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Service Manual Alltech Model 3300 ELSD

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2. Pin 11 Normally Closed NC Pins 9 10 and 11 on the Model 3300 ELSD can output a TTL contact closure signal to other instruments Consult the appropriate manuals for wiring details Fault Relay Pin 12 Normally Open NO Pin 13 Common Pin 14 Normally Closed NC Pins 12 13 and 14 on the Model 3300 ELSD can output a TTL contact closure signal to stop pump flow when an error occurs on the detector Consult the appropriate manuals for wiring details Gas Connection Connect the nitrogen gas supply tubing to the GAS INLET on the back panel The nitrogen gas supply should be regulated from 65 80 psig A stable gas flow and pressure are necessary for reproducible results The gas must be free of contaminants such as oil water particulates or any other non volatile substances A 0 1um gas filter is built into the instrument Liquid Connection Connect the column effluent line to the LIQUID INLET with a 1 16 male fitting The ID and length of the tubing between the column and the detector should be kept as small as possible to avoid band broadening 0 005 ID tubing is recommended for best results Tubing and fittings are included in the ELSD 3300 accessory kit Drain Setup Attach the drain tubing and clamp included with the detector to the DRAIN OUTLET on the right side of the front panel Extend the tubing to a drain waste container not included either at bench level if the detector is stacked or
3. gt Quartus Il Programmer Chain1 cdf File Edit Options Processing Help da Hardware Setup ByteBlasterll LPT1 Enable real time ISP to allow background programming for MAX II devices Mode Active Serial Programming y Progress JTAG In Socket Programming Passive Serial Add Device T Up 10 Click on the Hardware Setup button and select ByteBlaster LPT1 from the pull down menu 3 Quartus Il Programmer Chain1 cdf File Edit Options Processing Heip E Hardware Setup ByteBlasterll LPT1 m Enable real time ISP Hardware Setup Hardware Settings JTAG Settings Select a programming hardware setup to use when programming devices This programming hardware setup applies only to the current programmer window Currently selected hardware ByteBlasterll LPT1 Available hardware items Server Pot Add Hardware ByteBlasterll Add Device 4 Up Ai Dow System Ready 11 Click on the Add File button and locate the latest version of the FPGA file on your computer The file format should be pof ND Quartus Il Programmer Look in o FPGA Files ex El BE W My Recent Documents Desktop My Network File name 331 6 pof x j aces Files of type POF Files pof Y Cancel 12 Select the file and choose Open Bd NUM Z 13 In the file name row c
4. 17 Replace the preamp board and the 4 preamp board screws 18 Replace the preamp board cover and 4 preamp board cover screws 19 Reconnect the ribbon cable to the preamp board 20 Replace the instrument cover and tighten the cover screws The unit is now ready for use 1301 q 133HS A3H 90 v1 60 ALVA Nd 88 GSA0Udd 882000 ON ONIMVYC 43718 sells xV YONV Ol TYNOLLOVE ee 1 1 WIS oos WHE PIUUORMYYA SI0NVW3 101 TVH3N39 WIMALVN sasi SI YOa y Jo juesuoo JNOY IM sjuejuo2 Aiquiessy 19018 sondo NOLLdIH2S 3d Si JO BUIMDIP siu jo suonpoljipouu 0098 876 278 S1009 1I Pjey1eeg ppoy UDB3ANDM IG0Z CIm OU S89 DI2OSSy YIA Y Jo suojanpoidas uy ou s lpigossv yoay y Jo AjjedoJd ay si Buwbup siyl WLLNAGIANOO JOUSOM 4 Iouu lul YM M S Sdlilliud QvIVEOOG D2 Je SDAOA POSH UDd 1 B E X Z 9s ZLIE000 6c LOOVING J10 18ISDWNON J8USDM 4907 YJOOL 9 9120000 8c 5 6459669 11D9 J91SDNDN dil 8 09 uoqaly 1220000 ZZ J quinN K quuessy 9 vIZeo00 Sulmoig uoeiv DuulM GLY 490 8 sondo vIZE000 9c K quuessy JequunN HULIM esnJ oway 9 8Iz 000 Buimbig uoeillv pub sJeiped eBpunp 81ZE000 Sc M3J9S SUIYODW sdilliud c 9v1VO 16 1102 J8180N9A PDH ssnil 7 8 X ZE 9 981 000 vz J qunN K quuessy 8 c c 000 Buimbig uoeillv JIM punoJ9 A90 8 sondo ZETEOOO ez v EGIYZZZI6 440
5. 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument and set aside 6 Locate the connector s for the zones to be checked The connectors are located on the left side of the processor board at positions J22 J23 and J24 which correspond to lower drift tube upper drift tube and optics block respectively Refer to Section 7 7 1 Electronic Schematic for details 7 Disconnect the connector s from the Processor Board 8 Using a multimeter measure the resistance between the wires If there is infinite resistance then the RTD needs replacement Refer to Section 7 8 2 for details on replacing the RTD s If the RTD s are ok then replace the connectors back to their original positions and replace the 3300 ELSD cover and screws 7 8 1 3 CHECKING THE HEATERS Tools Needed e Anti static strap e Phillips screwdriver e Digital multimeter Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure Power off the unit from the back panel and disconnect the power cord Allow the unit to cool for at least 30 minutes Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel Remove the ELSD cover by carefully sliding it toward the back of the instrument and set aside Locate the connector s on the heater board for the zones to be
6. Dress the RTDs along the bracket and underneath the bracket Reconnect the three RTD connectors to the processor board making sure the RTD labeled 1 is at the top 19 Tie the RTDs wiring with cable ties at the drift tube outlet and the processor board bracket 20 Retighten the drift tube end plates with six screws 21 Reinstall the drift tube insulation making sure it adheres to itself 22 Replace the 3300 ELSD cover and screws 7 8 2 3 THERMOFUSE REPLACEMENT PROCEDURE Tools Needed Anti static strap Phillips screwdriver Scissors Replacement thermofuse s Wire stripper Soldering iron Heat shrink tubing Kapton tape Cable ties Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure 2 Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument 6 Disconnect the three wiring connectors from the heater board located at J4 J5 and J6 The heater wires for the drift tube are labeled Element 1 and Element 2 correspond to the lower drift tube heater zone Element 3 and Element 4 correspond to the upper drift tube heater zone The third unla
7. Replace gas source if necessary Check gas flow path for leaks and remedy Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Replace pressure switch The following errors occurred during initialization The device has not been configured Device heater gas flow and or laser have not been calibrated Please contact a technical service representative to recalibrate Error encountered while setting temperature gas flow or gain The following errors occurred during initialization Device heater gas flow and or laser calibration is out of date last calibrated mm dd yyyy hh mm ss AM PM Please contact a technical service to recalibrate INITIALIZATION ERRORS WHEN OCCURS CAUSES Laser preamp gas flow and or heaters have not been calibrated Unit requires its yearly recalibration 33 SOLUTIONS Calibrate the heaters gas flow and or laser preamp Refer to Section 7 6 for calibration procedures Recalibrate the heaters gas flow and or laser preamp as needed Refer to Section 7 6 for calibration procedures 6 2 PERFORMING DIAGNOSTIC TESTS 6 2 1 NEBULIZER GAS PRESSURE TEST 1 Make sure the inlet gas pressure is set between 65 and 80 psig before starting the test Turn off mobile phase flow Wait several minutes for the detector to stabilize In the software select Maintenance Tests Nebulizer Gas Pres
8. Journal of Liquid Chromatography 11 9 amp 10 1967 2004 1988 Effects of Wavelength of the Laser Beam on the Response of an Evaporative Light Scattering Detector Michel Righezza Journal of Liquid Chromatography 11 13 2709 2729 1988 69 CARBOHYDRATE APPLICATIONS Analysis of Carbohydrates using the Mass Detector R Macrae and J Dick Journal of Chromatography 210 138 145 1981 High Performance Liquid Chromatographic Deter mination of Mono and Oligosaccharides in Vegetables with Evaporative Light Scattering Detection and Refractive Index Detection J Lopez Hernandez M J Gonzalez Castro Naya Alba and C de la Cruz Garcia Journal of Chromatographic Science 36 292 298 1998 GLYCERIDE FATTY ACID OIL APPLICATIONS Determination of Nonvolatile Components of Heated Soybean Oils Separated with High Efficiency Mixed Bed Polystyrene Divinylbenzene Columns S L Abidi I H Kim and K A Rennick Journal of the American Oil Chemists Society 76 8 939 944 1999 Non Aqueous Reversed Phase High Performance Liquid Chromatography of Synthetic Triacylglycerols and Diacylglycerols J T Lin C L Woodruff and T A McKeon Journal of Chromatography A 782 41 48 1997 Simulated Distillation of Heavy Oils Using an Evaporative Light Scattering Detector D M Padlo and E L Kugler Energy amp Fuels 10 5 1031 1035 1996 Fast Monitoring of C20 C160 Crude Oil Alkanes by Size Exclusion Chromato
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10. 4 0L min using the keypad Gain Enter a value of 1 2 4 8 or 16 using the keypad Each increase in gain setting will produce twofold signal amplification over the previous setting Events Events can be added to the method in order to program timed gain changes or timed external output events Timed gain changes can be used so sample compounds of widely varying concentration can be on scale in the same chromatogram Timed external output events can be used to trigger events on other instruments NEW EVENT To add a new timed event use the up down arrows to highlight the New button and press Enter The New Event window will then appear Menu Edit Method Methad Method Pharmaceuticals New Event bo LLL Accept O cance O conca Mode Run Enter the Event Time from 0 60 minutes Enter the Event Type Change Gain or Set Control Relay If Change Gain has been selected then enter the Gain value 1 2 4 8 or 16 If Set Control Relay has been selected select On or Off for the External Contact Once the new event has been created press Accept to save the new event or press Cancel to cancel the new event EDIT EVENT To Edit an existing event use the up down arrows to highlight the event to be edited from the table Then use the right arrow to select Edit and press Enter The Edit Event table will then appear Menu Edit Method Method Method Pharmaceuticals Edit Event ALO Accept O cance
11. 60 to O minutes The y axis range is 500mV to 2 5V To go directly to Zoom from Pan press Enter USER DEFINED SCALE The User Defined Scale screen can be used to enter user defined x axis and y axis values for the chart scaling Select Operation Chart User Defined Scale using the arrows on the keypad and press Enter to reach the User Defined Scale Screen Menu Operation gt Method Method 1 Output 369 2 mY User Defined Scale NM b Jminutes 2000 _ TO Accept O Conca 4 50 3 50 3 00 4 00 5 00 Mode Run Enter the minimum and maximum x axis and y axis values in the window that appears The x axis range is 60 to O minutes The y axis range is 500mV to 2 5V Once the new chart values have been entered press Accept to save the new chart settings or press Cancel to return to the original settings 12 ENABLE DISABLE Y AXIS AUTOSCALE The Enable Y Axis Autoscale function causes the chart to automatically scale to the highest peak and ensures that the chromatogram trace will always be on scale Select Operation Chart Enable Y Axis Autoscale and press Enter to enable this feature Select Operation Chart Disable Y Axis Autoscale and press Enter to disable this feature RESET SCALE The Reset Scale function will zoom out the chart view to its maximum x axis and y axis values 60 to O min 500mV to 2 5V Select Operation Chart Reset Scale using the arrows on the keypad and press Enter to reset the
12. Afterwards the FTP window should look similar to amp CATEMPtapplication File Edit View Favorites Tools Help Back gt A Search y Folders d fr VM X x m Address ftp 192 158 70 10 ni u application iHT Select an item to view its description jaJP zh CN ena Elsd pp exe My Documents ELSDDiagsAPl dll My Network Places E My Network Places 8 ELSDHardware Pl dll My Computer 8 ELSDRemoteAPI dl al Enabled way a Manifest xml E MON EXE gt OpenNETCF dll 9 OpenNETCF Net dl e RemoteServer dll Mj SPLASH BMP 14 Close the FTP connection to the ELSD 15 Reboot the ELSD The normal splash screen should appear 53 7 5 2 PEN DRIVE SOFTWARE UPGRADE PROCEDURE The following procedure should be used to install new application and or OS software on the 3300 ELSD when an initial upgrade procedure isn t necessary Materials Needed e 128MB or less USB pen drive loaded with new software upgrade NOTE Pen drives with greater than 128MB are NOT compatible with the 3300 ELSD 1 First confirm that the new software upgrade files have been properly loaded onto the pen drive The software files should appear on the pen drive similar to the following a Main contents on the pen drive SER File Edit View Favorites Tools Help da Back gt GQSearch y Folders 4 US GS X A Ed Address E Update laa boot losh P ElsdUpgrade exe
13. Bad laser Replace laser and recalibrate preamp laser Refer to Section 7 6 3 for details Bad preamp board Replace preamp board and recalibrate preamp laser Refer to Section 7 6 3 Bad satellite board Replace satellite board Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Change in peak height or loss in Nebulizer drift tube and or optics are Clean the nebulizer drift tube and optics sensitivity dirty as needed Following the cleaning procedures in Sections 5 1 5 4 Autosampler needle not pulling up Repair or replace equipment as needed sample properly or sample loop blockage Bad laser Replace laser and recalibrate the laser preamp Refer to Section 7 6 3 for details Bad preamp board Replace preamp board and recalibrate preamp laser Refer to Section 7 6 3 Bad satellite board Replace satellite board Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Broad peaks Leak s especially between the column Check for loose fittings and tighten if and detector present necessary Tubing between column and detector is Use a shorter piece of 0 005 0 010 ID too long or too large of an ID tubing Cut off peaks Sample concentration too high Decrease sample concentration until peaks are on scale Gain set too hig
14. Materials Needed Crossover Ethernet cable WinCE OS setup files TeraTerm software downloaded onto a pc Serial cable Tftpd32 exe software downloaded onto a pc 1 Configure a standalone PC with a static IP address In these instructions the IP address of 159 97 84 210 is used It doesn t matter what address is used but the rest of the procedure will assume the above address NOTE Make sure this PC is not connected to any other network A DHCP server on the PC will be used to assign an IP address to the ELSD If this PC is connected to a network that already has a DHCP server running both DHCP servers will be assigning addresses to PC s on the network This will cause corrupting and confusion on the network 2 Connect the 3300 ELSD to the PC with a crossover Ethernet cable 3 Copy the OS setup files to a directory on your PC The setup files are boot losh setup losh nk bin 4 Disable any firewall software that may be running on your PC If you are unsure how to do this contact your IS department The firewall will most likely interfere with the DHCP and TFTP Servers 5 Connect the serial cable to the serial port on the 3300 ELSD and the serial port on the PC 6 Run TeraTerm Pro to create a serial connection to the ELSD 7 Power up the 3300 ELSD while holding down the q key on the PC keyboard This should produce output similar to the following KKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKKK LogicLoa
15. Output 32 2 mY Maintenance gt LO Accept kk CETTE TDI iu I Mode Run Equilibrating Next Cleaning mode EJ Low inlet gas pressure error Laser On Off Press 1 to toggle the Laser On or Off The current signal output value is displayed in mV Gas Flow On Off Press 2 to toggle the Gas Flow On or Off The current gas flow rate and nebulizer gas pressure are displayed Lower Drift Tube On Off Press 3 to toggle the Lower Drift Tube heater On or Off The current Lower Drift Tube Temperature value is displayed Upper Drift Tube On Off Press 4 to toggle the Upper Drift Tube heater On or Off The current Upper Drift Tube Temperature is displayed Optics Block On Off Press 5 to toggle the Optics Block heater On or Off The current Optics Block temperature is displayed The Optics Block heats to 90 of the drift tube temperature set point Press Accept to return to the main screen and the detector will return to its original settings 3 5 2 LOGS VIEW ERROR LOG Select Maintenance Logs View Error Log using the arrows on the keypad and press Enter The View Error Log screen will then appear Menu View Error Log iutput 5 mV Maintenance gt Low inlet gas pressure error LO aos s Each error log entry contains the time of the error the method loaded when the error occurred the mode the detector was in when the error occurred and the description of the error Use the left right arrows on the ke
16. Removable Disk E amp nk fix paffs bin Select an item to view its description Capacity 122 MB O Used 27 0 MB O Free 95 6 MB b Contents inside the Update folder on the pen drive E Update File Edt View Favorites Tools Help Back A Search L Folders ca S Le x r mee Select an item bo view its description See alza Iu Documents idu Network Places My Computer c Contents inside the App folder on the pen drive if Application will be upgraded otherwise this folder would be empty E Update App File Edit View Favorites Tools Help da Back gt QSearch Ly Folders 4 le GE X wd E Address E WUpdater App Select an item to view its description LJ jaJP zh CN en ElsdApp exe y Documents ELSDDiagsAPl dll My Network Places 3 ELSDHardware Pl dl My Computer ELSDRemoteAPI dll el Enabled way IE Manifest ml MON EXE gt OpenNETCF dll gt OpenNETCF Net dll Mf SPLASH BMP d Contents inside the OS folder on the pen drive if OS will be upgraded otherwise this folder would be empty E Update 0S File Edit View Favorites Tools Help sa Back gt j QSearch LY Folders 4 UE GE X A Ed Address E Update 0S a boot losh ES ManifestOS xml z nk bin a setup losh Select an item to view its description See also My Documents My Network Places My Computer 2 Power off the 3300 ELSD 3 Insert the pen drive cont
17. Set 40 0 C 1 5 L min 16 Temperature Output 5 3 mV Gas Flow Gain Low inlet gas pressure error The Operation screen is the main screen displayed during use of the instrument This screen provides the following information for the currently loaded method e Method Name Currently loaded method name e Temperature Set point and read value of the drift tube temperature in C The temperature range is from 25 0 to 120 0 C NOTE There are two heated zones in the drift tube a lower zone and an upper zone The value displayed on the main screen is the average value for the two zones The individual values are displayed in the Manual Control screen see Section 3 5 1 for details e Gas Flow Set point and read value of the nebulizer gas flow rate in L min The gas flow range is from 0 0 to 4 0L min e Gain Current gain setting Possible gain values are 1 2 4 8 and 16 A gain setting of 1 produces an unamplified signal and each increase in gain setting produces twofold signal amplification over the previous setting Signal Output The signal output in mV is displayed when the instrument is in Run or Cleaning modes The output is not displayed in Standby or Heating modes If the output value exceeds 2 5V the signal output will read High If output drops below 500mV the signal output will read Low e Method Run Time The elapsed time for the method run is displayed in the upper right corner if a method r
18. The Model 3300 ELSD can be configured for the following languages English Spanish French German Italian Chinese Simplified Korean and Japanese The detector must contain the proper software versions in order to be compatible with certain languages consult Grace Discovery Sciences for further details Select Configuration Language using the arrows on the keypad and press Enter The Language Configuration screen will then appear KA tls od Menu Mnthad r f l Language Configuration Output Configuration gt Enalish O Accept Cancel Boone MUUL gt oLaMuo y Use the up down arrows to select a language from the list Press Accept to save the new language configuration or press Cancel to cancel the new language configuration If Accept has been entered the Restart Device screen will then appear Menu Mathad Matf auilt Riathad Language Configuration Restart Device Enalisl Output Configuration gt O Accert cancel MEE MUU gt oLaMmuo y The unit must be restarted before the language change can take effect Select Yes to restart the device and change the language or select No and the new language will take effect the next time the unit is rebooted 16 3 4 8 PRESSURE UNITS Select Configuration Pressure Units using the arrows on the keypad and press Enter The Pressure Units Configuration screen will then appear Method Default Method Set Read Pressure Units Config
19. back of the instrument Disconnect the three connectors from the heater board located at J4 J5 and J6 The heater wires for the drift tube are labeled Element 1 and Element 2 correspond to the lower drift tube heater zone Element 3 and Element 4 correspond to the upper drift tube heater zone The third unlabeled connector contains the wires for the optics block heaters Cut the cable tie holding the heater wires by the heater board Remove the drift tube insulation by finding the seam and peeling it apart Loosen the drift tube end plates by removing six screws to rotate the drift tube assembly as needed Cut the Kapton tape wrapped around the drift tube If replacing the drift tube heater continue on to step 12 If replacing the optics block heaters proceed to step 17 Peel off the RTD s from the drift tube Peel off the heater from the drift tube Remove the resettable fuses and thermofuses from the drift tube Replace the drift tube heater assembly by peeling off the protective film Make sure the drift tube heater outer surface is clean to ensure good adhesion The wiring for Element 1 and Element 2 should be towards the front Tape the drift tube heater to the drift tube at the ends and middle with Kapton tape Tape the RTDs to the drift tube with Kapton tape Tape the resettable fuses and thermofuses to the drift tube with Kapton tape 18 19 20 21 22
