxima lies outside of the limits see Figure 57 on page 178 1220 Infinity LC 177 178 Test Functions an Figure 57 d Calibration Instrument Serial Number Operator Holmium Filter Test Results Wavelength 1 361 0 Wavelength 2 453 7 nz Wavelength 2 536 7 Test Failed Probable cause 1 2 Absorbing solvent or air bubble in flow cell Incorrect calibration Dirty or contaminated flow cell Dirty or contaminated optical components achromat windows Old or non Agilent lamp Specification Measured Result 360 262 nm 360 95 mm Passed 452 7 454 7 nm 452 4 nm Passed 35 7 5327 7 nm 526 8 nm Passed Holmium Oxide Test Results report Suggested actions Ensure the flow cell is filled with water Recalibrate see Wavelength Verification and Recalibration on page 185 and repeat the test Run the cell test see Cell Test on page 181 If the test fails exchange the flow cell windows Clean optical components with alcohol and lint free cloth or replace the parts see Intensity Test on page 174 Exchange the UV lamp 1220 Infinity LC Test Functions and Calibration 9 Spectral flatness test The spectral flatness test determines the maximum noise in mAU on the spectrum The test is run with the flowcell removed to eliminate effects due to absorbing solvent or a dirty flowcell First a detector balance is done Next a spectrum no
210. stem Description Variable Stroke Volume 90 Due to the compression of the pump chamber volume each plunger stroke of the pump generates a small pressure pulsation influencing the flow ripple of the pump The amplitude of the pressure pulsation is dependent mainly on the stroke volume and the compressibility compensation for the solvent in use Small stroke volumes generate pressure pulsations of smaller amplitude than larger stroke volumes at the same flow rate In addition the frequency of the pressure pulsations are higher This decreases the influence of flow pulsations on quantitative results In gradient mode smaller stroke volumes result in less flow ripple and improve composition ripple The pump uses a processor controlled spindle system to drive its plungers The normal stroke volume is optimized for the selected flow rate Low flow rates use a small stroke volume while higher flow rates use a larger stroke volume When the stroke volume for the pump is set to AUTO mode the stroke is optimized for the flow rate in use A change to larger stroke volumes is possible but not recommended 1220 Infinity LC Solvent Delivery System Description 5 Using the Pump Hints for successful use of the Agilent 1220 Infinity LC pump 1220 Infinity LC When using salt solutions and organic solvents in the Agilent 1120 Infinity LC pump it is recommended to connect the salt solution to one of the lower gradient valve ports and the or
211. stem 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 Suggested 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 1220 Infinity LC Shutdown 1220 Infinity LC Error ID 0063 Error Information 10 An external instrument has generated a shutdown 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 1 Leak detected in another module with a CAN connection to the system 2 Leak detected in an external instrument with a remote connection to the system 3 Shut down in an external instrument with a remote connection to the system Suggested actions Fix the leak in the external instrument before restarting the module Fix the leak in the external instrument before restarting the module
212. t be configured with valid TCP IP network parameters These parameters are e IP address e Subnet Mask 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 by automatically requesting the parameters from a network based DHCP Server using the so called Dynamic Host Configuration Protocol This mode requires a LAN onboard Module or a G1369C LAN Interface card see Setup DHCP on page 61 e by manually setting the parameters using Telnet 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 11 on page 56 54 1220 Infinity LC LAN Configuration 4 Configuration Switches 1220 Infinity LC The configuration switch can be accessed at the rear left side of the instrument The Agilent 1220 Infinity LC is shipped with switches 7 and 8 set to ON which means that the instrument is set to a default fixed IP address 192 168 254 11 To configure the LAN SW1 and SW2 must be set to OFF Table 10 Factory Default Settings Initialization Init Mode Using
213. t vial positions defined in the Check method settings vs installed tray method or sequence 3 Tray recognition defective dirty sample tray Ensure the coding surfaces of the sample tray or defective transport assembly flex board are clean located at the rear of the sample tray If this does not solve the problem contact your Agilent service representative Metering Home Failed 1220 Infinity LC Error ID 4054 4704 The metering piston has failed to move back to the home position The home position sensor on the sampling unit flex board monitors the home position of the piston If the piston fails to move to the home position or if the sensor fails to recognize the piston position the error message is generated Probable cause Suggested actions 1 Defective sensor or main board Please contact your Agilent service representative 2 Broken piston Exchange the metering piston and seal 3 Defective metering drive motor Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 215 10 Error Information 216 Missing Vial Error ID 4019 4034 4541 4706 No vial was found in the position defined in the method or sequence When the gripper arm picks a vial out of the sample tray the processor monitors the gripper motor encoder If a vial is present the closing of the gripper fingers is limited by the vial However if no vial is present the grippe
