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Agilent 1200 Series Handheld Control Module

1. Figure 22 Control Module 156 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide A Appendix Safety Information 158 Radio Interference 161 Agilent Technologies on Internet 161 phe Agilent Technologies 157 A Appendix Safety Information General The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation 158 Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the
2. PF 2 G3 CO 5 O f Navigation keys access different O software areas D Esc key reverses current i info key input entry or provides action context Numeric keys Alphanumeric keys specific information for current item selected enter numbers 0to9 press numbers 1 to 9 multiple times eg 1ABC 2DEF 3GHI Direction keys move the cursor in the screen display Enter key accepts current input entry or action Selection keys select settings values or alphabetic characters Figure 1 The Agilent 1200 Series Control Module A short description of the main keys and the product and serial number is located on the rear of the control module 1200 Series Handheld Control Module Users s Guide 17 1 18 The Agilent 1200 Series Control Module The display will show you a variety of menu buttons F1 F5 in the lower section or function buttons F6 F8 in the right hand section that can be accessed with the corresponding Navigation for menus and Action for functions keys In this context the expression button will always refer to a menu or function shown on the display whereas key refers to the actual keys on the keyboard The key corresponding to a certain button is shown in brackets F1 F8 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 The i info key Online Information System The online information system provide
3. Theta Correction describes the default angle of the transport arm towards the front back axis of the module rotation For detailed information on the axes consult your Autosampler reference manual 6 Select the Done button F6 to accept settings The new values will be valid after performing the next hardware initialization or reset 1200 Series Handheld Control Module Users s Guide Using the Autosampler 5 Tracking Autosampler History EMF limits 1 Select the Records button F4 in the System screen 2 Select Autosampler from the list 3 Press Enter You can check the number of Needle into Seat injections the autosampler has made and the number of injection valve cycles A limit can be specified for each function which you can use to schedule preventive maintenance Resetting the Autosampler 1 Select the Control button F1 in the System screen 2 Select Autosampler from the menu 3 Press Enter 4 Select the Reset button F7 to reset the autosampler hardware This resets the injection valve metering device and sampling unit Reset to Default Settings 1 Select the Settings button F1 in the Analysis screen 2 Select Autosampler from the menu 3 Press Enter 4 Select the Default button F7 to reset the autosampler settings to their default values 1200 Series Handheld Control Module Users s Guide 81 5 Using the Autosampler Troubleshooting the Autosampler 1 Select the Tests button F
4. 1200 Series Handheld Control Module Users s Guide Using the Autosampler 5 Entering Settings All autosampler settings can be entered in the Autosampler Settings screen You can access this screen by selecting the Settings button F1 in the Analysis screen From here you can access the timetable function to set up a timetable for the Autosampler only the runtimes screen and the injector program screen Commonly used settings such as injection volume and vial number can be set directly in the Analysis screen More specific settings draw speed eject speed draw position offset can be entered using the More button F1 and choosing the Settings option Setting the Injection Mode There are two modes which can be set e Standard without pre defined needle wash with pre defined needle wash wash vial number can be set If the pre defined needle wash function is enabled the needle moves prior to the injection with reagent in the needle into the wash vial to remove sample deposits from the needle outside This prevents sample stay in the seat and create memory effects on the next injection cycle e Injector Program See Running an Injector Program on page 149 1200 Series Handheld Control Module Users s Guide 71 5 78 Using the Autosampler Optimizing Autosampler Performance There are two optimization modes available on the autosampler called prefetch and overlap Both options allow to shorten the anal
5. 2 Turn on the detector lamp and pump using the On Off button F7 in the Analysis screen 3 For the quaternary pump turn on the degasser by pressing the line power switch 4 Purge the pump For more information see Chapter 3 Using the Pump Allow the detector at least 15 minutes to provide a stable baseline 6 Fill the contents of a Agilent Technologies isocratic standard sample ampoule into a vial and seal the vial with a cap Place the vial in position 1 of the autosampler tray 7 Pump the water acetonitrile 35 65 mobile phase through the column for 10 minutes at a flow rate of 2 ml min 1200 Series Handheld Control Module Users s Guide 125 10 Running a Gradient Analysis Entering Settings 126 To set up the gradient analysis you will set the LC system settings to default and then modify selected settings the other settings will remain with their default values You will then save these settings to a method called GRAD To set up the solvent gradient you will create a timetable in the method This is done using the Timetable screen accessed by selecting the Timetable button F2 in the Pump settings screen The example assumes that the Timetable is empty If the Timetable is not empty use the All Lines item accessed by pressing the Delete button Enter the Analysis screen Set the Vial Range as 1 to 1 Set the Number of Injections to 1 Skip the method name field Select the Settings button F1
6. 8 Select the Start button F8 in the Sequence screen Select the OK button to start the sequence 136 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Single Level Calibration Sequences The following procedure describes how to set up a calibration sequence for an analysis which uses single level calibration There is one calibration standard C and 9 samples S The analysis requires that each sample is analyzed in duplicate the calibration standard is analyzed once before the samples and re analyzed once after every 2 samples C SS C SS C SS C SS C S C the calibration standard is located in position 90 and the 9 sample vials are in positions 1 to 9 of the autosampler tray and the method called METH1 is used for the samples and standards The example assumes that the sequence table is empty If the sequence table is not empty use the All Lines item accessed by pressing the Delete button F6 1 2 Select the Sequence button F4 in the Analysis screen For sequence line 1 select the Insert button F7 and enter Vial Range 1to9 lnj 2 Inj Volume Default Method METH1 Select the Calibration button F1 to display the Calibration Settings screen for sequence line 1 and choose Edit 1200 Series Handheld Control Module Users s Guide 137 11 138 Running Multiple Vial Analyses 4 Enter the following information Calibration vial range 90 to 90 Number o
7. 94 1200 Series Handheld Control Module Users s Guide Using the Detectors 7 Troubleshooting the Detector 1 Select the Tests button F3 in the System screen 2 Select the Detector from the menu 3 Press Enter 4 Select the test you require The selection of tests depends on the For information about each test see the Reference Manual for the Agilent 1200 detectors The full test capability is only available from the LC ChemStation 1200 Series Handheld Control Module Users s Guide 95 7 Using the Detectors Tracking Detector History 1 Select the Records button F4 in the System screen 2 Select the Detector from the menu 3 Press Enter to display the logbook You can check change and reset the lamp burn time and number of ignitions For the FL detector the flash lamp lifetime and for the RI detector the time since last purge can be checked 96 1200 Series Handheld Control Module Users s Guide Using the Detectors 7 Resetting the Detector Select the Settings button F1 in the Analysis screen Select the Detector from the menu Press Enter Select the Default button F7 to reset the detector settings to their default values FPF O N 1200 Series Handheld Control Module Users s Guide 97 7 Using the Detectors Lamp Ignition Routine VWD only When the lamp is turned on the following routine is implemented e 1 minute warm up within this time the grating position is re initialized Check o
8. Figure 21 Wait for repeated external start request An Agilent 1200 variable wavelength detector or diode array detector will perform a balance provided that Auto Balance is set to Prerun in the More Settings screen when receiving a start command from the control module This will only happen in the Standard and Wait for single repeated start request modes In the Send single repeated start request modes a balance before the run will NOT be performed If regular balancing is required set the Auto Balance check box to Postrun 1200 Series Handheld Control Module Users s Guide 147 11 Running Multiple Vial Analyses Synchronizing Analyses with External Devices 148 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 12 Running an Injector Program Creating an Injector Program 150 Entering Injector Program Settings 151 Saving the Method 153 phe Agilent Technologies 149 12 Running an Injector Program Creating an Injector Program The injector program is part of the method The injector program screen can be accessed using the Inj Program button F3 in the Autosampler Settings screen This section describes an injector program to do sample preparation involving a precolumn derivatization reaction This is required when the analytes lack chromophores and in their original chemical structure cannot be detected with the required sensitivity To create this
9. 14 Enter the following values B 65 C OFF D OFF for quarternary pump If you have a binary pump set B to 65 15 Set the Flow to 1 5 ml min 16 Confirm by selecting Done to enter the Analysis screen 17 Enter the values shown in Table 4 in the Analysis screen Table4 Values in Analysis Screen Setting Value Detection wavelength 254 nm Injection volume Tul Stoptime 6 min 1200 Series Handheld Control Module Users s Guide Running an Isocratic Analysis 9 Entering Settings NOTE The channels of a pumping system are named A B C and D depending on the pump type A is automatically calculated by 100 B C D If no values for B C and D are entered A is always 100 1200 Series Handheld Control Module Users s Guide 117 9 Running an Isocratic Analysis Saving Settings in a Method 1 Select the Method button F3 in the Analysis screen 2 Select the Save As button F8 3 Enter the method name as ISO using the selection keys also see Specifying a Method Name on page 42 4 Press the Done button F6 to save the method 5 Press the Esc key to return to the Analysis screen 118 1200 Series Handheld Control Module Users s Guide Running an Isocratic Analysis 9 Observing the Chromatogram 1 Select the Plot button F6 in the Analysis screen 2 Press the Select button F6 3 Choose a Signal from the Available Signals list box 4 Press Enter You can choose several signa
10. 87 margins 55 maximize plot screen 51 menu buttons 18 method 24 deleting 45 deleting all 45 exchanching with PC card 45 loading 41 modifying 42 partial method 42 PC card 41 PC card load 45 printing 56 protecting 43 save to PC card 45 saving 44 118 128 specifiying a name 42 types 41 user ID 44 working with 41 method button 41 MIO interface 57 missing vial 76 modifying a method 42 166 module button 41 Module Status 25 move button 50 multiple wavelenght detector autobalance 92 bandwidth 92 peakwidth 92 slit width 92 multiple wavelength detector settings 92 multiple level calibration 139 multiple level recalibration muliple standards 141 multiple vial analysis 133 navigation key 21 needle seat volume 76 needle wash 77 numeric keypad 22 numeric keys 22 0 on error 38 on off 65 column compartment 102 degasser 72 diode array detector 90 fluorescence light detector 90 pump 64 variable wavelength detector 90 on off button 25 37 65 90 102 online help 19 online information system 19 operation time 53 optimizing autosampler 78 overlapped injections 78 P page button 55 page layout 55 paper size 55 parameter changes 53 partial method 42 PC card initialize 45 inserting and removing 40 method exchanging 45 method loading 45 method saving 45 PC card button 45 piston stroke 67 plot button 25 plot screen 31 50 active signa
11. Default button F7 to reset the pump settings to their default values 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 4 Using the Degasser Starting the Degasser 72 Removing Gas Bubbles 72 Changing Solvents 73 phe Agilent Technologies 71 4 Using the Degasser Starting the Degasser 3 Press the line power switch on the front panel Turn on your pump by selecting the On Off button F8 in the Analysis screen Observe the degasser status lamp on the front panel The status lamp is off when there is sufficient vacuum in the degasser During operation the status lamp may be yellow for several seconds This indicates there is insufficient vacuum in the online degasser and the vacuum pump is on to create sufficient vacuum Removing Gas Bubbles If you see gas bubbles in the solvent tubing or inside the solvent filter 1 2 3 4 5 Disconnect the solvent tube of the first solvent channel from your pump Connect the syringe adapter onto the syringe from degasser accessory kit Pull the syringe plunger to draw solvent through the degasser and tubing Continue to draw solvent through tubing until no gas bubbles are visible Disconnect the syringe adapter from the solvent tube Connect the solvent tube to your pump Repeat step 1 through step 5 for other solvent channels 72 1200 Series Handheld Control Module Users s Guide Using the De
12. F7 enables you to delete print jobs if several jobs are on the stack Additionally you may choose the number of copies to be printed In the Records screen you can choose the Print button F6 to create a Configuration Report including the modules product serial and firmware version numbers together with the operation time This button is also available from the System Log Error Log Main Log and EMF windows Print Method The current method settings can be printed out using the Print button F6 in the Method screen The print dialog as described above will appear This will print all method settings excluding vial range information Print Timetable Pressing the m menu key in the Timetable screen allows you to choose Print Timetable This will lead to the regular print dialog Print Sequence Entering the Sequence screen and pressing the m menu key offers the Print Sequence option Print Injector Program From the Autosampler Settings screen press the Inj Program button F3 to enter the Program screen Via the m menu key you have the option to print out the program 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Connecting External Devices There are several kinds of interfaces that enable the Agilent 1200 Series modules to communicate with a range of other output devices For some of them extra hardware needs to be installed Configuration of selected interface parameter
13. Select LC System from the menu Press Enter Select the Default button F7 and select the Yes button to load defaults Press the Esc key to enter the Analysis screen oo N OO oO F QON 10 Enter the following values in the Analysis screen Table5 Values in the Analysis Screen Setting Value Flow 1 5 ml minute Detection wavelength 254 nm Injection volume 1 ul Stoptime 5 min 11 Select the Settings button F1 12 Select BIN or QUAT pump from the menu 1200 Series Handheld Control Module Users s Guide Running a Gradient Analysis 10 If you have a quaternary pump set B to 65 C and D to OFF If you have a binary pump set B to 65 The channels of a pumping system are named A B C and D depending on the pump type A is automatically calculated by 100 B C D If no values for B C and D are entered A is always 100 13 Select the Pressure button 14 Set the upper pressure limit to 400 bar 15 Select the Done button 16 Select the Timetable button 17 Select the Insert button 18 Enter a value of 2 minutes and select Composition as the setting If you have a quaternary pump set the B composition to 65 C and D to 0 00 If you have a binary pump set the B composition to 65 19 Select the Enter button to accept entries Action Key F7 20 Enter the following information for another two lines time 4 B 95 time 5 B 65 21 Press the Done button and verify your timetable en
14. column compartment 109 detector 96 pump 69 i info key 19 icons EMF 27 53 ID tag 105 identify button 53 identify modules 53 initialize 45 injection mode 77 injection valve manual 83 injection volume 77 injector program 77 149 155 creating 150 156 entering settings 151 example 152 printing 56 insert button 135 1200 Series Handheld Control Module Users s Guide Index interfaces 57 76 APG remote 57 BCD 57 GPIB 57 MIO 57 serial RS232 57 interfaces button 57 internal diagnostics 39 internet 161 isocratic analysis 113 isocratic standard sample 114 K keypad 22 keys action 21 alphanumeric 22 direction 21 enter 21 esc 20 info 19 keypad 22 menu 20 navigation 21 numeric 22 overview 17 selection 21 L lamp button 90 lamp ignition routine 98 lamp on off diode array detector 90 fluorescence light detector 90 variable wavelength detector 90 LC system configuring 38 general functions 38 shut down 48 LED 53 liquimeter 69 logbook button 48 logbooks 53 165 Index column compartment 109 detector 96 error 54 maintenance 53 print 39 56 sequence 48 setting up 53 system 54 M m menu key 20 43 maintenance 16 53 maintenance logbook 53 manual injection valve 83 filling loops 85 filling sample loop 85 87 filling sample loop partially 86 making an injection 85 positions 84 sample 86
