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Clarus 600/680 GC User's Guide

1. 7 B To The T Amplifier Bead Transformer i Assembly COEGI le Lt fi 2i l Bead C gt uae Air Flame In Jet Hydrogen In Column Connector OO Figure 4 26 Nitrogen Phosphorus Detector NPD Setting Up a NPD To set up a NPD using PPC modules set the hydrogen and air flow as described below then condition the bead Set the Hydrogen Flow and Air Flow for PPC The pneumatics consists of PPC modules where the plasma gases are adjusted and set from the Clarus GC keyboard The PPC modules are calibrated at the factory to set the flows for an analysis follow the procedure below 1 Turn on the hydrogen at the tank and adjust the line pressure to 60 90 psig 2 Turn on the air at the source and adjust the pressure to 70 90 psig 4 45 Setting Up the Detectors 3 Inthe System Status screen touch the NPD button The following screen appears B NPD Events a A Torr oc Heater Off m temp 0 00 mv B POCO Owen 25 C Aten 4 g Method Editor Range poo E PERN Log Gas flow tril Sel Ar g 0 He 0 0 0 0 Ready start O w 3 4 To set the air and hydrogen touch the Tools button in NPD screen and touch Configuration from the displayed menu The Configuration displays 4 46 Clarus 600 680 User s Guide Configuraton Sep Preumalics Relays
2. Figure 6 2 Location of a restrictor on the PPC module 6 50 Clarus 600 680 GC User s Guide To zero the carrier and detector gases 1 From the PPC screen touch the PPC Configure button To proceed touch OK on the Caution message Configuration PPG Caulon To avoid damaging he PPG syster do not modify he setings unless Ine hardware configuration has changed Do you want bo proceed Select the channel you need in this example Channel A tab is selected Touch the Zero button Select any of the other tabs to Zero another Channel carrier gas detector or Aux 6 51 Using the Tools Menu Configure PPC Devices Carrier Detector ALK Channel 4 Channel B PPG 1 Garr Flow om _ _ _ Gas He Restictor a 9 Zero Calibrate PPG 11 Split Cr ferro Ready i OK Cancel If the value shown on the top line of the display is outside the range of 3 psi first verify that the supply gas pressure has bled to 0 If the supply gas pressure has bled to 0 and the value is still outside the range of 3 psi contact your local PerkinElmer Service Engineer CAUTION The module identifier 1A is defined as follows The number 1 12 indicates the specific PPC module The letter A or B indicates the pressure transducer within that module The flow CAUTION controller has two pressure transducers per module whereas the other modules
3. ral oo wo e 17 01 i Glose Disable Filler 50 Gas Flow SetPoint Actual Arf 0 o mmn Hef oo oo momin Recorder _ ntegrabor Ofset b ri a Ready Mar 4 4 OK Cancel 5 Inthe NPD Configuration screen set the Air to 450 mL min and the Hydrogen flow to 45 mL min by touching the field and using the up and down arrow or keypad al T buttons 4 47 Setting Up the Detectors 6 Set the Filter to 200 The default setting for the filter is 200 milliseconds If you want to improve the signal to noise change the setting to 800 milliseconds however the noise improves but the peak shapes broaden If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase 7 When all the settings are appropriate for your analysis touch OK The NPD tab screen will be now displayed with the changes you made in the configuration screen NOTE The flows listed in the above procedures for hydrogen and air are optimum for both capillary and packed column flow rates The optimum flow provides the best sensitivity signal to noise selectivity and bead life Any changes to these flows will affect all of these parameters Also when using capillary columns makeup gas is not required NPD Bead Activation Procedure Packed Column Setup Disconnect column and cap the oven end of the detector The recommended D
4. B Pkd wen B PID Events i 100 C Heater Off temp GOO mY 100 C Alen je AuloZero Range 20 Qutub Recorder ofset Yo Filter 200 mg Gas flow iml set Actual Make Up 10 1 Ready 17 0 Tools 5 Allow the system to stabilize until the background signal is steady Optimize the Lamp Intensity 1 As shown in the screen above go to the Atten Attenuation field Touch the downward arrow and select an attenuation value of 32 2 Make sure AutoZero is off 3 Locate the lamp intensity control knob see Figure 4 14 and slowly turn it clockwise increasing the signal until the background signal on your integrator or recorder whichever is configured suddenly decreases 4 42 NOTE Clarus 600 680 User s Guide Detector Output Signal lt lt lt lt lt _ _ _ lt Optimum x Control Ss Setting 8 ER Z Best Setting g Q Lamp Intensity Control Setting Figure 4 17 A typical intensity signal 4 Repeat steps 2 through 4 at different attenuations using the highest lamp intensity that corresponds to the lowest background signal If optimizing the lamp intensity cannot be done easily using the above procedure increase the lamp intensity until the noise is between 1 and 1 5 of full scale at an attenuation of x8 Setting Up a NPD To avoid injury Do Not turn on the hydrogen gas unless a column is connected to th
5. 17 0 Tools x When completed touch OK to close the screen When a run is started the system uses the initial range of 1 for 2 minutes then switches to a range of 20 for the duration of the run When the run completes the system switches back to the initial value of 1 When completed touch OK to close the screen 4 77 Setting Up the Detectors Setting the TCD Current Filament Current When the detector is not in use the temperature and current CAUTION must De off 1 From the System Status screen touch the TCD button S Ready blar 4 start Tools x In the TCD tab page touch the Current field Current 40 mA and use 2 the drop down menu to change the value TCD range options are Off 40 80 120 and 160 maximum sensitivity and 40 80 120 or 160 A negative value reverses the polarity 4 78 Clarus 600 680 User s Guide B TCD Events co i OFF e Heater OF B Pkd Oven temp M ooo my C Alten mo EJ I AutoZero Current 40 2 MA uput Recorder 160 Ofset 5 Filler 200 ms 17 01 gaa Tools d The TCD range values corresponding to bridge current are shown below Table 4 3 Correlation Between Bridge Current and Range Bridge Current mA Range Entry Py I a S O o G A The initial setting is the range that is used at all times unless the polarity is changed with a timed event during a GC run ir I 4 7