214. te accessory kit PTFE silicone septa 16mm pre silt 100 pk delivered quantity is 0 010 Syringe 50 0 pL FN LC tip Syringe Plastic Syringe adapter Screw Cap Vial clear 6 mL 100 PK delivered quantity is 0 010 Screw caps for 6 mL vials 100 PK delivered quantity is 0 010 Solvent bottle transparent Solvent bottle amber Bottle head assembly 1220 Infinity LC 1220 Infinity LC Installation 3 Accessory Kit Contents for G4290B C G4294B p n G4290 68755 0100 2562 0890 1195 0890 1711 5023 0203 5062 8535 9301 0411 9301 1337 9301 1420 9301 1450 G1311 60003 Description Accessory kit complete Fitting onepiece fingertight PTFE tubing 0 052 in i d Flexible tubing to waste 3 m Cross over network cable shielded 3 m for point to point connection Waste accessory kit Syringe Plastic Syringe adapter Solvent bottle transparent Solvent bottle amber Bottle head assembly Optional Tool Kit for Agilent 1220 Infinity LC p n G4296 68715 0100 1710 8710 0510 8710 1924 8720 0025 01018 23702 8710 2392 8710 2394 8710 2411 8710 2412 8710 0899 Description Tool kit complete Mounting Tool for Tubing Connections Wrench open 1 4 5 16 inch Wrench open 14 mm Wrench 1 2 inch amp 9 16 inch Insert tool Hex key 4mm15 cm long T handle Hex key 9 64 inch 15 cm long T handle Hex key 3 mm12 cm long Hex key 2 5 mm 15 cm long straight handle Pozidriv screwdriver 33 3 Installation
215. tem and Performing the Installation Check 48 Performing a Checkout Run 49 LAN Configuration 51 To do first 52 TCP IP parameter configuration 54 Configuration Switches 55 Initialization mode selection 56 Dynamic Host Configuration Protocol DHCP 60 Link configuration selection 63 Automatic Configuration with BootP 64 Storing the settings permanently with Bootp 74 Manual Configuration 75 Contents Solvent Delivery System Description 81 Overview 82 Degasser 83 Principles of Operation 84 Compressibility Compensation 88 Variable Stroke Volume 90 Using the Pump 91 Injection System Description 93 Manual Injector 94 Autosampler 97 Column Oven Description 109 Column Oven 110 Detector Description 111 Detector Types 112 Agilent 1220 Infinity LC Variable Wavelength Detector VWD 113 Agilent 1220 Infinity LC Diode Array Detector DAD 114 Match the Flow Cell to the Column 130 Test Functions and Calibration 135 Agilent 1220 Infinity LC System 137 Solvent Delivery System 139 Autosampler 149 Column Oven 155 Variable Wavelength Detector VWD 157 Diode Array Detector DAD 167 1220 Infinity LC Contents 10 Error Information 191 What are Error Messages 194 General Error Messages 195 Pump Error Messages 201 Autosampler Error Messages 213 General Detector Error Messages 222 VWD Detector Error Messages 225 DAD Detector Error Messages 230 1 Maintenance 237 PM Scope of Work and Chec
216. test to fail 160 1220 Infinity LC 1220 Infinity LC Test Functions and Calibration 9 Variable Wavelength Detector VWD Intensity Test Report VWD Intensity Spectrum Intensity counts 4 mm 175000 1800004 Specification Measured Result Accumulated lamp on time 94 35 h Highest intensity gt 320000 cts 7123680 cts Passed Average intensity gt 160000 cts 951488 cts Passed Lowest intensity gt 6400 cts 36384 cts Passed 161 9 162 Test Functions and Calibration Evaluating the VWD Intensity Test Table 39 Limits Intensity Limits counts Highest gt 320000 Average gt 160000 Lowest gt 6400 Table 40 Probable causes of test failure Cause Corrective action Lamp off Switch on the lamp Old lamp Exchange the lamp Absorbing solvent or air bubble in flow cell Ensure the flow cell is filled with water and free from air bubbles Dirty or contaminated flow cell Run the VWD Cell Test Description on page 157 If the test fails exchange the flow cell windows 1220 Infinity LC Test Functions and Calibration 9 Filter Grating Motor Test VWD Filter Grating Test Description The actual position of the filter motor and grating motor is defined as the number of steps from the reference sensor positions The VWD Filter Grating Test counts the number of motor steps required to move the filter motor and grating motor back to the reference sensor position If th
217. the error message is generated Probable cause Suggested actions 1 Defective pump drive assembly Please contact your Agilent service representative 2 Defective main board Please contact your Agilent service representative Missing Pressure Reading 1220 Infinity LC Error ID 2054 The pressure readings read by the pump ADC analog digital converter are missing The ADC reads the pressure signal of from the damper every lms If the readings are missing for longer than 10 s the error message is generated Probable cause Suggested actions 1 Damper disconnected Please contact your Agilent service representative 2 Defective damper Please contact your Agilent service representative 3 Defective main board Please contact your Agilent service representative 203 10 Error Information Motor Drive Power Error ID 2041 2042 The current drawn by the pump motor exceeded the maximum limit Blockages in the flow path are usually detected by the pressure sensor in the damper which result in the pump switching off when the upper pressure limit is exceeded If a blockage occurs before the damper the pressure increase cannot be detected by the pressure sensor and the module will continue to pump As pressure increases the pump drive draws more current When the current reaches the maximum limit the module is switched off and the error message is generated Probable cause Suggested actions 1 Flow path blockage in front