15. date and time It is automatically updated whenever an error message is generated by the respective module This logbook is stored permanently in the module but when memory is full the newest error will replace the oldest one System Logbook Here all relevant system or event messages are stored until the module is restarted or turned off EMF Early Maintenance Feedback In the Records screen the EMF indicator shows if a regular maintenance is needed The EMF limits can be scheduled by pressing the EMF button F1 in the Records screen and choosing Setup Limits Depending on the highlighted module you enter a window where the maintenance intervals can be set Consult the online information system on Setting EMF Limits You can also display EMF events by choosing the Show Events option This windows shows all EMF limits for the modules that have been operated beyond them This windows is only updated during startup 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Printing Screens You can connect a printer with an RS 232 interface to any module using the proper cable A converter from a serial RS 232 to a parallel Centronics connection is available from Agilent Technologies part number 5181 1529 The RS 232 settings in the 1200 module must be the same as set with the dip switches on the cable Serial 19200 baud 8 databits 1 stopbit no parity You can configure the printer by pres
16. example you can first run a method containing an injector program to do sample preparation followed by an analytical run to analyze a batch of samples You can then run a second method to analyze further samples with different analytical conditions A delay time can be set in the sequence line When the second method is loaded it waits for a specified time before starting the analysis allowing the column to equilibrate to the new conditions All sequence events can be traced in the Sequence Logbook available through the Logbook button F5 in the Sequence screen At the end of the sequence you can specify either to load a method e g to flush the LC system to remove buffer salts to avoid crystallization or to program a soft shut down method or to turn off the LC system using the End Actions button F1 If both options are selected the shut down method will be loaded to be available for the next user However it will not be executed before the turning off You can set up automatic recalibrations using the Calibration Settings screen This screen allows you to attach calibration settings to a sequence line The Calibration Settings screen is accessed by selecting the Calibration button in the Sequence screen You can recalibrate using one or more standards and have the flexibility of choosing various calibration intervals and patterns You can define within a sequence line the frequency to recalibrate and the order of calibration vial analys
17. injector program you will e set the LC system to the default settings e modify the injector program settings in the Inj Program screen the other settings will remain with their default values and e save the method with the name DERIV When the method called DERIV is started the program is executed followed by the analytical run The first step of the program involves drawing derivatization reagent into the needle capillary followed by sample and then reagent again To ensure the reagent and sample react efficiently the plunger in the metering device of the autosampler is moved back and forth This mixes the sample and reagent as they travel up and down the capillary Following mixing the derivatization requires a pause to allow the sample and reagent to fully react before the derivatized sample is injected onto the column 150 1200 Series Handheld Control Module Users s Guide Running an Injector Program 12 Entering Injector Program Settings Enter the Analysis screen Select the Settings button F1 Select LC System from the menu Select the Default button F6 and select the Yes button to load defaults Press Esc to go back to the Analysis menu Select the Settings button F1 Select Autosampler from the menu Select the Inj Program button F3 to display the Program screen oo nr OOo F WH For program line 1 select the Insert button F7 10 Select the DRAW function and enter the draw settings as describ
18. installed correctly So you can check the number of injections that have been made on the column in this screen 1200 Series Handheld Control Module Users s Guide 105 8 Using the Column Compartment Selecting Separated or Combined Mode This mode allows the temperature setting of both heaters independent from each other If not enabled both heaters are kept on the same temperature 1 Select the Settings button F1 in the Analysis screen 2 Select Column Comp from the menu 3 Enable the Separated mode by selecting the check box 4 To enable the Combined mode deselect the check box 106 1200 Series Handheld Control Module Users s Guide Using the Column Compartment 8 Selecting the Column Switching Valve optional The column switching valve is optional 1 Select the Settings button F1 in the Analysis screen 2 Select Column Comp from the menu 3 Press the Column Switch button 4 Select mode 1 or 2 5 Press the Done button F6 and leave this screen 1200 Series Handheld Control Module Users s Guide 107 8 Using the Column Compartment Troubleshooting the Column Compartment 1 Select the Tests button F3 in the System screen 2 Select Column Comp from the menu 3 Press Enter 4 Select the test you require You can select the Calibrate test to check the operation of the Column Compartment For information about the test see the Reference Manual for the Agilent 1200 Series column compartment 108 1200 Se
19. protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuseholders must be avoided 1200 Series Handheld Control Module Users s Guide Appendix A Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided as much as possible When inevitable this should be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious pers
20. some of the sample could be lost through port 6 if you try to inject too much An Alternative Way to Fill The Loop When the sample loop is completely filled you can either inject the sample into the loop or use the syringe to draw the sample through the loop 1 Move valve to LOAD position 2 Place vent tube from port 6 into sample vial 3 Insert needle of syringe into needle port until needle touches stator face Do not press too hard 4 Slowly draw sample into syringe 5 Leave syringe in position and move valve to INJECT position 6 Remove syringe If you use this method always flush the loading passages vent tube on port 6 after each injection to prevent cross contamination between injections Remember to flush port 6 and the vent tube the valve must be in the LOAD position 1200 Series Handheld Control Module Users s Guide 87 6 Using the Manual Injection Valve An Alternative Way to Fill The Loop 88 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 7 Using the Detectors Turning the Lamp On and Off 90 Entering Settings 91 Resetting the Baseline 93 Configuring the Detector 94 Troubleshooting the Detector 95 Tracking Detector History 96 Resetting the Detector 97 Lamp Ignition Routine VWD only 98 Configuring the Analog Channel Output 99 phe Agilent Technologies 89 7 Using the Detectors Turning the Lamp On and Off 90 To
21. start signal to the APG remote line That is after all the programming has been completed on the control module and the Start button F8 has been pressed a Start Request is issued before each run and the external device must give the Start command for the injection process START START START START SR SR SR SR Figure 19 Send repeated external start request to APG Remote time from Control Module Here too the module will simply track the progress of the analysis Wait for Single External Start Request After pressing the Start button F8 the autosampler will wait for a single external start request on the APG remote lines When the start request is received the complete vial range or sequence is done as in standard mode under the command of the control module to APG Remote SR START START START START from Control Module Figure 20 Wait for single external start request 146 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Wait for Repeated Start Request After pressing the Start button F8 the autosampler will wait for external start requests before each vial in the range or sequence They have to be generated by the external device This mode is necessary when the external device needs extra time to get ready for the next analysis and thus has to be in charge of the start event SR SR SR SR START START START START from Control Module to APG Remote time
22. the Calibration button F1 and choosing Edit Delete from the pop up menu You can specify a range of calibration vials number of injections injection volume calibration method and a wait time after method loading You can also enter specific recalibration parameters such as the recalibration interval and pattern The Online Information System provides accurate information on recalibration options 1200 Series Handheld Control Module Users s Guide 49 2 Working with the Control Module Displaying Data Graphically Using the Plot screen you have many opportunities to display a wide variety of signals on a graphic display while the analysis is performed Selecting Signals Among all the signals available up to 3 can be chosen for graphical display 1 From the Plot screen press the Select button F6 to show the Plot selection menu 2 Use the Direction and Selection keys to navigate within and between the Available Signals and Selected Signals list boxes 3 Exchange signals between the list boxes by pressing the Move button F8 or the Enter key On the right hand side from the Selected Signals list box you can see the legend to the signals You can also enter a time range X axis for the plot in this screen The different signals can be set up by pressing the Setup button F7 Depending on which signal is highlighted you can enter an individual Y Range setting here 4 When the signals and their X time and Y signal u
23. the postrun time Ready When all Agilent 1200 Series modules are ready for the next analysis this signal is on Other modules or external devices now can react e g by issuing a start request Prepare This causes the modules to get ready for the next analysis e g the detector will perform a balance Start Request This signal causes the modules to get ready for the analysis e q the autosampler will begin the injection cycle As soon as all conditions to start the analysis the injection needle is placed in the seat and the valve is in the proper position are fulfilled a Start signal is generated to inform the other modules that now the analytical run starts Start In standard mode only the autosampler creates this signal This sends an order to start run time controlled activities to all the modules connected to the APG remote bus From now on moment of injection the runtime counts up 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 GPIB With the GPIB interface included in all modules your system is able to communicate with a Personal Computer configured as the Agilent ChemStation Connect all modules with CAN cables and use one of them to connect to the Agilent ChemStation via an GPIB cable See Coexecution with Agilent ChemStation on page 61 for further details on how to operate the system using the GPIB interface Serial RS 232 Use a standard RS 232 cable t
24. to the value specified after a certain time in the timetable e g wavelength In other cases solvent composition these changes take place dynamically approaching the set value in a step wise and linear manner The timetable becomes part of the current method when the method is saved The timetable is accessed by selecting the Timetable button F2 in the Analysis screen A timetable line can be inserted by pressing the Insert button F7 and consists of the following e Time Set the time span between the instant of injection and the desired parameter change e Module Choose the module that controls the parameter you want to change e Setting Select the parameter to be changed e Value Enter the desired parameter value You can edit an existing timetable line by pressing the Enter key Use the Delete button F6 and make a choice from the pop up menu to delete either the selected line or the whole timetable You can copy and paste timetable lines by selecting the respective choices available from the context menu m key 1200 Series Handheld Control Module Users s Guide 47 2 Working with the Control Module Automating Analyses 48 You can use the Sequence screen to create completely automatic unattended analyses from sample preparation to injection The Sequence screen is accessed by using the Sequence button F4 in the Analysis or Samples screen Using the Sequence screen you can link several methods together For
25. working with methods 41 write button 105 X x yvalues 52 xaxis 51 x correction 80 1200 Series Handheld Control Module Users s Guide www agilent com In This Book This book provides information about the control module and how to operate the Agilent 1200 Series modules and system for HPLC e The Agilent 1200 Series Control Module e Working with the Control Module e Using the Pump e Using the Degasser e Using the Autosampler e Using the Manual Injection Valve e Using the Detectors e Using the Column Compartment e Running an Isocratic Analysis e Running a Gradient Analysis e Running Multiple Vial Analyses e Running an Injector Program Agilent Technologies 2000 2006 Printed in Germany 02 2006 0 61323 90010 Agilent Technologies
26. 0 5 minutes WAIT Wait for 0 5 minute for the mixture to completely react 9 INJECT Inject the mixture and start the analysis 152 1200 Series Handheld Control Module Users s Guide Running an Injector Program 12 Saving the Method 1 Select the Method button F3 in the Analysis screen 2 Select the Save As button F8 3 Enter the method name as DERIV using the selection keys also see Specifying a Method Name on page 42 4 Press the Done button F6 to save the method 5 Press the Esc key to return to the Analysis screen The injector program is now part of the method called DERIV and can be started by selecting the Start button F8 in the Analysis screen 1200 Series Handheld Control Module Users s Guide 153 12 Running an Injector Program Saving the Method 154 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 6 eece 13 e Maintaining the Control Module Control Module Parts 156 This chapter shows the repair items ot Agilent Technologies 155 13 Maintaining the Control Module Control Module Parts The Controll Module s repair level is shown below Table 7 Control Module Parts Item Description Part Number Control Module replacement part including cable G1323 67011 Plastic Housing Kit includes front back and a clamp 5065 9984 CAN cable Agilent module to control module G1323 81600
27. 155 S sample amount 86 sample loop completely filling 85 samples screen 30 printing 55 save as button 42 saving a method 44 saving method 118 128 screens analysis 23 24 25 config 55 method 56 plot 23 31 50 program 56 records 53 samples 23 30 sequence 48 status 23 29 system 23 27 timetable 42 views 24 search button 19 select button 50 select signals 50 selection keys 21 sequence 24 48 135 137 139 calibration 48 137 139 end actions 48 logbook 48 printing 56 recalibration 48 sequence button 48 sequence modes 144 1200 Series Handheld Control Module Users s Guide Index serial button 55 serial interface 57 serial number 17 53 settings detectors 91 diode array detector 91 fluorescence light detector 91 multiple wavelenght detector 92 refractive index detector 92 settings button 24 42 setup button 37 50 56 setup logbooks 53 setup view 38 shut down signal 57 shut down pump 68 signal unit axis 51 signals button 82 single level calibration 137 solvent composition 65 115 solvents 73 spooler button 56 standard isocratic sample 114 standard mode 144 start button 144 start request signal 58 144 145 external 146 start signal 58 144 start stop button 25 starting an analysis 121 131 status screen 29 stop signal 58 stroke volume 68 syringe volume 76 system logbook 54 system screen information 27 menu structure 28 T t
28. 3 in the System screen 2 Select Autosampler from the menu 3 Press Enter You can select a variety of injector steps to move individual parts of the autosampler The injector step functions can be used in troubleshooting to check the single steps of the injection cycle For a complete description of each step see the Reference Manual for the Agilent 1200 Series autosampler If you have a thermostatted autosampler you can also test the auxiliary signals by pressing the Signal button in the Test screen The auxiliary signals will be displayed graphically now see Setting up the Thermostatted Autosampler on page 79 82 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 6 Using the Manual Injection Valve About the Injection Valve 84 Making An Injection 85 Completely Filling the Sample Loop 85 Partially Filling the Sample Loop 86 How Much Sample Is Actually Injected 86 How Much Sample Do Need 87 An Alternative Way to Fill The Loop 87 phe Agilent Technologies 83 6 Using the Manual Injection Valve About the Injection Valve The injection valve has six ports and can be moved manually between two positions In the LOAD position the mobile phase is led from the pump directly to the column allowing you to inject your sample into the sample loop In the INJECT position the mobile phase is led through the sample loop flushing the contents of the loop on