20. connect it to the LIQUID INLET on the left side of the front panel on the detector The tubing between the column and the nebulizer should be a short as possible 0 005 ID tubing is recommended Turn the pump on to the desired flow rate Do not exceed the recommended maximum solvent rates Check connections for leaks and tighten the fittings if necessary Observe the signal output on the display and the recorded baseline After an initial large rise when the pump is turned on the signal level should drop close to the gas only level after several minutes If it remains high after sufficient equilibration time the mobile phase may be contaminated column fines buffers etc or the temperature or gas flow settings may be too low for optimal evaporation of the mobile phase Take corrective measures and allow the system to re equilibrate for a few minutes The detector is ready for sample analysis The first time the Model 3300 ELSD is used you may want to reproduce the Model 3300 ELSD QC procedure Refer to Section 7 9 for details 4 5 SHUTDOWN SEQUENCE 1 2 Turn off the mobile phase flow Allow gas only to flow for approximately five minutes to clear any remaining droplets Put the detector in Standby mode Operation Mode Standby Turn off the gas supply at the source if required Power off the ELSD using either the soft power button on the front panel or the main power switch on the rear panel If the E
21. 4 Optics Heating I Ig S 1uuu uuu iaa 37 6 275 Heater Stability Testa Y 38 6 2 6 Power SUDDIV Test toa a o See 39 6 5 Diagnosing Baseline NOS U U U u u u uu u 40 0 4 Troubleshooting ChartSu uyu u toe veo u uav aaa uuspayka qa rogus Yao CU sa Vra DAA la AEREA RA EUM a Vv 41 6 5 Software Troubleshooting Procedure U U u u uu u uu u 44 fi iuge minds a 45 ESO uere dada 45 7 2 ero ic odlarrergerr li o Meet EMT 45 La Replacement Parts neri carnicero caerle UE avr dina FROM LZ 46 LOT MES RIDERE I ILLE 46 7 5 Software Upgrade Procedures uoce u u Sc EN cardiaco cien 47 7 5 1 Complete Software Re Installation Procedure 47 1 9 1 1 FPGA Installation POCO UT ocio a E Y Cue xn xu eei agua Er Re 47 TOZ LOLO Upgrade Procedure iio icruden abe rige cce rur Rad laa 49 7 5 1 3 WinCE OS Initial Setup Procedure 50 7 5 1 4 Application Initial Setup Procedure 52 7 5 2 Pen Drive Software Upgrade Procedure e u 54 16 GaliDFation Procedures PE 56 7 6 1 Heater Calibration cor cscsenevescusaenszsuerensstaneussanteonensgutouunnebeqensecasnznesuasensersunaennssunnessasancneniatenmsianu
22. Ipd077 Fri Aug 12 10 08 23 CDT 2005 CPLD_CE_REG_REVISION 0x32 6 Examine the version number listed in step 5 If it begins with 2 0 5 or a larger number the procedure can be stopped no upgrade is necessary If the version begins with a number that is less than 2 0 5 continue with step 7 7 Install the LOLO upgrade file onto the PC 8 On the serial terminal run the following command update 49 The output should be send update file 9 On the PC using TeraTerm Pro a Select File gt Send File b Navigate to the directory where the LOLO upgrade files were placed c Inthe Send File dialog box make sure that Binary is checked under Option Look in C tmp da t E Ez 1004077_boot elf i UP E 1004077_lolo_ram elf 1004077 Release Notes txt Filename 1004077_lolo upd Files of type all Cancel Help Option M Binary d Doubleclick on the file that has an extension of upd to start the download e Inthe above image the name of the file is 1004077 1616 up 10 When the download has completed LOLO will automatically update itself The output should appear similar to the following erasing flash 100 burning flash update done 11 If running the complete software re installation continue on in Section 7 5 1 3 WinCE OS Initial Setup Procedure Otherwise the LOLO installation procedure is complete 7 5 1 3 WinCE OS INITIAL SETUP PROCEDURE
23. OM oem DS 5 Zc ANStalla On ias 6 21 What You WIIUNGGG es ii 6 2 2 UNPICKN ico 6 2 5 Controls ANG Feat fl6S oni comae car sevo creme uyasha EEL aE SU REVO EE FEE taveudeuss 7 2 52 J Eront Panely mua a nM S T UN 7 2 5 2 Back Panel olor 8 2 4 Making Electrical and Fluid Connections lle U U u u u u 9 3 Navigating the Software Interface iii ees dh eh ee ets 10 EMBED ETE Um 10 32 D o Eee p EE A uynuy o MM MIA M o IM Le 10 uM MM op eet 10 2 2 2 Ofart Stop RUN iieri aoo eO ineo 2 EOD eC cu ue COl ou PD UI Ete on Uc IRE Ec Lon ds buco Ac i 11 3 29 LOCKUNIOCK Detector oec dp pr 11 3 24 OF Ogee MST suu uM M MM CM M MU MEN III UE 11 5 2 9 AUTOZOIO doit a cmd sime dir uei sume ELI M DU NU E dd M VELIE 12 3 3 ip iet A A AA AAA A A uuu asqa aby 12 99 l NOW An A eS ey er ee eae er eee 12 992 GI err E 13 SEM MIO ee uz uu umu u tun Su sS skua Sta en ere u S hasa umasa usss 13 A Aero pee 14 xe WIZ d snr e apppustaqupapataspatusppuspussupappuuk qas atan qa qdpupayuamapupa 14 E sre Meer 14 SAT Alain oem 14 342 Serial NUImDOE nani FR a E 15 S elc AA A A AAA E A A do 15 CP MEDICAE 15 OAD Hed erS u uu basa T DL DLL 15 54 0 Date and TIME mee 16 JAS Language ista A da 16 54 8 Pressure UNS loo 16 OAD rolg str acia 16 3 4 10 Timed Mode Changes cruce A A A Rs 16 39 Mamtena e on a 17 3 54 Manual Control criar tl 17 9 9 2 o A o II A M od PLIN C DUE PIOS OD DEM De
24. RTD s if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater Check heater Replace heater if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater board Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 for details Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Optics block temperature not Thermal fuse may be blown Allow the resettable fuses 2 hours to reset Then reaching set point recheck the thermofuse and replace if necessary Refer to Section 7 8 for details Heater calibration is off Recalibrate heaters Refer to Section 7 6 1 for details 41 TROUBLESHOOTING continued 1 PROBLEM CAUSE SOLUTION Optics block temperature not Bad RTD s Check RTD s Replace RTD s if bad reaching set point continued and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater Check heater Replace heater if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater board Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 for details Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details No gas flow Gas source valve is closed Open gas valv
25. an analysis of 5 minutes The only peak will be Hydrocortisone eluting at 3 3 5 minutes Make three 20uL injections of Hydrocortisone at a concentration of 2 ug mL Measure the noise for three 0 2 0 4 minute regions on the baseline Use the average noise value to calculate the signal to noise ratio Calculate the average signal to noise ratio from all three injections The average signal to noise ratio should be equal to or greater than 15 with no more than two random spikes larger than the noise per injection Drift and Noise Evaluation C18 column in line and continue running the detector at the same conditions as in the Sensitivity section drift tube set to 40 C gas flow set to 1 5L min and gain set to 16 with mobile phase running 55 45 acetonitrile water at 1 0mL min Collect a baseline trace for 15 minutes From this 15 minute baseline trace determine the baseline drift by subtracting the lowest voltage reading from the highest voltage reading The baseline drift should be less than or equal to 5mV 66 4 Measure the highest and lowest mV readings in each of the three 2 minute intervals 2 2 2 min 7 7 2 min and 12 12 2 min in the 15 minute baseline trace to determine the system noise The average noise should be less than or equal to 2 mV during the 15 minute baseline trace Note Due to the sensitivity of the detector small random spiking will occur This is normal as long as the spikes are included in
26. at floor level Make sure the container is sealed to prevent solvent fumes from escaping Monitor the liquid level in the container during operation and decant excess liquid when the level approaches the top of the container CAUTION Do NOT allow the tubing to become submerged in the liquid inside the container Remember that the waste container will contain solvents from your mobile phase and should be disposed of properly Signal Output Connect the signal cable provided with the unit to the SIGNAL OUTPUT port on the back panel of the detector and connect to your data collection device 10 Exhaust Tubing Connect the exhaust tubing included with the unit to the EXHAUST outlet on the rear panel of the unit Extend the tubing to the hood ventilation system There should be no low spots in the tubing where condensate can collect NOTE Make sure the exhaust system provides adequate but not excessive suction Excessive suction can cause a noisy baseline 3 NAVIGATING THE SOFTWARE INTERFACE The Model 3300 software interface features a collapsible menu located in the upper left corner of the LCD screen The following sections describe the software menu options in detail The Help Button can be pressed in many software screens in order to access Help Screens which offer assistance with using the software functions 3 1 MAIN SCREEN 6 43 min Menu Operation gt Method Method 1 Read 40 0 C 0 0 L min
27. calibration issues i e if the unit is uncalibrated or if the calibration is out of date OPERATION ERRORS WHEN OCCURS CAUSES SOLUTIONS Drift tube temperature Drift tube temperature Bad RTD s Check RTD s Replace error reading is more than 10 C RTD s if bad and then off its set point recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater Check heater Replace heater if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater board Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 for details Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Blown thermofuse Allow the resettable fuse 2 hours to reset Then recheck the thermofuse and replace if necessary Refer to Section 7 8 for details Optics block temperature Optics block temperature Bad RTD Check RTD Replace RTD if error reading is more than 10 C bad and then recalibrate the off its set point heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater s Check heater s Replace heater s if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Bad heater board Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 for details 31 OPERATION ERRORS continued WHEN OCCURS CAUSES Opti
28. checked The connectors are located at positions J4 J5 and J6 which correspond to lower drift tube upper drift tube and optics block respectively Refer to Section 7 7 1 Electronic Schematic for details Disconnect the connector s from the Heater Board Using a multimeter measure the resistance between the heater wires The heater wires are located on the bottom two rows of the connector If there is infinite resistance between the pair of wires in a row then the heater needs replacement Refer to Section 7 8 2 1 Heater Replacement Procedure for details on replacing the heater s If the heater s are ok then replace the connector s back to their original position s and replace the 3300 ELSD cover and screws 63 7 8 2 HEATER RTD AND THERMOFUSE REPLACEMENT PROCEDURES 7 8 2 1 HEATER REPLACEMENT PROCEDURE Tools Needed Anti static strap Phillips screwdriver Scissors Replacement heater s Kapton tape Cable ties Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 10 11 12 13 14 15 16 17 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel Remove the ELSD cover by carefully sliding it toward the
29. ed Jay enl Ud WO Way WAL SQSVMO L 9 WALI JO SOVAYNS JAHNO NOLLISOd SALON MIEGWASSV MOO 18 SN3T1 dINVddd v S INDI 5 5 FUSE REPLACEMENT donc Only suitably qualified personnel should carry out these adjustments disc Shock hazard disconnect the power cord before replacing the fuse A WARNING Fire hazard only use the same type and rated CERTIFIED fuse 6 amp 4 250V 5A FP 1 Power off the detector from the back panel and unplug the power cord 2 Gently squeeze the side tabs of the fuse drawer and pull the fuse drawer straight out Refer to Figure 5 5 for details 3 Remove the blown fuse and replace with the new fuse Be sure to use the appropriate fuse 5 Amp 250V Make sure the replacement fuse is placed into the fuse slot on the right side of the fuse drawer 4 Replace the fuse drawer Make sure the fuse inserts into the fuse slot on the right side of the fuse block The correct slot has a metal contact inside the fuse block Figure 5 5 Model 3300 ELSD Fuse Block 30 6 DIAGNOSTICS AND TROUBLESHOOTING 6 1 ERRORS The main screen will list any errors currently occurring on the instrument in the lower right corner Operation error messages will remain until the error condition is remedied Operation errors relate to temperature and gas flow accuracy during operation Initialization errors will appear on bootup for 15 seconds and then disappear Initialization errors relate to
30. editing method Operation gt Configuration Maintenance gt Temperature 40 0 C Gas Flow 1 50 L min Gain 16 muut Kuri Finished The final screen in the Method Wizard provides the recommended Temperature Gas Flow and Gain settings based on the mobile phase solvent composition mobile phase flow rate and sample concentration Press Finish to continue creating the method and the New Method window will appear or press Cancel to cancel the Method Wizard 3 4 CONFIGURATION 3 4 1 ALARM The Alarm function can be used to sound an alarm when errors occur on the detector Select Configuration Alarm using the arrows on the keypad and press Enter to bring up the Alarm Configuration window Operation gt Method gt Alarm Configuration Output Configuration gt 378 2 mY Maintenance gt Alarm Disabled 4 500 0 60 00 Mode Run 50 00 40 00 30 00 20 00 14 Use the left right arrows to select Enabled or Disabled If Enabled the alarm will sound when errors occur on the unit and will continue to sound until the errors are remedied If Disabled the alarm will not sound when errors occur on the unit Press Accept to save the alarm configuration or press Cancel to return to the original alarm configuration 3 4 2 SERIAL NUMBER This function is available in Service Tech Mode only To configure the serial number on the detector first enter Service Tech mode by selecting Mainte
31. environment while performing this procedure Power off the unit from the back panel and disconnect the power cord Allow the unit to cool for at least 30 minutes 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel Remove the ELSD cover by carefully sliding it toward the back of the instrument and set it aside CAUTION The optics block and drift tube may still be hot 6 Disconnect the ribbon cable from the preamp board Allow it to hang inside the unit 7 Remove the 4 preamp cover screws using the Phillips screwdriver and remove the preamp cover 8 Remove the 4 preamp board screws using the Phillips screwdriver and remove the preamp board Set the preamp board aside 9 Remove the 4 preamp mount plate screws using the Phillips screwdriver and remove the preamp mounting plate 10 Remove the 4 screws connected to the preamp lens assembly using the 7 64 hex driver 11 Flip the preamp lens assembly and remove the 4 screws using the 3 32 hex driver 12 Remove the lens and clean with acetone and cleaning wipes until no fingerprints smudges or dirt remain 26 13 Carefully replace the lens make sure the curved surface faces toward the aperture 14 15 Replace the 4 screws to the preamp lens assembly Replace the preamp lens assembly onto the optics block with the 4 screws 16 Replace the preamp mount plate onto the optics block with the 4 screws
32. is loaded yet but WinCE is running and the ELSD can be accessed with telnet and FTP Continue on to Section 7 5 1 4 Application Initial Setup Procedure 7 5 1 4 APPLICATION INITIAL SETUP PROCEDURE Materials Needed e Crossover Ethernet cable e Application upgrade files e Tftpd32 exe software installed on a pc 1 Configure a standalone PC with static IP address In this example an address of 159 97 84 210 will be used It doesn t matter what address is used but the rest of the procedure will assume the above address NOTE Make sure that this PC is not connected to any other network A DHCP server will be run on the PC to assign an IP address to the ELSD If this PC is connected to a network that already has a DHCP server running both DHCP servers will be assigning addresses to PC s on the network This will cause corrupting and confusion on the network 2 Connect the crossover Ethernet cable to the 3300 ELSD and the PC 3 Start running the Tftpd32 exe software Make sure it is configured the same as described in Section 7 5 1 3 WinCE OS Initial Setup Procedure steps 9 13 4 Power up the 3300 ELSD 52 5 Prior to upgrading the application the IP address of the ELSD must be determined In step 15 of Section 7 5 1 3 WinCE OS Initial Setup Procedure the IP address of the ELSD was recorded Use this IP address The rest of this procedure assumes the ELSD was assigned the IP address 159 97 84 10 6 The ELS
33. psta DENS HOD LEAL CES 18 ERO A A IY Er 18 SEIT MENU ND E 18 9 5 5 Service A 19 356 CaliDFatlOM e 19 O 19 4 Routine Opera ON ossaa 20 ARM Safety PNE 20 4 2 Operating NOLES ainia aaa 20 4 3 Selecting Initial Operating Conditions U U u u u u u 20 AA SLAP Sequence uuu u L u tua Ec 20 4 5 Shutdown Se6quehCce uu uy uapa aisasasha payapa qasapuyasppusaqhsapstapsasaryapiaqppasaq squstaqapapansaugasqisaqapatatupapasa 21 4 0 Optimization Procedure uc uu u uta m u uuu suu suttu usss 21 Mucius nin 22 31 Cleaning Mode A A OS 22 5 2 Nebulizer Cleaning Procedure uni id 22 5 3 Drift Tube Cleaning Procardia 23 5 4 Optics Cleaning Procedures ona diia criada 24 5 4 1 Optics Block Cleaning Procedure uuu uuu da 24 5 4 2 Laser Window Cleaning Procedure U U u u u u 25 5 4 3 Photodiode Cleaning Procedure aa 25 5 4 4 Pre Amp Lens Assembly Cleaning Procedure 26 o AAA r a a 30 Diagnostics and Troubleshooting 31 Ol cicer de 31 6 2 Performing Diagnostic T OSES usina 34 6 2 1 Nebulizer Gas Pressure estu u uu aa a y ua h au anpi wauu a 34 0 2 2 Gas FIOW Iestuuuuy uuu ii 35 52 9 ODUCS TEST tarios 36 6 2
34. smo mac Q0 098 606 007293 77 1ps 159 97 94 190 mask 25955 255 259540 gw IL59 97 92 210 16 In the above output the IP address assigned to the ELSD is 159 97 84 10 Write down this address it will be needed during the application installation procedure If the IP address is all O s wait a few more seconds and try it again Next a YAFFS partition will be created in the flash on the card engine This partition will be used to store the OS image as well as the application and supporting data files To do this complete the following sequence of commands a Erase the flash that the partition will exist in erase 0x00040000 0x01fc0000 The expected output from this command is unlocking flash blocks erasing flash 100 erased dev flash0 start 0x40000 len 0x1fc0000 bytes ini x Current Directory Ftp Browse Server interface 159 37 84 210 Show Dir Help 51 b Create the partition add yaffs app nor 0x00040000 0x01fc0000 The expected output from this command is add yaffs inserted start 0x40000 len Ox1fc0000 c Mount the partition mount yaffs app The expected output from this command is Mounting a YAFFS partition Starting YAFFS file system Current YAFFS partition table er app 00000000 0000007e 0 e lt NULL gt 21 lt NULL gt a8 lt NULL gt YAFFS initialized 17 Next you need to load the OS image and initial boot files from the TFTP server The ELSD wil
35. test has failed refer to the following table Power Supply Test for possible fail messages and their solutions POWER SUPPLY TEST RESULTS RESULT CAUSE SOLUTION Fail 1 5 1 8 3 3 4 Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details 5 12 or 12V 6 3 DIAGNOSING BASELINE NOISE There are many causes for baseline noise Use the table Start diagnosing the noise at A and work down the table until below Diagnosing Baseline Noise to help identify the source the source of the baseline noise is determined DIAGNOSING BASELINE NOISE SYMPTOM SOLUTION A Noise from Column he column may be leaking silica or packing material e Column in line Replace the column e Mobile phase on e Nebulizing gas on e aser on Result Noise disappears when column is removed B Noise from Mobile Phase Current drift tube temperature and gas flow rate settings may e Column removed not be providing adequate evaporation of the mobile phase e Mobile phase on Re optimize gas flow and or drift tube temperature following e Nebulizing gas on the optimization procedure in Section 4 6 e Laseron The nebulizer drift tube and or optics may be dirty Refer to Sections 5 1 5 4 for cleaning procedures Result Noise disappears when pump is stopped The mobile phase may be contaminated with particulate matter Filter the current mobile phase or repl
36. the drift and noise measurements 7 10 VOLATILE MOBILE PHASE MODIFIERS VOLATILE BUFFERS AND MOBILE PHASE MODIFIERS PE MA e mme sm w _ Acids Trifluoroacetic Acid Formic Acid Acetic Acid Carbonic Acid Bases Ammonia 33 35 C Methylamine 16 6 C Ethylamine 6 3 C Triethylamine 89 3 C Buffers Ammonium Formate 3 0 5 0 Pyridinium Formate 3 0 5 0 Ammonium Acetate 3 8 5 8 Pyridinium Acetate 4 0 6 0 Ammonium Carbonate 8 0 adjusted used for reverse phase Ammonium Carbonate 5 5 7 5 and 9 3 11 3 lon Pair Reagents Pentafluoropropionic Acid 96 97 C Heptafluorobutyric Acid 120 C Nonafluoropentanoic Acid 140 C Pentadecafluorooctanoic Acid 189 C Tridecafluoroheptanoic Acid 67 7 11 WARRANTY RETURNS AND REPAIRS WARRANTY Grace Davison Discovery Sciences warrants its products against defects in workmanship or material under normal use or service for one year All obligations or liabilities under this warranty are limited to repair or replacement at Grace s option F O B Deerfield IL of parts that are returned freight prepaid and which are accepted as being defective upon inspection by Grace Components that are subject to normal wear and or are scheduled for routine replacement within the warranty period and or parts which are subjected to effects of corrosion or deterioration by chemical or other action are excluded from the above warranty for malfunction because of inadequate facilities operating