218. the module that hosts the LAN interface 4 Configure your Control Software e g Agilent ChemStation Lab Advisor Firmware Update Tool and use MAC address as host name e g 003043177321 The LC system should become visible in the control software see Note in section General Information DHCP on page 60 1220 Infinity LC LAN Configuration 4 Link configuration selection The LAN interface supports 10 or 100 Mbps operation in full or half duplex modes In most cases full duplex is supported when the connecting network device such as a network switch or hub supports IEEE 802 3u auto negotiation specifications When connecting to network devices that do not support auto negotiation the LAN interface will configure itself for 10 or 100 Mbps half duplex operation For example when connected to a non negotiating 10 Mbps hub the LAN interface will be automatically set to operate at 10 Mbps half duplex If the 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 15 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 1220
219. tions 1220 Infinity LC If holmium oxide filter is contaminated Description Screwdriver Pozidriv 1 PT3 Screwdriver flat blade Wrench 1 4 inch for capillary connections Pair of tweezers p n Description 1 79880 22711 Holmium oxide filter Turn the lamp s off Remove the front cover Remove the flow cell see Exchanging a Flow Cell on page 300 See also Declaration of Conformity for HOX2 Filter on page 371 11 The glass tends to build a film on its surface even under normal environmental conditions This is a phenomenon which can be found also on the surface of several other glasses and has something to do with the composition of the glass There is no indication that the film has an influence on the measurement Even in the case of a thick film which scatters the light remarkably no shift of the peak positions is to be expected A slight change in the absorbance might be possible Other components within the light path lenses windows are also changing their behavior over the time 311 11 Maintenance Diode Array Detector DAD 1 Unscrew the six screws and remove the flow cell cover 2 If not already in this position move the filter up e Q Ts W 7 L a 3 While releasing the holder with a screw driver at the top carefully remove the holmium oxide filter Do not scratch the
220. to evaluate the intensity spectrum The test is used to determine the performance of the lamps and optics see also Cell Test on page 181 When the test is started the 1 nm slit is moved into the light path automatically and the gain is set to zero To eliminate effects due to absorbing solvents the test should be done with water in the flow cell The shape of the intensity spectrum is primarily dependent on the lamp grating and diode array characteristics Therefore intensity spectra will differ slightly between instruments Figure 56 on page 175 shows a typical intensity test spectrum Intensity Test Evaluation The Agilent LabAdvisor ChemStation and Instant Pilot evaluate four spectral ranges automatically and display the limits for each range the measured intensity counts and passed or failed for each spectral range see Figure 56 on page 175 174 1220 Infinity LC 1220 Infinity LC Instrument G1315 c Serial Nurber DE60755000 Operator Date 3 17 2009 Time 1 24 38 PM Intensity Plot Intensity counts 140000 120000 100000 80000 Intensity Test Results Accumulated UV lamp Lowest intensity in Lowest intensity in Lowest intensity in Lowest intensity in on time range 190nm 220nm range 221inm 350nm range 351inm 500nm range 50inm 950nm Highest intensity in range 190nm 350mm Test Functions and Calibration Diode Array Detector DAD gt 2000 gt 5000 gt 2000 gt 20
221. to take control of the phase sequencing with the commutator If the rotor is unable to move or if the C position cannot be reached the error message is generated Probable cause Suggested actions 1 Disconnected or defective cable Please contact your Agilent service representative 2 Mechanical blockage of the module Remove the pump head assembly Ensure there is no mechanical blockage of the pump head assembly or pump drive assembly 3 Defective pump drive assembly Please contact your Agilent service representative 4 Defective main board Please contact your Agilent service representative 208 1220 Infinity LC Error Information 10 Stroke Length Error ID 2206 2216 The distance between the lower piston position and the upper mechanical stop is out of limits pump During initialization the module monitors the drive current If the piston reaches the upper mechanical stop position before expected the motor current increases as the module attempts to drive the piston beyond the mechanical stop This current increase causes the error message to be generated Probable cause Suggested actions 1 Defective pump drive assembly Please contact your Agilent service representative Temperature Limit Exceeded 1220 Infinity LC Error ID 2517 The temperature of one of the motor drive circuits is too high The processor continually monitors the temperature of the drive circuits on the main board If excessive current i