29. 3 Select the Calibration button F1 to display the Calibration Settings screen for sequence line 1 and choose Edit 4 Enter the following information Calibration vial range 1 to 3 Number of injections 2 Inj Volume Default Calibration method METH1 Recalibrate every 2 vials multi Before On After off 5 Select the Done button F6 to accept entries Move the highlighted bar to line 2 by pressing the Selection key down and press Enter 7 For sequence line 2 enter Vial Range 13 to 21 lnj 1 Inj Volume Default Method METH2 8 Select the Calibration button F1 to display the Calibration Settings screen for sequence line 2 and choose Edit 142 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 9 Enter the following information Calibration vial range 4to6 Number of injections 2 Inj Volume Default Calibration method METH3 Recalibrate every 3 vials multi Before On After Off 10 Select the Done button F6 to accept entries 11 Select the Start button F8 in the Sequence screen 12 Press Enter to start the sequence The autosampler now analyzes e three type A calibration standards in duplicate e type A samples in vials 7 and 8 e three type A calibration standards in duplicate e type A samples in vials 9 and 10 e three type A calibration standards in duplicate e type A samples in vials 11 to 12 e three type A calibration standards in duplicate e three type B
30. 9 1 20 The Agilent 1200 Series Control Module The m menu key You can use the m menu key on the control module keyboard to access selected functionality quickly wherever you are in the software For example from the Table of Contents you have quick access to the Print function In other screens you can easily select the Restart or Default functions or a schematic diagram for explanation purposes Press the Esc key to exit the menu See the Quick Reference Guide on the availability of context sensitive menus In Figure 3 Analysis Screen context menus are shown Depending on the active parameter entry field context sensitive menus provide different options Lamp On Off 2 8pectrum Aerea 2Reset 2Reset AStatus 3Status 5 Setup View 4Restart 6 Restart S 2 Bottle Filings MGEEETED 2Print Screen 3Reset 2 3 Setup View 4Restart viele 100E Wuece o ooi Ready Figure 3 Context Menus in the Analysis Screen The Esc key The Esc Escape key allows you to exit the current window or screen and leads you back to the last window or screen you were working with If you are in one of the main screens you can use Esc to toggle between the current and the previous screen In an edit field the previous value can be restored by pressing ESC 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 The Enter key With Enter you accept a current e
31. 9 10 Running a Gradient Analysis 9 Press the Plot button F6 to show the chromatogram A typical gradient chromatogram for this analysis is shown in Figure 17 mAU 350 300 250 200 150 100 50 pit ie Ge L 1 2 3 4 min Figure 17 Gradient Analysis of Isocratic Standard The exact profile of the chromatogram will depend on the column you have used Differences in retention times and areas of the peaks in your chromatogram and the one shown in Figure 17 might be a result of variations in the concentration of the sample from batch to batch the quality of the solvents used and the column temperature If you compare this chromatogram with the one from Chapter 9 Running an Isocratic Analysis you will notice the solvent gradient has reduced the elution time of the fourth peak in the chromatogram You can rescale the plot using the Rescale button F7 or the cursor keys or you define the plot window within the Setup 130 1200 Series Handheld Control Module Users s Guide Running a Gradient Analysis 10 Starting the Analysis The analysis can be started by pressing the Start button F8 from the Samples screen the System screen or the Status screen 1 Enter the Analysis screen 2 Select the Start button F8 3 Select OK to confirm the vial range and injection number and press Enter to start the analysis 1200 Series Handheld Control Module Users s Guide 131 10 Running a Gr
32. A method that is stored in the individual LC modules can be loaded modified saved and run from the control module e The PC card method The method parameters are stored on a PC card A method that is stored on the PC card can be loaded to the LC modules or transferred to another LC system Methods cannot be run directly from the PC card The method must first be loaded from the PC card before it can be run When the PC card method is loaded it becomes a module method Unless stated otherwise the following sections refer to module methods Loading a Method A method can be loaded using the Method button F3 in the Analysis or Samples screen 1 Enter the Analysis or Samples screen 2 Select Method the current parameters are displayed 3 Press the Module button F1 4 Select a method from the list 5 Press Enter You can also load a method directly from the Analysis screen by using the selection keys and changing the method in the method list The Method Module screen lists all methods that are stored in the modules For each method there is a date when the method was last changed and a short user description When a method is loaded it becomes the current method 1200 Series Handheld Control Module Users s Guide 41 2 42 Working with the Control Module A method might be identified as partial method This means that there is a mismatch between the actual and the original system configuration for example when a modul
33. Agilent 1200 Series Handheld Control Module User s Guide Eee Agilent Technologies Notices Agilent Technologies Inc 2000 2006 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Microsoft Microsoft is a U S registered trademark of Microsoft Corporation Manual Part Number G1323 90010 Edition 02 2006 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn Germany Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connec tion with the furnishing use or per formance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that con
34. It refers only to the active signal indicated at the top of the screen e Use the selection keys to change the scaling of the Y axis by a factor of 2 respectively 1 2 Using the m menu key and choosing maximize you can enlarge the diagram to full display size Press the Restore button F6 to return to the regular view 1200 Series Handheld Control Module Users s Guide 51 2 Working with the Control Module Toggling Signals You can monitor up to 3 different signals from different modules in real time updates every second on the Plot screen Although all 3 signals are shown in the display the Rescale button F7 only refers to the active signal The active signal is shown in the Plot screen title and can be toggled by pressing the 1 2 3 keys on the numeric keypad Displaying Exact Signal Values Selecting the Cursor button F8 in the Plot screen displays the X and Y value of the current cursor position for the active signal In this mode using the Selection keys you can rescale the Y axis Using the Direction left right keys you can move the cursor along the graph in an X direction in order to find the position you want Print Graph If a printer is connected to your system you can print the contents of the Plot screen by pressing the m menu key and selecting Print Plot This works also for the maximized view 52 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Logbooks The c
35. RID cell temperature in the Analysis screen Temperature Peakwidth polarity and automatic recycling can be set in the RI detector settings screen This screen is accessed by selecting the Settings button F1 in the Analysis screen Automatic zero and automatic purge can be set by selecting the More button F1 under RI Settings Only the G1323B version of the control module allows control of the Refractive Index Detector The G1323A will display resident or unsupported module if a RI detector is configured in the Agilent 1200 system 1200 Series Handheld Control Module Users s Guide Using the Detectors 7 Resetting the Baseline You can reset the baseline using the Balance button F1 Zero button F1 when using the Refractive Index Detector in the Detector Control screen Please note that this procedure is not available for the Fluorescence Light Detector 1 Select the Control button F1 in the System screen 2 Select the Detector from the menu 3 Press Enter 4 Select the Balance button F1 You can achieve the same using the m menu key in the Detector Settings window available from the Analysis screen 1200 Series Handheld Control Module Users s Guide 93 7 Using the Detectors Configuring the Detector 1 Select the Configure button F2 in the System screen 2 Select the Detector from the list 3 Press Enter You can now configure the detector analog output s lamp on at power on and the interfaces
36. Settings you can enter autobalance settings and the margin for negative absorbance The option Spectrum allows you to enter a wavelength range for a sample spectrum Fluorescence Light Detector For the fluorescence light detector the following settings can be entered Excitation wavelength emission wavelength and Multi wavelength settings can be set in the regular Settings screen With the More button F1 you can specify further detector settings i e peakwidth and PMT Gain baseline behaviour reference polarity spectral range fit multi wavelength settings spectrum excitation range 3D scanning settings excitation and emission ranges and phosphorescence detection mode settings 1200 Series Handheld Control Module Users s Guide 91 7 92 Using the Detectors Multiple Wavelength Detector The wavelength for signal A can be entered in the Analysis screen The wavelength for signal B slit width and peak width can be entered in the MW Detector Settings screen This screen is accessed by selecting the Settings button F1 in the Analysis screen Additional signals and functions are accessed by selecting the More button F1 under MW Settings Only the G1323B version of the control module allows control of the Multiple Wavelength Detector The G1323A will display resident or unsupported module if a RI detector is configured in the Agilent 1200 system Refractive Index Detector The control module allows to set the
37. a value between 20 and 100 ul When the stroke is set to AUTO the pump uses large strokes at high flow and shorter strokes at low flow rate This can improve the mixing performance and gradient linearity by reducing the size of the solvent packets to be mixed The stroke volume can be accessed by using the Settings button F1 in the Analysis screen selecting the pump and then pressing More The amplitude of the pressure pulsation is directly proportional to the stroke volume Decreasing the stroke volume decreases the pulsation amplitude giving a better signal to noise ratio with flow sensitive detectors To maintain the flow the pumping frequency is increased increasing the frequency of the pressure pulsation Increasing the pump frequency gives better peak area reproducibility at low flow rates Automatic Shut down At the end of a sequence you can set the pump to be automatically turned off using the Sequence End Actions button F1 in the Sequence screen You can turn off the pump completely or load a specific shut down method Troubleshooting the Pump 68 1 Select the Tests button F3 in the System screen 2 Select Pump from the menu You can now select various tests to check the pump For further information about these tests see the Reference Manual for the Agilent 1200 Series pump 1200 Series Handheld Control Module Users s Guide Usingthe Pump 3 Tracking Pump History Pump EMF Limits 1 Select the Records b
38. adient Analysis Starting the Analysis 132 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 11 Running Multiple Vial Analyses Analyzing Multiple Vials Using the Same Method 134 Analyzing Multiple Vials Using Different Methods 135 Single Level Calibration Sequences 137 Multiple Level Calibration Sequences 139 Recalibrating With the Same Group of Standards 139 Recalibrating With Multiple Groups of Standards 141 Synchronizing Analyses with External Devices 144 lt Agilent Technologies 133 11 Running Multiple Vial Analyses Analyzing Multiple Vials Using the Same Method 134 This section describes how to set up a 25 vial analysis with one injection from each vial You will use a previously created method The samples are located in positions 1 to 25 of the autosampler tray For details Working with Methods on page 41 1 ao ao FF WwW N Enter the Analysis screen Set the Vial Range from 1 to 25 Set the number of injections to 1 Select the method you want to use with the scroll buttons 4 Y Select the Start button F8 Select OK to confirm the vial range and injection number and press Enter to start the analysis 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Analyzing Multiple Vials Using Different Methods This section describes how to set up a 50 vial analysis using three methods which yo
39. ag 105 tests autosampler 80 82 column compartment 108 167 Index detector 95 tests button 68 80 82 108 thermostatted autosampler 79 ambient temperature 79 auxiliary signals 79 display signals 79 heat sink 79 heat sink fan 79 parameters 79 plot 79 settings 79 signals 79 theta correction 80 time and date 37 time axis 51 time programming 47 timeout 38 timetable 24 47 autosampler 77 copy paste 47 printing 56 setting 47 timetable button 47 toggling signals 52 transport arm aligning 80 trays 76 troubleshooting autosampler 82 column compartment 108 control module 39 detectors 95 logbook 39 pump 68 turning on off column compartment 102 U units 38 updating firmware 60 user ID 44 V valve 168 column compartment 107 Y filling sample loop 85 87 filing sample loop partially 86 yaxis 51 making an injection 85 manual 83 Z opening 64 zero button 93 positions 84 sample 86 87 variable wavelength detector 89 analog output 94 balance 93 interfaces 94 lamp ignition routine 98 lamp on off 90 98 resetting 97 resetting the baseline 93 settings 91 signal polarity 91 spectrum 91 tests 95 tracking history 96 troubleshooting 95 wavelength 91 wavelength calibration 99 views 24 views button 23 WwW wash mode 77 wash vial 77 washing the needle 77 wavelength calibration 99 wear count 69 working with control module 35
40. an Injector Program 149 Creating an Injector Program 150 Entering Injector Program Settings 151 Injector Program Lines 152 Saving the Method 153 13 Maintaining the Control Module 155 Control Module Parts 156 A Appendix 157 Safety Information 158 General 158 Operation 158 Safety Symbols 159 Radio Interference 161 Test and Measurement 161 Agilent Technologies on Internet 161 Index 163 1200 Series Handheld Control Module Users s Guide 13 Contents 14 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 1 The Agilent 1200 Series Control Module Control Module Features 16 Control Module Keys 17 Control Module Software 23 Control Module Versions 32 ot Agilent Technologies 15 1 The Agilent 1200 Series Control Module Control Module Features 16 The control module provides complete local control and monitoring of a single module or an entire Agilent 1200 Series system You have easy access on every supported function you can easily control all parameters and settings and you can configure various communication channels with other devices in order to comfortably analyze the generated data Install any desired configuration of Agilent 1200 Series modules The control module software will reflect which modules are present in the LC system and adjust the screens accordingly Enter parameter settings for every module perform reset and on off funct
41. and enter Vial Range 10 to 24 lnj 2 Inj Volume Default Method METH1 1200 Series Handheld Control Module Users s Guide 139 11 Running Multiple Vial Analyses 3 Select the Calibration button F1 to display the Calibration Settings screen for 5 6 7 sequence line 1 and choose Edit Enter the following information Calibration vial range 90 to 92 Number of injections 2 Calibration method METH1 Recalibrate every 5 vials multi Before On After Off Select the Done button F6 to accept entries Select the Start button F8 in the Sequence screen Press Enter start the sequence The autosampler now analyzes 140 the three calibration standards in duplicate sample vials 10 through 14 the three calibration standards in duplicate sample vials 15 through 19 the three calibration standards in duplicate sample vials 20 through 24 and the three calibration standards in duplicate 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Recalibrating With Multiple Groups of Standards There are two different types of samples A and B that need to be analyzed The analysis for sample type A requires a 5 ul injection and a stoptime of 8 minutes The analysis of sample type B requires a 2 ul injection and a stoptime of 5 minutes For sample type A there are 3 calibration standards of different concentrations and 6 samples each sample must be analyzed once the calibr
42. artment Resetting the Column Compartment 112 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 9 Running an Isocratic Analysis What You Will Need 114 Preparing the LC System 115 Entering Settings 116 Saving Settings ina Method 118 Observing the Chromatogram 119 Starting the Analysis 121 phe Agilent Technologies 113 9 Running an Isocratic Analysis What You Will Need Instruments Agilent 1200 Series isocratic binary or quaternary pump autosampler and a UV detector Column A 125 mm x 4 0 mm Hypersil ODS 5 um Agilent Technologies part number 7982618 564 Solvents For the isocratic pump a solvent mixture of LC grade bidistilled water 35 and acetonitrile 65 Sample The Agilent Technologies isocratic standard sample Agilent Technologies part number 01080 68704 This contains 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl and 0 03 wt o terphenyl dissolved in methanol 114 1200 Series Handheld Control Module Users s Guide Running an Isocratic Analysis 9 Preparing the LC System 1 For the isocratic pump fill the solvent bottle with the mixture of LC grade bidistilled water 85 and acetonitrile 65 For the binary or quaternary pump fill one solvent bottle with bidistilled water channel A and the other with acetonitrile channel B 2 Turn on the detector lamp and pump using the On Off button F7 in th