37. to Run mode for sample analysis CLEANING MODE Menu Operation gt Method gt Configuration gt Maintenance gt Method Cleaning Read Lan al le 2 0 L min Set TIM USE Gas Flow 2 0 L min Gain 1 Temperature Output 17 4 mY mi 1 500 0 500 0 500 0 60 00 50 00 40 00 Mode Cleaning Select Operation Mode Cleaning using the arrows on the keypad and press Enter to put the detector into Cleaning mode In Cleaning mode the heaters gas flow and laser are on Temperature is set to 110 C gas flow is set to 2 0L min and Gain is set to 1 The detector should be run with 100 water or other suitable solvent at 1 0mL min for at least one hour to clean the detector Cleaning mode can be used for routine cleaning of the detector to prevent any buildup of sample materials inside the drift tube and optics A dirty drift tube and optics can cause excess baseline noise 3 2 2 START STOP RUN Select Operation Start Run using the arrows on the keypad and press Enter to manually start a method run The method elapsed time will then appear in the upper right corner of the screen above the output and the timed events programmed in the method will start This function should be used only if timed events will be used with the method Select Operation Stop Run and press Enter to manually stop the method run Refer to Section 3 3 1 for more information on programming timed method events Alternately method timed event
38. 2 13 14 15 16 17 18 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel Remove the ELSD cover by carefully sliding it toward the back of the instrument Disconnect the three connectors from the processor board located at J22 J23 and J24 Two of the connectors are labeled 1 corresponds to the lower drift tube heater zone and 2 corresponds to the upper drift tube heater zone The third connector unlabeled corresponds to the optics heater zone Cut the cable ties holding the RTD wires Remove the drift tube insulation by finding the seam and peeling it apart Loosen the drift tube end plates by removing the six screws to rotate the drift tube assembly as needed Cut the Kapton tape wrapped around the drift tube If replacing the drift tube RTDs continue on to step 12 If only replacing the optics block RTDs continue on to step 13 Peel off the existing RTD from the drift tube Replace with the new RTD by peeling off protective film and adhering it to the drift tube If also replacing the optics block RTDs continue on to step 13 Otherwise continue on to step 18 Remove the retaining bracket and screws from the optics block near the drift tube outlet Remove the existing RTD from the center hole on the optics block Replace the new RTD by inserting it into the center hole of the optics block Install the retaining bracket with two screws
39. 23 24 25 26 27 28 29 30 If also replacing the optics block heaters continue on to step 19 Otherwise proceed to step 25 Remove the retaining bracket screws located by the drift tube outlet from the optics block Remove the clamp and screws holding the thermofuse assembly underneath the optics block Remove the 2 existing cartridge heaters from the optics block outer holes Replace the optics heater assembly by installing 2 new cartridge heaters back into the optics block outer holes Replace the retaining bracket with the two screws Replace the clamp and screws underneath the optics block Dress the heater wiring assembly against the drift tube and tape it with Kapton tape Retighten the drift tube end plates with six screws Reinstall the drift tube insulation making sure it adheres to itself Cable tie the heater wires by the heater board Reconnect the three wiring connectors to the heater board Replace the 3300 ELSD cover and screws 64 7 8 2 2 RTD REPLACEMENT Tools Needed Anti static strap Phillips screwdriver Scissors Replacement RTD s Kapton tape Cable ties Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 10 11 1
40. 4 hex head screws Make sure the light trap has the proper orientation so the magnetic interlock makes the proper connection Refer to Figure 5 1 for details Carefully replace the insulation and light trap sweep gas tubing Replace the instrument cover and tighten the cover screws The unit is now ready for use PS w Board Magnetic Tut Switch N ROS NON Laser A f z amp bel J F gt Drift Tube if m S 5 Optics Block Sweep Gas Connection Figure 5 1 Optics Block Cleaning Procedure 5 4 2 LASER WINDOW CLEANING PROCEDURE A WARNING Use of controls adjustments or performance of procedures other than those specified herein may result in hazardous exposure to laser light A WARNING Class 3B laser radiation when optics are open and interlocks defeated Avoid exposure to beam Materials Needed Anti static strap Phillips screwdriver Hex ball driver 3 32 HPLC grade acetone Cleaning wipes References Figure 5 2 and Figure 5 3 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure 2 Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument and set it aside CAUTION The optics b
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42. A 2113967 2113968 2114811 2107480 2107476 2107511 2114472 2114584 2113962 2113961 2113963 2114471 2113960 8606365 2113966 2114652 2114711 2114712 2113943 2114671 2113643 2113956 2113965 2113954 2113964 2113959 2113958 2113952 2113953 2113955 2113957 2113951 ee LL Ll LI LI LL Ll LI lI lI lI lI l2 n L LL LL LO LL LI LI LI LI LI LI LI LI Ll LI Ll Ll lI Ll lI Ll Ll Ll ll 3300 ELSD Accessory Kit includes all parts listed above the divider Signal Cable Power Cord 110V Open End Wrench 3 8 x 7 16 Open End Wrench 1 4 x 5 16 Ball Driver 3 32 Ball Driver 7 64 Drift Tube Cleaning Brush PEEK Tubing 1 16 OD x 0 005 ID 10 SofGrip Fittings 10 pk Gas Tubing 10 1 8 Brass Nut 1 8 Brass Ferrule Drain Tubing 5 Clamp for Drain Tubing Exhaust Tubing 20 Exhaust Adaptor Fuse 5 Amp Model 3300 ELSD Operating Manual 3300 ELSD ChemStation Driver CD Nebulizer Nebulizer Wear Band Nebulizer Chemraz O Ring 25 x 9 Aperture 31 x 74 Aperture 36 x 4 Aperture Processor Board Pre Amp Assembly includes sensor Display Board Card Engine Board Heater Board Satellite Board Inverter for Display Board Gas Filter Optics Block Thermofuse Complete Assembly Drift Tube Heater Assembly Optics Block Heater Assembly Magnetic Switch Assembly Gas Pressure Sensor Membrane Switch Panel Front Service Door Nebulizer Cartridge Inlet Gas Fitting Im
43. D will power up to a white screen 7 Wait about 30 seconds before continuing This gives WinCE enough time to launch the OS and start the FTP and telnet servers 8 Next establish an FTP connection to the ELSD This procedure assumes that Windows is being used to FTP to the ELSD Open My Computer and type the following into the address bar ftp lt IP gt Where lt IP gt is the IP address from step 5 192 168 70 10 File Edit View Favorites Tools Help T 7 ur E DD EA b x i E Address g ftp 192 166 70 10 m E Mame Size Type Modified Capp File Folder 1 1 1998 6 00 AM My Documents File Falder 12 31 2079 6 00 PM profiles File Folder 12 31 2079 6 00 PM 5 Program Files File Folder 12 31 2079 6 00 PM Cj Temp File Folder 12 31 2079 6 00 PM Windows File Folder 12 31 2079 6 00 PM The screen should look similar to the above 9 Next change to the app directory There should be four files listed in it These are the initial boot files tp 192 168 70 10 app B x File Edit View Favorites Tools Help Ok G x t Address Ftp 192 168 70 1D app boot losh 818 bytes LOSH File 5 27 2056 11 36 PM E nk bin 10 2 MB BIN File 5 27 2056 11 36 PM El setup losh 170 bytes LOSH File 5 27 2056 11 36 PM a splash bmp 450 KB GIMP image 5 27 2056 11 36 PM 10 Next the setup splash screen bitmap file will be removed This will be replaced by th
44. Grace Davison Discovery Sciences Service Manual Alltech Model 3300 ELSD Manual Part No 33001005M 8 15 2007 A Important Safety Guidelines for the Model 3300 ELSD Please read the following cautions and warning statements carefully before using the Model 3300 ELSD A Warning The equipment must be used as specified by the manufacturer otherwise overall safety will be impaired A Warning All service must be completed by qualified personnel only A Warning Only use the power supply cord recommended by the manufacturer A Warning Fire hazard only use the same type and rated CERTIFIED fuse 250V 5A P Ax warming Shock hazard disconnect power before replacing the fuse A Warning Remove power cord from the power module to disconnect electrical power from the unit A Warning Check the MSDS forms and dispense and dispose of all reagents in accordance with local and national regulations A Warning Be sure to provide proper ventilation for all solvent vapors A Warning Avoid open flames and sparks when using flammable solvents A Warning If the unit is damaged and does not function properly stop the unit safely and contact the manufacturer immediately AA warning Class 3B LASER radiation inside can cause severe eye damage Do not open or defeat interlocks Avoid exposure to the beam Table of Contents T MEOdUCHUON meet CS 4 1 Aboutthe Model 3300 ES Bisa iii oi 4 1 27 IPHINGIDIS OF ORC Atl
45. INE OPERATION 4 1 SAFETY Please use the following guidelines to insure safe operation of the Model 3300 ELSD lie A warning Be sure to provide proper ventilation for all solvent vapors 2 Warning Use a fume hood or other ventilation device to prevent the inhalation of any solvent fumes expelled through the exhaust tube 3 Warning Avoid open flames and sparks when using flammable solvents 4 Warning Always power off before removing the cover 5 Warning Laser Radiation Avoid exposure to beam Class IIIB laser A CLASS 1 LASER PRODUCT Contains a class 3B 30mW 650nm laser Designed to comply with 21CFR 1040 10 1040 11 and IEC60825 with amendments as of date of manufacture No user serviceable components inside Refer servicing to qualified personnel 4 2 OPERATING NOTES 1 The internal drain reservoir must be filled with liquid water prior to using the detector The reservoir can be filled through the EXHAUST port on the back panel Once water is visibly draining from the DRAIN port on the right side panel the internal drain reservoir has been filled Monitor the liquid level in the drain waste container and remove excess liquid when necessary Never let the end of the drain tubing become submerged in the liquid inside the container Mobile phase should not be flowing when the drift tube is not at proper vaporization temperature or when the nebulizer gas is turned off Only volatile buf
46. LSD will not be used for several days disconnect the column from the nebulizer inlet and plug the inlet Flush the column before reconnection Instrument power may be left on when the instrument is not in use The laser may be turned off by putting the detector into Standby or Heating mode 21 4 6 OPTIMIZATION PROCEDURE 1 Set the drift tube temperature gas flow and gain to the initial settings recommended in Section 4 3 Start mobile phase flow and allow the system to equilibrate Increase the drift tube temperature by 1 C increments if necessary until adequate evaporation of the mobile phase is achieved indicated by a stable baseline Inject the sample and obtain peak areas for each of the components Choose a sample concentration that shows a peak that is on scale with baseline noise Change the gas flow rate in 0 2L min increments from the recommended set point and observe the change in peak area with each change The optimal gas flow rate will produce the largest peaks with the lowest amount of baseline noise Plot the signal to noise ratio vs peak area to help in identifying the optimal gas flow rate 9 MAINTENANCE 5 1 CLEANING MODE Cleaning mode can be used for routine cleaning of the detector to prevent any buildup of sample materials inside the drift tube and optics A dirty drift tube and optics can cause excess baseline noise To put the detector into Cleaning mode select Operation Mode Clea
47. Service Tech using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept Once in Service Tech mode select Configuration Heaters using the arrows on the keypad and then press Enter The Heater Configuration screen will then appear Menu Method Method 1 Set Heater Configuration Output Configuration gt 1 500 0 500 0 E Accept O Cancel YI A 500 0 min 40 00 30 00 20 00 0 00 40 50 00 60 00 Mode Standby Enter a value for the Optics Heating in the blank provided The default value is 90 The Optics Block will heat to this of the Drift Tube temperature setting Press Accept to save the new Heater setting or press Cancel to cancel the changes 3 4 6 DATE AND TIME Select Configuration Date and Time using the arrows on the keypad and press Enter The Date and Time Configuration screen will then appear Menu Date and Time Configuration Method Default Method Configuratio GMT 06 00 Central Time US amp Canada 4 O a O cena 3 UU DUU UU p UL SUU Z UU 1 00 IUU ERIT AUU DUU D M o d e S t an d b y Enter the Date month day and year and the Time hour minute and second using the keypad Use the up down arrows to tab across the entry blanks Select the Time Zone from the list using the left right arrows Press Accept to save the new date and time configuration or press Cancel to cancel the changes 3 4 7 LANGUAGE
48. ZEOOO g DumtJ uj usnd eqni v 01 8 1 uolun pnbaun 1962000 y Ep m 01 60620 n N d Jeuuubd ejo2 Jew4 S09 481000 NX Dumi4 ur usng eqn c Z 4 19MJOJ 8 1 01 LdN 8 1 881 anims uoupug ejpuje4 g90e000 z JOQUUNN ZOZE000 quuessy Buy YMS eunsseJd 702 000 san 1 1 X dl 91 1 X dO 8 l JEQUUNN Bulmolg Yo9 V V BUIMDIJ uoeiv BUIMDIJ uoeiv JOQUUNN jyuong Uolsinay Jou adh jey enit od Wo wey MO14 JHL 40 NOI193810 JHL HLIM 9NLLNIOd SMOHMV 3A1193dS38 WISH E HLIM Z ONY S SWALI 39V Td SQV38HL LdN TIVA TIV OL 3dV1 344d aav SALON C JION 335 NOI1L9 3810 MO 13 310N 335 C ilON 335 i e NOILLO3MIO MO 13 310N 335 c SION 345 NOILLO3MIO MO 13 7 DOS SH E JILVIN3HOS MO ld SVO c Z Z 7 8 HEATERS RTDS AND THERMOFUSES 7 8 1 CHECKING THE THERMOFUSES RTDS AND HEATERS 7 8 1 1 CHECKING THE THERMOFUSES Tools Needed e Anti static strap e Phillips screwdriver e Digital multimeter Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure Power off the unit from the back panel and disconnect the power cord Before checking the thermofuses first allow the resettable fuses 2 hours to reset Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back pa
49. ace it with freshly prepared and filtered mobile phase The mobile phase may contain excess air bubbles Degas the mobile phase The pump may be the source Check pump for pulsations Make sure the pump has been sufficiently purged to remove air Incorporate a pulse dampener into the system if necessary Examine the pump check valve and seals and replace as necessary C Noise from Gas The gas supply may be contaminated with particulates e Column removed Replace with better quality higher purity gas e Mobile phase off The nebulizer drift tube and or optics may need cleaning e Nebulizing gas on Refer to Sections 5 1 5 4 for cleaning procedures Laser on Result Noise disappears when gas is turned off D Noise from Flow Optics Block he optics may need cleaning Refer to Section 5 4 for optics e Column removed cleaning procedure e Mobile phase off Check data cable for noise e Nebulizing gas off Check light trap for condensation Refer to Section 5 4 for e Laseron details on removing the light trap Result Noise disappears when laser is turned off E Noise from Electronics e Column removed Preamp board is bad Replace the preamp board and then e Mobile phase off recalibrate the preamp laser Refer to Section 7 6 3 for e Nebulizing gas off details e Laser off Processor board is bad Replace the processor board and then recalibrate the heaters gas flow and laser preamp Result Baseline noise persists u
50. aining the upgrade files into the USB Host port on the back panel of the 3300 ELSD 4 Power up the 3300 ELSD 5 The software installation should begin automatically Follow the instructions on the front panel as the procedure continues The screens should appear similar to the following software version numbers may differ a In the first step the update procedure determines if the pen drive contains a new Application software version If so the existing Application version and the new Application version on the pen drive are displayed ELSD Update 0 19 b Press Yes to continue with the upgrade and the update procedure will continue on through the following steps Verifying checksum for ELSD application Backing up application Updating application a These steps may take several minutes to complete c Once the Application update is completed the following screen will appear ELSD Update d Press OK and the update procedure will then determine if the pen drive contains a new OS image upgrade If so the following screen will appear that displays the existing version on the unit and the new version on the pen drive ELSD Update 0 19 If this is the first time a pen drive upgrade has been performed on the unit the existing version will be listed as Unknown This is normal 55 e Press Yes to continue on with the OS image upgrade If the existing OS version on the unit was 0 99 3 or a
51. al flow meter 7 6 3 LASER PREAMP CALIBRATION Tools Needed Anti static strap Phillips screwdriver Hex driver 3 32 Magnet Preamp calibration fixture including SMB cable Digital multimeter Small screwdriver for adjusting potentiometers Procedure 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this calibration 2 Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument 6 Use a 3 32 hex driver and a Phillips screwdriver to remove the preamp and laser from the ELSD and install both onto the calibration fixture 7 Verify the calibration setup a Laser is plugged into the processor board b Preamplifier board is plugged into the processor board Preamplifier ribbon cable is grounded SMB cable is connected to the preamplifier board SMB cable is connected to the voltmeter gt 0 20 Voltmeter is set to read DC millivolts Magnet is on outside of chassis next to the magnetic switch Do not center magnet on the switch Place it near one of the studs ae h Marked interlock on the instrument is replaced with the fixture interlock I Coveris installed on the preamp 8 Power on the ins
52. ase if the mobile phase has not been completely evaporated Detector settings must be carefully selected to ensure adequate mobile phase evaporation DETECTION The non volatile sample particles emerge from the drift tube in the mobile phase vapor and enter the light scattering cell In the optical cell sample particles scatter light emitted by a laser light source The scattered light is detected by a silicon photodiode generating a signal proportional to sample mass This signal is sent to the analog output for data collection The advanced design of the Model 3300 ELSD optical components provides excellent sensitivity for HPLC analysis 1 US Patent 6229605 other patents pending 2 INSTALLATION 2 1 WHAT YOU WILL NEED In addition to the Model 3300 ELSD detector and its accessories the following will be needed for installation of a complete chromatographic system Exhaust System eA fume hood or other ventilation device located close to the detector to remove the detector exhaust from the laboratory NOTE Make sure the exhaust system provides adequate but not excessive suction Excessive suction can cause a noisy baseline Gas Supply eA supply of clean dry nebulization gas preferably nitrogen regulated from 65 to 80 psig 99 9 purity or better is recommended The gas source can be a high pressure gas cylinder high pressure liquid tank or a nitrogen generator HPLC System Components eAn HPLC pump
53. aser preamp Refer to Section 7 6 for details Fail Offset between laser on and laser off Is too high Optics may need Following the optics cleaning procedure in Section 5 4 cleaning Bad preamp board Replace preamp board and then recalibrate the preamp laser Refer to Section 7 6 3 for details Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 OPTICS TEST RESULTS continued RESULT Fail Offset between laser on and laser off is too high continued Fail Offset between laser on and laser off is too low Fail Noise level at laser on is too high CAUSE Apertures have rough edges Laser is not powering on Bad laser Bad processor board Optics may need cleaning Bad preamp board Bad processor board 6 2 4 OPTICS HEATING TEST 1 SOLUTION Rotate apertures 90 Make sure interlocks are activated including cover Replace laser and then recalibrate the preamp laser Refer to Section 7 6 3 for details Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Following the optics cleaning procedure in Section 5 4 Replace preamp board and recalibrate the preamp laser Refer to Section 7 6 3 for details Replace processor board and then recalibrate the heaters gas flow and la
54. beled connector contains the wires for the optics block heated zone 7 Cut the cable tie holding the wires by the heater board 8 Remove the drift tube insulation by finding the seam and peeling it apart 9 Loosen the drift tube end plates by removing the six screws to rotate the drift tube assembly as needed 10 Cut the Kapton tape wrapped around the drift tube 11 If replacing the drift tube thermofuse s continue on to step 12 If only replacing the optics block thermofuse continue on to step 14 12 Cut the two drift tube thermofuse assembly wires about two inches from the connector and strip ends about 1 2 13 Replace the drift tube thermofuse assembly by stripping the wire ends about 1 4 and soldering them together to the wires on the connector Then install shrink tubing over the solder points If also replacing the optics block 65 thermofuse continue on to step 14 otherwise continue on to step 18 14 Cut the two optics block thermofuse assembly wires from the connector about two inches from the connector and strip ends about 1 2 15 Remove the clamp and screws holding the assembly underneath optics block 16 Replace the optics block thermofuse assembly by stripping the wire ends about 1 2 and soldering them together to the wires on the connector Then install shrink tubing over the solder points 17 Install the clamp and screws underneath the optics block 18 Dress the thermofuse wiring against t