222. to the DCGV and from there to the inlet valve The pump assembly comprises two substantially identical plunger chamber units Both plunger chamber units comprise a ball screw drive and a pump head containing one reciprocating sapphire plunger A servo controlled variable reluctance motor drives the two ball screw drives in opposite directions The gears for the ball screw drives have different circumferences ratio 2 1 allowing the first plunger to move at twice the speed of the second plunger The solvent enters the pump head close to the bottom limit and leaves it at its top The outer diameter of the plunger is smaller than the inner diameter of the pump head chamber allowing the solvent to fill the gap in between The first plunger has a stroke volume in the range of 20 100 uL depending on the flow rate The microprocessor controls all flow rates in a range of 1 uL min 10 mL min The inlet of the first plunger chamber unit is connected to the inlet valve which is opened or closed allowing solvent to be drawn into the first plunger pump unit The outlet of the first plunger chamber unit is connected through the outlet ball valve and the damping unit to the inlet of the second plunger chamber unit The outlet of the purge valve assembly is then connected to the chromatographic system 1220 Infinity LC Solvent Delivery System Description 5 Principles of Operation Chamber 1 Chamber 2 Purge valve gt Tocolumn Inlet valv
223. ton and insert the straightened paper clip into the slit a j 1220 Infinity LC 283 11 Maintenance Autosampler 3 Rotate the gripper arm slowly from left to right and apply a gentle pressure to the paper clip The clip will engage on an internal catch and the rotation of the arm will be blocked 4 Hold the paper clip in place press the gripper release button and rotate the gripper arm to the right S 6 Replace the gripper arm by holding the paper clip in place pushing the gripper arm into the holder and rotating the gripper arm to the left LAK NY Next Steps 7 On completion of this procedure Install the front cover 8 Turn the power to the Instrument ON 284 1220 Infinity LC Maintenance 11 Variable Wavelength Detector VWD Introduction This section describes simple maintenance and repair procedures for the detector that can be carried out without opening the main cover Table 46 Detector maintenance and repair Procedure Typical Frequency Notes Exchanging the deuterium If noise and or drift exceeds your application A VWD test should be performed after lamp limits or lamp does not ignite replacement Exchanging the flow cell If the application requires a different flow cell A VWD test should be performed after type replacement Repairing the flow cell If leaking or if intensity drops due to contaminated A pressure tightness test s
224. tor Detector G4288C G4290C A Solvent Selection Valve SSV Upgrade Kit G4280 68708 is available 1220 Infinity LC 11 1 Introduction Early Maintenance Feedback 12 EMF counters for the pump The user settable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements The wear of pump components is dependent on the analytical conditions Therefore the definition of the maximum limits needs to be determined based on the specific operating conditions of the instrument The Agilent 1220 Infinity LC pump provides a series of EMF counters for the pump head Each counter increments with pump use and can be assigned a maximum limit that provides visual feedback in the user interface when the limit is exceeded Each counter can be reset to zero after maintenance has been done The pump provides the following EMF counters Pump liquimeter The pump liquimeter displays the total volume of solvent pumped by the pump head since the last reset of the counters The pump liquimeter can be assigned an EMF maximum limit When the limit is exceeded the EMF flag in the user interface is displayed Seal wear counters The seal wear counters display a value derived from pressure and flow both contribute to seal wear The values increment with pump usage until the counters are reset after seal maintenance Both seal wear counters can be assigned an EMF maximum limit When the
225. trance slit the grating and the photodiode array with front end electronics The spectrograph lens refocuses the light beam after it has passed through the flow cell The sampling interval of the diode array is lt 1 nm over the wavelength range 190 950 nm Depending on the wavelength this varies from 1 0 to 1 25 diodes per nanometer for example a diode every 0 8 to 1 nm For a small wavelength range the small non linearity could be neglected With the wavelength range from 190 950 nm a new approach is required to achieve wavelength accuracy over the full range Each spectrograph is calibrated individually The calibration data is stored in the spectrograph on an EEPROM Based on these data the built in processors calculate absorbance data with linear intervals 1 0 2 0 between data points This results in an excellent wavelength accuracy and instrument to instrument reproducibility The micro slit system makes use of the mechanical properties of silicon combined with the precise structuring capabilities of bulk micro machining It combines the required optical functions slit and shutter in a simple and compact component The slit width is directly controlled by the micro processor of the instrument and can be set as method parameter 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 refl