43. ation standards must be analyzed in duplicate and re analyzed after every 2 samples C1 C2 C3 S7 S8 C1 C2 C3 S9 S10 C1 C2 C3 S11 S12 C1 C2 C3 The calibration standards of type A are in positions 1 2 and 3 of the autosampler tray and the 6 sample vials are in positions 7 to 12 and the samples and the calibration standards use the same method called METH1 For sample type B there are 3 calibration standards of different concentrations and 9 samples each sample must be analyzed once the calibration standards must be analyzed twice and re analyzed after every 3 samples C1 C2 C3 13 S15 C1 C2 C3 16 S18 C1 C2 C3 19 S21 C1 C2 C3 the calibration standards of type B are in positions 4 5 and 6 of the autosampler tray and the 9 sample vials are in positions 13 to 21 and the samples and calibration standards of type B use different methods The samples use METH2 and the calibration standards use METHS These methods contain the same analytical parameters and differ only in the analysis stoptime 1200 Series Handheld Control Module Users s Guide 141 11 Running Multiple Vial Analyses The example assumes that the sequence table is empty If the sequence table is not empty use the All Lines item accessed by pressing the Delete button F6 1 Select the Sequence button F4 in the Analysis screen 2 For sequence line 1 select the Insert button F7 and enter Vial Range 7to 12 lnj 1 Inj Volume Default Method METH1
44. calibration standards in duplicate e type B samples in vials 13 14 and 15 e three type B calibration standards in duplicate e type B samples in vials 16 17 and 18 e three type B calibration standards in duplicate e type B samples in vials 19 20 and 21 and e three type B calibration standards in duplicate 1200 Series Handheld Control Module Users s Guide 143 11 Running Multiple Vial Analyses Synchronizing Analyses with External Devices With an APG remote connector the system can be connected to external devices in order to synchronize the analyses This is necessary when an external device needs some time in order to get ready for a new analysis and when transmitting of a start request is required see Connecting External Devices on page 57 for further information on interfaces When executing an analysis by pressing the Start button F8 you will see a window where sequence modes can be chosen In any case do all the analysis preparation using the control module A Start command is used to start the analytical run from the point of injection and is usually issued by the autosampler A Start Request command causes the autosampler to take the next vial and place it under the injection needle also see APG Remote on page 57 and Optimizing Autosampler Performance on page 78 The Start button F8 on the control module is used to start a vial range or sequence analysis Standard In t
45. ces and computers and wait 1 minute and then restart or e try to use just one Agilent 1200 Series module If the problem still remains call Agilent Technologies 1200 Series Handheld Control Module Users s Guide 39 2 Working with the Control Module Inserting and Removing PC cards 1 Insert the connecting side of the PC card into the PC card slot of the control module until you feel it will not go in any further 2 Switch to the Analysis System or Sample screen press the m key and select Restart to restart the control module 3 To remove the PC card press the card eject button on the left hand side of the module The control module supports PCMCIA 2 0 type and II memory cards In general only cards up to a capacity of 128 MB are supported Compatible cards are SanDisk CompactFlash Memory Cards SDCFBx yy with SanDisk CompactFlash PC Card Adapter SDCF yy SanDisk Flash Disk PCMCIA PC Card ATA SDP3Bx yy Card eject button Figure 14 Inserting and Removing the PC card 40 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Working with Methods A method contains a complete set of injection separation and detection parameters including the timetable and injector program Vial range information is not part of the method There are two types of methods The module method The method parameters are stored in the individual LC modules and not in the control module
46. creen also allows you to enable disable the option always keep transport arm next to last used vial 1200 Series Handheld Control Module Users s Guide Using the Autosampler 5 Setting up the Thermostatted Autosampler If a thermostatted autosampler is part of your system you can enter specific setting using the Thermostat option in the settings screen Using this option you can set the temperature of the airflow into the autosampler This setting is available in the Analysis screen too Activate the check box to have the temperature controlled as soon as the cooled autosampler is turned on Using the More option in the Settings screen and selecting Signals you can choose among several thermostat parameters ambient temperature heat sink heat sink fan etc that will be referred to as Autosampler Auxiliary in the Plot Signals screen This allows you to access a variety of thermostatted autosampler signals without overloading the Available Signals list box see Plot Screen on page 31 1200 Series Handheld Control Module Users s Guide 79 5 Using the Autosampler Aligning Transport Arm Gripper 80 1 Press the Tests button F3 in the System screen 2 Choose Autosampler from the list 3 Press the Align button F1 4 Choose Transport 5 Enter the desired values in the corresponding fields The field X Correction sets the default value for the axis parallel to the front panel left right motion
47. ctor baseline resetting 93 diode array 89 fluorescence light 89 variable wavelength 89 diode array detector 89 analog outputs 94 autobalance 91 balance 93 bandwidth 91 interfaces 94 lamp on off 90 peakwidth 91 resetting 97 resetting the baseline 93 settings 91 slit width 91 tests 95 tracking history 96 troubleshooting 95 wavelength 91 1200 Series Handheld Control Module Users s Guide direction keys 21 display 50 contrast 37 settings 37 displayed modules 38 dot key 43 draw position offset 77 draw speed 77 E early maintenance feedback EMF 16 27 69 indicator 53 logbook 54 setting limits 54 eject speed 77 EMF button 54 end actions 48 end actions button 48 enter key 21 error logbook 54 esc key 20 external devices 57 F features 16 firmware version number 53 firmware update 60 control module 61 fluorescence light detector 89 3D scan 91 analog outputs 94 emission wavelength 91 excitation wavelength 91 history 96 interfaces 94 lamp on off 90 multi wavelength 91 peakwidth 91 phosphorescence detection 91 PMT Gain 91 resetting 97 resetting the baseline 93 settings 91 troubleshooting 95 fluorescence light detectors tests 95 function buttons 18 G general functions 37 GLP compliance 16 GPIB interface 57 gradient analysis 123 126 130 graphical display 50 graphs 50 gripper 80 help 19 history autosampler 81
48. d for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Select Products Chemical Analysis 1200 Series Handheld Control Module Users s Guide 161 A Appendix Agilent Technologies on Internet 162 1200 Series Handheld Control Module Users s Guide Index A action key 21 active signal 52 add button 38 53 adjusting view 38 Agilent ChemStation 57 features 61 restricions 62 Agilent on internet 161 align transport arm 80 alphabetic characters 22 alphanumeric characters 21 43 alphanumeric keypad 22 analog output diode array detector 99 fluorescence light detector 99 variable wavelength detector 99 analysis automated 48 gradient 123 isocratic 113 multiple vial 133 start 121 131 time programming 47 analysis screen 23 displayed modules 38 information 24 menu structure 25 printing 55 settings 24 setup view 38 APG Remote interface 57 power on 57 prepare 58 ready 58 shut down 57 start 58 start request 58 stop 58 automated analyses 48 auto on 38 autosampler align transport arm 80 auxiliary signals 79 configuration 76 defaults 81 draw position offset 77 draw speed 77 eject speed 77 entering settin
49. d samples on the tray image Vial Range Vial 4 to 1 nj 1 Method Stoptime min O Sequence Une Figure 11 Samples Screen This screen is only available if an autosampler is part of your system 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 Plot Screen The Plot screen provides an online plot You can view various signals depending on the modules in the system e g a chromatogram pressure signal or temperature signal Directly from the Plot screen you can use a cursor to pinpoint information and you can observe information like run time status pressure ripple or composition Using the Direction and Selection keys of the control module you can change the scale of the plot window With the Rescale button F7 you can optimize the screen according to the selected signal and parameter ranges Pressure OLEA EE Time o ooie Ready 8 1715 MAU Cursor for exact Cursor values Rescale for fullscale plot Select Signal source time range scaling Figure 12 Plot Screen 1200 Series Handheld Control Module Users s Guide 31 1 The Agilent 1200 Series Control Module Control Module Versions With the introduction of the Agilent 1100 Multiple Wavelength Detector and the Refractive Index Detector the Control Module G1323B was introduced To find out which version you possess check the part number label on the back side of your con
50. e Analysis screen Use Action keys then to select the module 3 For the quaternary pump turn on the degasser by pressing the line power switch 4 Purge the pump For more information see Chapter 3 Using the Pump Allow the detector at least 15 minutes to provide a stable baseline 6 Fill the contents of a Agilent Technologies isocratic standard sample ampoule into a vial and seal the vial with a cap Place the vial in position 1 of the autosampler tray 7 Pump the water acetonitrile 35 65 mobile phase through the column for 10 minutes at a flow rate of 2 ml min 1200 Series Handheld Control Module Users s Guide 115 9 Running an Isocratic Analysis Entering Settings 116 To set up the isocratic analysis you will set the LC system settings to default and then modify selected settings the other settings will remain with their default values You will then save these settings to a method called ISO Enter the Analysis screen Set the vial range as 1 to 1 Set the number of injections to 1 Press Enter to skip the method name section Select the Settings button F1 Select LC System from the menu Select the Default button F7 and select the Yes button to load defaults Press Esc Select the Settings button F1 10 Select the pump from the menu either ISO BIN or QUAT 11 Press the Pressure button F3 oo N OOo F WwW NB 12 Enter 400 as the upper pressure limit 13 Select the Done button F6
51. e changes the current value according to Figure 4 O STU VWX YZ_ JKL MNO POR ABC DEF GHI O ieee ji Figure 4 Keypad of the Control Module 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 Control Module Software The Control Module User Interface In a basic configuration of modules there are at least three main screens the Analysis Status and System screens You can move between these screens using the Views button F5 If an Autosampler is part of your system a fourth screen called Samples can be accessed Another important screen is the Plot screen which is accessible via an Action button F6 F8 depending on the active screen ie i ae se ae PS Se 1 1 1 Figure 5 Main Screens of the Control Module From these screens other menus can be accessed When a certain menu is selected by using a Navigation key in some cases the control module user interface prompts you with a pop up menu before proceeding From there you have to make a choice in order to go on either by using the up down Selection keys or by pressing the corresponding number on the Numeric Alphanumeric keys The latter will give you quicker access to the choices in most cases Mostly these pop up menus will distinguish between the different modules in your system or in the case of the Views button F5 between screens Analysis Screen The Analysis screen provides access to a
52. e from the Agilent ChemStation To have a method available on both controllers proceed as follows If the method is on the Agilent ChemStation and should be saved on the control module or PC card load the method on Agilent ChemStation and then save the method on the control module or PC card with Method Save As If the method is on the control module or PC card and should be saved on the Agilent ChemStation first load method DEF_LC M on the Agilent ChemStation to have no additional parameter in the format and then load the required method on control module Then save the method on the Agilent ChemStation with the same name WARNING A method that is available on the control module as protected method can be modified by the Agilent ChemStation and then be saved on the control module without any warning 62 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 3 Using the Pump Turning the Pump On and Off 64 Entering Settings 64 Purging the Pump 64 Purging Procedure 65 Adjusting Compressibility 66 Adjusting Stroke Volume 68 Automatic Shut down 68 Troubleshooting the Pump 68 Tracking Pump History Pump EMF Limits 69 Resetting the Pump 70 Resetting the Pump Settings 70 lt Agilent Technologies 63 3 Using the Pump Turning the Pump On and Off To turn the pump on or off you can use the 0n Off button F7 in the Analysis or System scree
53. e keys 1 to 9 several times e g 1ABC 2DEF 3GHI See also Figure 4 on page 22 5 Move the cursor to the next entry position using the right direction key and repeat step 4 6 Repeat step 4 and step 5 until you have specified your method name 7 Select the Done button F6 to accept the method name The left arrow key can be used as backspace the right arrow key is used to move to the next character position Protecting a Method To protect the current method 1 Select the Method button F3 in the Analysis screen 2 Select Module from the menu 3 Select the Save As button F8 4 Select the Protected check box 5 Select the Done button F6 The method is now protected against inadvertent changes Any changes to the method will not be accepted until the method is unprotected by saving it again without protection For further protection remove the Control Module from the Instrument and store it in a secure place Any unauthorized method or instrument changes can be traced by the system logbook 1200 Series Handheld Control Module Users s Guide 43 2 44 Working with the Control Module Saving a Method Although it may seem that methods are stored within the control module in fact all data concerning methods is stored in the modules themselves The control module generates a list of all available methods that can be loaded The number of methods that can be stored depends on the number of timetable and inj
54. e was added to or removed from the system A partial method can not be loaded as the current method Modifying a Method A method can be modified by changing the settings in the Analysis or Settings screens Many of the commonly used method settings flow injection volume column temperature wavelength and stoptime can be modified in the Analysis screen Other less commonly used method settings such as eject speed can be modified using the Settings button F1 This button displays the Settings menu from which all LC system and module settings can be accessed If you change a method setting the value is immediately downloaded to the LC module An asterisk will appear in the right corner of the status line to indicate the current method has been modified The time programmable settings can be modified in the Timetable screen The injector program settings can be modified in the Injector Program screen accessed from the Autosampler Settings screen Specifying a Method Name 1 Select the Method button F3 in the Analysis or Samples screen 2 Select the Save As button F8 3 Press the Selection key up to enter the letter input mode 4 Select the required letter or number in the method name entry box using the Selection keys Numbers and the minus sign can be entered directly 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Alphanumeric characters can be entered also by pressing th
55. ector program lines included In general about 15 methods may be stored which contain about 50 timetable lines per module With differing method contents the actual amount of methods to be stored may change significantly Use PC cards in order to store infinite numbers of methods for future use or exchange between LC instruments see Transferring Methods Between LC Systems on page 46 To save the current method 1 Select the Method button F3 in the Analysis screen 2 Select Save As using the Action keys 3 Enter a name as described in Specifying a Method Name on page 42 or simply continue with the next step if you want to keep the current method name 4 Press Enter Optionally you may fill in further data Activate the Protected check box in order to protect the method By entering a User ID you can identify your personal modules more quickly You can also enter a personal comment 5 Select the Done button F6 to store the method in the modules Select Yes to confirm save in case you are overwriting an existing method The stored method now contains all the current LC system and module settings The method settings are stored in the individual modules e g all the pump method settings are stored in the pump and not in the control module If you disconnect the control module from one LC system and connect it to another LC system the current method and settings are now shown for the new LC system To transfer methods f
56. ed in Table 6 on page 152 11 Select the Enter button F7 to accept entries 12 Repeat the procedure for the other functions to complete the program 13 Press the Esc key until you are back in the Settings screen 1200 Series Handheld Control Module Users s Guide 151 12 Running an Injector Program Injector Program Lines Table 6 describes the program lines which will complete the required derivatization reaction Table 6 Injector Program Lines Line Function Parameters Comment 1 DRAW 2 pl AMOUNT from Air Draw 2 ul from air into the needle SOURCE capillary to separate the mobile phase sitting in the capillary from the sample 2 DRAW 1 pl AMOUNT from vial Draw 1pl from derivatization reagent 1 SOURCE from vial 1 in the autosampler tray into the needle capillary 3 WASH in vial 2 VIAL 1 time Wash the needle tip in the wash vial 2 Cycles 4 DRAW 2 pl AMOUNT from sample Add 2 ul of the sample in the SOURCE autosampler tray to the derivatization volume already in the needle capillary 5 WASH in vial 2 VIAL 1 time Wash the needle tip in the wash vial 2 CYCLE 6 DRAW 1 pl AMOUNT from vial 1 Add 1 pl of derivatization reagent from SOURCE vial 1 in the autosampler tray to the derivatization reagent and sample already in the needle capillary 7 MIX 6 pl AMOUNT in seat Mix 6 pl with a repetition of 8 times at a SOURCE at 500 l min speed of 500 ul minute in the seat SPEED 8 times REPEAT 8 WAIT