6. 6 64 Clarus 600 680 GC User s Guide down field is inactive GC Tune 1s only available if it is downloaded A successful tune must be performed in order for GC tune to be enabled Only those channels for which a valid tune exists will be available on the drop down list The selection will be made from the external GC Tune software but the user may override this The actual temperature under the single point radio button 1s the time averaged actual oven temperature Allow the oven temperature to equilibrate for at least 30 minutes by setting the time in the Equilibrate field Press OK The displayed temperature will approach 100 00 C or the oven temperature you entered in step 4 and the thermometer readout will approach a value close to 100 00 C Enter the Required Offset Value l After the temperature has stabilized subtract the thermometer reading from the actual oven temperature shown on the previous screen Using the plus and minus keys enter a value into the above screen then press OK For example if the thermometer reads 101 55 C and the oven temperature reads 100 10 C type a value of 1 45 C Remove the Thermometer Probe After temperature calibration is satisfactory l Open the oven door and allow the oven to cool until the fan stops 2 Remove the temperature probe 3 Fill in any hole left by the probe in the oven insulation 4 Replace the left side instrume
7. 25 C a m E AutoZera Current 40 gt mA Gutput Recorder Offset To Filter 200 mS gas flow tril set Actual Ref i i None a Ready 2700 EEE Tools ad The gas flows output offset and filter are shown above as reference fields and they cannot be changed in this screen lt 7 17 Setting up a Typical Analysis 7 Ifthe gas flows output offset and filter have to be changed touch the Tools button and touch Configuration from the drop down menu B Pkd Oven BTCD Events wE l OFF C Heater Ci temp 0 00 mY 25 C Aten 4 Method Editor Current 40 ma fe Event Log hiaintenance Configuration Gas flow mL ilies Sel Arta Ret 0 0 None a Ready ZU A lnjector Z e a p Run Sebp Pneumatics Relays a Ready 00 Close 7 18 8 9 10 Clarus 600 680 GC User s Guide Touch the TCD button and as shown in the screens below the Configuration screen will allow you to modify the gas flows output offset and filter fields as your application requires B LHE Disable Filter 200 e Deine Gas Sources SetPoint Actual Reference 0 0 m Linin Gas Flow uput Fecorder _ylhbegrator Ofset E Yo 2 00 OK cancel Once you have modified the Configuration screen touch OK and the new values will now be visible on the TCD tab screen If timed events have to be added or modified in the Active Method touch the E
8. Configure Injector A Type PSSI EJ Capillary Control Carrier Control On a Flow afset Auto Fixed ofset 1 00 mutmin HS Control 1701 FEE OK Cancel Now you can only pressure program your capillary injector If you wish to program the Capillary control for more than just pressure skip to step 9 4 Under Flow Offset select either the Auto or Fixed 3 30 Configure Injector A Type PSSI g Capillary Control Carrier Control Pressure Configure Injector A Type FSS l Capillary Control Carrier Control Pressure g Flow Ofset amp uo Fixed Leak Limit 0 0 mLinin Flow Offset Auto wy Fixed Ofset 1 00 mbimin H5 Control HE control hlar 4 17 0 aa OK Cancel 22 OK Cancel The Auto mode is the preferred mode of operation If you want to shorten the overall run time at the expense of some area precision then use the Fixed mode Clarus 600 680 User s Guide We recommend that if you are operating with a split vent flow of 50 mL min or less select the Auto mode Before each injection in the Auto mode the system briefly closes the split vent and measures the total flow With the split vent off this flow is the column flow plus the septum purge flow The septum purge flow is maintained due to a mechanical restrictor and the split vent flow and split ratio are maintained for each injection In the Fixed mode you enter an offset value whic
9. Four tungsten rhenium filaments are connected in a bridge circuit two in each channel The TCD is set up with the same amount of carrier gas flowing through both channels The presence of a sample component in the carrier gas flowing through the analytical channel changes the resistance of the filaments in that channel This unbalances the bridge and produces a signal proportional to the amount of sample Reference Out ia Reference In Carrier Out Carrier In Figure 4 10 Thermal Conductivity Detector TCD 4 28 NOTE Clarus 600 680 User s Guide TCD Setup Setting up a TCD requires that you equalize carrier gas flows through both channels followed by balancing the current through the two filaments The TCD is nondestructive and can be used in series with other detectors The TCD is a universal detector that is concentration sensitive The TCD sensitivity depends on the filament current component concentrations and the difference in thermal conductivity between the carrier gas and the component To prevent TCD filament damage shut off the filament current before disconnecting columns or turning off gas flows To set up a TCD read the TCD setup summary then follow the steps TCD Setup Summary To set up a TCD e Ensure that a column is installed e Turn on the ov
10. Alpha Num Accent Katakana ee A Pe jit jis jie E E E Pm E E E e e O ee Ook cancel M Enter the password and touch OK or touch the x close symbol or Cancel to close the keypad and continue setup Language drop down menu English En Rae French Fr spanish 5p talian It German Ge Japanese Jpn w Touch the language option The list box closes and the selected language is immediately displayed throughout the application Brightness field The field is selected Brightness 75 z 6 29 Using the Tools Menu Use the up and down arrow or keypad nd aj za3 buttons to increment the brightness values up or down The settings take effect immediately Date Time Set Date Time 1 Touch the Date Time button to display the Time and Date screen 2 To set the Date and Time highlight the field then use the up and down arrow or keypad al 22 buttons to enter the values Time and Date i r l Time 17 01 Date Sep H 2 2006 Ready Sen 8 vl aI gag OK Cancel BEE BEE BEE 6 30 Clarus 600 680 GC User s Guide Startup 1 Touch the Startup button to display the Startup screen 2 Select the Method field then using the arrow button e select your desired method Time 08 50 Pr Pe Repeat Once J Always N FEF aK Cancel 3 To set the Date and Time highlight the field then use the up and down arrow or keypad
11. Her Edit Delete Stabs change sepium Q of 10 days Ready 17 0 T ai Close When done touch the Close button When the Count value equals the number assigned to the task a dialog box displays the reminder Malntenance Task Reminder Clean the Synnge Plunger Count 500 injections OK 8 Touch OK to close the reminder Using the Tools Menu Configuration To access Configuration from the System Status screen touch the Tools menu and select Configuration The Configuration screen appears This section describes how to configure and then shows the various GC configuration screens Configuration Method Editor Event Log d Maintenance A Injector Run Selp Pneumatics Relays Ready 12 00 34 Tools x Close Injectors Deconfiguring and Configuring Injectors Occasions may arise when you may not be using one of the injectors for an extended period of time Instead of turning off the injector heater you may find it more convenient to deconfigure the unused injector When you do this the injector temperature screen for the deconfigured injector will not appear in the method Every Clarus GC has been configured at the factory for the specific injector s that have been installed You can check the injector configuration of your Clarus GC from the Configuration Mode If one of the detectors has been deconfigured analog data from the remaining detector will be route