226. ts and evaluates the results automatically The following tests are run e Filter Test Slit Test Dark Current Test e Intensity Test Wavelength Calibration Test Holmium Test e Spectral Flatness Test ASTM Noise Test optional The self test can be run once or repetitively When set up to run repetitively the tests run in series continually until stopped by the user Running the test repetitively is useful when troubleshooting problems which occur intermittently The ASTM noise test determines the detector baseline noise 254 nm while pumping water at 1 mL min The test requires approximately 20 minutes to run and can be included or excluded from the self test sequence as required Setup of the self test is done in the Self Test dialog box Select either Single Test or Repetitive Tests Check the ASTM Noise Test checkbox to include the noise test in the self test 167 9 Test Functions and Calibration Diode Array Detector DAD Fy Agilent G1315 Self Test Results More INFO Limits Measured Result 0 005 0 5 AU 0 27 AU 07 13 1 08 Passed 0 12000 cts 7977 8026 cts Min intensity 190nm 220nm gt 2000 cts 18042 cts Min intensity 221 nm 350nm gt 5000 cts 28451 cts Min intensity 351nm 500nm gt 2000 cts 16886 cts Min intensity 501nm 950nm gt 2000 cts 14683 cts Max intensity 190nm 350nm lt 450000 cts 89461 cts Max intensity 700nm 950nm lt 300000 cts 63609 cts Max intensity D
227. ty decrease is not detected the error message is generated Probable cause 1 Motor is not connected 2 Defective motor 3 Defective missing grating or filter 4 Cable connector defective Filter Missing Error ID 7816 The filter motor is not detected Probable cause 1 Filter motor is not connected 2 Cable connector defective 226 Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Please contact your Agilent service representative Suggested actions Please contact your Agilent service representative Please contact your Agilent service representative 1220 Infinity LC Error Information 10 Grating or Filter Motor Errors Error ID Grating 7800 7801 7802 7803 7804 7805 7806 7808 7809 Filter 7810 7811 7812 7813 7814 7815 7816 The motor test has failed Test 0 Failed Filter motor Test 1 Failed Grating motor During the motor tests the detector moves the motor to the end position while monitoring the end position sensor If the end position is not found the error message is generated Probable cause Suggested actions 1 Motor is not connected Please contact your Agilent service representative 2 Defective motor Please contact your Agilent service representative 3 Defective missing grating or filter Please contact your Agilent service
228. u know little about the analytes in your sample use both lamps and store all spectra over the full wavelength range This provides full information but fills up your disk space rather quickly Spectra can be used to check a peak s purity and identity Spectral information is also useful to optimize wavelength settings for your chromatographic signal The detector can compute and store at run time up to 8 signals with these properties e sample wavelength the center of a wavelength band with the width of sample bandwidth BW and optionally e reference wavelength the center of a wavelength band with the width of reference bandwidth The signals comprises a series of data points over time with the average absorbance in the sample wavelength band minus the average absorbance of the reference wavelength band Signal A in the detector default method is set to sample 250 100 reference 360 100 that is the average absorbance from 200 300 nm minus the average absorbance from 300 400 nm As all analytes show higher absorbance at 200 300 nm than at 300 400 nm this signal will show you virtually every compound which can be detected by UV absorbance Many compounds show absorbance bands in the spectrum Figure 40 on page 120 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 s
229. uch the electrical components Always use ESD protection for example an ESD wrist strap when handling electronic boards and components WARNING Eye damage by detector light 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 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 1220 Infinity LC 241 11 Maintenance Solvent Delivery System 242 Introduction The Agilent 1220 Infinity LC pump is designed for easy repair The procedures described in this section can be done with the pump in place in the rack The most frequent repairs such as exchanging the plunger seals or purge valve seal can be done from the front of the pump Table 44 Simple repair procedures overview Procedure Typical frequency Notes Checking and cleaning the solvent filter Exchanging the Passive Inlet Valve Exchanging the Outlet Ball Valve Exchanging the Purge Valve Frit or the Purge Valve Exchanging the Purge Valve Frit or the Purge Valve Exchanging the Pump Seals Seal Wear in Procedure Removing the pump head assembly Exchanging the Plungers If solvent filte