55. ble cleaning solvent NOTE Use only the drift tube cleaning brush included with the unit This brush has been specially selected so it will not travel too far down the drift tube which could splash the optics and result in additional noise Do not attempt to force the brush further into the drift tube than it was designed to go 1 Power off the unit from the back panel and disconnect the power cord 2 Allow the detector to cool for at least 30 minutes 3 Remove the front door by gently pulling it towards you from the handle and set aside 4 Disconnect the stainless steel liquid inlet line from the nebulizer using the 1 4 wrench 5 Disconnect the quick connect gas tubing from the front panel Push in and then pull out to remove the tubing 6 Remove the nebulizer from the drift tube by pushing in and turning it firmly counterclockwise Set the nebulizer aside 7 Use the hex ball driver to remove the two screws on the removable cartridge on the front panel of the unit Pull out the cartridge and set aside 8 Using water or other suitable solvents wet the drift tube cleaning brush and carefully insert the brush into the drift tube from the front panel NOTE Use only the cleaning brush provided with the unit 9 Carefully clean the sides of the drift tube with the cleaning brush loosening any particles that adhere to the drift tube 10 Once the drift tube has been cleaned reinsert the impactor cartridge an
56. bove the upgrade will continue through the following steps If the existing OS version is below 0 99 3 then the update procedure may involve a few extra steps including a reboot In that case follow the instructions on the screen and press Yes or OK when indicated Updating OS image Verifying checksum for OS Image ELSD Update f The pen drive upgrade procedure is complete Power off the 3300 ELSD and remove the pen drive g Reboot the 3300 ELSD and confirm the new software versions on the unit by selecting Maintenance About 7 6 CALIBRATION PROCEDURES These functions are available in Service Tech mode only NOTE The detector must be in Standby mode in order to be calibrated IMPORTANT If the processor board has been replaced the serial number and date time must be re configured first BEFORE the calibration procedures are performed Otherwise the calibration will not be saved Refer to Section 3 4 2 for details on configuring the serial number and refer to Section 3 4 6 for details on configuring the date time 7 6 1 HEATER CALIBRATION Tools Needed Anti static strap Phillips screwdriver Temperature calibration box Temperature probe Claw with thermometer Reference Section 7 7 1 Electronic Schematic Procedure 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this calibration 2 Power off the unit from the back panel and discon
57. ccept to exit the Manual Control screen and return to the main screen 23 Replace the RTDs Make sure they are installed in order from top to bottom RTD 1 RTD 2 and RTD 3 24 Physically check the temperatures using the temperature probe claw in the three heater regions and inside the drift tube at three set points at 40 C 70 C and 100 C When taking external temperature measurements make sure the temperature probe is in direct contact with the copper tube and the heater Write down these temperature measurements 57 7 6 2 GAS FLOW CALIBRATION Tools Needed Anti static strap Phillips screwdriver External gas flow meter Sierra 822S or equivalent 1 2 open end wrench 7 16 open end wrench Reference Section 7 7 2 Gas Flow Path Schematic Procedure 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this calibration Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel Remove the ELSD cover by carefully sliding it toward the back of the instrument and set aside Connect the external flow meter in line between the internal flow meter and the flow valve Flow direction is from meter to valve Connect a nitrogen gas line regulated to 80psi to the Gas Inlet on the back panel of the 3300 ELSD 6 Turn on the unit and wait for it to boot up 7 Select Maintenance Service Tech Enter Service Tech Pass
58. ccur during the Heater Stability Test e Minimum maximum and average temperature values for the Lower Drift Tube Upper Drift Tube and Optics Block are determined e Test results are displayed Menu Heater Stability Test Maintenance gt iutput 51 7 mV 6 Passing requirements for the Heater Stability Test are e Temperature stability for the Lower Drift Tube Upper Drift and Optics Block must be within 1 C during the testing period If the test has failed refer to the following table Heater Stability Test Results for possible causes and solutions 8 Once the test is completed press Done to return to the main screen or press Test to repeat the test HEATER STABILITY TEST RESULTS RESULT CAUSE Detector is still equilibrating Fail Lower Drift Tube Upper Drift Tube and or Optics Block Blown thermofuse Bad RTD s Bad heater s SOLUTION Wait for the detector to equilibrate and then repeat the test Allow the resettable fuse 2 hours to reset Then recheck the thermofuse and replace if necessary Refer to Section 7 8 Check RTD s Replace RTD s if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Check heater Replace heater if bad and then recalibrate the heaters Refer to Sec 7 8 amp 7 6 1 HEATER STABILITY TEST RESULTS continued RESULT CAUSE SOLUTION Bad heater board Fail Lower Drift Tube Upp
59. ce Tech Password Menu iutput Maintenance gt Mode Standby Enter the new password in the blank provided using the keypad Press the down arrow to reach the second blank and then re enter the new password Press Accept to save the new Service Tech password or press Cancel to cancel the changes If Accept is pressed a Success screen will then appear indicating that the Service Tech password has been changed Press Accept to confirm the new Service Tech password RESET SERVICE TECH PASSWORD To restore the Service Tech password to its default setting atat select Maintenance Service Tech Reset Service Tech Password using the arrows on the keypad and then press Enter A Success screen will then appear press Accept to confirm that the Service Tech password will be restored to its default setting 3 5 6 CALIBRATION This function is available in Service Tech Mode only To enter Service Tech mode select Maintenance Service Tech Enter Service Tech Password using the arrows on the keypad and press Enter Enter atat as the Service Tech password and press Accept Refer to Section 7 6 for details on the calibration procedures 3 5 7 ABOUT The About screen displays the current software versions on the detector and the serial number of the unit Select Maintenance About using the arrows on the keypad and press Enter The About screen will then appear Alltech Press Accept to return to the main screen 4 ROUT
60. ce Tech mode it is possible to access service functions that cannot be reached in the normal operation mode ENTER SERVICE TECH PASSWORD To enter Service Tech mode select Maintenance Service Tech Enter Service Tech Password using the arrows on the keypad and press Enter The Authorize Service Tech screen will then appear Method Method 1 Authorize Service Tech Menu iutput Maintenance gt 9 Accept Cancel 0 00 Mode Standby Enter the Service Tech password using the keypad and then press Accept or Cancel The default Service Tech password is atat Once Accept has been pressed the detector is now in Service Tech Mode Service Tech mode provides additional functions for Configuration and Maintenance serial number configuration optics block heater configuration calibration heater stability and power supply tests export service log and service log LOG OUT SERVICE TECH To log out of Service Tech mode select Maintenance Service Tech Log Out Service Tech using the arrows on the keypad and press Enter The detector will then return to normal operation mode and Service Tech functions will no longer be accessible CHANGE SERVICE TECH PASSWORD To change the Service Tech password from its default setting atat select Maintenance Service Tech Change Service Tech Password using the arrows on the keypad and press Enter The Change Service Tech Password screen will then appear 19 Method Method 1 Change Servi
61. chart axes 3 2 5 AUTOZERO The Autozero function can be used to zero the output on the detector To autozero select Operation Autozero using the arrows on the keypad and press Enter The autozero value will depend on the full scale voltage setting on the detector For a 1V full scale voltage setting the default Autozero value is 5mV For a 10mV full scale voltage setting the default Autozero value is OmV If the Custom Autozero Output has been enabled the detector will be autozeroed to the value selected from O to 100mV Refer to Section 3 4 3 for more details on setting the Custom Autozero Output value 3 3 METHOD Methods are created to set the temperature gas flow gain and event settings on the detector 3 3 1 NEW Select Method New using the arrows on the keypad and press Enter to bring up the New Method window Menu New Method Methad Method Method 1 Default Method LO accept O conce Mode Run Enter the Method Name Temperature Gas Flow Gain and Timed Events using the keypad Use the up down arrows to tab through the method parameters Method Name The Method Name may include the following characters A Z a z 1 9 space or period Rapidly press a button on the keypad to cycle between letter and number options For upper case press Shift and then enter the letter Temperature Enter a temperature value between 25 120 C using the keypad Gas Flow Enter a value between 0 0
62. conditions or utilities Equipment and components may only be returned with Grace s prior approval and must bear a Grace Return Authorization Number Call the Grace Customer Service Department to obtain a Return Authorization Number Guarantee Warranties on accessories and equipment included by Grace from other manufacturers are limited to the guarantees given on such equipment by the respective manufacturers Any modifications made to equipment covered by this warranty without written permission from Grace will void the warranty Grace reserves the right not to honor this warranty if the products are obviously mishandled by the user Grace assumes no responsibility for consequential economic or incidental damages of any nature or on site reinstallation costs arising out of future alleged failure of any of its products or their accessories This warranty supersedes any and all previous warranties unless otherwise agreed upon at the time of sale such as for customized equipment 68 SHIPMENTS All shipments are made F O B Deerfield IL DAMAGED SHIPMENTS The Interstate Commerce Commission has held that carriers are responsible for both concealed and visible damage occurring during transit Unpack the shipment upon receipt and check for concealed damage even if no visible damage is apparent If concealed damage is discovered stop unpacking the unit request an immediate inspection by the local carrier agent and obtain a writt
63. cs block temperature error continued Optics block temperature reading is more than 10 C off its set point Bad processor board Blown thermofuse Gas flow error Gas flow reading is more than 0 3L min off its set point Gas source may be low or empty Regulator pressure setting is too low Nebulizer may be blocked Gas leaks may exist inside unit Bad gas flow valve and or flow meter Bad processor board Inlet gas pressure is low Inlet gas pressure is lower than 40 psig Regulator pressure setting is too low Gas source may be low or empty Gas leaks may exist inside unit Bad processor board Bad pressure switch Any errors not included in this list 32 SOLUTIONS Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Allow the resettable fuse 2 hours to reset Then recheck the thermofuse and replace if necessary Refer to Section 7 8 for details Check gas source and replace if necessary Adjust regulator pressure to 65 80psig Clean nebulizer Refer to Section 5 2 for details Check gas flow path for leaks Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Adjust regulator pressure to 65 80psig
64. d Method 1 Optics Block Temp Calibration High iutput Maintenance gt 27 For the heated zones that are out of tolerance only O contine O coca MEME enter the temperature values obtained in step 20 for v n SR Gs ass 0 00 temperature set points of 40 C and 100 C It is ok to was leave the blanks empty for the zones that are within tolerance but values must be entered for both temperature set points for a given zone 18 Flip the third switch to 96 C The Raw Value should increase again Press Continue to reach the final step of the calibration 28 Once the temperature values have been entered press Accept to modify the heater calibration Method Method 1 Finished 29 Re measure the temperatures of the heated zones pil using the temperature probe and repeat the Maintenance gt i Temperature Correction Procedure if necessary until the heated zones are within tolerances Mode Standby 19 Press Finish to complete the heater calibration and return to the main screen 20 To check the calibration select Maintenance Manual Control and press Enter to reach the manual control screen 21 Flip each of the 3 toggle switches back and forth between 17 C and 96 C and observe the values on the screen The temperatures should be 17 C 0 2 C and 96 C 0 2 C If the temperature readings do not meet the 17 C 0 2 C and 96 C 02 C requirements the unit must be recalibrated 22 Press A
65. d tighten the screws Make sure the drain hole is located on the bottom of the tube as it is inserted 23 CAUTION The drain hole located on the bottom of the impactor cartridge must be aligned with the drain hole inside the unit when the cartridge is reinserted Otherwise flooding could occur inside the unit 11 12 13 14 Replace the nebulizer back into the unit by aligning the grooves and turning clockwise until the nebulizer locks firmly into place Reattach the nebulizer gas tubing to the quick connect fitting Reconnect the liquid inlet line to the nebulizer Replace the front door The unit is now ready for use 5 4 OPTICS CLEANING PROCEDURES 5 4 1 OPTICS BLOCK CLEANING PROCEDURE The optics block can become dirty over time from sample and mobile phase materials Dirty optics can cause increased baseline noise and decreased sensitivity The following procedure can be used to clean the optics block A WARNING Use of controls adjustments or performance of procedures other than those specified herein may result in hazardous exposure to laser light A WARNING Class 3B laser radiation when optics are open and interlocks defeated Avoid exposure to beam Materials needed Insulation Anti static strap Phillips screwdriver Hex ball driver 3 32 Suitable cleaning solvent Cleaning swabs wipes Reference Figure 5 1 1 Precaution must be taken use of an anti static foot strap in a grou
66. dby to save the new laser preamp calibration Power off the instrument Remove the magnet from the chassis Replace the interlock switch m Reinstall the laser and preamp in the 3300 ELSD and replace the cover and screws 40 i 13718 E JST SST NT EA m OLLVA3HOS ON ONIMVEC ws sss aos 90 91 80 LW OM d3A0YddV WM NMVSO SINTO MEND wd TEN O 9 SIN3NOdWOO OLLVWSHOS TWOIMLOATA OOEE NOLLdIHOS3Q sio Baro sun so suo 0096 GPS TG ena ben SI009 71 plauasq ppoy upbBexnoM IS0c OU sejDI20SSy uoeiv IVILN3GIJNOO a n u HO LIMS Quvog n INVEBNIN o AIdANS i O ell YIMOd 135330 O c O O UU NNV9 Quvog TWNOIS diAV 3Md 90 IVNV TINON AMINA INdNI YaMOd YaMOd Oo ann YALYSANI 097 P n quvog m O O O dS O i qug S35n3OWH3HL a IJ31V3H sado em SISMIONYIHL 193 LYH 38n1 O E O O O 13180 yaaan tef K O O YO LOSNNOO SISNIONS3HL trn vod Ie31V2H ae SINdLNO NO LLOG C 134180 H3M01 ISLNANI d vog 3NI9N3 13538 O O 13N93H13 7 o B 391130 8sn 53 r s quvog ale HOLIMS a ALITTALVS SO Ld0 AYNSSAYd 1SOH 8SN 5 k GLY SEN NV d 14190 Wadd GLY SNL 14180 H3MO1 ZEZSY INdLNO TYNIIS F E 7 L THa WAP B q LA O O O O YOSN3S YINVIAS JUNSSIWA w SN X00 H31NI LECEN d Ll OLL3NO VA TEMOR u3sv1 YALAW MO ld AN WA MO 13 JILVIN3HOS DINOHLIO3 TSI Z Z SOLLVINHHOS ZZ
67. der c Copyright 2002 2005 Logic Product Development Inc All Rights Reserved Version 2 0 6 LLH7a404 11 0001 deck oe oe ke oe ke oe ehe k Kk k k k k k ke ke ee k IO IO IO ee eee eek losh gt 8 Run the following command ifconfig sm0 up 9 Start the TFTP DHCP server by launching Tftpd32 exe The first time that Tftpd32 is started there may be some error dialogs about not being able to bind the BOOTP 50 port Click OK to accept the dialogs and continue with step 10 to configure software 10 After starting the screen below will appear Tftpd32 by Ph Jounin B x Current Directory Ftp Browse Server interface 159 97 84 210 Show Dir Tip Server Tftp Client DHCP server Syslog server Current Action Listening on port 69 Settings Help Next Tftpd32 will need to be configured Click on the Settings button on the bottom of the window This will present a new screen Tftpd32 Settings Baze Director F tftp Browse Global Settings Iv TFTP Server w Syslog Server I TFTP Client e DHCP Server SHTP server Syslog server Save syslog message File TFTP Security TFTP configuration f Mane f Standard High t Read Only Timeout seconds Max Retransmit B S m E THp port Advanced TFTP Options lif Option negotiation PXE Compatibility W Show Progress bar Translate Unis file names Hide window at startup Crea
68. e Source gas pressure is too low Adjust source pressure to 65 80psig Gas source may be low or empty Replace gas source Gas flow meter and or valve error Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details Bad pressure switch Replace pressure switch Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details No power Blown fuse Replace fuse Refer to Section 5 5 Fuse Replacement for details No LCD display Display cable is loose Check for loose display cable Bad LCD display Replace LCD display Bad processor board Replace processor board and_ then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details No peak s detected Sample is below the detection limit Increase the sample concentration or injection volume and re inject Sample is volatile at current detector Lower temperature settings are needed for conditions semi volatile compounds Refer to Section 4 6 Optimization Procedure for details Sample is being retained on the Use a different column for your separation column Gain is set too low Increase the gain value 42 TROUBLESHOOTING continued 2 PROBLEM CAUSE SOLUTION No peak s detected continued Autosampler needle is not pulling up Repair or replace equipment as needed sample properly or sample loop blockage
69. e Phase Solvents Use the left right arrow keys to select from the list of solvents Use the up down arrows to tab down the table Enter a percentage for each solvent The total percentage must add up to 100 Once the solvents percentages have been entered press Continue to continue on to the next screen in the Method Wizard or press Cancel to cancel using the Method Wizard Menu m m Method Mande Mobile EE Flow Rate Operation gt Method gt Please select the mobile phase flow rate Configuration Maintenance gt Mobile Phase Flow Rate 1 0 mL min 4 Continue e Cancel ju mMuue Kull Mobile Phase Flow Rate Select the Mobile Phase flow rate using the left right arrows Possible choices are 0 2 0 5 1 0 2 0 and 3 0mL min Press Continue to continue on to the next Method Wizard screen or press Cancel to cancel the Method Wizard Menu aad method METE Hans Concentration Operation gt Method gt Please select the sample concentration Press Continue to Configuration gt determine method settings Maintenance gt Sample Concentration 0 50 ng 4 O Continue O Cancel 0 muue Kuri Sample Concentration Use the left right arrows to select the sample concentration from the list Press Continue to reach the next Method Wizard screen or press Cancel to cancel using the Method Wizard Method Wizard Finished The method settings have been calculated Press Finish to continue
70. e application splash screen Select splash bmp and delete it 11 Locate the folder where the ELSD application is stored amp CATEMP File Edit View Favorites Tools Help Back gt GQSearch C Foldes 4 MG G2 X A Edy Address CATEMP L C3 application EY 3300 ELSD Grace Davison Discovery Sciences Select an item to view its description See also My Documents My Network Places 16 Verify that the version numbers of the software My Computer installed are correct To display the version numbers go to the menu option Maintenance About 12 Go into the application directory as shown in step 11 17 The application upgrade procedure is complete The complete software installation procedure is also gt C TEMP application complete File Edit View Favorites Tools Help Back ASearch Folders 4 4 GS X Ed Address CATEMPt application C de DE L1 en US es ES application Select an item to view its description See also My Documents My Network Places fr FR it IT jaJP zh CN FElsd pp exe ELSDDiags amp Pl dll 2 ELSDHardwareAPI dll My Computer 8 ELSDRemote P dl el Enabled waw ES Manifest xml 7 MON EXE OpenNETCF dli OpenNETCF Net dll is RemoteS erver dll My SPLASH BMP 13 Select all of the files and directories and drag them to the FTP window from step 4 The copy should only take a minute or so