12. PID screen and then touch Configuration from the drop down menu Clarus 600 680 User s Guide This displays the PID Configuration screen Disable Fiter 200 Gas Flow SetPoint Actual blake up 10 1 rniLirnin dupult Fecorder ylnteqrator oftset E Yo 17 01 OK Cancel 3 Inthe PID Configuration screen set the Make Up gas line pressures to 60 90 psig by using the up and down arrow or keypad nd aj 22 buttons 4 As shown in the example above use the up and down arrows ma to set the Filter to 200 The default setting for the Filter is 200 milliseconds If you want to improve the signal to noise change the setting to 800 milliseconds however the noise improves but the peak shapes broaden If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase 5 Use the up and down arrow or keypad al 22 buttons to set the Offset to 5 6 When all the settings are appropriate for your analysis touch OK The PID screen will now display the changes you made in the Configuration screen Turn on the UV lamp 1 Lift the detector cover to expose the PID see Figure 4 14 4 41 Setting Up the Detectors 2 Turn the lamp intensity control knob fully counterclockwise 3 Turn the UV lamp switch ON 4 From the PID Tab make sure that AutoZero is off the box is not checked If it is On touch the field to remove the check mark
13. To increase the bead life turn off the bead if the NPD is not continually in use When you turn off the bead keep the detector temperature hydrogen flow and air flow set to operating conditions If the column remains connected to the injector and detector in the oven make sure the carrier gas is flowing through the column If the column is disconnected from the detector make sure the Swagelok cap is installed on the NPD fitting Prior to using the NPD adjust the bead background to the same millivolt setting that you were using Run your standards to determine if the NPD bead 1s responding at a level of sensitivity equal to the previous run If not then reactivate the NPD bead To reactivate a NPD bead follow the activation procedure above Operating Notes The bead is operated as a conventional NPD bead following these instructions will increase the bead lifetime Baseline Set the baseline to a level of between 0 4 0 5 A lower baseline will help to extend bead lifetime Studies have shown that the signal to noise will not be adversely affected by the lower baseline 4 53 Setting Up the Detectors Column bleed Material from the column can effect bead lifetime Keep the maximum oven temperature as low as possible for each application Between run operation If the NPD bead is not in use for a few days it is best to simply lower the potentiometer setting to 600 and maintain the detector temperature at 200 deg C or g
14. Enabled Disabled Type _ Autosampler anual Type _ Aubosampler anual Method Method 5 B Method Method 5 El 1 Select hlethiod Wait until Ready 1 Select Method Wait until Ready Injecton Countdown 2 Touch ihe start buton 2 Inject when you hear the final tone Injecton Countdown w Enable Injection Countdown v Enable Ready Mar 4 Not Ready 17 01 o jam mew ORELE Go to a temp prograrn step cancel 2 10 Clarus 600 680 GC User s Guide Stop Menu Stop Immediately Touching this button immediately stops the Active Method and closes the Stop Menu dialog Go to a temp program step Displays the Go to Temp dialog for you to select the step you wish to go to at this time Then press OK to activate the selected step Cancel Cancels this Stop Menu dialog and returns you to the Active Method Signal Button The Signal icon displays the graphic signal for the active method If the system 1s not running a baseline appears on the graph Channel B TCD Raw signal 50 C 0 0 psi O00 mw feet E m co Processed signal 260 a fero Display Auloero Ready 17 01 Start o 4 aa Tools The Signal screen displays the selected detector signal over a fixed time period 2 minutes with you selecting the scaling factor using the up and down arrow buttons The raw signal is unprocessed and can appear slightly larger than the processed sig
15. Events Heater Of LA Ea 256 C temp init Prograrn ij Carrier Gas O41 psi 6 00 mum 119 0 cmisec ces 0 0 emee wel init Split total flow 0 tri Liri E ratio fio Frogram a Ready Ea i start O w Fe Tools w A PSSI Oven AFID Events i OFF C Heater Off temp 0 00 mY 25 C Alten 20 Jv AutoZera Range f s Output Recorder Offset Filter 200 mS A FI t 010 my Gas flow mL See ee ee Set Actual Ar 0 0 6 H 00 0 0 Ignite Ready Ready 17 01 2 14 Clarus 600 680 GC User s Guide Oven Button Clicking the oven button provides access to the oven program settings and graph You can set to 10 program steps and up to 9 ramp rates Use the up and down scroll buttons to the right of the oven entries to view program steps 5 10 Method 5 CHC ALA A Pkd Oven A FID I Events Temp Time t it 75 1 00 mo al C o io 100 e D 4 150 too END w i o fka 150 E 2 660 oe ged ven Off Eee ee nee 0 YOO 14 00 E daw 3 Ready 17 01 a Equilibrating 0 06 min tal If both channels are running and the Oven is accessed from the Status screen it defaults to Channel A The oven program screen displays the same tabs and navigation icons as the injector and detector active method screens Aux Zone Buttons If a heated Aux Zone is configured pressing the Aux button displays a sc
16. Her Edit Delete 17 01 OK Cancel The last item accessed is automatically selected The tasks are listed in the order they were entered Use the scroll bar to display additional entries Each entry includes the name of the task and the Count at which it is set to prompt a reminder message The buttons below the list allow the user to add edit and delete tasks The current count field displays the value and type of interval associated with the selected item l Clarus 600 680 GC User s Guide To add an entry touch the New button The New Maintenance Task screen appears The interval options are Injections Hours and Days Nem haintenance Task Count Injections Ca Days J Hours Message pee 17 01 rer OK Cancel Touch the Count interval field and then enter a value using up and down arrow or keypad nd aj 22 buttons Enter a message by touching the Message field This displays the alphanumeric keypad for you to enter a message Using the Tools Menu Data Entry Alpha Num Accent Katakana ae ae es ee es E a a Se Bae e es eae _y _z __ i Type the message For example Change Septum Click OK to save the message Ifa maintenance task has already been assigned to the selected number a dialog box will ask if you want to overwrite it Clarus 600 680 GC User s Guide Maintenance 100 Days Change Septurni