230. uilt in Test Chromatogram This function is available from the Agilent ChemStation Lab Advisor and Instant Pilot The built in Test Chromatogram can be used to check the signal path from the detector to the data system and the data analysis or via the analog output to the integrator or data system The chromatogram is continuously repeated until a stop is executed either by means of a stop time or manually The peak height is always the same but the area and the retention time depend on the set peakwidth see example below Procedure Using the Agilent LabAdvisor This procedure works for all Agilent 1200 Infinity detectors DAD MWD VWD FLD and RID The example figure is from the RID detector 1 Assure that the default LC method is loaded via the control software 2 Start the Agilent Lab Advisor software B 01 03 SP4 or later and open the detector s Tools selection 3 Open the test chromatogram screen Tools Test Chromatogram Current Status Disabled Switch Test Chromatogram on Switch Test Chramatogram off 4 Turn the Test Chromatogram on 5 Change to the detector s Module Service Center and add the detector signal to the Signal Plot window 1220 Infinity LC 183 9 Test Functions and Calibration Diode Array Detector DAD 6 To start a test chromatogram enter in the command line STRT Set heater temperature 35 Send Generic command line stor 7 Send A Signal configuration Available signals Signal A mA G
231. unter autosampler 13 detector 14 injection valve 13 liter 12 needle movement 13 sealwear 12 cuvette holder 292 D D A converter 188 DAC Agilent LabAdvisor 188 Instant Pilot 189 dark current 158 test 172 data evaluation 20 declaration of conformity 371 degasser exchange 148 delay volume 21 86 87 delivery checklist 30 description 94 detection type 24 detection compound classes 126 detector EMF counters 14 features 113 DHCP general information 60 setup 61 diagnostic tables 138 dimensions 19 diode array 116 116 width 26 draw 151 drift ASTM and noise 26 374 drift 24 DSP notrunning 234 dual plunger in series design 82 dual channel gradient valve 260 E Early maintenance feedback 20 EE 2060 206 electronic waste 370 electrostatic discharge ESD 241 243 EMF pumphead 12 EMF counters pump 12 encoder missing 201 entrance slit 116 environment 18 error message ADC hardware error 225 error messages arm movement failed 213 calibration failed 225 compensation sensor open 195 compensation sensor short 195 diode current leakage 231 DSP notrunning 234 encoder missing 201 fan failed 196 filter check failed 226 filter missing 226 grating missing 227 grating filter motor defective 227 heater current missing 228 heater failed 222 heater power at limit 222 holmium oxide test failed 228 233 illegal temperature value from sensor at air inlet 223 illegal value from sensor on main board 223
232. ure 37 on page 104 for motor identification Motor 0 temperature X axis motor Motor 1 temperature Z axis motor Motor 2 temperature Theta gripper rotation motor Motor 3 temperature Gripper motor motor for gripper fingers The processor monitors the current drawn by each motor and the time the motor is drawing current The current drawn by the motors is dependent on the load on each motor friction mass of components etc If the current drawn is too high or the time the motor draws current is too long the error message is generated Probable cause Suggested actions 1 Mechanical obstruction Ensure unobstructed movement of the transport assembly 2 High friction in the transport assembly Please contact your Agilent service representative 3 Motor belt tension too high Switch OFF the autosampler at the power switch Wait at least 10 min before switching on again 4 Defective motor Please contact your Agilent service representative 5 Defective transport assembly flex board Please contact your Agilent service representative 1220 Infinity LC 217 10 Error Information Needle Down Failed Error ID 4018 The needle arm failed to move down into the needle seat The lower position of the needle arm is monitored by a position sensor on the sampling unit flex board The sensor detects the successful completion of the needle movement to the needle seat position If the needle fails to reach the end point or if t
233. urrent exceeds the upper limit the error message is generated Probable cause 1 Defective PDA optical unit 2 Defective connector or cable UV Ignition Failed 1220 Infinity LC Error ID 7452 The UV lamp failed to ignite Suggested actions 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 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 231 10 Error Information 232 UV Heater Current Error ID 7453 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
234. valve 2 Using the 14 mm wrench loosen the valve and remove it from the pump body 3 Check that the new valve is assembled correctly and that the gold seal is present if the gold seal is deformed it should be replaced Figure 66 Outlet ball valve 4 Reinstall the outlet valve and tighten the valve 248 1220 Infinity LC Maintenance 11 Solvent Delivery System 5 Reconnect the valve capillary Valve capillary Outlet valve 1220 Infinity LC 249 11 Maintenance Exchanging the Purge Valve Frit or the Purge Valve When Frit when plunger seals are exchanged or when contaminated or blocked pressure drop of gt 10 bar across the frit at a flow rate of 5 mL min of H20 with purge valve opened Purge valve if internally leaking Tools required Description Wrench 1 4 inch Wrench 14mm Pair of tweezers OR Toothpick Parts required p n Description 1 01018 22707 PTFE frits pack of 5 1 G4280 60061 Purge valve Preparations Switch off pump at the main power switch Remove the upper front cover 1 Using a 1 4 inch wrench disconnect the pump outlet capillary at the purge valve 2 Disconnect the waste tube Beware of leaking solvents due to hydrostatic pressure 3 Using the 14 mm wrench unscrew the purge valve and remove it 4 Remove the seal cap from the purge valve 250 1220 Infinity LC Maintenance 11 Solvent Delivery System 5 Using a pair of tweezers or a toothpick remove the frit Val