71. eetene 56 7 6 2 Gas FIOW Calibration ini PEOR 58 760 3 Lasetr Preamp Calibration ccc ees a 59 Lh SSC MEM AU CS in O a 60 FAA Electronic Schematll unica ol 60 rov M Gas FOW Patl u uuu unum au a aut aaa a a ata tateuttats 61 7 8 Heaters RTDs and Thermolfuses U U U U eee 62 7 8 1 Checking the Heaters RTDs and Thermotfuses 62 KOLT CHECKING the Heaters isidro nio rotar 62 1 8 1 2 Checking the TDS usan 62 7 8 1 3 Checking the Thermofu ses yuu u u u u yu nnn n nnn nnn n nnn nnn nnn nnn nns 63 7 8 2 Heater RTD and Thermofuse Replacement Procedures 63 7 8 2 1 Heater Replacement Procedure 11 u uuu enhn nnne nnn nnn nnn nnn 63 7 8 2 2 RTD Replacement Procedure 1 ee eceeeieeeeseeeeiee nennen nnn nnn nhan nnn nnn nn 64 7 8 2 3 Thermofuse Replacement Procedure 65 7 9 Model 3300 EESD QC Procedure uni 66 7 10 Volatile Mobile Phase Modifliers J U U U U nennen u nn nnn nnn u u 67 7 11 Warranty Returns and Repairs U U u u u u u u u 68 TAZ Useful RETEFEN COS o o AS 69 1 INTRODUCTION 1 1 ABOUT THE MODEL 3300 ELSD The Alltech Mod
72. egulator Power up the Model 3300 ELSD When the Operation screen appears set up the desired method and configuration as indicated in Sections 3 3 and 3 4 Put the detector into Run mode Operation Mode Run Allow the detector to equilibrate The Equilibrating indicator will appear next to the Mode in the lower left corner until the Lower Drift Tube heater Upper Drift Tube heater Optics Block heater and Gas Flow reach their set points Once the detector has equilibrated record a gas only baseline for 10 15 minutes Observe the signal output displayed on the front panel and on the chromatogram You should get a stable low noise baseline The noise should be in the millivolt range within 2mV 8 If the baseline is unstable and or drifting the unit may need longer equilibration time 9 If the noise is higher than expected you may want to perform the optics test to determine if there is a possible laser or electronics problem Refer to Section 6 2 3 for details on the optics test Ts 12 13 14 15 Flush the column with mobile phase before connecting it to the detector The length of purging will depend on how long the column was in storage and what type of sample and mobile phase were used It is very important that the column is free from silica fines or other contaminants before connecting to the ELSD The Model 3300 ELSD will detect the contaminants with great sensitivity After flushing the column
73. el 3300 ELSD is designed for use with High Performance Liquid Chromatography HPLC systems to analyze any sample compound that has sufficiently lower volatility than the mobile phase Some of its possible application areas include carbohydrates pharmaceuticals lipids triglycerides underivitized fatty and amino acids polymers surfactants nutraceuticals and combinatorial libraries Evaporative light scattering detection eliminates common problems associated with other HPLC detectors Refractive Index RI detectors can be complicated by solvent front interferences baseline instability and gradient incompatibility RI detectors can also have a less sensitive response than ELSD Low wavelength UV can suffer baseline drift with steep gradients and also requires that the analyte contains a chromophore ELSD does not have these limitations It can achieve stable baselines with multisolvent gradients for improved resolution and faster separations Also since ELSD response does not depend on the samples optical characteristics the sample does not require a chromophore or fluorophore for detection The Model 3300 ELSD features the most advanced evaporative light scattering detection technology available It provides sensitivity in the low nanogram range An intuitive Windows based software interface provides a nested menu of options for detector operation including Method Wizard for simplified method development multiple languages and bu
74. en report of the findings to support a claim This request must be made within 15 days of receipt otherwise the claim will not be honored by the carrier Do not return damaged goods to Grace without first obtaining an inspection report and calling Grace for a Return Authorization Number FILING OF CLAIMS After a damage inspection report has been obtained Grace will cooperate in replacing damaged goods and in handling of claims which have been initiated by either party RETURNS If it is necessary to return any material to Grace please call Grace s Customer Service Department for a Return Authorization Number and forwarding instructions No returns may be made without a Return Authorization Number REPAIRS Grace is the only organization authorized to service or repair the Model 3300 ELSD Any repairs performed without notifying Grace will void the warranty To obtain repair service call Grace s Customer Service Department for instructions and a Return for Repair Number 7 12 USEFUL REFERENCES THEORY AND REVIEWS Evaporative Light Scattering Detection Solves Common HPLC Detection Problems M J Wilcox International Labmate 23 6 35 36 1998 Modified Laser Light Scattering Detector for Use in High Temperature Micro Liquid Chromatography R Trones T Andersen Hunnes and T Greibrokk Journal of Chromatography A 814 55 61 1998 Improved Modification of Laser Light Scattering Detector for Use in Packed Capilla
75. ent to be edited or press Cancel to cancel the editing If Accept has been selected the Edit Timed Mode Change Event window will appear Method Default Method Edit Timed Mode Change Event Menu Output Configuration gt Change to standby mode 4 Mode Standby Next Cleaning mode 1 7 2005 17 00 Make the desired changes to the Timed Mode Change Event Press Accept to save the changes or press Cancel to cancel the changes DELETE TIMED MODE CHANGE Select Maintenance Timed Mode Changes Delete using the arrows on the keypad and press Enter The Delete Timed Mode Changes Event screen will then appear 17 hAnthoad Menu Mathad Mafart hs Delete Timed Mode Change Event Output Standby mode once at 17 00 on 04 23 Cleaning mode at 17 00 on Friday each week Configuration gt Accept Cancel AA FAT a ag BIB J MUUEe gt OLAMuo y Next vIedririu Mute Ly f Z2UUS Use the up down arrows to highlight the event to be deleted from the table Once the event has been highlighted press Accept to delete the selected event or press Cancel to cancel deleting the event 3 5 MAINTENANCE 3 5 1 MANUAL CONTROL The Manual Control screen can be accessed in order to view the current status on the detector for laser gas flow and heated zones Select Maintenance Manual Control using the arrows on the keypad and press Enter to reach the Manual Control screen Menu Method Default Method Manual Control
76. er Drift Tube and or Optics Block continued Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 Bad processor board Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details 6 2 6 POWER SUPPLY TEST This function is available in Service Tech Mode only This test can be run to test the voltages on the processor board 1 5V FPGA Voltage 1 8V Card Engine Voltage 3 3V Digital Voltage 4V Laser Power Supply Voltage 5V Digital Voltage 12V Analog Voltage 12V Analog Voltage Contact Grace Alltech for more details 1 Enter Service Tech mode by selecting Maintenance Service Tech Enter Service Tech password and entering atat using the keypad Select Maintenance Tests Power Supply Test using the arrows on the keypad and press Enter The Power Supply Test screen will then appear Menu Power Supply Test iutput Maintenance gt Press Test and the Power Supply Test will begin The test will run until Done is pressed The results for the test are then displayed The values are updated in real time Power Supply Test iutput Maintenance gt 39 5 Passing requirements for the Power Supply Test are e Each voltage value must be 5 of its theoretical value Once the test is completed press Done to return to the main screen or press Test to repeat the test If the
77. er and set aside 7 Disconnect the nebulizer gas inlet fitting with gas tubing attached from the nebulizer using the 5 16 wrench and set aside 8 Place the nebulizer methanol water solution in a beaker filed with 50 50 9 Sonicate the nebulizer in an ultrasonic bath for 10 minutes NOTE Do NOT sonicate the orange wear band the nebulizer gas inlet fitting or the gas tubing 10 If the nebulizer is still completely blocked connect a high pressure air line to the nebulizer inlet to help remove the blockage 11 If the nebulizer is permanently blocked or cannot be cleaned the nebulizer should be replaced 12 Replace the nebulizer wear band and nebulizer gas inlet fitting with gas tubing attached 13 Replace the nebulizer back into the unit by aligning the grooves and turning clockwise until the nebulizer locks firmly into place 14 Reattach the nebulizer gas tubing to the quick connect fitting 15 Reconnect the liquid inlet line to the nebulizer 16 Replace the front door The unit is now ready for use 22 5 3 DRIFT TUBE CLEANING PROCEDURE The drift tube can become dirty over time from sample and mobile phase materials A dirty drift tube can cause increased baseline noise and decreased sensitivity The following procedure can be used to clean the drift tube Materials Needed Open end wrench 1 4 x 5 16 Hex ball driver 3 32 Drift tube cleaning brush HPLC grade water or other suita
78. fers are allowed in the mobile phase Non volatile buffer particles will be viewed as sample by the detector causing unwanted baseline noise Refer to Section 7 10 Volatile Mobile Phase Modifiers for a list of suitable buffers 20 4 3 SELECTING INITIAL OPERATING CONDITIONS Use the recommendations provided by the Method Wizard for initial method settings The Method Wizard can be reached by selecting Method Wizard in the software interface Refer to Section 3 3 5 for details Semi Volatile Compounds The recommendations provided by the Method Wizard are based on non volatile sample compounds If the sample compound is semi volatile it may require a lower drift tube temperature than the Method Wizard recommends Some experimentation may be necessary Gradient Separations Choose operating conditions based on the least volatile portion of the mobile phase when performing gradient separations Unlisted Solvents For any solvents not listed in the Method Wizard please refer to the solvent s boiling point and vapor pressure in a reference book such as the Merck Index or Handbook of Chemistry and Physics Use the temperature and gas flow rate for the solvent that most closely matches the boiling point and vapor pressure of the solvent of interest 4 4 STARTUP SEQUENCE 1 Set up the unit as described in Section 2 4 Making Electrical and Fluid Connections Turn on the nebulizer gas supply between 65 and 80 psig Set the r
79. g the arrows on the keypad and press Enter The zoom tool will then appear in the lower left corner of the screen Method Method 1 Read 40 2 C 1 5 L min Set 40 0 C 1 5 L min 16 Temperature Output 376 2 mY Gas Flow Gain 8 0 4 0 0 0 5 00 geome Mode Run Use the up arrow to Zoom out the Y axis use the down arrow to Zoom in the Y axis use the left arrow to zoom in the X axis or use the right arrow to zoom out the x axis Once the desired chart view has been achieved press Accept to save the new chart view or press Cancel to return to the original chart view The x axis range is 60 to O minutes The y axis range is 500mV to 2 5V To reach Pan directly from Zoom press Enter PAN The Pan function can be used to pan left right up or down on the chromatogram trace Select Operation Chart Pan using the arrows on the keypad and press Enter The Pan tool will then appear in the lower left corner of the screen Method Method 1 Read 40 1 C 1 5 L min Set 40 0 C 1 5 L min 16 Temperature Output 373 6 mv Gas Flow Gain 5 00 Run Cancel Mode Use the up arrow to Pan up the Chart use the down arrow to Pan down the Chart use the left arrow to Pan left on the Chart or use the right arrow to Pan right on the Chart Once the desired chart view has been achieved press Accept to save the new chart view or press Cancel to return to the original chart view The x axis range is
80. gan Analytical Chemistry 70 1 389A 395A 1998 Quantitation of Combinatorial Libraries of Small Organic Molecules by Normal Phase HPLC with Evaporative Light Scattering Detection C E Kibbey Molecular Diversity 1 4 247 258 1996 An Alternative Method for the Determination of Chloride in Pharmaceutical Drug Substances Using HPLC and Evaporative Light Scattering Detection D S Risley J A Peterson K L Griffiths and S McCarthy LC GC 14 12 1040 1047 1996 A High Performance Liquid Chromatography Method for the Quantitation of Impurities in an NMDA Antagonist Using Evaporative Light Scattering Detection D S Risley and J A Peterson Journal of Liquid Chromatography 18 15 3035 3048 1995 Trace Analysis of a Weak UV Absorbing Pharmaceutical Compound in Swab Samples Using HPLC with Evaporative Light Scattering Detection D S Risley K F Hostettler and J A Peterson LC GC 16 6 562 568 1998 POLYMER AND SURFACTANT APPLICATIONS Universal Detection and Quantitation of Surfactants by High Performance Liquid Chromatography by Means of the Evaporative Light Scattering Detector G R Bear Journal of Chromatography 459 91 107 1988 Chemical Characterization of Cellulose Acetate by Non Exclusion Liquid Chromatography T R Floyd Journal of Chromatography 629 243 254 1993 Acrylic Block Copolymer Analysis by Adsorption Chromatography with ELSD B L Neff H J Spinelli Journal of Applied Polymer Sc
81. graphy Evaporative Light Scattering Detection Performed with Silica Columns L Carbognani Journal of Chromatography A 788 63 73 1997 Analysis of Human Milk Triacylglycerols by High Performance Liquid Chromatography with Light Scattering Detection S M Pons A I Castellote Bargallo and M C Lopez Sabater Journal of Chromatography A 823 475 482 1998 Evaluation by High Performance Liquid Chromatography of the Hydrolysis of Human Milk Triacylglycerides During Storage at Low Temperatures S M Pons A I Castellote Bargallo and M C Lopez Sabater Journal of Chromatography A 823 467 474 1998 Prediction of Relative Retention Times of Triacylglycerols in Non Aqueous Reversed Phase High Performance Liquid Chromatography J T Lin L R Snyder and T A McKeon Journal of Chromatography A 808 43 49 1998 Analysis of Lipoxygenase Kinetics by High Performance Liquid Chromatography with a Polymer Column A Nunez and G J Piazza Lipids 30 2 129 133 1995 Gradient Reversed Phase High Performance Liquid Chromatography of Saturated Unsaturated and Oxygenated Free Fatty Acids and Their Methyl Esters J T Lin T A McKeon and A E Stafford Journal of Chromatography A 699 85 91 1995 Comparative High Performance Liquid Chromatographic Analyses of Cholesterol and Its Oxidation Products Using Diode Array Ultraviolet and Laser Light Scattering Detection S Kermasha S Kubow and M Goetghebeur Journal of Chro
82. h Reduce gain value until peaks are on scale 43 6 5 SOFTWARE TROUBLESHOOTING PROCEDURE Use the following procedure to help customers troubleshoot the software on the 3300 ELSD 1 Obtain the following information from the customer a A detailed description of the error including any error messages displayed on the unit b Serial number of the detector c Software versions on the detector The software versions on the detector can be obtained by going to Maintenance About on the unit d Configuration Error Log and Method files exported from their unit These files can be exported by inserting a USB pen drive must be 128MB or less pen drives with greater than 128MB are not compatible with the 3300 ELSD into the USB Host port on the back panel of the unit Then select Maintenance Files Export in the software to export the files The pen drive can then be removed and the files can be sent via email to Grace Alltech Technical Support technicalservice alltech grace com e The information obtained from the customer will then be forwarded to the Grace Alltech Engineering department who will provide further assistance 44 7 APPENDIX 7 1 SPECIFICATIONS MODEL 3300 ELSD SPECIFICATIONS Light Source Laser diode with collimating optics 650nm max output less than 30mW Class IIIB Product Class Class 1 laser product Detector Element Silicon photodiode Temperature Range Ambient to 120 C in 0 1 C increment
83. he drift tube and tape it with Kapton tape 19 Tighten the drift tube end plates with the six screws 20 Reinstall the drift tube insulation making sure it adheres to itself 21 Cable tie the heater wires by the heater board 22 Reconnect the three wiring connectors to heater board 23 Replace the 3300 ELSD cover and screws 7 9 MODEL 3300 ELSD QC PROCEDURE Materials Needed HPLC system with the ability to perform an accurate and precise 20 uL injection HPLC grade Water and Acetonitrile one liter pre mixed H2O ACN 45 55 for the mobile phase Hydrocortisone standard Sigma part number H 4001 stock solution of 1000ug mL made in 10096 acetonitrile Further dilutions made with HPLC grade Water for a final concentration of 2 ug mL Alltech Alltima C1 8 5 um 250 x 4 6mm column Grace part number 88056 Universal Mini Filter 1 2uL Internal Volume Porosity 0 5um Grace part number 77166 connected to Liquid Inlet on detector Data collection device that can accept an analog signal Procedure A 1 Leave the Alltima Sensitivity Connect the Alltima C18 column between the injector and detector Make sure the 0 5um filter is connected to the Liquid Inlet on the detector Program the ELSD 3300 to run with a drift tube temperature set to 40 C gain set to 16 and the nitrogen flow set to 1 5 L min Equilibrate the column with mobile phase for at least 1 hour Program the data station for
84. heck the Program Configuration and Verify boxes gt Quartus Il Programmer Chain1 cdf File Edit Options Processing Help s Hardware Setup ByteBlasterll LPT1 Mode Active Serial Programming y Progress Enable real time ISP to allow background programming for MAX II devices A MENU Chechen Use Eomae veto pes Eramine O C Documents and Setti EPCS4 06308 438 00000000 5 Change File i Gave File 14 Press Start in the Altera software and monitor the Progress bar in the upper right corner gt Quartus II Programmer Chain1 cdf File Edit Options Processing Help ByteBlasterll LPT1 low background programming for M Program Configure v Examine 22 Info Device 1 silicon ID is 0x12 4 Info Erasing ASP configuration device s SD Info Programming device 1 15 When the Progress bar reaches 100 power off and unplug the unit and remove the FPGA cable from J14 W Quartus Il Programmer Chain1 cdf File Edit Options Processing Help Mode Active Serial Programming y Progress Enable real time ISP to allow background programming for MAX II devices wa j ae esa E ETE Im El C Documents and Setti EPCS4 063CB438 00000000 X Hardware Setup ByteBlasterll LPT1 Performing verification of type standard on device 1 Device 1 silicon ID is 0x12 Successfully performed operationis Ended Programmer ope
85. hen appear Menu Edit Method Method Method Pharmaceuticals 0 00 Control On 5 00 Gain 2 TO Accept O Conc Mode Run Use the up down arrows to tab through the method parameters and enter a new Method Name Temperature Gas Flow Gain and or Events using the keypad Press Accept to save the new method settings or press Cancel to return to the original method settings 3 3 4 DELETE To Delete a method select Method Delete and press Enter The Delete Method window will then appear Operation gt Configuration gt Maintenance gt LA Delete Method Please select a method to delete 01 Pharmaceuticals 02 Carbohydrates 03 Polymers Output High yuu Kuri Select a method to delete from the list using the up down arrows or by entering cycling a number Press Accept to delete the method or press Cancel to cancel deleting the method 3 3 5 WIZARD The Method Wizard can help provide initial detector settings based on the mobile phase solvent composition mobile phase flow rate and sample concentration Select Method Wizard and press Enter and the first Method Wizard screen will appear Menu LEES P mil munn momo bi l 5 Method Wizard Select Mobile Phase Solvents Operation gt Method gt Please select the solvents in your mobile phase and enter a Configuration Percentage for each Maintenance gt S Total Continue e Cancel ju mMuue Kull Select Mobil
86. his procedure 2 Complete the LOLO Upgrade Procedure in Section 2 Power off the unit from the back panel and disconnect 7 5 1 2 the power cord 3 Complete the WinCE OS Initial Setup Procedure in 3 Using a Phillips screwdriver remove the cover screws l Section 7 5 1 3 1 on each side and 4 on the back panel 4 Remove the ELSD cover by carefully sliding it toward the 4 Complete the Application Initial Setup Procedure in backoff the in irument and set aside Section 7 5 1 4 5 Connect the FPGA cable to connector J14 on the processor board inside the unit J14 is a 10 pin connector located in the lower left corner of the processor board The red wire of the FPGA cable should be towards the back panel of the unit 6 Connect the FPGA cable to the parallel port LPT1 on the PC 7 Reconnect the power cord and power up the unit 8 Start the Altera Quartus ll Programmer software on the PC The following screen will appear 3 Quartus Il Programmer Chain1 cdf File Edit Options Processing Help hi Hardware Setup ByteBlasterll LPT1 Mode JTAG v Progress 0z Enable real time ISP to allow background programming for MAX Il devices File Device Checksum Usercode Becta Verify aa Examine nm Auto Detect 2b Add File AM Change rie Bi severe Add Device System Ready NUM 9 In the Mode drop down menu at the top of the screen select Active Serial Programming 47