17. PSSI M Capillary Contral Carrier Control Pressure H Carrier Control Pressure e Program _ Oventrack Program Oventrack Golurin Lengi 25 00 mo ILD 260 urm Split mode Flow Ofset Flow Offset Fow _ Rato Auto a Fixed Aubo J Fixed Ofset 166 mUtmin Leak Lirit 0a mbin T HE Control I vacuum Compensation HS Control M Vacuum Compensation Sep a Ready Mar 4 ok Cancel a FB o ce Cancer After selecting Program you must enter your column dimensions as described in the following steps 9 Use the up and down arrow or keypad nd aj s2a buttons to enter a Column Length which is measured in meters 10 Use the up and down arrow or keypad aj PEE Diameter which is measured in micrometers not millimeters buttons to enter an Internal 11 Then view the calculated linear gas velocity by selecting Utilities from the Tools menu and selecting the Column Flow Calc 3 32 Clarus 600 680 User s Guide Column Flow Cale column Length Calc P O Background Cormpert Sbopwabt Ready 17 01 The Column Carrier Gas Calculator screen appears Column Carrier Gas Calculator Column Parameters Length 25 om Temp 50 0 ge Diameter Ea uri Carrier Gas Inlet Press 50 psig Gas He l J Flow Rate 040 mLimin Split A velociby q253 cmi t c24 min suggested Velocity 20 To 40 cms autet Press Ambient A Vacuum _ oiher 147 psia Ready p
18. Please read NRC Regulation 10 C F R Section 20 402 and 20 403 Appendix I These describe your duties should the radioactive material Ni 63 in the ECD cell be lost stolen or released or should any person be exposed to radiation Other Requirements Regulation 10 C F R Section 31 5 see Appendix I does not permit you to abandon the ECD cell or export it It may not be transferred except to a person specifically licensed to receive it Within thirty days of such a transfer you must report to the Director of Nuclear Material Safety and Safeguards U S Nuclear Regulatory Commission Washington D C 20555 the name and address of the transferee However no report is needed to transfer a used or defective ECD cell to PerkinElmer in order to obtain a replacement You may transfer the ECD cell to another general licensee like yourself only when it remains at the same location to which it was shipped by PerkinElmer Give the transferee a copy of these instructions and the regulations in Appendix I and report to the commission as required in Regulation C F R Section 31 5 The ECD cell may only be removed for repair from the chromatograph if a specific license has been obtained THE W ARNING CELL SHOULD NEVER BE DISMANTLED 4 19 Setting Up the Detectors United Kingdom Regulations In the U K registration is required under the Radioactive Substances Act of 1960 for anyone keeping or using radioactive materials Applicatio
19. a E Close NOTE If you incorrectly enter a column length or internal diameter the resulting flow and pressure may be incorrect For example a 0 25 mm column may actually be 0 22 mm To verify that you have entered the correct values you can measure the linear gas velocity by injecting methane and calculating the linear gas velocity 3 33 Using the Active Method 3 34 column length cm Retention Time of Methane sec 12 Return back to the Configure Injector screen and select either a Flow or Ratio Split Mode Configure Injector A Type PSS gH M Capillary Control Carrier Control Pressure p Program J Oventack column bengh 25 00 m LO 260 um Split mode Flow J Ralo Flow Offset wub J Fixed Leak Limit 0 0 mbinin HS Control Vacuum Compensation hiar 4 aa OK Cancel If you select Flow you will enter a split flow in your method The software controls and calculates the split ratio If you select Ratio you enter the split ratio in your method The software controls the ratio and calculates the split flow 13 Select a Flow Offset of either Auto or Fixed 14 Clarus 600 680 User s Guide Configure Injector A Configure Injector A Type P551 M Capillary Control Type FSS M Capillary Control Carrier Control Pressure e Carrier Control Pressure Program J Oventrack Program 3 Ovwenkrack column Length 25 00 rn LD 260 urm Column Len
20. temp M 0 00 m 25 C are I gt fe AuloZero OupuE Recorder afset 5 Eis Filter 200 mS Gas fow iLi gel Actual hake Up Q 0 Ready har 4 EE aa BRE BBE I 190 c In the ECD page touch the temp field P and use the up and down arrow or keypad al 22 buttons to set an ECD temperature appropriate for the analysis to be run To turn the heater on or off just touch the Heater button SEES The message on the button will toggle to either on or off and will be visible on the screen 4 73 Setting Up the Detectors Setting the Range Setting the FID PID or NPD Range The initial FID PID or NPD range is set from the FID PID or NPD Range screen The example below uses FID but the following procedure can also be used for PID or NPD 1 From the System Status screen touch the FID button a this will bring you to the FID tab screen page AFPSSI Oven AFID Events iy il OFF C Heater f i temp 0 00 mv 25 C J Aulozero Ouput Recorder afset w Filler 200 mS Flameout O 10 rmi Gas fow iml Sel Acal A Ar H 0 0 o 0 Ignite 17 0 Tools x 20 2 To change the range touch the Range field ii Select a range from the drop down menu for the detector FID PID and NPD range options are 1 or 20 where is the most sensitive setting and 20 is 20 times ess sensitive The value that you enter will always be used unless you c
21. viscosity Contral 0 Solvent Pre titash Pre Inject 2 Fost Inject E Putrip pA Sample Rinse Before Ready EDI E OK Cancel 6 After you touch OK on the Autosampler Configuration screen the main autosampler screen will appear again Touch Start to begin the run Touch the Signal icon to get to the Signal screen 7 24 Clarus 600 680 GC User s Guide On the Signal screen you will be able to observe the peaks as they are coming out during the analysis If at any time you need to stop the analysis touch the Stop button Channel B TCD K G O00 fri AG gignal rr 100 aj al zero Display Aulo ero Ready Oct 12 e xa FR rosy 7 25 Setting up a Typical Analysis 7 26 Index A Abbreviations screen 1 6 About This Manual 1 3 Active Method editing 3 4 parameters editing 3 4 Attenuating detector signal 4 87 4 90 Auto ignition FID 4 9 Autosampler 7 22 using with TCD 3 63 4 35 vials waste amp wash 3 62 AutoSystem controlling 3 3 glossary 1 8 Aux Zone 2 31 B Background calibration options multi 6 75 off 6 75 once 6 75 Background compensation overview 6 75 Background Compensation 6 74 Balancing TCD bridge current 4 34 Bridge current range 4 33 Bridge current vs range 4 34 C Calibrating oven temperature 6 60 6 65 reference thermometer 6 60 Calibrating PPC module carrier gas 6 54 detector