235. ve appropriate safety procedures for example wear goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used CAUTION Electronic boards and components are sensitive to electrostatic discharge ESD ESD can damage electronic boards and components gt In order to prevent damage always use an ESD protection when handling electronic boards and components 1220 Infinity LC 243 11 Maintenance Checking and Cleaning the Solvent Filter WARNING Small particles can permanently block the capillaries and valves of the pump Damage to the Agilent 1220 Infinity LC pump gt Always filter solvents gt Never use the pump without solvent inlet filter If the filter is in good condition the solvent will freely drip out of the solvent tube hydrostatic pressure If the solvent filter is partly blocked only very little solvent will drip out of the solvent tube 244 1220 Infinity LC Maintenance 11 Cleaning the Solvent Filter When If solvent filter is blocked Parts required Description Concentrated nitric acid 65 Bidistilled water Beaker Preparations Remove solvent inlet tube from the inlet valve 1 Remove the blocked solvent filter from the bottle head assembly and place it in a beaker with concentrated nitric acid 65 for one hour 2 Thoroughly flush the filter with LC gr
236. ve body PTFE frit Gold seal Plastic cap Figure 67 Purge Valve Parts 6 Place a new frit into the purge valve with the orientation of the frit as shown above 7 Reinstall the cap with the gold seal NOTE If the gold seal is deformed exchange it before reinstalling 8 Insert the purge valve into the pump head and locate the pump outlet capillary and the waste tube 1220 Infinity LC 251 11 Maintenance Solvent Delivery System 9 Tighten the purge valve and reconnect outlet capillary and waste tubing Outlet capillary Purge valve Waste tube Figure 68 Exchanging the purge valve 252 1220 Infinity LC Maintenance 11 Removing the Pump Head Assembly When Tools required Preparations Before exchanging the seals Before exchanging the plungers p n Description 8710 0510 Wrench open 1 4 5 16 inch 8710 2392 Hexagonal key 4 0 mm 15 cm long T handle Switch off pump at the main power switch Starting the pump when the pump head is removed may damage the pump drive gt Never start the pump when the pump head is removed 1220 Infinity LC Remove the upper front cover Using a 1 4 inch wrench remove the outlet capillary Disconnect the capillary from the outlet valve 1 2 3 4 Remove the waste tubing and disconnect the inlet valve tubing 5 Remove the capillary at the bottom of the pump head 6 Using a 4 mm hexagonal key loosen the two pump head screws stepwise and
237. ventional 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 WL3 wa i a 3a WLI WL2 Wavelength nm Figure 45 Wavelength Selection for Peak Suppression With a UV visible detector based on a diode array and the correct choice of a reference wavelength setting quantitative detection is possible To 1220 Infinity LC 125 8 Detector Description suppress caffeine the reference wavelength must be set to 282 nm At this wavelength caffeine shows exactly the same absorbance as at 222 nm When the absorbance values are subtracted from each another any indication of the presence of caffeine is eliminated In the same way hydrochlorothiazide can be suppressed if caffeine is to be quantified In this case the wavelength is set to 204 nm and the reference wavelength to 260 nm Figure 46 on page 126 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 and caffeine Wavelength 204 nm No reference Hydrochlorothiazide and caffeine Wavelength 222 nm No
238. w cell 6 mm 5 pL 120 bar 12 MPa 1 G1315 60024 Micro flow cell 3 mm 2 pL 120 bar 12 MPa 1 G1315 60015 High pressure flow cell 6 mm 1 7 uL 400 bar 40 MPa 1 G1315 68716 Nano flow cell kit 6 mm 80 nL 5 MPa Turn the lamp s off Remove the front cover 1 Open the front cover to gain access to the flow cell area 2 Open the flow cell cover Depending on the system setup the inlet capillary might be routed directly from the module above or below to the cell and not to the capillary holder 300 1220 Infinity LC 4 Loosen the thumb screw 1 and remove the flow cell Maintenance 11 Diode Array Detector DAD 3 Disconnect the flow cell inlet capillary top and the waste tubing bottom from the unions outlet capillary bottom with the union 2 is 6 Insert the flow cell while pressing the flow cell holder 5 Remove the flow cell while pressing the flow cell holder NOTE The label attached to the flow cell provides information on part number path length volume and maximum pressure 1220 Infinity LC 301 11 Maintenance 7 Insert the flow cell capillaries into the union holder top is inlet bottom is outlet Tighten the thumb screw and reconnect the waste tubing bottom to the union To check for leaks establish a flow and observe the flow cell outside of the cell compartment and all capillary connectio