87. ience 42 595 600 1991 Use of an Evaporative Light Scattering Detector in Reversed Phase High Performance Liquid Chrom atography of Oligomeric Surfactants Y Mengerink H C De Man S J Van Der Wal Journal of Chromatography 552 593 604 1991 MISCELLANEOUS APPLICATIONS Determination of the Mass Extractable in Organic Solvents by Light Scattering Detection Katherine S Hammond Joanne Shatkin Brian P Leaderer Applied Occupational Environmental Hygiene 7 1 49 54 January 1992 Determination of Decyldimethyl Ammonium Chloride on Wood Surfaces by HPLC with Evaporative Light Scattering Detection C R Daniels Journal of Chromatographic Science 30 497 499 December 1992 Newer Method for the Characterization of Higher Molecular Mass Coal Derivatives Keith D Bartle Erdol und Kohle Erdgas Petrocheme Vereinigt mit Brennstoff 36 1 January 1983 ALLTECH is a trademark registered in the United States and or other countries of Alltech Associates Inc SOFGRIP is a trademark of Alltech Associates Inc GRACE and GRACE DAVISON are trademarks registered in the United States and or other countries of W R Grace amp Co Conn GRACE DAVISON DISCOVERY SCIENCES is a trademark of W R Grace amp Co Conn WINDOWS is a trademark of Microsoft Corporation This trademark list has been compiled using available published information as of the publication date of this brochure and may not accurately reflect c
88. ilt in Diagnostic tests for troubleshooting The Model 3300 ELSD also features compact stackable dimensions allowing it to fit easily into limited laboratory space 1 2 PRINCIPLE OF OPERATION The unique detection principle of evaporative light scattering detection involves a three step process nebulization of the column effluent to form an aerosol solvent evaporation within a heated drift tube and detection of the non volatile solute particles in the light scattering cell NEBULIZATION EVAPORATION DETECTION NEBULIZATION The column effluent from an HPLC separation enters the nebulizer where it is mixed with a steady stream of nebulizing gas usually nitrogen to form an aerosol The aerosol consists of a uniform distribution of droplets whose size is dependent on the gas flow rate used for the analysis The lower the gas flow rate used the larger the resulting droplets will be Larger droplets scatter more light and increase the sensitivity of the analysis but they are also more difficult to evaporate in the drift tube There will be an optimum gas flow rate for each method which will produce the highest signal to noise ratio Lower mobile phase flow rates will require lower gas flow rates for optimal nebulization Substitution of a 2 1mm ID column for your standard 4 6mm ID column will allow you to greatly reduce the mobile phase flow rate while also increasing the sensitivity of the analysis EVAPORATION Eva
89. in 0 2L min at each gas flow set point 1 0 2 0 3 0 and 4 0L min 7 Once the test is completed press Done to return to the 6 22 GAS FLOW TEST main screen or press Test to repeat the test 1 Make sure the inlet gas pressure is set between 65 and 80psig before starting the test 8 If the test has failed refer to the following table Gas Flow Test Results for possible fail messages and their solutions 2 Turn off mobile phase flow Wait several minutes for the GAS FLOW TEST RESULTS detector to stabilize RESULT CAUSE SOLUTION 3 In the software select Maintenance Tests Gas Flow Test and press Enter The testing screen will then appear Fail Gas flow is Unstable inlet unstable gas pressure Check stability of gas source and remedy if necessary Menu Gas Flow Test iutput Maintenance gt Gas flow meter or valve error Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details 4 Press Test and the Gas Flow Test will begin The test takes 4 minutes to complete A timer bar will appear showing how much time is left for the test Nebulizer may need replacement Replace nebulizer Menu Gas Flow Test utput Fail Gas flow is lower than the set point Gas supply is low or empty Check gas supply and replace if necessary Gas Flow Test Maintenance gt A Gas supply valve is closed Open gas supply valve Bl
90. ion Plug the power cord provided with the unit into the power module on the back panel of the detector The module is autoselecting for 85 265V diens Only use the power supply cord recommended by the manufacturer 5 14 Pin Connector Insert the 14 pin connector into the port on the back panel Make the appropriate wiring connections to the 14 pin connector depending on which of the following functions are needed Start Pin 1 Ground Pin 2 Signal Pins 1 and 2 on the Model 3300 ELSD can accept a TTL contact closure signal to start a method run on the detector Standby Pin 3 Ground Pin 4 Signal Pins 3 and 4 on the Model 3300 ELSD can accept a TTL contact closure signal to put the detector into Standby mode Gas Shutoff Pin 5 Ground Pin 6 Signal Pins 5 and 6 on the Model 3300 ELSD can accept a TTL contact closure signal to turn off gas flow at the end of a run This signal is typically sent from an autosampler or a data collection system Consult the appropriate manuals for wiring information Autozero Pin 7 Ground Pin 8 Signal Pins 7 and 8 on the Model 3300 ELSD can accept a TTL contact closure signal from a start signal cable to autozero the detector This signal is typically sent from an autosampler or a manual injection valve with a position sensing switch Consult the appropriate manuals for wiring information External Output Pin 9 Normally Open NO Pin 10 Common
91. ion 6 2 for details on these tests 3 5 4 FILES Files can be imported or exported from the unit using a pen drive inserted into the USB Host port on the back panel of the unit The USB pen drive must be 128MB or less for the import export function to work properly EXPORT To Export files from the detector insert a pen drive into the USB Host port on the back panel of the unit Select Maintenance Files Export Configuration Methods Service Log Service Tech mode only or Error Log using the arrows on the keypad and press Enter A message will then appear indicating that the files have been successfully exported press Accept and then the pen drive containing the files can be removed To enter Service Tech mode select Maintenance Service Tech using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept IMPORT To Import files to the detector insert a pen drive containing the files into the USB Host port on the back panel of the unit Select Maintenance Files Import Configuration or Methods and press Enter A message will then appear indicating that the files have been successfully imported press Accept and the pen drive can then be removed The files to be imported must be located inside a folder named Alltech on the pen drive in order for the import to be successful 3 5 5 SERVICE TECH Service Tech functions are reserved for qualified personnel only By entering Servi
92. iquid Tubing Impactor Cartridge Nebulizer LCD Liquid Crystal Display The LCD displays the software interface screens The Model 3300 ELSD can be powered on off from the front panel of the unit using the soft power button NOTE The power button on the back panel must be set to the On position in order for the front panel button to be active Liquid Inlet The column effluent tubing connects to the LIQUID INLET with a 1 16 male fitting The stainless steel tubing carries the column effluent to the liquid inlet of the nebulizer The cartridge can be removed in order to access the drift tube for cleaning Refer to Section 5 3 Drift Tube Cleaning Procedure for details The column effluent and nitrogen gas are combined within the nebulizer to form an aerosol The nebulizer is easily removed for cleaning by pushing in and using a counterclockwise twisting motion 10 Nebulizer Gas Tubing The gas tubing carries nitrogen gas to the nebulizer gas inlet Drain Port The DRAIN port is located on the right side of the front panel The drain tubing and clamp included with the unit are connected to the DRAIN port and then directed to a waste reservoir not included located at bench level if the unit is stacked or floor level NOTE The drain tubing must not be submerged in the liquid inside the reservoir during operation Keypad The keypad is used to interact with the software interface screens Rem
93. isocratic or gradient capable of low pulsation solvent delivery at a flow rate ranging from at least 0 1 to 1 5mL min against pressures of at least 3 000 psig Lower flow rate capabilities may be necessary for smaller bore columns eAn autosampler or manual injection valve eA column capable of separating the compounds of interest If you are uncertain which column to use contact your Grace Davison Discovery Sciences representative or the Grace Technical Support Group for assistance Phone 1 800 33 SOL VE eA guard column or cartridge compatible with the separation column is recommended to prolong separation column lifetime eA column heater if needed eA data system or integrator capable of accepting analog voltage data 0 10mV or 0 1000mV systems can be used Other eHPLC grade mobile phase solvents NOTE Only volatile buffers may be used in the mobile phase Refer to Section 7 10 Volatile Mobile Phase Modifiers for a list of suitable buffers eSolvent reservoirs tubing inlet filters paper etc required for pump and data system operation Consult the appropriate manuals for requirements 2 2 UNPACKING The Model 3300 ELSD detector and its accessories are shipped in the same container Unpack components carefully making sure all items in the list below have been included and are in good condition Save the container and packing material for future use The Model 3300 ELSD shipping container should c
94. iutput Maintenance gt a 0 00 Mode Standby 14 Flip the left switch to 96 C The Raw Value should significantly increase Press Continue to reach the next step of the calibration Upper Drift Tube Temp Calibration Low Method Method 1 Upper Drift Tube Temp Calibration Low iutput Maintenance gt s 0 00 Mode Standby 15 The middle switch should be set to 17 C Press Continue to reach the next step of the calibration Upper Drift Tube Temp Calibration High Method Method 1 Upper Drift Tube Temp Calibration High iutput Maintenance gt Mode Standby 16 Flip the middle switch to 96 C The Raw Value should increase again Press Continue to reach the next step of the calibration Optics Block Temp Calibration Low Menu Method Method 1 25 If the measured temperatures are within tolerance Optics Block Temp Calibration Low 2 C at 40 C and 70 C and 3 C at 100 C then iutput heater calibration is finished If any measured value is not within tolerance continue on to step 26 26 Select Maintenance Calibration Heaters Correction using the arrows on the keypad and press Enter to reach the Temperature Correction screen oer gt 0 00 Mode Standby Menu Temperature Correction 17 The third switch should be set to 17 C The raw value should decrease Press Continue to reach the next step of tput the calibration Optics Block Temp Calibration High TEE Metho
95. l Fe cancel Mode Run Make the desired changes to the Event Time Event Type Gain or External Contact Press Accept to save the event changes or press Cancel to cancel the changes 13 DELETE EVENT To Delete an event use the up down arrows to highlight the event to be deleted from the table Then use the right arrow and the down arrow to select Delete and press Enter The event will then be deleted Once all method parameters have been entered press Accept to save the new method The Save Method window will then appear Menu Method gt Ea PLE DEALER KA EIS AH Save Method Output 01 Pharmaceuticals pt HEBES min O accept Cancel ERIS MUUe otar IUD Yy Use the up down arrows or the keypad to select a method number for the new method Press Accept to save the new method or press Cancel to cancel the new method 3 3 2 OPEN Select Method Open using the arrows on the keypad and press Enter to open an existing method The Open Method window will then appear Open Metho Method gt Dutnut 170 7 mV 01 Pharmaceuticals 103 Polymers iuue KUT Use the up down arrows or enter the method number on the keypad to select a method from the list Press Accept and the method will then load on the main screen or press Cancel to cancel loading the method 3 3 3 EDIT To Edit an existing method select Method Edit using the arrows on the keypad and press Enter The Edit Method window will t
96. l need to know the IP address of the PC running the TFTP server The TFTP server displays that information on its main screen In the example screen above the IP address is 159 97 84 210 Replace that address in the command below with the one from your TFTP server screen Do the following sequence of commands a Copy the boot script cp tftp 159 97 84 210 boot losh app boot losh The expected output from this command is cp tftp 159 97 84 210 boot losh app boot losh done b Copy the serial EEPROM setup script cp tftp 159 97 84 210 setup losh app setup losh The expected output from this command is cp tftp 159 97 84 210 setup losh app setup losh done c Copy the OS image Gp Z tftp 159 97 84 210 nk bin app nk bin This command may take a minute to run The expected output from this command is cp Jtftp 159 97 84 210 nk bIm gt app nk bin done 18 Next the serial EEPROM will be updated to mount the YAFFS filesystem on power up and boot the OS Run the following command source app setup losh The expected output from this command is Setup serial EEPROM for booting from YAFFS echo LOLOadd yaffs app nor 0x00040000 0x01fc0000 mount yaffs app cd app source boot losh exitirin dev serial eeprom 19 The OS image has been installed the ELSD can be rebooted 20 Once the ELSD reboots a white screen should appear The ELSD will appear to halt at this screen This is because no application
97. lock and drift tube may still be hot 6 Remove the 4 screws connecting the laser to the optics mount using the hex ball driver and remove the laser Allow the laser to hang inside the unit 7 Remove the 4 screws on the optics mount using the hex ball driver and remove the optics mount 8 Remove the laser window Clean the window with acetone and cleaning wipes until no residue remains 9 Replace the laser window 10 Reattach the optics mount 11 Reconnect the laser Make sure the laser is oriented so the magnetic interlock makes the proper connection 12 Replace the instrument cover and tighten the cover screws The unit is now ready for use 25 5 4 3 PHOTODIODE CLEANING PROCEDURE A WARNING Use of controls adjustments or performance of procedures other than those specified herein may result in hazardous exposure to laser light A WARNING Class 3B laser radiation when optics are open and interlocks defeated Avoid exposure to beam Materials Needed e Anti static strap e Phillips screwdriver e HPLC grade acetone e Cleaning wipes References Figure 5 2 and Figure 5 3 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure 2 Power off the unit from the back panel and disconnect the power cord ad Allow the unit to cool for at least 30 minutes Using a Phillips screwdriver remove the cover screws 1 on each side and 4 o
98. matography A 685 229 235 1994 A Qualitative Method for Triglyceride Analysis by HPLC Using an ELSD W S Letter Journal of Liquid Chromatography 16 1 225 239 1993 Fatty Acid Composition of Human Milk Triglyceride Species Possible Consequences for Optimal Structures of Infant Formula Triglycerides Cheil H Winter Edda B Hoving Frits A J Muskier Journal of Chromatography 616 9 24 1993 Analysis of Triglycerides in Oils and Fats by Liquid Chromatography with Laser Light Scattering Detector Andrzej Stolywho Henri Colin Georges Guiochon Analytical Chemistry 57 1342 1354 1985 Lipase G Catalyzed Synthesis of Monoglycerides in Organic Solvent and Analysis by HPLC Casmir Akoh Carolyn Cooper Chigozie Nwosu Journal of the American Oil Chemists Society 69 9 March 1992 Determination of the Positional Distribution of Fatty Acids in Butter Fat Triacylglycerols S Kermasha S Kubow M Safari A Reid Journal of Chromatographic Science 70 169 173 1993 A New Variety of Low Linolenic Rapeseed Oil Characteristics and Room Odor Tests A Prevot J L Perin G Laclaverie P H Auge Coustille J L Journal of the American Oil Chemists Society 67 3 161 March 1990 Analysis of Tocopherols and Phytosterols in Vegetable Oils by HPLC with Evaporative Light Scattering Detection K Warner T L Mounts Journal of the American Oil Chemists Society 67 11 November 1990 Analysis of Dimer Acids U
99. n the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument and set it aside CAUTION The optics block and drift tube may still be hot 6 Disconnect the ribbon cable from the preamp board Allow it to hang inside the unit 7T Remove the 4 preamp cover screws using the Phillips screwdriver and remove the preamp cover 8 Remove the preamp board screws using the Phillips screwdriver and remove the preamp board 9 Flip the preamp board to access the photodiode sensor Use acetone and cleaning wipes to clean the surface of the photodiode until there is no visible residue 10 Replace the preamp board and preamp screws 11 Replace the preamp cover and preamp cover screws 12 Reconnect the ribbon cable to the preamp board 13 Replace the instrument cover and tighten the cover screws The unit is now ready for use 5 4 4 PRE AMP LENS ASSEMBLY CLEANING PROCEDURE A WARNING Use of controls adjustments or performance of procedures other than those specified herein may result in hazardous exposure to laser light A WARNING Class 3B laser radiation when optics are open and interlocks defeated Avoid exposure to beam Materials Needed e Anti static strap Phillips screwdriver Hex ball driver 3 32 Hex ball driver 7 64 HPLC grade acetone Cleaning wipes References Figure 5 2 and Figure 5 4 1 Precaution must be taken use of an anti static foot strap in a grounded
100. nance Service Tech using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept Once in Service Tech mode select Configuration Serial Number The Serial Number Configuration screen will then appear Menu Serial Number Configuration iutput Configuration gt 33000206005 Enter the serial number using the keypad The serial number can contain numbers only Press Accept to save the new serial number or press Cancel to cancel the changes If Accept is pressed a Success screen will appear indicating that the new serial number has been set Press Accept to confirm that the new serial number will be saved 3 4 3 OUTPUTS Select Configuration Outputs using the arrows on the keypad and press Enter The Outputs Configuration screen will then appear Menu Method Pharmaceuticals Outputs Configuration Output Enabled 4 gt 380 0 mV Enabled 4 gt Configuration gt 500 0 ooo O Accept e Cancel 1 00 Mode Run FAULT RELAY Use the left right arrow keys to select Enabled or Disabled for the Fault Relay setting If Enabled the detector will output a signal to stop a pump if errors occur on the unit The proper wiring must be connected for the Fault Relay to work Refer to Section 2 4 for wiring details If Disabled errors will not trigger an output to a pump for pump shutdown FULL SCALE VOLTAGE Use the left right arrows to select 10mV or 1V for the full scale
101. nded environment while performing this procedure 2 Power off the unit from the back panel and disconnect the power cord 3 Allow the unit to cool for at least 30 minutes 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument and set aside CAUTION The optics block and drift tube may still be hot 6 Disconnect the sweep gas tubing from the light trap The connection is a quick connect fitting push in the plastic ring and then pull the tubing towards you to remove 7 Remove the insulation from the light trap by gently pulling it away from the optics block 8 Using the hex ball driver remove the 4 hex head screws connecting the light trap to the optics block and carefully remove the light trap Refer to Figure 5 1 for details To clean inspect the inside of the light trap for residue Swab the inside of the light trap as necessary with a suitable solvent to clean any residue The inside of the light trap should be black 24 11 12 Light Trap Interlock With the light trap removed the optics block can be accessed for cleaning Inspect the inside of the optics block for residue Swab the inside of the optics block with a suitable solvent to clean any residue The inside of the optics block should be black Once the optics have been cleaned reattach the light trap and replace the
102. nder the above conditions Refer to Section 7 6 for details 40 6 4 TROUBLESHOOTING CHARTS Consult the following charts to assist in troubleshooting your system TROUBLESHOOTING PROBLEM CAUSE SOLUTION Baseline drift Detector has not fully equilibrated Wait for detector to fully equilibrate Refer to Section 4 4 Start Up Sequence for equilibration procedure Baseline noise Follow the procedure in Section 6 3 Diagnosing Baseline Noise to determine the source of the problem and possible solutions Drift tube temperature and or gas flow Re optimize the drift tube temperature and gas rate set too low flow rate following the optimization procedure in Section 4 6 Gas source contaminated or low Use clean dry inert gas usually 99 996 pure purity nitrogen Mobile phase contaminated or made Replace with fresh filtered higher quality of low quality material mobile phase Nebulizer drift tube and or optical cell Refer to Sections 5 1 5 4 for cleaning dirty procedures Improper nebulization Nebulizer may be partially obstructed Refer to Section 5 2 for nebulizer cleaning procedure Drift tube temperature not Thermal fuse s may be blown Allow the resettable fuses 2 hours to reset Then reaching set point recheck the thermofuse and replace if necessary Refer to Section 7 8 for details Heater calibration is off Recalibrate heaters Refer to Section 7 6 1 for details Bad RTD s Check RTD s Replace