22. 10 10 50 2 125 100 100 B TCD Events Time Fale mit 75 1 00 100 al 382 C o 100 too 50 3 126 i00 100 B Pkd F s 3 Go to Temp init j je a a4 35 OK iW we Running Rate 2 s iso io END Oven Off Ovetre 0 47 min a Running Time 2 Stop TE Tools EIN j i FE Ja 310 Cancel 1400 1 48 min Tools x s is ro E Over Off 1 22 min B Running Time 4 Stop 4 Tools 2 From this window touch the button for the temperature level that you want to hold Touch OK Modify the temperature on the Oven tab screen using the up and down arrow or keypad al screen 3 12 buttons When completed return to the system status Clarus 600 680 User s Guide The oven heats ballistically to the temperature value for oven Temp 2 and holds instead of executing the time associated with oven Temp 2 Oven 3 empo Oven 2 Temp pa ee intial Oven jen nee Time 7 Rare 7 Time 3 hial Time Figure 3 2 Oven Temperature Program for Rate 1 To hold the oven program at a specific time during or before a run use an oven HOLD timed event See the section on Timed Events 3 13 Using the Active Method Setting Injector Temperatures Packed Capillary Split Splitless Programmed On Column and Programmed Split Splitless The examples in this section were derived by editing the Active
23. 2 40 Configuration Screen Ta I Disable Fiter so S Gas Flow SetPoint Actual Air 450 4 mLimin He 45 0 45 riLitnin uput Recorder j Integrator Ofset 5 wo acti FEF OK Cancel FPD Clarus 600 680 GC User s Guide In the Flame Photometric Detector FPD the column effluent 1s mixed with hydrogen and then burned in air Light emitted from the flame passes through a lens a filter and to a photomultiplier tube which generates an electrical signal The Flame Photometric Detector is used for detecting sulfur phosphorus or tin compounds which produce chemiluminescent reactions with emissions at wavelengths characteristic of the S2 Sn and HPO species The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method A PSS Oven M ooo my 250 C Alten 2 fe Aulo ero w PRIT On id Linearizer Off Filler 200 m5 Ouhput Recorder FMT Voltage 10 0 Offset oo Gas flow inL set Actual Ar a 9 He Toi EE Ready 17 0 val z Tools hd Configuration Screen Disable Fiter 200 Unearize PRIT voltage 10 0 Gas Flow SetPoint Actual Air a J mLimin H TOD T5 m Linin uput Recorder _ Integrabor Ofset E oo 17 01 33 OK Cancel 2 41 Touch Screen Navigation Timed Events Events Tab A PSS Owen A FPD Events Tine Evert Value Aux
24. Autozero is On indicated by a check mark in the box the system will autozero the detector to the offset specified during configuration whenever the system becomes READY or when a run is started The example below uses the ECD detector but the following procedure can also all the detectors 1 Inthe System Status screen touch the ECD button 2 Inthe ECD Tab you will see the AutoZero field E meee To turn on the AutoZero touch the field and a check mark will appear 4 93 Setting Up the Detectors B Fkd Oven B ECD Ewents pa I OFF ta Healer Off temp O 000 my 25 C rE i fe Aulo ero uput Recorder afset a Filler 200 ns Gas fow mL gel Arual Make Up 9 g Ready 17 01 NOTE When Autozero is Off the output signal is never autozeroed 4 94 Using the 5 Method Editor Using the Method Editor Clarus 600 680 GC User s Guide Method Editor To access the Method Editor display the System Status screen From this screen touch the Tools button as shown above This displays the following options Using the Method Editor Method Editar To access Method Editor touch Tools menu and touch Event Log the first option Method Editor Maintenance The Method Editor screens are similar to the Active Configuration Method screens The differences are noted in this Utilities section Felease You can access and edit the first five methods The pete fift
25. He 0 0 Ready 3 To turn on the photomultiplier tube touch the Tools button in FPD tab screen and touch Configuration from the displayed menu This will bring you to the Configuration screen page Conhiguraton B Injector A Injechor ae oe i A a Run selip Prieurniaics Relays la Ready 17 01 close 4 67 Setting Up the Detectors 4 On this page touch the FPD button a to display the FPD Configuration page EO I Disable Filter 200 B Unearize r00 w Alr a0 4 mLinin H TBD T5 mimin uput Recorder j Integrator Offset 5 Fo har 4 OK Cancel 5 Inthe PMT Voltage field set the percentage see note below by using the up and down arrow or keypad aj z2 buttons This will turn on the photomultiplier tube NOTE The voltage to the photomultiplier tube has been set in the factory to approximately 70 You can change this setting from the Clarus GC touch screen You may want to change this setting as the photomultiplier tube ages and the signal diminishes The signal to noise ratio may vary with each photomultiplier tube therefore increasing the voltage may not increase the signal to noise ratio After installing a replacement photomultiplier tube the noise should be about 2 when the Clarus GC integrator output is set to attenuation 8 x8 and the Linearizer off See the Clarus 600 680 GC Customer Hardware and Service Guide Maintenance chapter for this proce
26. NOTE Jf you wish to conserve carrier gas set the initial flow to 0 3 49 Using the Active Method If you are using pressure pulse injection you must set the split flow on just prior to when the inlet pressure begins to drop to the operating setpoint CAUTION For example if the inlet pressure is programmed to start decreasing one minute after injection use a split flow event time of 0 98 minutes At the end of a run the split flow resets to the original setting Setting a Value of 50 mL min minimizes contamination by keeping the splitter on during cool down NOTE The timed event that you set up or valve settings that you make become part of the method The timed event is automatically saved if you are editing the Active Method NOTE When operating in the splitless mode the recommended measured flow out of the vent is 30 50 mL min when the split vent is ON 3 50 Clarus 600 680 User s Guide Contolling the Autosampler NOTE The autosampler will not respond to commands if the autosampler door is opened Only sample vials and syringes distributed by PerkinElmer should be used with the Clarus GCs Plungers are not interchangeable from syringe to syringe The autosampler contains three basic parts an autosampler tower a carousel and a sample tray see the following two figures The autosampler tower can contain either a 0 5 5 0 or 50 0 uL syringe Figure 3 9 View of the Clarus GC with autosampler towe