57. eens e g System Status Sampels or Sequence screen 1 Enter the Analysis screen 2 Select the Start button F8 3 Select OK to confirm the vial range and injection number and press the Enter key to start the analysis 1200 Series Handheld Control Module Users s Guide 121 9 Running an Isocratic Analysis Starting the Analysis 122 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 10 Running a Gradient Analysis What You Will Need 124 Preparing the LC System 125 Entering Settings 126 Saving Settings ina Method 128 Observing the Chromatogram 129 Starting the Analysis 131 phe Agilent Technologies 123 10 Running a Gradient Analysis What You Will Need Instruments Agilent 1200 Series binary or quaternary pump autosampler UV detector and degasser Column A 125 mm x 4 0 mm Hypersil ODS 5 um Agilent Technologies part number 7982618 564 Solvents LC grade bidistilled water and acetonitrile Sample The Agilent Technologies isocratic standard sample Agilent Technologies part number 01080 68704 This contains 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl and 0 03 wt o terphenyl dissolved in methanol 124 1200 Series Handheld Control Module Users s Guide Running a Gradient Analysis 10 Preparing the LC System 1 Fill one solvent bottle with bidistilled water channel A and the other with acetonitrile channel B
58. eld Control Module Users s Guide Contents 69 Contents 10 Resetting the Pump Settings 70 Using the Degasser 71 Starting the Degasser 72 Removing Gas Bubbles 72 Changing Solvents 73 Using the Autosampler 75 Configuring the Autosampler 76 Configuring Interfaces 76 Entering Settings 77 Setting the Injection Mode 77 Optimizing Autosampler Performance 78 Setting up the Thermostatted Autosampler 79 Aligning Transport Arm Gripper 80 Tracking Autosampler History EMF limits 81 Resetting the Autosampler 81 Reset to Default Settings 81 Troubleshooting the Autosampler 82 Using the Manual Injection Valve 83 About the Injection Valve 84 Making An Injection 85 Completely Filling the Sample Loop 85 Partially Filling the Sample Loop 86 How Much Sample Is Actually Injected 86 How Much Sample Do I Need 87 An Alternative Way to Fill The Loop 87 1200 Series Handheld Control Module Users s Guide Contents 7 Usingthe Detectors 89 Turning the Lamp On and Off 90 Entering Settings 91 Diode Array Detector 91 Variable Wavelength Detector 91 Fluorescence Light Detector 91 Multiple Wavelength Detector 92 Refractive Index Detector 92 Resetting the Baseline 93 Configuring the Detector 94 Troubleshooting the Detector 95 Tracking Detector History 96 Resetting the Detector 97 Lamp Ignition Routine VWD only 98 Configuring the Analog Channel Output 99 8 Using the Column Compartment 101 Turning the Column Compart
59. emp 102 tests 68 80 82 95 108 timetable 24 47 views 23 24 write 105 zero 93 C calibration 48 137 139 detector 99 multiple level 139 sequence 137 139 single level 137 wavelength 99 calibration button 48 CAN Controller Area Network 36 164 changing solvents 73 channels 65 chromatogram 129 130 coexecution 61 column 114 column compartment column 114 column ID 110 column identification 105 column switching valve 107 configuration 104 heater modes 106 ID tag 105 modes 106 on off 102 resetting 111 settings 103 tests 108 tracking history 109 tracking ID history 110 troubleshooting 108 using 101 column ID button 105 column ID module 105 column switch button 107 column switching valve 107 compressibility 66 configure 38 context menu 20 contrast 37 control module Agilent ChemStation 61 available modules 38 coexecution 61 contrast 37 display 37 displayed modules 38 features 16 firmware update 61 general functions 37 installing 36 keys 17 overview 17 product number 17 restrictions 62 serial number 17 software 23 troubleshooting 39 user interface 23 working with 35 Control Module Versions 32 G1323A 32 G1323B 32 cursor 52 cursor button 52 D date and time 37 degasser changing solvents 73 on off 72 removing gas bubbles 72 starting 72 status lamp 72 using 71 deleting a method 45 deleting all methods 45 dete
60. es from the Selected Modules to the Available Modules list boxes and vice versa depending on which module is highlighted Configuring the LC System The LC system is self configuring to a large extent It recognizes automatically which modules are installed The layout of the Analysis screen changes according to the modules present You can use the Configure button F2 in the System screen to configure various features such as the Auto on for the system or Loading a method and After Error Condition If an error event occurs you can configure the LC system to load a specified method or turn off the LC system using the After Error Condition setting 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Troubleshooting Internal diagnostics continuously monitor the module s condition and record any unusual events in an electronic logbook For example missing vials or leaking solvent will signal errors and record the errors in the logbook together with the time and date the errors occurred The logbook is self updating where the newest entry replaces the oldest entry If a printer is connected you can easily print out the logbook Troubleshooting the Control Module If your control module does not work correctly disconnect the module CAN connector from the rear of the Agilent 1200 Series module it is attached to and reconnect it If the problem still remains then e power down all connected devi
61. es how to analyze the Agilent Technologies isocratic standard sample using a gradient analysis Running Multiple Vial Analyses This chapter descibes how to setup multiple vial analyses using the same method and different methods Running an Injector Program This chapter descibes how to create an injector program Maintaining the Control Module This chapter shows the repair items 1200 Series Handheld Control Module Users s Guide A Appendix This chapter contains safety information Related Documents Each HPLC module is supplied with a Reference Manual or User Manual The control module is supplied with the following e User s Guide Software Overview Guide 1200 Series Handheld Control Module Users s Guide Contents 1 The Agilent 1200 Series Control Module 15 Control Module Features 16 Control Module Keys 17 The i info key Online Information System The m menu key 20 The Esckey 20 The Enterkey 21 Navigation keys 21 Action keys 21 Selection keys 21 Direction keys 21 Numeric Alphanumeric keys 22 Control Module Software 23 The Control Module User Interface 23 Analysis Screen 23 System Screen 27 Status Screen 29 Samples Screen 30 Plot Screen 31 Control Module Versions 32 2 Working with the Control Module 35 Installing the Control Module 36 General Functions 37 Turning On Off LC System and Modules 37 Setting Date and Time 37 1200 Series Handheld Control Module Users s Guide Conte
62. f injections 1 Calibration method METH1 Recalibrate every 2 vials multi Before On After On 5 Press the Done button F6 until the Sequence screen appears 6 Select the Start button F8 in the Sequence screen 7 Press Enter to start the sequence 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Multiple Level Calibration Sequences The following sections describe how to set up calibration sequences for analyses which use multiple level calibration Recalibrating With the Same Group of Standards There are three calibration standards of different concentrations C1 C2 C3 and 15 samples S The standards and samples are analyzed using the same method The analysis requires that e each sample is analyzed once e the calibration standards are analyzed twice before the samples and re analyzed twice after every 5 samples C1 C2 C3 10 S14 C1 C2 C3 15 S19 C1 C2 C3 820 824 C1 C2 C3 e the calibration standards are located in positions 90 to 92 of the autosampler tray e the 15 sample vials are located in positions 10 to 24 of the autosampler tray and e the samples and standard are analyzed using a method called METH1 The example assumes that the sequence table is empty If the sequence table is not empty use the All Lines item accessed by pressing the Delete button F6 1 Select the Sequence button F4 in the Analysis screen 2 For sequence line 1 select the Insert button F7
63. f wavelength setting at 656 nm emission must be within 1 nm at reference side only to have no influence from flow cell condition If not correct a message for calibration is displayed Perform a wavelength calibration available within VWD Tests e Check of intensity at 250 nm without cut off filter inserted at 250 nm with cut off filter inserted If the intensity check is not OK the cut off filter operation is not OK 98 1200 Series Handheld Control Module Users s Guide Using the Detectors 7 Configuring the Analog Channel Output You may use the LC Series 1200 detectors to test or monitor optical parameters on external analog equipment connected via the analog output Fluorescence Light Diode Array and Multiple Wavelength Detectors have two analog outputs Variable Wavelength Detector and Refractive Index Detector have one at the back side of the module To configure the analog outputs 1 Press the Settings button F1 in the Analysis screen 2 Choose the detector and press enter 3 Press the Analog button F3 4 Either select the signal you want to monitor from the signal source drop down list Or if you have a variable wavelength detector fluorescence light detector choose the signal s from the list s to be routed to the analog output s 5 Enter the values for Zero Offset sets a baseline offset in order to recognize negative drifts and Attenuation sets an absorbance range for each of the two connecto
64. flict with these terms the warranty terms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or disclo sure of Software is subject to Agilent Tech nologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a haz ard It calls attention to an operat ing procedure practice or the like that if not correctly performed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION
65. gasser 4 Changing Solvents If you are changing to a solvent that is immiscible with the solvent currently in the tubing 1 Replace the current solvent with iso propanol if current solvent is organic or with water if current solvent is an organic buffer or salt 2 Flush the online degasser and all tubing thoroughly 3 Replace the iso propanol or water with the new solvent 1200 Series Handheld Control Module Users s Guide 73 4 Using the Degasser Changing Solvents 74 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 5 Using the Autosampler Configuring the Autosampler 76 Entering Settings 77 Aligning Transport Arm Gripper 80 Tracking Autosampler History EMF limits 81 Resetting the Autosampler 81 Troubleshooting the Autosampler 82 phe Agilent Technologies 75 5 Using the Autosampler Configuring the Autosampler 76 1 2 3 Select the Configure button F2 in the System screen Select Autosampler from the menu Press Enter You can configure the syringe volume seat capillary volume action on missing vial trays interfaces etc Configuring Interfaces ao A O N Select the Configure button F2 in the System screen Select Autosampler from the menu Press Enter Select the Interfaces button F1 Select the interfaces you want to operate see Connecting External Devices on page 57 Select the Done button F6
66. gs Method method management functions load save delete Sequence multiple method analyses and Views other screens Samples easy access on vials Status most important parameters during analysis and System control configuration tests and records 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 The Start Stop button F8 starts or stops a single injection or a multiple injection analysis The On Off button F7 turns the pump detector lamp heater and thermostatted column on or off The Plot button F6 provides direct access to the Plot screen where all important parameters can be displayed graphically It is possible to display several parameters at the same time Using the m menu key in the Analysis screen prompts context sensitive menus depending on the active parameter entry field see Figure 3 on page 20 The Module Status on the top right hand side of the screen and on top of the individual module tabs indicates whether the system module is ready or not ready only applicable for individual modules indicates that a vital error has occurred in the module The following diagram shows the functionality available in the Analysis screen for an LC system comprising a pump an autosampler a thermostatted column compartment and a detector e g Variable Wavelength Detector Diode Array Detector Multiple Wavelength Detector 1200 Series Handheld Contro
67. gs 77 external contacts 76 injection modes 77 injection volume 77 injector program 77 interfaces 76 missing vial 76 needle seat volume 76 needle wash 77 optimization 78 overlapped injections 78 prefetch 78 resetting 81 runtimes 77 sample throughput 78 shortening analysis time 78 syringe volume 76 tests 82 thermostat 79 theta correction 80 timetable 77 tracking history 81 trays 76 troubleshooting 82 using 75 1200 Series Handheld Control Module Users s Guide wash mode 77 wash vial 77 x correction 80 auxiliary signals 79 available modules 38 available signals 50 backspace 43 balance 93 balance button 93 banner text 55 baseline resetting 93 baudrate 55 BCD interface 57 buttons 65 add 38 53 align 80 analog 99 balance 93 calibration 48 column ID 105 column switch 107 configure 38 copy gt gt 45 cursor 52 delete 47 EMF 54 end actions 48 function 18 identify 53 initialize 45 insert 47 135 interfaces 57 76 lamp 90 logbook 48 menu 18 163 Index method 24 41 module 41 move 50 on off 25 37 64 72 90 102 page 55 PC card 45 plot 25 previous 19 print 56 printer 55 records 53 related 19 remove add 38 rescale 31 51 130 reset 70 81 restore 51 right 105 save as 42 search 19 select 50 sequence 24 48 serial 55 settings 24 42 setup 37 50 56 signal 82 spooler 56 start 144 start stop 25 t
68. he standard mode the analysis is under the command of the control module The control module will issue a Start Request command to the autosampler as soon as all modules are ready for the next analysis The autosampler issues the Start command at the point of injection With an Agilent 1200 Autosampler integrated in the system and no external devices this is the normal operation mode 144 1200 Series Handheld Control Module Users s Guide Running Multiple Vial Analyses 11 Send Single Start Request After you start the analysis with the control module it will generate a single start request on the APG remote lines This allows to trigger the external device which will start each injection by sending a start signal The vial range or sequence will be started by the control module but for every new injection the external device must give the start command to APG Remote SR START START START START from Control Module Figure 18 Send single external start request In this mode the control module will simply track the progress of the vial range or sequence It will indicate the proper sample change sequence lines load methods or other sequence related actions for each run 1200 Series Handheld Control Module Users s Guide 145 11 Running Multiple Vial Analyses Send Repeated Start Request This will cause the control module to generate start requests before each run The external device starts each injection then by sending a
69. ilent 1200 Series Modules This part describes how to use the individual HPLC modules to run isocratic gradient and multiple vial analyses using a single method or more than one method Using the Pump This chapter contains operational details for the Agilent 1200 Series pumping systems Using the Degasser This chapter contains operational details for the Agilent 1200 Series vacuum degasser Using the Autosampler This chapter contains operational details for the Agilent 1200 Series autosampler 1200 Series Handheld Control Module Users s Guide Part 3 10 11 12 13 Using the Manual Injection Valve This chapter contains operational details for the Agilent 1200 Series manual injection valve Using the Detectors This chapter contains operational details for the Agilent 1200 Series variable wavelength multiple wavelength refractive index fluorescence light and diode array detectors Using the Column Compartment This chapter contains operational details for the Agilent 1200 Series thermostatted column compartment Using the Agilent 1200 Series LC System With Control Module This part describes how to run isocratic gradient and multiple vial analyses using a single method or more than one method Running an Isocratic Analysis This chapter describes how to analyze the Agilent Technologies isocratic standard sample using a single injection analysis Running a Gradient Analysis This chapter describ
70. ions as well as calibration and configuration settings in a self explanatory and intuitive way Define automated analyses including methods timetables injector programs method sequences and automated calibration settings using the control module Protect your method from any inadvertent keyboard changes by setting method protection Use PC cards to store and transfer methods and sequences between Agilent1200 systems Monitor all operations and error events using the self updating logbooks Use the context sensitive online information system to get further information on all topics Use the context sensitive menu function to have the quickest access on related functions To help comply with Good Laboratory Practice GLP regulations you can select a variety of module tests that will check the performance of the LC system The early maintenance feedback EMF limits can be used for scheduling maintenance work Display data graphically using the Plot screen where as many as three different signals can be monitored at the same time Print information to a PCL3 compatible printer connected to the serial RS232 port of a Agilent1200 module 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 Control Module Keys Action keys execute specific operations and access Plot screen m menu key provides navigational shortcuts and actions 00