103. nect the power cord Allow the unit to cool for at least 30 minutes Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel 5 Remove the ELSD cover by carefully sliding it toward the back of the instrument 6 Disconnect the three RTDs DT1 DT2 and Optics from the processor board positions J22 J23 and J24 respectively 7 Connect the Temperature Calibration Box to the processor board by connecting the left middle and right cables to positions J22 J23 and J24 respectively 8 Set all three switches on the Temperature Calibration Box to 17 C 9 Power on the 3300 ELSD and wait for the instrument to boot up 10 Select Maintenance Service Tech Enter Service Tech Password using the arrows on the keypad and press Enter 11 Enter the password atat and press Accept to enter Service Tech mode 12 Select Maintenance Calibration Heaters Calibration using the arrows on the keypad and press Enter The first screen of the heater calibration will then appear Lower Drift Tube Temp Calibration Low 56 Method Method 1 Lower Drift Tube Temp Calibration Low iutput Maintenance gt rg S 0 00 Mode Standby 13 The left switch on the Temperature Calibration Box should be set to 17 C Press Continue and the next screen in the calibration procedure will appear Lower Drift Tube Temp Calibration High Method Method 1 Lower Drift Tube Temp Calibration High
104. nel Remove the ELSD cover by carefully sliding it toward the back of the instrument and set aside Locate the connector s on the heater board for the zones to be checked The connectors are located at positions J4 J5 and J6 which correspond to lower drift tube upper drift tube and optics block respectively Refer to Section 7 7 1 Electronic Schematic for details Disconnect the connector s from the Heater Board Using a multimeter measure the resistance between the thermofuse wires The thermofuse wires are located on the top row of each connector If there is infinite resistance between the wires the thermofuse needs replacement Refer to Section 7 8 2 3 Thermofuse Replacement Procedure for details on replacing the thermofuse s If the thermofuse s are ok then replace the connector s back to their original position s and replace the 3300 ELSD cover and screws 62 7 8 1 2 CHECKING THE RTDS Tools Needed e Anti static strap e Phillips screwdriver e Digital multimeter Reference Section 7 7 1 Electronic Schematic 1 Precaution must be taken use of an anti static foot strap in a grounded environment while performing this procedure 2 Power off the unit from the back panel and disconnect the power cord 3 Before checking the thermofuses first allow the resettable fuses 2 hours to reset 4 Using a Phillips screwdriver remove the cover screws 1 on each side and 4 on the back panel
105. ning and press Enter In Cleaning mode the heaters gas flow and laser are on Temperature is set to 110 C Gas Flow is set to 2 0L min and Gain is set to 1 The detector should be run with 100 water or other suitable solvent at 1 0mL min for at least one hour to clean the detector The detector will remain in Cleaning mode until the detector is switched to another mode CA Method Cleaning Set Read Temperature TIMORE 110 129 Output Gas Flow 2 0 L min 2 0 L min 17 4 mV Maintenance gt Gain al 500 0 60 00 50 00 Mode Cleaning 5 2 NEBULIZER CLEANING PROCEDURE The nebulizer can become blocked over time with sample and mobile phase materials A dirty or blocked nebulizer can cause increased baseline noise and decreased sensitivity The following procedure can be used to clean the nebulizer Materials Needed e Open end wrench 1 4 x 5 16 e HPLC grade 50 50 methanol water solution e Sonication bath 1 Power off the unit from the back panel and disconnect the power cord 2 Remove the front door by gently pulling it towards you from the handle and set aside 3 Disconnect the stainless steel liquid inlet line from the nebulizer using the 1 4 wrench 4 Disconnect the quick connect gas tubing from the front panel Push in then pull out to remove the tubing 5 Remove the nebulizer from the drift tube by pushing in and turning it firmly counterclockwise 6 Remove the orange wear band from the nebuliz
106. ockage or leaks in gas line before the detector Check gas line for blockage and leaks remedy replace as necessary 5 The following steps occur during the Gas Flow Test e Gas flow is set to 1 0 2 0 3 0 and 4 0L min and allowed to stabilize at each flow rate Gas flow meter and or valve error Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details e Minimum maximum and average gas flow rate values are determined at each flow rate e Test results are displayed The gas flow is returned to its pre testing set point Gas flow calibration is off Recalibrate gas flow Refer to Section 7 6 2 for details 35 GAS FLOW TEST RESULTS continued RESULT CAUSE SOLUTION Fail Gas flow Gas flow calibration is higher than the set point Recalibrate gas flow Refer to Section 7 6 2 for details Gas flow meter and or valve error Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details 6 2 3 OPTICS TEST 1 Make sure the inlet gas pressure is set between 65 and 80psig before starting the test Turn off mobile phase flow Wait several minutes for the detector to stabilize In the software select Maintenance Tests Optics Test and press Enter The Optics Test screen will then appear Menu Optics Test Maintenance Orem Qee 4 Press Test and the Optics Test will begin The test take
107. of Wheat Flour Lipids Using an Evaporative Light Scattering Detector F Conforti Carolyn H Harris Janet T Rinehart Journal of Chromatography 645 83 88 1993 Determination of Cholesterol in Milk Fat by Reversed Phase High Performance Liquid Chromatography and Evaporative Light Scattering Detection George A Spanos Steven J Schwartz LC GC 10 10 774 777 1992 NUTRACEUTICAL PHARMACEUTICAL APPLICATIONS Determination of Fumonisins B B B and B by High Performance Liquid Chromatography with Evaporative Light Scattering Detection J G Wilkes J B Sutherland M I Churchwell and A J Williams Journal of Chromatography A 695 319 323 1995 High Performance Liquid Chromatographic Analysis of Ginseng Saponins Using Evaporative Light Scattering Detection M K Park J H Park S B Han Y G Shin and I H Park Journal of Chromatography A 736 77 81 1996 A Facile Separation of Nonactin and Its Homologues T Herlt Journal of Liquid Chromatography and Related Technologies 20 8 1295 1300 1997 Simultaneous Resolution and Detection of a Drug Substance Impurities and Counter lon Using a Mixed Mode HPLC Column with Evaporative Light Scattering Detection M D Lantz D S Risley and J A Peterson Journal of Liquid Chromatography amp Related Technologies 20 9 1409 1422 1997 71 High Throughput Characterization of Combinatorial Libraries Generated by Parallel Synthesis J N Kyranos and J C Ho
108. ons 7 8 and 7 6 1 for details Replace heater board and then recalibrate the heaters Refer to Section 7 6 1 OPTICS HEATING TEST RESULTS continued CAUSE RESULT Fail The Optics Block temperature is xx x of the drift tube temperature It should be XX X continued Bad processor board 6 2 5 HEATER STABILITY TEST Blown thermofuse SOLUTION Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Allow the resettable fuse 2 hours to reset Then recheck the thermofuse and replace if necessary Refer to Section 7 8 for details This function is available in Service Tech Mode only 1 Menu Make sure the detector is set to Run mode and is fully equilibrated before running the test Enter Service Tech mode by selecting Maintenance Service Tech Enter Service Tech password and entering atat using the keypad Select Maintenance Tests Heater Stability using the arrows on the keypad and press Enter The Heater Stability Test screen will then appear Heater Stability Test iutput 71 3 mV 2 ee ee Maintenance gt 4 Press Test and the Heater Stability Test will begin The test takes 2 minutes to complete A timer bar will appear that shows how much time is left for the test Heater Stability Test iutput 71 5 mY Heater Stability Test Maintenance gt 38 T 5 The following steps o
109. ontain the following Model 3300 ELSD Model 3300 ELSD Operating Manual Model 3300 ELSD Performance Documents Model 3300 ELSD Driver for Agilent ChemStation CD Power Cord Signal Cable PEEK Tubing 1 16 OD x 005 ID 10 SofGrip Fittings 10 pk Gas Tubing 10 Gas Fittings 1 8 Brass Nut and Ferrule Drain Tubing 5 Reservoir not included Drain Tubing Clamp Exhaust Adaptor Exhaust Tubing 20 14 Pin Connector Open End Wrench 3 8 x 7 16 Open End Wrench 1 4 x 5 16 Hex Ball Driver 3 32 x 5 1 4 Hex Ball Driver 7 64 x 4 Drift Tube Cleaning Brush Fuse 5 Amp The 3300 ELSD Driver for Agilent ChemStation CD can be used with Agilent ChemStation to control and collect data from the 3300 ELSD Agilent ChemStation must be purchased separately The Model 3300 ELSD has been carefully shipped to ensure that it is received in proper condition Any damage to the container or its contents should be reported immediately to your local distributor or to Grace Davison Discovery Sciences Please refer to Section 7 11 Warranty Returns and Repairs for more information Refer to Section 7 3 Replacement Parts for part numbers if replacement parts are needed 2 3 CONTROLS AND FEATURES Alltech 3300 ELSD u 25 79 mv Output a PRODUCTOF GRACE Davison Figure 2 1 Front Panel of 3300 ELSD Door Removed 2 3 1 FRONT PANEL FIGURE 2 1 1 Soft Power Button Nebulizer L
110. ospholipids and Glycolipids Using Light Scattering Detection G A Picchioni A E Watada and B D Whitaker Lipids 31 2 217 221 1996 Separation of Synthetic Phosphatidylcholine Molecular Species by High Performance Liquid Chromatography on a Cs Column J T Lin C L Woodruff T A McKeon and J A Singleton Journal of Chromatography A 824 169 174 1998 New Procedures for Rapid Screening of Leaf Lipid Components from Arabidopsis W W Christie S Gill J Nordback Y lItabashi S Sanda and A R Slabas Phytochemical Analysis 9 53 57 1998 Characterization of Rabbit Myocardial Phospholipase A Activity Using Endogenous Phospholipid Substrates O Vesterqvist C A Sargent G J Grover B M Warrack G C DiDonato and M L Ogletree Analytical Biochemistry 217 210 219 1994 Separation of Lipid Classes from Plant Tissues by High Performance Liquid Chromatography on Chemically Bonded Stationary Phases W W Christie and R A Urwin Journal of High Resolution Chromatography 18 97 100 1995 Separation of Neutral Lipids by High Performance Liquid Chromatography Quantification by Ultraviolet Light Scattering and Fluorescence Detection E J Murphy T A Rosenberger and Lloyd A Horrocks Journal of Chromatography B 685 9 14 1996 A Rapid Method for Phospholipid Separation by HPLC Using a Light Scattering Detector W S Letter Journal of Liquid Chromatography 15 2 253 266 1992 High Performance Li
111. ovable Door not shown The front door can be opened or removed to access the nebulizer and drift tube for cleaning To remove the door gently pull the door towards you 2 3 2 BACK PANEL FIGURE 2 2 USB Devi 4 7 l Eg Exhaust Ethernet B Start Standby lI 2 3 4 e Gas Shuoff Auto Zero g NO ocou External Output I N 2 NO seu Faut Relay HN 0000000000000 Figure 2 2 Model 3300 ELSD Back Panel Signal Output The signal cable included with the unit is connected to the SIGNAL OUTPUT port on the back panel of the unit and is used to send the analog signal to the data collection device RS 232 This port is currently reserved for service tech functions only USB Host A pen drive not included can be inserted into this port for file importing exporting and software upgrades USB Device This port is currently reserved for service tech functions only Ethernet This port can be used with the 3300 ELSD Driver for Agilent ChemStation This port is also used for service tech functions 14 Pin Connector Outputs TTL contact closure signals or accepts signals from peripheral equipment 7 Exhaust Outlet Nebulizer gas mobile phase vapor and solute mist or particles produced during an analysis will exit the detector through the EXHAUST outlet The exhaust outlet accepts the exhaust adaptor and exhaust tubing included with the unit which must be then directed to a f
112. pactor Light Trap Light Trap Cover Light Trap Gasket Light Trap ND Filter Laser Power Entry Module Fuse Drawer 46 mem 3300 ELSD Service Kit includes all parts listed below 3300100SM 3116580 8617092 3116671 2107799 2113972 2114102 3112023 2113971 2107268 2114101 2113970 2113969 v A A A A A A A L1 lI 3300 ELSD Service Manual Pre Amp and Laser Calibration Fixture Temperature Calibration Box Drift Tube Temperature Device Claw Magnet for Magnetic Switch 128MB Flash Drive Jumper for Cal Box SMB Cable FPGA Cable 3 32 Standard Ball Driver Small Flat Screwdriver for Pots Crossover Cable Serial Modem Cable 7 5 SOFTWARE UPGRADE PROCEDURES 7 5 1 1 FPGA INSTALLATION PROCEDURE 7 5 1 COMPLETE SOFTWARE RE INSTALLATION Materials Needed PROCEDURE e Anti static strap e Phillips screwdriver The software re installation procedure should be completed e FPGA cable e Altera Quartus Il programming software downloaded e if the processor board has been replaced onto a pc _ e if the existing software files on the unit have e New FPGA software file pof become corrupted l l l Reference Section 7 7 1 Electronic Schematic These steps must be followed in order for the re installation to be successful Procedure 1 Precaution must be taken use of an anti static foot 1 Complete the FPGA Installation Procedure in Section strap in a grounded environment while performing a t
113. poration of the volatile components in the aerosol occurs in a heated stainless steel drift tube The optimum drift tube temperature setting for an application will depend on mobile phase composition mobile phase flow rate and on sample volatility Highly organic mobile phases require lower drift tube temperatures for evaporation than highly aqueous mobile phases Lower mobile phase flow rates require lower drift tube temperatures than higher mobile phase flow rates Semi volatile analytes require the use of much lower drift tube temperatures to obtain optimum sensitivity The optimum temperature should be determined by observing the signal to noise ratio with respect to temperature Within the Model 3300 ELSD drift tube a PTFE coated stainless steel impactor plate is located three inches from the nebulizer The plate is perpendicular to the aerosol path so as the aerosol contacts the plate larger droplets exit through the drain tube on the side panel The remaining droplets pass around the impactor and travel through the drift tube to the optical cell for detection The removal of the larger droplets allows operation of the Model 3300 ELSD at low temperatures making it ideal for the analysis of semi volatile compounds Non volatile impurities in the mobile phase or nebulizing gas will produce noise Using the highest quality gas solvents and volatile buffers preferably filtered will greatly reduce baseline noise Noise will also incre
114. quid Chromatography of Lipids for the Identification of Human Metabolic Disease Thomas C Markello Juanru Gu and William A Gahl Analytic Biochemist 198 368 374 1991 Detection of HPLC Separation of Glycophospholipids Part 1 J V Amari P R Brown J G Turcotte American Laboratory 23 29 February 1992 Optimization of Detection for HPLC Separations of Glycerophospholipids Part 2 J V Amari P R Brown J G Turcotte American Laboratory 26 33 March 1992 HPLC Analysis of Phospholipids by Evaporative Light Scattering Detection T L Mounts S L Abidi K A Rennick Journal of the American Oil Chemists Society 69 5 438 432 May 1992 High Performance Liquid Chromatography of Phosphatidic Acids and Related Polar Lipids S L Abidi Journal of Chromatography 587 193 203 1991 An Improved Method for the Identification and Quantitation of Biological Lipids by HPLC Using Laser Light Scattering Detection B S Lutzke J M Braugler Journal of Lipid Research 31 2127 2130 1990 Rapid Separation and Quantification of Lipid Classes by High Performance Liquid Chromatography and Mass Light Scattering Detection W H Christie Journal of Lipid Research 26 507 512 1985 Analysis of Neutral Lipids and Glycerolysis Products from Olive Oil by Liquid Chromatography Baokang Yang Jyhping Chen Journal of the American Oil Chemist Society 68 12 December 1991 High Performance Liquid Chromatographic Analysis
115. r or bad processor board Gas source may be low or empty Regulator pressure may be too low Gas leaks may be present before the nebulizer Bad gas pressure sensor or bad processor board Nebulizer may be blocked Inlet gas pressure is unstable Gas flow meter or valve error SOLUTION Follow the nebulizer cleaning procedure in Section 5 2 Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Check gas source and replace if necessary Adjust regulator pressure to 65 80psig Check gas connections for leaks and tighten fittings if necessary Replace processor board and then recalibrate the heaters gas flow and laser preamp Refer to Section 7 6 for details Follow the nebulizer cleaning procedure in Section 5 2 Check stability of gas source and remedy if necessary Replace flow meter and or valve and then recalibrate the gas flow Refer to Section 7 6 2 for details Menu Gas Flow Test NEBULIZER GAS PRESSURE TEST RESULTS continued iutput Maintenance gt RESULT CAUSE SOLUTION Fail Gas pressure is Bad gas pressure sensor or bad processor board Replace processor board and then recalibrate the heaters gas flow 6 unstable continued and laser preamp Refer to Section 7 6 for details Passing requirements for the Gas Flow Test are e Gas flow must be with
116. ration at Fri Oct 13 19 59 30 2006 48 16 Replug in and power up the unit and wait for the main screen to load 17 Select Maintenance About in the software and verify that the new FPGA version has been loaded 18 If running the complete software re installation continue on in Section 7 5 1 2 LOLO Upgrade Procedure Otherwise the FPGA installation procedure is complete 7 5 1 2 LOLO UPGRADE PROCEDURE Materials Needed e TeraTerm Pro software program installed on a pc e Serial cable e LOLO upgrade files 1 Start the TeraTerm Pro software program on the PC Select Setup Serial Port and make sure the settings are Baud Rate 115200 Data 8 bit Parity None Stop 1 bit Flow Control None Transmit Delay Omsec char and Omsec line 2 Connect the serial cable between the 3300 ELSD and the PC 3 Power up the 3300 ELSD while holding down the q character on the PC keyboard The following should appear in the serial terminal screen kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk LogicLoader c Copyright 2002 2005 Logic Product Development Inc All Rights Reserved Version 2 0 3 LLH7a404_11 0001 kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk losh gt qqqqqqqqqq 4 Press Enter to reach the next line in the serial terminal 5 Run the following command info version The response should be similar to the following Version 2 0 3 LLH7a404_11 0001 Build
117. ry High Temperature Liquid Chromatography Roger Trones Thomas Andersen Tyge Greibrokk Journal of High Resolution Chromatography 22 5 283 286 1999 The Evaporative Light Scattering Detector S L Hansen and W E Artz Inform 6 2 170 176 1995 Detect Anything Your LC Separates P A Asmus Research amp Dev 2 96 98 1993 Evaporative Light Scattering Detectors for HPLC GPC SEC SFC A Review Bonnett P G nternational LabMate 15 5 27 29 1990 Use of Light Scattering as a Detector Principle in Liquid Chromatography A Stolyhwo H Colin G Guiochon Journal of Chromatography 265 1 18 1983 A Light Scattering Detector for Liquid Chromatography P B Stockwell B W King American Laboratory 19 24 August 1991 Evaporative Analyzer as a Mass Detector for Liquid Chromatography John M Charlesworth Analytical Chemistry 50 11 1414 1420 September 1978 Study of the Qualitative and Quantitative Properties of the Light Scattering Detector A Stolynwo H Colin M Martin G Guiochon Journal of Chromatography 288 253 275 1984 Influence of Various Parameters on the Response Factors of the Evaporative Light Scattering Detector for a Number of Non Volatile Compounds Georges Guiochon Anne Moysan Christopher Holley Journal of Liquid Chromatography 11 12 2547 2570 1988 Effects of the Nature of the Solvent and Solutes on the Response of a Light Scattering Detector Michel Righezza
118. s Nebulizer Gas Up to 4L min nitrogen preferred 65psig min pressure 80psig max pressure Mobile Phase Flow Rate 50uL 3 0mL min Analog Outputs Selectable for either O 1V or 0 10mV full scale Communications Remote Inputs TTL Contact closure Autozero Gas Shutoff Start Standby Outputs Contact closure Fault Relay External Output RS232 USB Device USB Host Ethernet Operating Parameter Windows Based Graphical Selection amp Display LCD with alphanumeric keypad Power Requirements 120 240V 50 60Hz 5A Dimensions 11 6 H x 10 3 W x 19 5 D 29 5cm H x 26 2cm W x 49 5cm D Environmental Operating Temperature 15 to 40 C Relative Humidity 10 90 Non Condensing 45 7 2 CONTACT INFORMATION Grace Davison Discovery Sciences Alltech Associates Inc 2051 Waukegan Road Deerfield IL 60015 USA Phone 847 948 8600 Fax 847 948 1078 Web www discoverysciences com www elsd com Technical Support 1 800 33 SOLVE technicalservice alltech grace com Ordering Information 1 800 ALLTECH Additional information for the 3300 ELSD including software updates can be obtained from the www elsd com website 7 3 REPLACEMENT PARTS 7 4 SERVICE KIT MODEL 3300 ELSD REPLACEMENT PARTS MODEL 3300 ELSD SERVICE KIT 5136931 2112995 2112993 2107259 2106694 2107268 2112992 2112880 2110773 5126955 2110623 2111502 2111503 2112997 2112990 3112777 2108384 2112994 2112996 N
119. s 60 seconds to complete and a timer bar appears indicating how much time is remaining on the test Menu Optics Test iutput 8 1 mY Optics Test Maintenance gt A The following steps occur during the test e The laser is turned off and the detector is allowed to stabilize at Gain 1 e Minimum maximum and average signal data are collected for laser off The laser is turned on and the detector is allowed to stabilize e Minimum maximum and average signal data are recorded for laser on 36 e The offset between laser on and laser off and the amount of variation in laser signal are determined e Test results are displayed Menu Optics Test iutput 4 9 mV H Maintenance gt 6 Passing requirements for the Optics Test are e Laser on off offset must be between 0 5 80mV e Laser off stability must be within 1 5 mV e Laser on stability must be within 1 5 mV 7 Once the test is completed press Done to return to the main screen or press Test to repeat the test 8 If the test has failed refer to the following table Optics Test Results for possible fail messages and their solutions OPTICS TEST RESULTS RESULT CAUSE SOLUTION Fail Noise level Bad preamp at laser off is too board high Replace preamp board and recalibrate the preamp laser Refer to Section 7 6 3 Bad processor board Replace processor board and then recalibrate the heaters gas flow and l