27. You are now able to select any of the options displayed in the menu Using the Tools Menu Method Editor To access Method Editor touch the Tools button and then touch the first option Method Editor For detailed Method Editor information see Chapter 4 Using the Method Editor in this guide A hdaintenance configuration Jiliies 6 4 Event Log Clarus 600 680 GC User s Guide To access Event Log from the System Status screen touch the Tools button and touch the second option in the list Event Log Event Log J Aulosampler Fun Run Report Se ee eee 0 10 Alten B ge hielo O20 Valve on bieta 0 20 Valve 4 Or Wethod 0 40 AuloZero B Of hielo 060 Aulofero B On Method 0 60 Range B 1 WIA Ready editable 17 0 Close In the Event Log screen you can select either the Autosampler or current Run log The list box displays the contents of the selected log The logs are not Using the Tools Menu Maintenance To access the Maintenance screen from the System Status screen touch the Tools button and then touch Maintenance The maintenance feature provides you with the ability to set up to eight task reminders For each item you can enter the name of the task and specify the condition that prompts the reminder When the criteria are met a dialog box displays the message Maintenance Mew Maintenance Task Court _ Injections 10 Days J Hours hlessage Change septurn al
28. illustration of an installed PID The optimum operating temperature for a photoionization detector is 250 C PIDs may be operated at 350 C for short periods of time with a subsequent loss in lamp life The PID is equipped with a glass lined inlet and exhaust that permits series operation with another detector Lj we P g Lamp ON OFF Switch Lamp Intensity j Control Figure 4 14 PID installed in the Detector 2 position PID Setup To set up a PID read the PID setup summary then follow the steps PID Setup Summary To set up a PID e Turn on the oven and the detector heaters e Adjust the make up gas 4 37 Setting Up the Detectors Adjust the make up gas flow if using a capillary column at flows of lt 10 mL min e Turn on the UV lamp e Optimize the lamp intensity Turn On the Oven and the Detector Heaters NOTE A PID can only be installed in the Detector 2 position rear 1 Close the oven door This turns on the oven heater 2 From the System Status screen touch the PID button 3 Inthe PID page touch the temp field one and use the up and down arrow or keypad al ssa buttons to add a PID temperature appropriate for the analysis to be run 4 38 4 NOTE Clarus 600 680 User s Guide If you require the heater on for your analysis just touch the heater button and it will toggle to heater on e hae B Pkd Oven B PID E a dog C
29. the example in the above screen will allow you to enter an inlet pressure and calculate the flow rate and velocity from this and the other entries Use the up and down arrow or keypad a 7 buttons to add the flow rates 5 Press the Split button and the next screen appears This screen allows you to calculate the split flow settings may The Close button on this second screen brings you back to the above screen 6 68 Clarus 600 680 GC User s Guide Column Flow Fate ost m Limin Spit Flow Rate 50 0 mLimin Column 1 0 220 UII Injector Liner 1 0 ao tirti Split Flow Kato 5 2 oplit Velocity Raio 0 25 ithe Close Column Flow Calc Main Screen Length This field is normally entered in meters 1 to 1000 in 1m increments The calculator should also support techniques such as PreVent and heart cutting etc and so shorter columns tubes should be supported If the value scrolls below 1m then the units should change to mm 1 to 1000 in 1mm increments The default value will be 30m For the calculation this value should be converted to cm Diameter Column diameter should be entered in um 1 to 1000um in lum increments The default will be 320um Value converted to cm for calculations Temp Normal GC oven temperature range in C 99 to 450 C in 1 C increments The default will be 50 C Value converted to K for calculations 6 69 Using the Tools Menu Name The name of the carr
30. 1 Bridge Current Range vs Max Detector Operating Temperature Bridge Current Range Recommended Operating Temperatures for the Following Detectors Up to 100 Do not Use 4 Do not Use 4 st z 4 33 Setting Up the Detectors The correlation between bridge current and range is in Table 4 2 Table 4 2 Correlation Between Bridge Current and Range Bridge Current mA Range Entry NOTE Entering a negative number reverses the detector polarity For examples of reversing the polarity see the Clarus 600 680 GC Customer Hardware and Service Guide Maintenance Chapter section Practical Hints Balance the Bridge 1 Inthe System Status Screen touch the Signal button m to display the Signal screen This will allow you to observe the signal as you adjust the potentiometer Method 5 CMC mD Channel E TOD RO G O00 pr Method 5 132 8 Signal gm T 55 E i Aus dus zero Display Auer a Ready 17 91 Feady 17 0 Lii rosy E lE easy F 4 34 4 5 Clarus 600 680 User s Guide Allow the system to stabilize for about 20 min then open the detector cover Locate the TCD Balancing Potentiometer see Figure 4 11 Adjust the potentiometer until the Autozero display reads between 0 0 and 20 0 mV Wait for drifting to stop as indicated by a constant reading on the display Reset the potentiometer to produce a reading between 0 0 and 20 0 mV Using a TCD with the Autosampler
31. 4 56 NOTE NOTE Clarus 600 680 User s Guide Setting Up the FPD To set up a FPD using PPC modules follow the steps below FPD Setup Summary To set up a FPD e Configure the linearizer and signal filter e Set the FPD temperature e Set the hydrogen flow and air flow for PPC e Turn on the photomultiplier tube e Ignite the flame Configure the Linearizer and Signal Filter The signal for sulfur is a function of the square of the sample quantity injected That is if twice as much sample is injected the response is quadrupled When the linearizer is turned on the software calculates the square root of the signal and sends that value to the integrator or recorder If Linearization is set to ON the Autozero function must be checked off on the FPD tab screen If Linearization is set to ON set the Clarus GC integrator attenuation to x64 If Linearization is set to OFF set the Clarus GC integrator attenuation to x8 1 From the System Status screen touch the FPD button 4 57 Setting Up the Detectors B FPD Events BPOCO Oven nS OFF ie Healer Off temp 0 00 mv 25 C Aten 4 e M Aulozero w PAT On m Linearizer Off Filler 200 mg uput Recorder PMT Voltage OFF 6 Offset i Gas flow tril set Actual Ar 0 Q He 0 0 0 0 Ready o Mard 4 58 Clarus 600 680 User s Guide 3 For Linearizer the default value is Off To change the value to O