71. is screen for example to 5 ml min If a flow rate of more than 5 ml min is used on a quaternary pump redefine the upper pressure limit to 200 bar Accessible from the Analysis screen press the Settings button F1 choose pump from the list and press the Enter key Then choose More 5 Set the first channel to be purged to 100 We recommend you start with the organic solvent channel first Channel A will automatically be set to 100 when all other channels are set to zero or OFF 6 Turn on the pump using the 0n Off button F7 in the Analysis screen 7 Wait until a continuous stream of solvent comes out of the outlet tube from the purge valve 8 Turn off the pump using the On Off button F7 in the Analysis screen and then close the purge valve 9 Repeat the procedure for the other channels you need to purge The channels of a pumping system are named A B C and D depending on the pump type A is automatically calculated by 100 B C D If no values for B C and D are entered A is always 100 To purge the pump you have to go through steps step 5 to step 8 individually for each of the channels setting the composition to 100 for the channel to be purged 1200 Series Handheld Control Module Users s Guide 65 3 Adjusting Compressibility 66 Using the Pump Liquid chromatographic solvents are compressible under pressure This solvent compressibility produces a change in flow rate as the pressure change
72. is using the Alter and Multi settings Alter analyzes the calibration vials alternately Multi analyzes the calibration vial or vials in complete groups according to the calibration interval 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 A sequence line consists of the following Line Number Starting with 1 the sequence lines are automatically counted up Vial Range Information Just like in the Analysis screen you can specify a range of vials together with the number of injections per vial Injection Volume Although the injection volume is stored as a method parameter a sequence has its own injection volume setting overriding method information If DEF is specified here the volume as set in the method is kept Method Name Choose a method stored in the modules from the method list box see Working with Methods on page 41 The method has to contain all the relevant parameters as well as timetable or injector program settings In the Sequence screen you create a program of several methods to be executed in a specified order Editing of methods or their components timetables injector programs etc is not possible Wait Time Specify a wait time that creates a gap between method loading and execution This allows certain module parameters to stabilize before the next analysis is performed Calibration Settings For each sequence line you can define calibration settings by pressing
73. l 52 cursor 52 display exact values 52 maximize 51 print 55 print graph 52 rescale 51 signal unit axis 51 time axis 51 toggling signals 52 x yvalues 52 x axis 51 y axis 51 pop up menu 23 power on signal 57 prefetch 78 prepare signal 58 previous button 19 print delete job 56 graph 52 interface 57 logbooks 56 number of copies 56 plot 55 print button 56 printer button 55 printer setup 55 printing screens 55 product number 17 53 protecting a method 43 pump 63 1200 Series Handheld Control Module Users s Guide adjusting compressibility 66 channels and composition 65 127 on off 64 piston 67 purging 64 resetting 70 resetting settings 70 settings 64 shut down 68 stroke 68 tracking history 69 troubleshooting 68 using 63 valve 64 purge procedure 65 pump 64 valve 64 ready signal 58 recalibration 139 alter multi 48 recalibration with same group of standards 139 records nutton 53 refractive index detector automatic recycling 92 cell temperature 92 peakwidth 92 polarity 92 settings 92 zero 93 related button 19 remove button 38 rescale button 31 51 130 rescale plot screen 51 reset button 70 81 resetting autosampler 81 autosampler defaults 81 baseline 93 column compartment 111 detector 97 pump 70 pump settings 70 restore button 51 right button 105 RS232 interface 57 running an analysis 113 running injector program 149
74. l Module Users s Guide 25 1 The Agilent 1200 Series Control Module table 4HPLS System 2QUAT Pump Autosampler 4Column Comp 5 Detector LC System Runtimes Timetable Defaults Pump Flow Pressure Solvent Composition Autosampler Inj Program Inj Vol Draw Speed Optimization Column Comp Temperature Left Right Temp Range DA MW VW FL or RI Detector Wavelengths Peakwidth Auto Balance Spectrum Figure 7 Set parameters time dependent from instant of injection Flow Solvent Composition Temperature Wavelength Balance also available from Settings screens Handle methods Combine methods onmodulesorPC for automated cards analysis Save As End Actions Load Calibration Print Manage PC card User ID Sequence Logbook Comment Where to go from the Analysis Screen Menu Structure 1200 Series Handheld Control Module Users s Guide The Agilent 1200 Series Control Module 1 System Screen The System screen provides access to non routine settings and provides error checking control testing and tracking usage for LC system and modules This screen displays the logbook together with the LC system and module status The EMF Early Maintenance Feedback icon will flash to indicate when an EMF limit is exceeded On off indicators of other modules Current status EE eee Puinp i Temp Lamp ee o oR READY M
75. ld Control Module Users s Guide The Agilent 1200 Series Control Module 1 Status Screen This screen shows the most important parameters of the system in an easy to read style Included parameters are flow pressure column temperature absorbance units detector wavelength elapsed time etc depending on the LC system configuration The screen content is updated in short intervals of roughly one second You can also monitor the LC system and module status using the Status bar at the top of each screen The content of the Status bar varies depending on the screen and is very limited The status for each module can also be displayed In the respective Setting screen press the m menu key In the appearing context menu select Status Status Niel Inj fies o oE Ready snow O 000 Te 20 00 90 0 0 271 mu Pressure Qbar Ripple 0 0 A 254 nm I Elapsed 0 00 min i Figure 10 Status Screen 1200 Series Handheld Control Module Users s Guide 29 1 30 The Agilent 1200 Series Control Module Samples Screen Operating from this screen you have easy access on the sample tray Using the Vial Range function you can specify the vials you want to analyze and the desired method A graphical image of the tray offers a good view of the vials chosen The Sequence option gives you control over the execution of specified analysis sequence steps programmed before While the analysis is running you can view the processe
76. le of syringe into needle port until needle touches stator face Do not press too hard 5 Slowly inject sample 6 Leave syringe in position and move valve to INJECT position 7 Remove syringe How Much Sample Is Actually Injected 86 When the sample loop is completely filled the amount of sample injected is equal to the volume of the sample loop plus the volume of the valve passages 1 in rotor and 2 in stator This means that the actual amount of sample injected will be different to the nominal value designated to your sample loop However since both standards and samples are analyzed using the same loop you rarely need to know the absolute volume of the loop If you do need to know the actual volume of a sample loop we recommend you calibrate it fitted to the valve so that you also take the valve passages into account 1200 Series Handheld Control Module Users s Guide Using the Manual Injection Valve 6 How Much Sample Do Need To completely fill the sample loop an excess of sample is required This is about 2 to 3 loop volumes of sample to achieve 95 of the maximum loop volume the remainder is residual mobile phase in the sample loop Determine the optimum number of loop volumes experimentally for your particular application When you partially fill the sample loop do not inject more than half of the sample volume As you inject your sample into the loop the sample mixes with the solvent already in the loop and
77. les Table 2 Firmware Update Tools Update via Control Module G1323B LAN RS 232 Update Tool 2 00 Module and a PC with LAN or RS 232 Control Module G1323B Y PC card Y via the HPLC system HPLC Modules Y PC card Y requires LAN RS 232 The installation of older firmware might be necessary e to keep all systems on the same validated revision or e if third party control software requires a special version To upgrade downgrade the firmware 1 Download the firmware and the documentation from the Agilent web http www chem agilent com scripts cag_firmware asp The use of the LAN RS 232 Update Tool 2 00 is also possible It is also available via the above mentioned Agilent web For systems that still use GIPB use the Firmware Update Tool 4 00 2 Load the firmware into the module s as described in documentation provided with the Firmware Update Tools 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Coexecution with Agilent ChemStation Features e Both user interfaces the control module and the Agilent ChemStation can be connected to a Agilent 1200 Series system at the same time e Parameter entry is possible from both user interfaces Parameters will be updated on the other user interface within a few moments e An Agilent ChemStation sequence can be stopped and aborted from the control module and vice versa The Agilent ChemStation can generate data files from a cont
78. ll LC analytical settings The most commonly used settings are displayed with their corresponding set and actual values Since space on the display is limited you will only see a selection of important parameters The screen layout will depend on the modules that are included in the system and on the modules selection the user did in the Setup View dialog accessible via the m key the maximum of visible modules on this screen is 4 1200 Series Handheld Control Module Users s Guide 23 1 The Agilent 1200 Series Control Module parameter vial range setting number of injections setting Pump parameter flow rate setting system pressure solvent composition 24 The other less used settings of the current method appear in further screens to be accessed from the Settings button F1 The actual values are updated continuously Vial range status information vial number injection number run time status module status modification flag method in use stoptime 4 ber B3 COFF Ta OFF Autosampler parameter Thermostatted Column Detector parameter injection volume setting Compartment parameter wavelength setting drawing volume temperature setting actual wavelength actual temperature left right Figure 6 Analysis Screen Information The screen provides access to Settings all LC analytical system and module settings Timetable time programmable settin
79. loop Autosampler G2258A Agilent 1100 1200 Preparative Autosampler G2260A G2261A 32 1200 Series Handheld Control Module Users s Guide Table 1 The Agilent 1200 Series Control Module 1 Control Module Versions Version controls G1323B Firmware B 03 22 1100 module firmware revision up to A 05 xx Agilent 1100 Isocratic G1310A Quaternary G1311A and Binary G1312A pump Agilent 1100 Autosampler G1313A and Thermostatted Autosampler G1330A Agilent 1100 Variable Wavelength Detector G1314A Agilent 1100 Diode Array Detector G1315A B C Agilent 1100 Thermostatted Column Compartment G1316A Agilent 1100 Fluorescence Detector G1321A Agilent 1100 Preparative Pump G1361A Agilent 1100 Fraction Collector G1364 Agilent 1100 Refractive Index Detector G1362A Agilent 1100 Multiple Wavelength Detector G1365A B Agilent 1100 Well plate Autosampler G1367A Agilent 1100 Capillary Pump G1376A Agilent 1100 Micro Well plate Autosampler G1377A G1368A Agilent 1100 Dual loop Autosampler G2258A Agilent 1100 Preparative Autosampler G2260A G2261A G1323A Firmware A 02 10 1100 module firmware revision up to A 05 xx Agilent 1100 Diode Array Detector G1315A Agilent 1100 Fluorescence Detector G1321A Agilent 1100 Variable Wavelength Detector G1314A Agilent 1100 Quaternary G1311A Binary G1312A and Isocratic G1310A pump Agilent 1100 Thermostatted Column Compartment G1316A Agile
80. ls at a time The plot function will display all signals that are shown in the Selected Signals list box Use the selection keys to navigate within the list boxes and press the Enter key to move Signals from one box to the other Select the Done button F6 to display the chromatogram Press the Esc key to go back to the Analysis screen Press the Start button F8 Select OK to confirm the vial range and injection number and press Enter to start the analysis on oo ol 1200 Series Handheld Control Module Users s Guide 119 9 Running an Isocratic Analysis 9 Press the Plot button F6 to show the chromatogram A typical chromatogram for this analysis is shown in Figure 16 mAU 350 4 300 4 250 4 200 4 150 4 100 4 50 4 1 2 3 4 5 6 min Figure 16 Analysis of Isocratic Standard Sample The exact profile of the chromatogram will depend on the column you have used Differences in retention times and areas of the peaks in your chromatogram and the one shown in Figure 16 might be a result of variations in the concentration of the sample from batch to batch the quality of the solvents used and the column temperature You can rescale the plot using the Rescale button F7 or the cursor keys or you define the plot window within the Setup 120 1200 Series Handheld Control Module Users s Guide Running an Isocratic Analysis 9 Starting the Analysis The analysis can be started from various other scr
81. ment On and Off 102 Entering Settings 103 Configuring the Column Compartment 104 Configuring the Column ID Module 105 Selecting Separated or Combined Mode 106 Selecting the Column Switching Valve optional 107 Troubleshooting the Column Compartment 108 Tracking Column Compartment History 109 Tracking Column ID History 110 Resetting the Column Compartment 111 1200 Series Handheld Control Module Users s Guide 11 Contents 12 10 11 Running an Isocratic Analysis 113 What You WillNeed 114 Preparing the LC System 115 Entering Settings 116 Saving Settings ina Method 118 Observing the Chromatogram 119 Starting the Analysis 121 Running a Gradient Analysis 123 What You Will Need 124 Preparing the LC System 125 Entering Settings 126 Saving Settings in a Method 128 Observing the Chromatogram 129 Starting the Analysis 131 Running Multiple Vial Analyses 133 Analyzing Multiple Vials Using the Same Method 134 Analyzing Multiple Vials Using Different Methods 135 Single Level Calibration Sequences 137 Multiple Level Calibration Sequences 139 Recalibrating With the Same Group of Standards 139 Recalibrating With Multiple Groups of Standards 141 Synchronizing Analyses with External Devices 144 Standard 144 Send Single Start Request 145 Send Repeated Start Request 146 Wait for Single External Start Request 146 1200 Series Handheld Control Module Users s Guide Contents Wait for Repeated Start Request 147 12 Running
82. n 1 Enter the Analysis or System screen 2 Select the On Off button F7 3 Select the Pump button F8 4 Choose the desired function either with the Action buttons F6 F8 or by selecting the On Off buttons in the pop up window Uncheck the to Standby mode only if you want to turn the pump on or off without going to standby mode You can also access this function from the Settings button F1 available in the Analysis screen or the Control button F1 in the System screen Entering Settings All pump settings can be entered in the Pump Settings screen You can access this screen by selecting the Settings button F1 in the Analysis screen and then choosing the pump Commonly used settings such as flow and solvent composition can be set directly in the Analysis screen The choices available there depend on how many other modules are installed Purging the Pump 64 By opening the purge valve you can redirect the solvent flow from the pump out through the valve exit instead of passing through the injection valve and column This purging process removes any undegassed or previously used solvent within the pumping system 1200 Series Handheld Control Module Users s Guide Using the Pump 3 Purging Procedure 1 Ensure that an outlet tube is connected from the purge valve to a waste solvent bottle 2 Open the purge valve Enter the Analysis screen 4 Set the purge flow rate in the regular flow rate section of the Analys
83. nit ranges have been specified press the Done button F6 to switch to the graphic view 50 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Rescaling the Plot Screen X time axis To rescale the X time axis there are several possibilities e Enter a time in the Plot Selection windows available from the Plot screen via the Select button F6 e Perform a rescale directly in the Plot screen by pressing the Direction left right keys The right key will shorten the time range by the factor 2 The left key will enlarge the range by the same factor Press the keys several times to set up the appropriate time frame The time range is indicated at the bottom of the Plot screen This setting is independent from the active signal Y signal unit axis To rescale the Y signal unit axis there are several possibilities e From the Plot Selection windows available from the Plot screen via the Select button F6 choose a signal from either list box and press the Setup button F7 You can specify a Y range separately for each signal This setting can also be made for signals not being part of the Selected Signals list box Rescaling directly from the Plot screen will overwrite these settings e Use the Rescale button F7 in the Plot screen to adjust the Y axis according to the minimum and the maximum signal value within the set time range Using this function provides the optimum signal display