120. s New using the arrows on the keypad and press Enter to bring up the New Timed Mode Change Event window Menu Method Default Method New Timed Mode Change Event Output Configuration gt Change to standby mode 4 Once 4 b O Accept O Cancel IP Mode Standby Select an Event Type from the list using the left right arrows keys Change to Standby mode Change to Heating mode Change to Run mode or Change to Cleaning mode Select the Recurrence using the left right arrow keys Once Weekly or Monthly For a Recurrence of Once enter the Day of Month Month Hour Year and Minute Use the up down arrows to tab through the entry blanks For Weekly Recurrence enter the Day of Week Hour and Minute For Monthly Recurrence enter the Day of Month Hour and Minute Press Accept to save the new event settings or press Cancel to cancel the new event settings EDIT TIMED MODE CHANGE To Edit a Timed Mode Change Event select Configuration Timed Mode Changes Edit using the arrows on the keypad and press Enter The Edit Timed Mode Change Event screen will then appear Menu por athad Nafa hAnthad veal hs Edit Timed Mode Change Event Output Standby mode once at 17 00 on 04 23 2006 Cleaning mode at 17 00 on Friday each week Configuration gt O Accept O Cancel BUD FEAT a SEU A MuUUL otal IUUY Next vIedririu Moug Lz f u Use the up down arrows to select an event from the table Press Accept to select the ev
121. s can be started by connecting the proper wiring to the Start input pins on the back panel of the unit Refer to Section 2 4 for details 11 3 2 3 LOCK UNLOCK DETECTOR The Lock Detector option can be used to lock the method settings on the detector to prevent unwanted method changes during operation Method Method 1 Lock Detector Method gt Configuration Enter new PIN then press Accept or Cancel Maintenance PIN ABC Retype PIN ABC Operation gt Lu e gt rz w 2 Tew em Mode Run Select Operation Lock Detector using the arrows on the keypad and press Enter to reach the Lock Detector screen Enter and then re enter the PIN using the keypad Press Accept to lock the detector or press Cancel to cancel locking the detector Method Polymers Unlock Detector Enter PIN then press Accept or Cancel Operation gt Method gt Configuration gt Maintenance gt PIN ABC wee Mode Standby ITIN CTI ITI ToT To unlock the detector select Operation Unlock Detector and press Enter to bring up the Unlock Detector screen Enter the PIN created when the detector was locked to unlock the detector The detector can also be unlocked by recycling the power on the unit 3 2 4 CHART The Chart displays a scalable chromatogram trace of up to 60 minutes ZOOM The Zoom function can be used to zoom in out on the chromatogram trace Select Operation Chart Zoom usin
122. ser preamp Refer to Section 7 6 for details The detector must be in Run mode and the heaters equilibrated before the Optics Heating Test is run In the software go to Maintenance Tests Optics Heating Test and press Enter The testing screen will then appear 37 Menu Maintenance gt Optics Heating Test iutput 7 mV 3 Press Test to run the Optics Heating Test The test takes 1 second to complete The results screen will then appear Menu Maintenance gt Optics Heating Test iutput 2 mV O re Qoo DITS 4 Pass requirements for the test are e Optics Block must be 90 2 of the Drift Tube Temperature set point 5 f the test has failed refer to the following table Optics Heating Test Results for possible causes and solutions OPTICS HEATING TEST RESULTS RESULT Fail The Optics Block temperature is xx x of the drift tube temperature It should be XX X CAUSE Detector is in Standby mode Detector is still equilibrating Bad optics block RTD Bad optics block heater Bad heater board SOLUTION Put the detector in Run mode allow it to equilibrate and then repeat the test Wait for the detector to equilibrate and then repeat the test Check RTD s Replace RTD s if bad and then recalibrate the heaters Refer to Sections 7 8 and 7 6 1 for details Check heater Replace heater if bad and then recalibrate the heaters Refer to Secti
123. sing HPLC and the Evaporative Light Scattering Detector Peter Bonnett Lipid Technology 96 97 July August 1992 Comparison of Detectors for Size Exclusion Chromatography of Heavy Oil Related Samples S Coulombe Journal of Chromatographic Science 26 1 6 1988 LIPID APPLICATIONS Estimation of Free Glycolipids in Wheat Flour by HPLC J B Ohm and O K Chung Cereal Chemistry 76 6 873 876 1999 Fractionation of Soybean Phospholipids by High Performance Liquid Chromatography with an Evaporative Light Scattering Detector Tong Wang Earl G Hammond James L Cornette and Walter R Fehr Journal of the American Oil Chemists Society 76 11 1313 1321 1999 70 Rapid Analysis of Oxidized Cholesterol Derivatives by High Performance Chromatography Combined with Diode Array Ultraviolet and Evaporative Laser Light Scattering Detection Kyoichi Osada Amir Ravandi and Arns Kuksis Journal of the American Oil Chemists Society 76 7 863 871 1999 Reversed Phase Separations of Nitrogenous Phospholipids on an Octadecanoyl Poly Vinyl Alcohol Phase S L Abidi and T L Mounts Journal of Chromatography A 773 93 101 1997 Quantitative Analysis of Phosphatidylcholine Molecular Species using HPLC and Light Scattering Detection Jos F H M Brouwers B M Gadella L M G van Golde and A G M Tielens Journal of Lipid Research 39 1 10 1998 Quantitative High Performance Liquid Chromatography Analysis of Plant Ph
124. sure Test and press Enter The Nebulizer Gas Pressure Test screen will then appear Nebulizer Gas Pressure Test iutput 2 mV Maintenance gt E O Dore r 4 Press Test and the Nebulizer Gas Pressure Test will begin The test takes 60 seconds to complete A timer bar will appear showing how much time is left for the test Nebulizer Gas Pressure Test Nebulizer Gas Pressure Test utput Maintenance gt 5 The following steps occur during the Nebulizer Gas Pressure Test e Gas flow is set to 2 0L min and allowed to stabilize e Minimum maximum and average nebulizer gas pressure values are determined e Test results are displayed The gas flow is returned to its pre testing set point Nebulizer Gas Pressure Test iutput Maintenance gt 6 Passing requirements for the Nebulizer Gas Pressure Test are e Nebulizer gas pressure must be between 3 30psig e Pressure variation must be less than 3 psig during the testing period 34 Once the test is completed press Done to return to the main screen or press Test to repeat the test lf the test has failed refer to the following table Nebulizer Gas Pressure Test Results for possible fail messages and their solutions NEBULIZER GAS PRESSURE TEST RESULTS RESULT Fail Gas pressure is too high Fail Gas pressure is too low Fail Gas pressure is unstable CAUSE Nebulizer may be blocked Bad gas pressure senso
125. t 40 0 C 1 5 L min 16 Temperature Output Gas Flow Gain 0 0 2 50 Mode Standby Select Operation Mode Standby using the arrows on the keypad and press Enter to put the detector into Standby mode In Standby mode the heaters gas flow and laser are off The signal output is not displayed and the chromatogram trace is not active The detector enters Standby mode after power up with the last saved method conditions RUN MODE Operation gt Method Method 1 Read 40 0 C 1 5 L min Set 40 0 C 1 5 L min 16 Temperature Output 5 3 mV Gas Flow Gain Select Operation Mode Run using the arrows on the keypad and press Enter to put the detector into Run mode In Run mode the heaters gas flow and laser are on The signal output is displayed and the chromatogram trace is active Run mode is used for sample analysis HEATING MODE Menu Method Method 1 Read 40 0 C Method gt Configuration gt Maintenance gt Set 40 0 C 1 5 L min 16 Temperature Gas Flow Output Gain 5 00 Mode Heating Select Operation Mode Heating using the arrows on the keypad and press Enter to put the detector into Heating mode In Heating mode the heaters are on but the gas flow and laser are off The signal output is not displayed and the chromatogram trace is not active Heating mode keeps the detector in a ready state so the user won t have to wait for temperature equilibration when switching
126. te dir txt files Beep for long transfer W Use Tftpd32 only an this interface 459 97 94 210 Use anticipation window of Bytes Allow As virtual root seo ee 12 Configure the settings to match those shown above Be sure the IP address matches the IP address on the PC in this example the address is 154 97 84 210 Also make sure to set the base directory to the location where the OS setup files were saved from step 3 above Then click OK to save the settings If the IP address was changed you ll be prompted to restart the Tftpd32 software do so now 13 Next the DHCP server needs to be configured Click on the DHCP Server tab and edit the settings to match those shown below and click the Save button Thtpd3 by Ph Jounin ftp Server T tp Client DHCP server Syslog server IP pool starting address f 29 97 84 10 Size of pool ho Boot File Ce WINS DNS Sever 159 97 84 210 a Default router 1159 97 84 210 z Mask 255 255 255 0 i Domain Name Additional Option Settings 14 Next the ELSD needs to be configured with an IP 15 address Run the following command ifconftig sm0 dhcp Once the command returns to the losh prompt the machine will have an IP address within a few seconds To check the address that was assigned wait a few seconds and then run the following command ifconfig sm0 The expected output from this command is sm0 up 100M full duplex 425
127. trument a Using the arrow keys navigate through the menus to select Maintenance Service Tech Enter Service Tech Password and hit Enter b Enter the password atat and press Accept c Select Maintenance Calibration Laser Preamp and press Enter The first screen of the laser preamp calibration procedure will appear 59 j k Press Finish Press Continue to Method Laser Preamp Calibration Laser On iutput Maintenance gt TO cominue O conce wwe PR 20 00 Mode Standby Adjust the gain pot until a maximum voltage is measured with the multimeter Laser is on Press Continue to reach the next screen in the laser preamp calibration Method Default Method Laser Preamp Calibration Laser Off iutput Maintenance gt TO continue 2 conce rrr awww 70 00 Mode Standby Adjust the Offset pot until the multimeter reads 10mV Laser is off Adjust the multimeter to read in Volts DC reach the next screen in laser preamp calibration Method Default Method Laser Preamp Calibration Laser On iutput Maintenance gt Mode Standby I The target gain voltage is dependent on the fixture being used Adjust the Gain pot until it matches the value listed on the fixture Laser is on Press Accept to reach the final in the laser preamp calibration procedure Method Default Method Finished step iutput Maintenance gt Mode Stan
128. ume hood Fan Provides cooling airflow through the instrument Do not block Power Module The power module contains a socket for the incoming power cord It also contains the main power switch which is used to turn the system power On Off and the line fuse The module is autoselecting for 85 265V and contains a 5 Amp fuse 10 Gas Inlet The GAS INLET accepts the nebulizer gas supply tubing The inlet features a quick connect port which requires no additional fittings Gas pressure should be regulated from 65 80psi 2 4 MAKING ELECTRICAL AND FLUID CONNECTIONS 1 Unpacking the Unit Remove the ELSD from its shipping container and position it on a level surface near the column outlet of your HPLC system and the fume hood Make sure there is free flow of air to the bottom of the ELSD and to the cooling fan at the back panel of the ELSD Allow the detector to warm to ambient temperature if necessary Save the shipping container for future use Exhaust Adaptor Screw in the threaded exhaust adaptor provided in the accessory kit to the EXHAUST port on the back panel of the unit Fill the Internal Drain Reservoir Place a beaker under the DRAIN port on the right side panel Using a water bottle or pipette add water into the EXHAUST port on the back panel of the unit until excess liquid is seen exiting the DRAIN port Filling the internal drain reservoir prevents gas from escaping the drift tube 4 Power Connect
129. un has been started The time value will remain until the method run has been stopped e Chart The chromatogram trace of up to 60 minutes will be active for Run and Cleaning modes e Mode The current mode of the detector is displayed Standby Run Heating or Cleaning Equilibrating Indicator If the detector is in Run mode and the heaters and gas flow have not reached their set points the screen will display Equilibrating next to the 10 Mode status until the equilibration requirements are met The equilibration requirements are lower drift tube upper drift tube and optics block must be within 1 5 C of their set points gas flow must be within O 3L min of its set point the temperatures and gas flow must meet the requirements for 60 seconds before the message disappears e Timed Mode Change Reminder not shown If a timed mode change has been scheduled a reminder for the event will be displayed next to the Mode status e Errors Any errors that occur on the instrument will be displayed in the lower right corner of the screen The software Menu is located in the upper left corner of the screen There are four main Menu headers Operation Method Configuration and Maintenance The following sections describe the software functions within these headers 3 2 OPERATION 3 2 1 MODE The Model 3300 ELSD has four operational modes Standby Run Heating and Cleaning STANDBY MODE Operation Method Method 1 Se
130. uration Output Configuration gt O tar Or 00 5 00 4 00 3 00 2 00 1 00 DO 8 00 7 00 6 ES TA i Select Bar or Psi and the new pressure unit setting will take effect 3 4 9 NETWORK To configure the Ethernet port on the back panel of the detector first connect an Ethernet cable between the Ethernet port and a PC Then select Configuration Network using the arrows on the keypad and press Enter The Network Configuration window will then appear Menu Method Default Method Network Configuration Output Disabled 4 _ 192 168 70 10 Configuration gt 255 255 255 0 192 168 70 1 524 0 O Accert cancel 6 00 5 00 4 00 3 00 2 00 1 00 10 00 9 00 8 00 7 00 Mode Standby Use the left right arrows to select DHCP Enabled or Disabled If Disabled is selected enter the IP address Subnet Mask and Gateway settings If Enabled is selected the IP address Subnet Mask and Gateway will be grayed out and should fill in automatically once the connection is made Press Accept to save the new settings or press Cancel to cancel the new settings 3 4 10 TIMED MODE CHANGES Timed Mode Change Events can be used to put the detector into another operation mode using a timer This can be convenient to schedule routine cleaning heating etc events A reminder for the next Timed Mode Change will be displayed on the main screen next to the Mode NEW TIMED MODE CHANGE Select Configuration Timed Mode Change
131. urrent trademark ownership Grace Davison Discovery Sciences is a product group of W R Grace amp Co Conn Alltech Associates Inc is a wholly owned subsidiary of W R Grace amp Co Conn Copyright 2007 Alltech Associates Inc All rights reserved 72 www discoverysciences com Grace Davison Discovery Sciences Regional Headquarters In the Americas 2051 Waukegan Road Deerfield Illinois 60015 1899 Tel 847 948 8600 Fax 847 948 1078 Email contact alltech grace com Web www discoverysciences com In Europe Brandstraat 12 B 9160 Lokeren Belgium Tel 32 0 9 340 65 65 Fax 32 0 9 340 65 60 Email info lokeren alltech grace com Web www discoverysciences com be In Asia 19th Floor K Wah Center 1010 Hua Hai Zhong Road Shanghai 200031 P R C Tel 86 21 54674678 Fax 86 21 54051500 Email dsbiz asia grace com Web www discoverysciences com cn In Australia 30 Brookhollow Avenue Baulkham Hills New South Wales 2153 Australia Tel 1300 36 24 12 Fax 1300 36 24 11 Email custcare syd discoverysciences grace com Web www discoverysciences com au 73
132. voltage depending on your data collection system 15 CUSTOM AUTOZERO Use the left right arrows to select Enabled or Disabled for the Custom Autozero If Enabled the user can select an Autozero Offset from 0 100mV f Disabled the Autozero will be based on the full scale voltage setting on the detector 5mV for 1V FS OmV for 10mV FS AUTOZERO OFFSET If the Custom Autozero has been enabled enter a value from O 100mV for the Autozero offset This is the signal output that will be displayed when the detector is autozeroed If the Custom Autozero has been disabled then the Autozero Offset will be grayed out Press Accept to save the changes to the Outputs Configuration or press Cancel to cancel the changes 3 4 4 DISPLAY Select Configuration Display using the arrows on the keypad and press Enter The Display Configuration screen will then appear Menu Method Default Method Set Read 40 0 C AA Temperature 42 2 C Output Configuration gt E mc Display Configuration O accent 524 0 E Mode 0 00 9 00 Standby Use the up down arrows to adjust the Display Contrast The up arrow lightens the display and the down arrow darkens the display Press Accept to save the new Display settings and return to the main screen 3 4 5 HEATERS This function is available in Service Tech Mode only To configure the optics block heating on the detector first enter Service Tech mode by selecting Maintenance
133. word using the arrow keys and press Enter 8 Enter the password atat and press Accept 9 Select Maintenance Calibration Gas Flow using the arrows on the keypad and then press Enter to reach the first screen of the Gas Flow calibration procedure Method Default Method Gas Flow Calibration Step 1 8 tutput Maintenance gt n 20 00 Mo d e Stan d b y 10 Allow the gas flow to equilibrate and then take the reading on the external flow meter Enter the value into the Observed Value box on the screen The first reading should be around 0 5 L min Then press Continue 11 Repeat the same procedure for the next seven screens pressing Continue after each step is complete 12 When the last step in the calibration is reached press Finish to finalize the calibration 13 Check the calibration a Select Operation Mode Run and then press Enter to put the detector into Run mode b Select Method Edit and press Enter 58 Enter a gas flow rate of 1 0L min in the method and then press Accept Allow the instrument to stabilize and watch the output of the external flow meter t should read within 0 15 L min of the set point Check the gas flow for the additional set points of 2 0 3 0 and 4 0 L min If the unit is out of spec repeat the gas flow calibration Disconnect the external flow meter from the instrument and re connect the internal flow valve to the intern
134. ws on the keypad and press Enter The Create Service Log screen will then appear Menu Create Service Log iutput Maintenance gt Laser replaced 8 24 2006 O accept O Cancel il Enter text for the log using the keypad on the front panel or by connecting a USB keyboard to the back panel Service Log entries can contain numbers letters and or symbols Press Shift before entering a letter to create an upper case character Once the log has been created press Accept to save the new Service Log entry or press Cancel to cancel the changes 3 5 3 TESTS Diagnostic tests can be run to help troubleshoot the unit The available tests are e Nebulizer Gas Pressure Test e Gas Flow Test e Optics Test e Optics Heating Test e Heater Stability Test Service Tech mode only e Power Supply Test Service Tech mode only To access the diagnostic tests select Maintenance Tests Nebulizer Gas Pressure Test Gas Flow Test Optics Test or Optics Heating Test using the arrows on the keypad and press Enter To access the Heater Stability Test and the Power Supply Test the detector must be in Service Tech mode first To enter Service Tech mode select Maintenance Service Tech Enter Service Tech Password using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept Once in Service Tech mode select Maintenance Tests Heater Stability Test or Power Supply Test and press Enter Refer to Sect
135. ypad to navigate Error Logs Use the up down arrows to fully view the contents of each log VIEW SERVICE LOG This function is available in Service Tech Mode only To view the Service Logs on the detector first enter Service Tech mode by selecting Maintenance Service Tech Enter Service Tech Password using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept Once in Service Tech mode select Maintenance Logs View Service Log using the arrows on the keypad and press Enter The View Service Log screen will then appear View Service Log iutput Maintenance gt Service tech logged out Use the left right arrows on the keypad to navigate through the Service Logs Use the up down arrows to fully view the contents of each log Each Service Log contains the time the log was created the file and entry number and the log information Service logs contain information on calibration and configuration changes Press Accept to exit the Service Log and return to the main screen CREATE SERVICE LOG ENTRY This function is available in Service Tech Mode only To create a Service Log Entry on the detector first enter Service Tech mode by selecting Maintenance Service Tech using the arrows on the keypad and press Enter Enter atat for the Service Tech password and then press Accept Once in Service Tech mode select Maintenance Logs Create 18 Service Log Entry using the arro
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Service Manual Alltech Model 3300 ELSD

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