239. w speed and injection volume Performance Specifications Agilent 1220 Infinity LC Column Oven 1220 Infinity LC Table6 Performance Specifications Agilent 1220 Infinity LC Column Oven Type Specification Temperature range 5 C above ambient to 60 C 5 C above ambient to 80 C min FW Rev B 06 50 Temperature stability 0 15 C constant Composition and Flow Rate Temperature accuracy 0 8 C Column capacity one 25 cm column Internal volume 6 uL 23 2 24 Site Requirements and Specifications Performance Specifications Agilent 1220 Infinity LC VWD Table 7 Performance Specifications Agilent 1220 Infinity LC VWD Type Specification Comments Detection type Double beam photometer Light source Wavelength range Short term noise ASTM Drift Linearity Wavelength accuracy Maximum data rate Band width Flow cells Analog outputs Deuterium lamp 190 600 nm See Specification Conditions on page 27 lt 0 25 10 AU at 230 nm See Specification Conditions on page 27 lt 1 104 AU h at 230 nm gt 2 AU 5 upper limit See Specification Conditions on page 27 1nm Self calibration with deuterium lines verification with holmium oxide filter 80 Hz 6 5 nm typical Standard 14 pL volume Can be repaired on component 10 mm cell path length and level 40 bar 580 psi pressure maximum High pressure 14 pL volume 10 mm cell path length and 400 ba
240. ween the DAD and the other 1220 modules CAN connection between DAD an instrument mainboard MAC address label LAN connector RS232 serial and remote connectors CAN port Configuration dip switches for boot mode selection A D signal output DAD board only Fuses Power plug Figure 7 Connections of the Agilent 1220 Infinity LC with DAD 42 1220 Infinity LC Installation 3 Connecting and Configuring the Instrument to the Chromatographic Data System The instrument is compatible to the following software for control and data evaluation Agilent ChemStation for LC e EZChrom Software 1 Install your Chromatographic Data System CDS Please refer to the installation documentation that has been delivered with the CDS 2 Start your CDS 3 At the instrument configuration screen enter the Instrument name free of choice and the Instrument type Agilent Compact LC 4 For configuring the module choose Auto Configuration 1220 Infinity LC 43 3 Installation Connecting the Agilent 1220 Infinity LC to the PC The AGILENT 1220 Infinity LC is delivered from factory with the default network configuration settings Configuration dip switches 7 amp 8 set to ON This enables you to quickly connect it via the crossover patch cable part of the accessory kit with your PC Factory default IP address 192 168 254 11 LAN port 06 k Eia D 3 Configuration dip switches S d 3 aby BS piep ple oE c
241. with other fittings When retightening the fittings make sure that they are carefully tightened handtight plus 1 4 turn with a wrench Otherwise damage of the flow cell body or blockage may result 306 1220 Infinity LC Maintenance 11 1 Identify the inlet and outlet capillaries To replace the inlet capillary continue with step Jo replace the inlet capillary use a 4 mm wrench for the fitting J fo j A K YN 9 j y Wy f Vr gt Inlet if C 3 Y Outlet 2 After replacing the outlet capillary fix it handtight first Then do a 1 4 turn with a 4 mm wrench a F bin 7 AAT OW D f j Y 7 Da Outlet 3 To replace the inlet capillary use a 4 mm wrench for the 4 Unscrew the cell body from the heat exchanger and the fitting heat exchanger from the clamp unit Y N lt b lt A N A 3 a N N gh N A O KY Ys RSS OW 3 S XA I OK lt NR 1220 Infinity LC 307 11 Maintenance Dio Arr ay Detector D A D 5 Use a small flat screw driver to carefully lift off the I D tag Shown is the default orientation See Note at the beginning of this section Bs 4 aq 6 Unscrew the fixing screw and unwrap the inlet capillary from the grove in the flow cell body Inlet capillary with heat exchanger 7 Take the new inlet capillary and bend it 90 about 35 mm from its end 8 Bend the capillary again b
242. y 90 as shown below 308 1220 Infinity LC Maintenance 11 Diode Array Detector DAD 9 Insert the capillary into the hole between fixing screw and the inlet fitting 10 The capillary lays in the grove and should be tied around the body in the grove 5 times 11 Insert the fixing screw so that the capillary cannot leave the grove Screw Inlet capillary with heat exchanger 12 Carefully insert the I D tag into the new heat exchanger Shown is the default orientation See Note at the beginning of this section 1220 Infinity LC 309 11 Maintenance 13 Fix the heat exchanger to the clamp unit and the flow cell body to the heat exchanger 14 Fix the inlet capillary to the flow cell body handtight first Then do a 1 4 turn with a 4 mm wrench N N IN N lt NN Om N G N Al Ni 15 Check for a centered holder vs hole If required adjust with the holder screws Next Steps 16 Reconnect the capillaries see Exchanging a Flow Cell on page 300 17 Perform a leak test 18 Insert the flow cell 19 Replace the front cover 20 Perform a Wavelength Verification and Recalibration on page 185 or a Holmium Oxide Test on page 177 to check the correct positioning of the flow cell 310 1220 Infinity LC Maintenance Cleaning or Exchanging the Holmium Oxide Filter When Tools required Parts required Prepara

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