84. notice until the indicated conditions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated condi tions are fully understood and met 1200 Series Handheld Control Module Users s Guide In This Guide This book describes how to operate the Agilent 1200 Series modules and systems for HPLC using the control module Solvent cabinet Vacuum degasser Control module Autosampler Column compartment Detector 1200 Series Handheld Control Module Users s Guide Part 1 Part 2 The control module provides complete local control and monitoring of a single module or an entire Agilent 1200 Series system There is no data evaluation in the control module The control module allows you to do a variety of HPLC tasks including automated sample preparation and injection isocratic gradient and multiple method analyses Chapter Overview Using the Agilent 1200 Series Control Module This part describes the control mode its features and its functionality The Agilent 1200 Series Control Module This chapter gives an overview over the Agilent 1200 Series control module Working with the Control Module This chapter describes how to use the Agilent 1200 Series control module Using the Ag
85. nt 1100 Autosampler G1313A and Thermostatted Autosampler G1330A 1200 Series Handheld Control Module Users s Guide 33 1 34 The Agilent 1200 Series Control Module Control Module Versions 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 2 Working with the Control Module Installing the Control Module 36 General Functions 37 Troubleshooting 39 Inserting and Removing PC cards 40 Working with Methods 41 Time Programming 47 Automating Analyses 48 Displaying Data Graphically 50 Logbooks 53 Printing Screens 55 Connecting External Devices 57 Firmware Updates 60 Coexecution with Agilent ChemStation 61 phe Agilent Technologies 35 2 Working with the Control Module Installing the Control Module WARNING The CAN connectors are similar to LAN adapter connectors Do not insert LAN connectors into the CAN or vice versa since the CAN uses 24 V and might blow up the LAN card Connect the CAN controller area network connector of the control module cable to one of the two CAN connectors on one of the Agilent 1200 Series modules CAN connector Figure 13 Connecting the CAN Connector to Rear Panel 36 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 General Functions Turning On Off LC System and Modules Use the On Off button F7 in the Analysis screen to turn on or off either the complete sys
86. ntry or action When entering a parameter into a certain field Enter leads you on to the next accessible entry field In this case it has the same function as the right Direction key Navigation keys These 5 keys F1 F5 allow you to switch between the menus Within these menus the relevant parameters can be set and certain functions can be accessed The Navigation keys always correspond to a button displayed above them on the screen The menus accessed via the buttons vary according to the screen you are working with In some cases pressing a button will cause a list box to appear From there you must make a choice in order to proceed Action keys The 3 Action keys F6 F8 trigger a variety of functions The available functions depend on the screen you are working with Selection keys With the Selection keys arrow up down you can select settings in various list boxes You can also change values in certain parameter entry fields or enter alphanumeric characters Direction keys With the Direction keys arrow left right you can move back and forth between the entry fields 1200 Series Handheld Control Module Users s Guide 21 1 22 The Agilent 1200 Series Control Module Numeric Alphanumeric keys These keys allow you to enter numeric values in parameter entry fields In certain fields where alphabetical characters may be entered you can use the Numeric Alphanumeric keys to do so Pressing them several times in sequenc
87. nts Setting Display Contrast 37 Adjusting View 38 Configuring the LC System 38 Troubleshooting 39 Troubleshooting the Control Module Inserting and Removing PC cards 40 Working with Methods 41 LoadingaMethod 41 Modifying a Method 42 Specifying a Method Name 42 Protecting a Method 43 Savinga Method 44 Deleting a Method 45 Exchanging Methods With the PC Card 39 45 Transferring Methods Between LC Systems 46 Time Programming 47 Automating Analyses 48 Displaying Data Graphically 50 Selecting Signals 50 Rescaling the Plot Screen 51 Toggling Signals 52 Displaying Exact Signal Values 52 Print Graph 52 Logbooks 53 Maintenance Logbook 53 Error Logbook 54 System Logbook 54 EMF Early Maintenance Feedback Printing Screens 55 Print Plot 55 54 8 1200 Series Handheld Control Module Users s Guide Print Logbooks 56 Print Method 56 Print Timetable 56 Print Sequence 56 Print Injector Program 56 Connecting External Devices 57 APG Remote 57 GPIB 59 Serial RS 232 59 MIO 59 BCD 59 External Contacts 59 Firmware Updates 60 Coexecution with Agilent ChemStation 61 Features 61 Restrictions 62 3 UsingthePump 63 Turning the Pump On and Off 64 Entering Settings 64 Purging the Pump 64 Purging Procedure 65 Adjusting Compressibility 66 Adjusting Stroke Volume 68 Automatic Shut down 68 Troubleshooting the Pump 68 Tracking Pump History Pump EMF Limits Resetting the Pump 70 1200 Series Handh
88. o connect a printer to the serial interface included in all modules The module communication is enabled with the CAN cables Choose one module to connect the printer to MIO This interface enables the Agilent 1200 Series modules to communicate with PCs configured as Agilent ChemStations using a local area network LAN You can use the MIO interface if the respective extension board is installed in one of your modules and your system is integrated in a LAN BCD If the appropriate extension board is part of your system you can use this output to inform external devices about the vial number currently processed External Contacts With an optional external contacts board you can use various opportunities to synchronize LC activities with external devices 1200 Series Handheld Control Module Users s Guide 59 2 Working with the Control Module Firmware Updates 60 The firmware updates can be done using the control module and a PC card The firmware is loaded from a PC card either into the control module itself or into the modules of the system You can also update the firmware using a Personal Computer configured as the Agilent ChemStation and connected via the GPIB cable or LAN connection All Agilent 1200 LC modules can be updated using a Personal Computer and the G1323B control module The firmware of Agilent HPLC modules or the Control Module can be updated using the Control Module and a PC card that holds the firmware fi
89. odule Message Date Time HPLC System Sequence wait 0 30 min IND 12 241 15 05 03 HPLC System Sequence started IND 12 24 15 05 03 Col Comp Column switching valve column 1 IND 12 24 15 04 55 DA Detector Parameter changed IMD 12 24 15 04 58 Parameter changed IND 12 24 15 04 55 Conf nReady System logbook shows all messages from all modules with date and time Figure 8 System Screen Information The screen provides access to e LC system and module controls for example pump on off lamp on off heater on off and injector reset e LC system and module configuration e module tests and e LC system and module records 1200 Series Handheld Control Module Users s Guide 27 1 The Agilent 1200 Series Control Module The following diagram shows the functionality available from the System screen for an LC system comprising a pump autosampler diode array detector variable wavelength detector and thermostatted column compartment Reset Balance Home Figure 9 28 2QUAT Pump 3 Autosampler 4Golumn Comp 5 Detector Auto On Pressure Test On Error Leak Test Printer Setup Temperature Display Settings Calibration User Settings Change Arm Interfaces Wavelength Column Calibr Identific DAC Test System Log Error Log EMF Data Maintenance log Firmware Update Identify Print Where to go from the System Screen Menu Structure 1200 Series Handhe
90. onal injury are present in this instrument Use extreme caution when handling testing and adjusting Safety Symbols Table 8 shows safety symbols used on the instrument and in the manuals Table8 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal Eye damage may result from directly viewing the light produced by the Xenon flash lamp used in this product Always turn the xenon flash lamp off before removing it a Os 1200 Series Handheld Control Module Users s Guide 159 A Appendix A warning alerts you to situations that could cause physical injury or damage to the equipment Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A caution alerts you to situations that could cause a possible loss of data Do not proceed beyond a caution until you have fully understood and met the indicated conditions 160 1200 Series Handheld Control Module Users s Guide Appendix A Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and or use
91. ontrol module keeps track of all kinds of system parameter changes error messages and maintenance data You can access the logbooks by pressing the Records button F4 in the System screen Information on this screen includes the module product and serial number firmware version number and the operation time from power on until now Additionally an EMF Early Maintenance Feedback indicator shows if maintenance is required You can identify the individual modules by highlighting them in the Records screen and pressing the Identify button F8 For several seconds the module s LED will be blinking Logbook settings may be entered by pressing the m menu key in the System screen and choosing the Setup Logbook option In the appearing logbook settings menu you can choose which events are to be displayed in the logbooks Choose a module from the list box and press the button F1 F4 corresponding to the type of logbook you want to open Maintenance Logbook On the screen you see the most recent maintenance work together with date and time Use the Add button F7 to record maintenance work and update the logbook The contents of this logbook is permanently stored in the respective modules but when memory capacity is exceeded the newest entry replaces the oldest entry 1200 Series Handheld Control Module Users s Guide 53 2 54 Working with the Control Module Error Logbook This logbook displays the most recent error messages with
92. py methods from and to the PC card 1200 Series Handheld Control Module Users s Guide 45 2 Working with the Control Module If you want to store the current method on PC card you have to use the Save As function see Saving a Method on page 44 in order to store it in the modules first From there you can copy it to PC card as described in this section Transferring Methods Between LC Systems Methods can be transferred from one LC system to another using a PC card 1 Save the method you want to transfer onto a PC card See section Exchanging Methods With the PC Card on page 45 2 Remove the PC card from the control module 3 Insert the PC card into the control module of the other LC system If this system does not have a control module connected use any available control module 4 Restart the control module using the Restart function via the m menu key available from the main screens 5 Load the method from the PC card See section Exchanging Methods With the PC Card on page 45 46 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Time Programming To time program selected settings during the analysis you can create a timetable Using the Timetable screen you can create a time based program that will automatically control the pump detector column compartment and external contacts In some cases the settings will change instantaneously from the initial value
93. ries Handheld Control Module Users s Guide Using the Column Compartment 8 Tracking Column Compartment History 1 Select the Records button F2 in the System screen 2 Select Col Comp from the list 3 Press the System or Maint Log button F4 to display the logbook 1200 Series Handheld Control Module Users s Guide 109 8 Using the Column Compartment Tracking Column ID History 1 Select the Configure button F4 in the System screen 2 Select Column Comp from the list 3 Press Enter to enter the Column Compartment Configuration screen 4 Press the Column ID button F2 to enter the Column ID screen If no column tag is sensed the parameter entry fields are not active the left right tag sign is crossed out and the More button is unavailable By selecting the More button F1 you can enter values and check a variety of features for the installed column For example the maximum pressure allowed and the maximum recommended temperature You can check the number of injections that have been made on the column 110 1200 Series Handheld Control Module Users s Guide Using the Column Compartment 8 Resetting the Column Compartment Select the Settings button F1 in the Analysis screen Select Column Comp from the menu PressEnter Select the Default button F7 to reset the detector settings to their default values FP WwW N 1200 Series Handheld Control Module Users s Guide 111 8 Using the Column Comp
94. rol module method or sequence In this case the pre fix and file name counter in the Single Sample Info section of the Agilent ChemStation must be enabled protocol mode only e Ifthe control module starts an analysis the Agilent ChemStation is the slave monitor system In general however it is not recommended to run both the Agilent ChemStation and the Control Module at the same time Since the Agilent ChemStation offers a wider variety of controls over the LC Series system and handling it is much more comfortable it should be preferred over the Control Module Since problems in diagnosis and verification may occur in some configurations the following restrictions apply 1200 Series Handheld Control Module Users s Guide 61 2 Working with the Control Module Restrictions If a parameter window is open for parameter entry on the Agilent ChemStation this specific entry field is disabled on the control module If an analysis is running with the control module the Agilent ChemStation should not be turned on or rebooted If the Agilent ChemStation starts an analysis the control module is the slave monitor system Parameter changes to a method will be identified on the other user interface as modification The control module and the Agilent ChemStation have a different method handling Agilent ChemStation method can have more information than the method on the control module e g additional DAD parameters that are only accessibl
95. rom one LC system to another use a PC card 1200 Series Handheld Control Module Users s Guide Working with the Control Module 2 Deleting a Method Select the Method button F3 in the Analysis screen Select Module from the menu Select the method from the method list Select the Delete button F6 oF Ww N Choose Selected Method from the pop up menu If you want to delete all methods choose All Methods Press Enter 7 Select Yes to confirm the deletion by pressing the Enter key Exchanging Methods With the PC Card To store and retrieve methods from PC card you can use a comfortable screen that allows easy copying to and from PC card 1 Insert the PC card into the control module as described in Inserting and Removing PC cards on page 40 Methods from a freshly installed PC card are not available Restart the control module using the Restart function via the m menu key from the main screens 2 Select the Method button F3 in the Analysis or Samples screen 3 Select the PC card button F2 Use the Initialize button F1 available in this screen in order to initialize a pre formatted PC card for use with the control module This has to take place prior to first use in the control module Be aware that all data on the PC card will be lost 4 Use the Selection and Direction keys to navigate within and between the method list boxes 5 Use the Copy gt gt and Copy lt lt buttons F7 F8 to co
96. rs 6 Press the Done button F6 1200 Series Handheld Control Module Users s Guide 99 7 Using the Detectors Configuring the Analog Channel Output 100 1200 Series Handheld Control Module Users s Guide Agilent 1200 Series Handheld Control Module User s Guide 8 Using the Column Compartment Turning the Column Compartment On and Off 102 Entering Settings 103 Configuring the Column Compartment 104 Configuring the Column ID Module 105 Selecting Separated or Combined Mode 106 Selecting the Column Switching Valve optional 107 Troubleshooting the Column Compartment 108 Tracking Column Compartment History 109 Tracking Column ID History 110 Resetting the Column Compartment 111 phe Agilent Technologies 101 8 Using the Column Compartment Turning the Column Compartment On and Off 102 You can turn the column compartment on and off by using the 0n Off button F7 in the Analysis screen 1 Enter the Analysis screen 2 Select the On Off button F7 3 Select the Temp button F7 The same can be achieved through the Settings or Control buttons F1 in the Analysis or Systems screens 1200 Series Handheld Control Module Users s Guide Using the Column Compartment 8 Entering Settings The temperature can be entered in the Analysis screen The temperature for left and or right heater can be entered in the Column Compartment Settings screen This screen is accessed by selecting the Settings button F1 in