32. 43 Using the Tools Menu Connect PPG Device Function Position carr Flow e B secondary Position spiten S 11 S aie Press OK to close the dialog box and implement the changes The Connect PPC Device screen appears Dialog Define Detector If Detector A is selected on the Connect PPC Device the dialog shown below pops up Since the PPC has yet to be configured the primary module is undefined and the secondary module entry is disabled Connect PPC Device Position Air Det Flow S fz al Position ra OK Cancel 6 44 Clarus 600 680 GC User s Guide Note that the dialog title bar contains the detector name and that the primary and secondary function boxes are now labeled with the default gases for this type of detector For a detector that only requires a single gas ECD PID and External the secondary module line is hidden The only valid option for a detector is a Detector flow module The following screen shows that once Detector flow has been selected the position combo box is recalculated and offers positions 3 and 4 Connect PPC Device PPC Define Detector A FID Position Air Det Flow f 3 Hydrogen Position Det Flow effe EEE OK Cancel Once Position 3 is assigned to the primary module however this location is no longer available for use with the secondary module Press OK to implement the changes and return to the co
33. Clarus 600 680 GC User s Guide Zero Display Button The Zero Display button offsets the current signal level to 5 f s d on the display Heated Zones The Status screen displays graphic icons to represent the devices installed in the system Ready Iro at tars v Each type of injector and detector is represented with a customized graphic as well as a text label Heated zone buttons display a status light indicator in the lower right corner The indicator lights for individual zones follow the same convention as the system status light that appears in the Status bar Steady green indicates that the zone is ready A red blinking light indicates that the zone is not ready Injector and Detector Buttons The screen is organized with Channel B devices above Channel A to reflect the position of the channels on top of the GC Injector and detector buttons display 2 13 Touch Screen Navigation the active method settings for each device Touching a device icon displays the selected screen as well as a row of tabs to allow easy access to the injector oven detector and events for that channel Touching the alternate channel icon on the top navigation bar displays the active screen and associated tabs for the other channel if it is installed and configured The active method screens include navigation icons on the title bar that allow you to access the same elements available from the Status screen Oven A FID
34. Healer Off temp 0 00 my 100 C ajen he gi AutoZero Fange 20 Output Recorder afset i Filler 200 ms Gas fow iiL gel Actual Make Up 10 Not React 17 01 Tools gt Adjust the Make up Gas Make up gas is required when using capillary columns at low flows 10 mL min or less Since a PID is concentration sensitive make up gas flow should be kept to a minimum to obtain the best peak shapes and sensitivity Use make up gas only if you are using a capillary column at flows of lt 10 mL min The following procedures describe how to adjust the make up gas using PPC pneumatics 4 39 Setting Up the Detectors l The PID flow module for make up gas is calibrated with helium gas at the factory You must recalibrate the PID flow module if CAUTION you are using a reference gas other than helium With the make up gas is set from the Clarus GC touch screen The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure B Pkd Oven B PID Events a i 100 C Healer Off temp 0 00 mY Method Edibor Event Log 100 C 16 AutoZero l Aten Maintenance Range 20 e Oulput Recorder Configuration Offset oo Utilities Filler 200 mS Gas flow mL Release Set Actual Fleset bake Up 10 Log Out Tool 2 To set the Make up and Reference gases touch the Tools button Tools gt in 4 40
35. NOTE Setting Up the Detectors If you want to switch between an FID and an ECD when using the same packed column injector use nitrogen as the carrier gas for both detectors Argon methane is not recommended for use with an FID because it produces a high background more noise and a wandering baseline To minimize detector contamination run the ECD hot at a temperature of at least 373 C You may experience high background readings when working with capillary columns The high background may be caused by liquid phase bleeding off the detector end of the column at a typical temperature of 375 C or higher In some cases the polyimide coating of the column may also cause a high background reading when using the ECD You can correct this situation by installing a glass lined receiver P N N6000968 The glass lined receiver terminates in a 1 16 inch fitting so that it can accept capillary columns with an i d of 530 microns or less If you suspect that the background is caused by column liquid phase bleeding install the glass lined receiver in the detector base Then insert the column end just beyond the ferrule and connect it to the receiver If you suspect that the background is caused by the polyimide insert the column through the glass lined receiver until it is flush with the end of the receiver Then insert the receiver into the detector base This shields the column from the make up gas flow ECD Set Up To set up an ECD r
36. PK ccises gscactestatetacecastuaeciataiadec ceca are A A 2 24 POC oaea E E E a titan 2 28 Capillary Cap lin Cor eiti E E 2 29 CVV o R EE EI he usta EEIE AA E E EIEE EE E EA EE tet 2 30 AUX ZONE eaea a a a n alte tan toere tat 2 31 NSTC CLOTS ipn ap sielts undon a a E Gon tyoohide N 2 32 PDair eee 2 32 TE Deraan E ia ee oe ee eee 2 36 GB ervey nnn ere ree er arte e nr ys eer rte Mere ter er aro enter rey ee re meron err erent rey 2 37 IPI cstttiesc ssa tbat Danet a actin ct oe aces Ueaehs a dee Donan acted eect Nenes ae dae onan eek ated eure eae oe ade onan ecee 2 39 NPD ceenscsusiceaap adda senasuensn E O 2 40 FED Saepaeeeneaee E vest ret aer re E E etm eer a nr res te Stentor re ent ee e 2 41 TEE VEM aaa ODE eens eR AoE RSIS ere MES E 2 42 iii Eyo 21 2 ee eee an ee aI Bn RE RED ONCE OORT ORSON NOT ER ORE OR OP SD OEE EMT R REINO Me Sen OMEN OEE EE 2 42 Mime Events Tal essa octtsvicaenaapnnsatauedaantsachased seaanee SaannasaYeasiaad veep daetstiacaaaenawhttalaintes 2 43 Usme The A Cty eV COO ia isisisi aeia 3 1 OVEN IE W css a sais dacet aa es kaaatod sat han pea adsndeons at sie a Gane manats 3 3 F Gite The ACO 6 MEMO acetates serrata E aaa E NS 3 4 Getting Ready to Edit the Active Method cccccccecccccecceeeeeeececeeeeeeeeeeeeeeeeeeeees 3 5 Setting Up Oven and Inlet Temperature Programs ccccccccccccccceeceeeeceeeeeeeeeeeeeeeeeeeees 3 6 Configuring the Equilibration Time Init ccccccccccceeeeeeeeeeee