97. s To compensate for this effect you can use the pump compressibility setting to maintain a uniform and accurate flow regardless of the system pressure The compressibility setting can be accessed by using the Pump Settings button F1 in the Analysis screen Table 3 lists compressibility values for common solvents used in LC Table 3 Compressibility Values for Common LC Solvents Solvent Compressibility 1076 per bar Acetone 126 Acetonitrile 115 Benzene 95 Carbon tetrachloride 110 Chloroform 100 Cyclohexane 118 Ethanol 114 Ethyl acetate 104 Heptane 120 Hexane 150 Isobutanol 100 lsopropanol 100 Methanol 120 1 Propanol 100 Toluene 87 Water 46 1200 Series Handheld Control Module Users s Guide Using the Pump 3 When the compressibility setting is set to Off the pump makes no compensation for the compressibility of the mobile phase For each particular compressibility value the piston stroke distance piston moves and the speed at which the piston moves are adjusted accordingly compensating for the solvent compressibility For a mixture of solvents we recommend that you choose the compressibility value of the solvent that is present in the highest amount 1200 Series Handheld Control Module Users s Guide 67 3 Using the Pump Adjusting Stroke Volume The stroke volume defines the volume of mobile phase which is displaced by one stroke of pump piston 1 You can set the stroke volume to AUTO automatic or
98. s a quick and convenient way to look up information about a task you are doing or a feature or screen you would like to know more about The online information system is context sensitive and provides information related to the current topic You can access the online information system by using the i info key on the control module keyboard Some words are underlined which indicates available further information By pressing the Enter key you can display screens providing more specific information about the underlined word Some words have a dotted underline which indicates there is an available definition of the word By pressing Enter you can display a small overlay screen with information You can remove this overlay screen by pressing Enter To exit from the online information system press Esc e To find out what other information topics are available select the Search button F8 From there you can choose between Contents and Index See ORE olka oiu o ooie Tabl Or Settings Timetable Program Method Sequence Samples Plot Status System Control Configure Tests Records Software Structure Figure 2 Online Information System Table of Contents e To access further screens containing related information on the currently selected screen select the Related button F7 e To move back to the previous information screen select the Previous button F6 1200 Series Handheld Control Module Users s Guide 1
99. s is possible using the Interfaces button F1 available from the Configure button F2 in the System screen This is handled individually for each module since some interfaces are only available from certain modules depending on installation For further information on interfaces see the corresponding sections in the modules reference manuals APG Remote Via the 9 pin APG remote connector included in all modules the system can communicate with external devices in order to synchronize the analyses This is necessary when an external device needs some time in order to get ready for a new analysis and thus transmitting of a start request is required see also Synchronizing Analyses with External Devices on page 144 for details on sequence modes Detailed descriptions of the APG Remote connector are available in the modules reference manuals Among the available signals are Power On This signal is active as soon as all modules connected to the system are switched on Shut Down When the system has a serious problem e g a leak occurs this alerts all modules to stop relevant operation in order to reduce safety risks 1200 Series Handheld Control Module Users s Guide 57 2 58 Working with the Control Module Stop This signal asks all modules to reach the ready state as soon as possible It works only during the analytical run controlled by the stoptime setting and causes the system to begin counting down
100. sing the Configure button F2 in the System screen and then selecting LC System In the following Config screen press the Printer button F1 to open the respective dialog In this dialog you can choose the printer model and the module it is connected to Define a page layout including paper size a banner text and the margins using the Page button F8 Use the Serial button F7 to enter settings for the RS 232 connection such as baudrate bits and parity This setting can be made individually for each module in the respective configuration settings see Connecting External Devices on page 57 If the setup is complete you may print a test page using the corresponding button In many cases a print function is provided via the context menu to be accessed with the m menu key e g from the vial range entry fields in the Analysis screen from the Samples screen and from the online information system Print Plot In the Plot screen you can create a screen hard copy using the m menu key and selecting Print Plot from the context menu The printout will also include a legend and the date and time 1200 Series Handheld Control Module Users s Guide 55 2 56 Working with the Control Module Print Logbooks Using the m menu key to show the context menu in the System screen allows you to choose the Print Logbook function In the following dialog you can also configure the printer using the Setup button F8 The Spooler button
101. tem or each module individually Setting Date and Time You can set the date and time using the context menu m key while the System screen is active Choose the Date amp Time option and press Enter Press Setup button F6 to change the settings Press Done F6 to confirm the new entries Alternatively choose Configure and select LC System Press Date amp Time F4 When date and time are changed in the control module the settings are automatically stored in all the connected modules The date and time are backed up by a battery in each module The control module does not have a clock of its own Upon startup the modules synchronize their internal clocks The clocks can also be synchronized by an external chromatographic data system like the Agilent ChemStation Setting Display Contrast From the System screen choose Configure and select LC System Press Display and then use the Selection keys to enter values between 0 and 31 to adjust the display contrast according to your personal and location requirements Then press Done 1200 Series Handheld Control Module Users s Guide 37 2 38 Working with the Control Module Adjusting View Pressing the m key in the Analysis screen and selecting Setup view allows to select the modules that will be displayed in the Analysis screen Choosing this option enables you to select the modules present in the Analysis screen By pressing the Remove Add buttons F7 F8 you can move the modul
102. the Analysis screen Additional settings are accessed by selecting the More button F1 under Column Compartment Settings 1200 Series Handheld Control Module Users s Guide 103 8 Using the Column Compartment Configuring the Column Compartment 1 Select the Configure button F2 in the System screen 2 Select Column Comp from the list 3 PressEnter You can now configure the leak detection mode temperature on at power on the interfaces and the column identification module 104 1200 Series Handheld Control Module Users s Guide Using the Column Compartment 8 Configuring the Column ID Module oa FF Ww N m Select the Configure button F2 in the System screen Select Column Comp from the list Press Enter to enter the Column Compartment Configuration screen Press the Column ID button F4 to enter Column ID screen To toggle between left and right column press the Left Right button F8 If no column tag is sensed the record fields are not active and the left right tag sign in the upper right corner or the window is crossed out Enter your column data into the fields as required Additional fields are available by pressing the More button F1 Pressing the Write button F7 will transfer the information into the column tag Pressing the Right button F8 will show the information fields of the right column tag if column is installed The column ID information is updated as soon as a column with ID tag is
103. to the column Load Inject Figure 15 Valve Positions Valve Positions 1to6 valve ports 7 inlet from pump 8 outlet to column 9 needle port 10 vents 11 sample loop 84 1200 Series Handheld Control Module Users s Guide Using the Manual Injection Valve 6 Making An Injection The sample loop can be either completely or partially filled This depends on the amount of sample you have Completely Filling the Sample Loop This is the conventional method in which an excess of sample is used to fill the sample loop completely The volume of the loop determines the injection volume 1 Fill syringe with sample 2 Move valve to LOAD position 3 Insert needle of syringe into needle port until needle touches stator face Do not press too hard 4 Slowly inject sample Leave syringe in position and move valve to INJECT position Remove syringe 1200 Series Handheld Control Module Users s Guide 85 6 Using the Manual Injection Valve Partially Filling the Sample Loop Use this method when only small quantities of sample are available In this method the syringe determines the injection volume 1 With valve in INJECT position use needle port cleaner to flush needle port with about 1 ml of mobile phase this will reduce residual contamination from previous injection 2 Move valve to LOAD position 3 Fill syringe with required volume of sample not more than half of loop volume 4 Insert need
104. tries 22 Press the Esc key until you are in the Analysis screen Use Enter to store timetable lines Use Done when all lines have been entered By pressing the Esc key you return to the previous screen 1200 Series Handheld Control Module Users s Guide 127 10 Running a Gradient Analysis Saving Settings in a Method 1 Select the Method button F3 in the Analysis screen 2 Select the Save As button F8 3 Enter the method name as GRAD using the selection keys also see Specifying a Method Name on page 42 4 Press the Done button F6 to save the method 5 Press ESC to return to the Analysis screen 128 1200 Series Handheld Control Module Users s Guide Running a Gradient Analysis 10 Observing the Chromatogram 1 Select the Plot button F6 in the Analysis screen 2 Press the Select button F6 3 Choose a Signal from the Available Signals list box 4 Press Enter You can choose several signals at a time The plot function will display all signals that are shown in the Selected Signals list box Use the selection keys to navigate within the list boxes and press the Enter key to move Signals from one box to the other Select the Done button F6 to display the chromatogram Press Esc to go back to the Analysis screen Press the Start button F8 Select OK to confirm the vial range and injection number and press Enter to start the analysis on al 1200 Series Handheld Control Module Users s Guide 12
105. trol module The G1323A version allows to control only a limited set of Agilent HPLC modules see Table 1 The G1323B version additionally controls a wide set of other Agilent HPLC modules see Table 1 There is no difference in the user interfaces or other functionality The Control Module G1323B does not control certain Agilent 1200 Modules the Binary Pump SL G1312B the Variable Wavelength Detector SL G1314B and the Thermostatted Column Compartment G1316B These require the Agilent 1200 Instant Pilot G4208A as controller or the Agilent ChemStation B 02 01 Table 1 Control Module Versions Version controls G1323B 1100 1200 module firmware revision A 06 xx B 01 xx and above Agilent 1100 1200 Isocratic G1310A Quaternary G1311A and Binary G1312A Firmware pump B 04 02 Agilent 1100 1200 Autosampler G1313A and Thermostatted Autosampler G1330A Agilent 1100 1200 Variable Wavelength Detector G1314A Agilent 1100 1200 Diode Array Detector G1315A B C Agilent 1100 1200 Thermostatted Column Compartment G1316A Agilent 1100 1200 Fluorescence Detector G1321A Agilent 1100 1200 Preparative Pump G1361A Agilent 1100 1200 Fraction Collector G1364 Agilent 1100 1200 Refractive Index Detector G1362A Agilent 1100 1200 Multiple Wavelength Detector G1365A B Agilent 1100 1200 Well plate Autosampler G1367A Agilent 1100 1200 Capillary Pump G1376A Agilent 1100 1200 Micro Well plate Autosampler G1377A G1368A Agilent 1100 1200 Dual
106. turn the lamp on and off use the On Off button F7 in the Analysis screen 1 Enter the Analysis screen 2 Select the On Off button F7 3 Select the Lamp button F6 The same can be achieved by using the On Off button F8 in the Detector Settings or Control screen available through the Analysis or System screens When the lamp is turned on a lamp ignition routine is started For more information Lamp Ignition Routine VWD only on page 98 1200 Series Handheld Control Module Users s Guide Using the Detectors 7 Entering Settings All detector settings can be entered in the Detector Settings screen You can access this screen by selecting the Settings button F1 in the Analysis screen and choosing the appropriate detector Commonly used settings such as wavelength can be set directly in the Analysis screen Diode Array Detector The wavelength for signal A can be entered in the Analysis screen The sample wavelength reference wavelength bandwidth peakwidth and slit width can be entered in the DA Detector Settings screen This screen is accessed by selecting the Settings button F1 in the Analysis screen Additional entries autobalance etc and the spectrum settings range threshold are accessed by selecting the More button F1 under DA Detector Settings Variable Wavelength Detector Settings for this detector include the wavelength peakwidth and signal polarity Pressing the More button F1 and choosing
107. u have previously created called e g METH1 METH2 and METHS For example METH1 and METH2 have the same analytical settings but differ in the injection volume and stoptime values METHS uses a different temperature and requires a wait time of 30 minutes for the LC system to equilibrate This way of combining methods is called Sequence e The first 20 vials are analyzed using METH1 with one injection per vial e the next 20 vials are analyzed using METH2 with two injections per vial e the last 10 vials are analyzed using METH3 with three injections per vial The vials are located in positions 1 to 50 of the autosampler tray The example assumes that the sequence table is empty If the sequence table is not empty use the All Lines item accessed by pressing the Delete button F6 1 Select the Sequence F4 in the Analysis screen 2 For sequence line 1 select the Insert button F7 and enter Vial Range 1 to 20 lnj 1 Inj Volume Default Method METH1 3 VSelect the Enter button to accept entries 4 For sequence line 2 enter Vial Range 21 to 40 lnj 2 Inj Volume Default Method METH2 1200 Series Handheld Control Module Users s Guide 135 11 Running Multiple Vial Analyses 5 Select the Enter button to accept entries For sequence line 3 enter Vial Range 41 to 50 lnj 3 Inj Volume Default Method METH3 Wait 30 minutes 7 Select the Done button F6 to enter sequence line 3 settings and complete the sequence
108. utton F4 in the System screen 2 Select Pump from the list 3 Press Enter You can now check the amount of solvent the pump has delivered liquimeter and the wear count The liquimeter displays the total volume of solvent that the pump has delivered since it was last reset You can use the liquimeter limit to set up a preventive maintenance schedule for the pump For example make a note of the total number of liters pumped when you change the piston seals This volume is a benchmark reflecting the lifetime of the seals for your solvents and application When the limit is exceeded an early maintenance feedback message will appear indicating it is time to change the seals Changing the seals in advance will prevent you having to repeat analyses due to leaking seals The wear count displays a calculated value indicating the wear of the pump seals You can also use the seal wear limit to set up a preventive maintenance schedule for changing the pump seals when the limit is exceeded 1200 Series Handheld Control Module Users s Guide 69 3 Using the Pump Resetting the Pump FPF O N Select the Control button F1 in the System screen Select Pump from the menu Press Enter Select the Reset button F7 to stop the pump operation and perform a hardware initialization Resetting the Pump Settings 70 A WO N Select the Settings button F1 in the Analysis screen Select Pump from the menu Press Enter Select the
109. ysis time for operations that require a high sample throughput The optimization modes can be chosen from the Analysis screen 1 Press the Settings button F1 2 Choose the Autosampler from the list 3 Select the More button F1 4 Choose Optimization from the list 5 In the appearing window the optimization mode can be chosen from the list box as well as a delay time If you choose the Prefetch Sample Vial option the next vial for multiple injections the same vial will be moved close to the injection port after the specified elapsed runtime The injection cycle will not be started This procedure reduces the total injection time without interfering with the current run By choosing the Overlap Injection Cycle option the next vial will be placed in the injection port after the selected elapsed runtime The following restrictions apply when using the Overlap option e The elapsed runtime entry before the sample is processed must not interfere with the current running analysis e Overlapping works only for a given vial range e g within one sequence line e The first run for a new vial range is done without overlap e Injector programs using valve switching commands must not be executed when overlapping is selected They will fail with an error message Since all injector programs created with the Agilent ChemStation require such commands in order to function correctly none of them will work in the overlap mode The s

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