37. Run button provides roe screen will displav a baseline access to the Autosampler and Manual Inject settings Channel B appears above The Icon buttons provide quick Channel A to emulate the access to all configured areas of the instrument An indicator d t f the GC ea eae s light shows the ready not ready status of each heated zone The Start button appears so you can start or stop a run FID The status bar displays the EE 3 f Aux overall ready not ready status Ready 1701 as well as text messages and the real time clock date am Tas x The bottom bar displays the Tools pop up menu When the system is running the Stop button also appears 2 5 Touch Screen Navigation Tabs Some of the active method screens include tabs to allow you to switch views associated with a specific channel Navigation Bar A Tabs Active Navigation Bar B Tabs Active amp Ha ke Defauk Method y m A P55 Oven A FID Events A Pkd Oven B TCD Events Non Configured Devices If a device is installed but not configured or configured as None both the graphic and light are grayed out Touching the button prompts the following dialog box Non Configured Device This device is not configured Close Clarus 600 680 GC User s Guide The following screen capture shows the drop down list on the injector Configuration screen used to set a device to None Method 5 Configure I
38. The parameter values used in the example are shown below 100 Cimin Inj Temp 2 250 C inj Time 2 Inj Rate 2 End 0 C min To set up a one ramp injector program 1 From injector tab screen touch the temp program button Snare 3 19 Using the Active Method Gm tap A PSSI oven AFID Events j Heater Off 296 C temp init Progratri a Carrier Gas 1 2 psi Split botal flowy 0 OFF Funning Time 1 O12 min 3 The temp program screen appears for the selected injector Use the up and down arrow buttons or numeric keypad button to program the temperature time and rate Refer to the table on the previous page for some examples for values to set up a one ramp injector program OFF Prograrri 4 When you have completed setting up the program touch Close button then the system icon a on the navigation bar to return to the System Status screen NOTE You can enter Rate 2 Temp 3 and Time 3 to set up a second ramp An entry of 999 for Rate l or 2 will cause the injector to ballistically heat up NOTE f the Injector Time is set with the default value of 999 the injector temperature will hold at the current temperature until the end of the oven program Otherwise the injector temperature will hold for the time you have entered or until the run ends NOTE Jf you have the subambient option the POC and PSS injectors are linked to the oven subambient option therefore you
39. Type PSSI S M Capillary Control A PSSI Oven AFID Events Heater of Carrier Control Pressure EI LA a DEE Op z oer amp Program J Oventack ternp init Program RB o Carrier Gas Column Len th 25 00 tri LO 260 urm i 0 1 psi jou l Ao psi Split mode Flow Ofset e A 0 0 cmsec press init Program Flow J Ralo JA Fixed 2 est afset 1 00 mbtnin J tatal flowy 100 Lin HE Control Vacuum Compensation ratio 0 i g Ready 17 01 Not Ready 17 01 K Cancel Start Bae Tools Temperature Program You can set injector inlet temperature programs by selecting the program In the inlet programmed mode the injector is first heated to the injector temperature that is entered in the method The injector then follows the injector temperature program that you defined The oven programmed mode is the default mode of operation In this mode the injector setpoint equals the oven setpoint plus 5 C 2 19 Touch Screen Navigation The temperature graph displays the set point value The label below the graph displays the current step The text to the left of the graph displays the actual temperature Current o EES a aa 0 0 00 0 00 i 265 E temp ime rate Injector Ternperatre Prograrn hit Time OOO m End 1 67 mi Close To modify the temperature program during a run touch the program button You can modify the temperature time or rate H
40. a carrier or makeup gas mixture of 95 argon 5 methane When using capillary columns at low flows 5 mL min or less helium or hydrogen may be used as the carrier gas provided nitrogen or argon methane is used as the make up gas The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configuration Screen gps I Disable Filler 200 B Pkd Oven B ECD st i 100 ie Healer Off temp 0 00 mY 100 C ae le I AuloZero Ouput Recorder afset wo Filler 200 mg Gas Flow SetPoint Actual hake up D Q m Limin Gas fow mL Output upu gel Achal Make Up 5 Fecorder j Integrabor Ofset z Yo 17 0 FE OK Cancel Read 17 01 Tools ad 2 38 PID Clarus 600 680 GC User s Guide The Photoionization Detector PID is designed to allow the effluent from a chromatographic column to be ionized by ultraviolet light provided the ionization potential of the effluent is less than that of the UV source The current produced by the ion flow is measured by the detector and is proportional to the concentration of the ionized material The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method B Pkd Oven B PID Events a i OFF C Heater Off lemp 0 00 mY 25 C stenje 2 Range fi I Autozero QuUUE Rec
41. acct osetyeeaat dacesaa tt anetee Senet seh beatae daseanca a aneuee toeduasosnautadaeadnshimenanisensenielees 6 18 CLC TONS asan a E A 6 20 Run AMOS ai Plier Feders a T a 6 26 SEUD ara E E E TE 6 28 Poena e Seea N tenner iyi ve Mente ene i nee onenTr or ve Terie eet 6 33 Connectine the PPC WMOGUIGS crassi 52 ich cusses Pee dcasunets a N ada 6 35 Reference SELUNGS wasapi p aa ia 6 48 TG LAS a E acids eerie say ees eee 6 48 Zeroing and Calibrating the PPC Modules cccccccccccccceceeceeeeeeeeeeeeeeeeeeeeeeeees 6 49 Heroine tne RPC Gas Modules sccexiarecstce nce ca crets helenae tena are dole yeatacet 6 49 Setting the Reference Temperature and Pressure cccccseeesessseesessesssesesseeeens 6 53 Calibrating the Carrier Gas Modules ccccccccccccccccceeceeceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeees 6 54 Calibrating the Detector Gas Modules aswxseswiicazesnicsxctapeleastiniveeuericastetieee etic 6 57 Calibrate the Oyen Tempera 2 35225 se Sesser care os Geetielaneseeses sererereene ese eaeneene 6 60 Calibrate the Reference Thermometer iccesccncsi ods ccvenGacteliccse nati meen Gaenk 6 60 Place the Thermometer Probe it the Oven vcs cdcevecere sid weleseacteeatil en 6 61 Equilibrate the Oven Temperature ccccccccccccccccccccccccceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeee es 6 62 Enter the Required Offset V ale cect cscvncetintevdiceeavnceu tees diidendveaptiniavlseeacducen testes 6 65 Remove the Thermometer Pro WC ices sess AA 6
42. all fitting connections have been leak tested WARNING Flame Ionization Detectors FID use hydrogen gas Before you turn on the hydrogen gas to the FID ensure that a column is connected to the FID fitting inside the oven Turning on the hydrogen gas without first connecting a column to the FID could create the possibility of an explosion in the oven Turn off the hydrogen gas before disconnecting a column from the FID When two FIDs are installed but only one FID has a WARNING column connected to it plug the inlet of the FID without a column with a 1 8 inch stainless steel plug P N N930 0061 to prevent hydrogen from back diffusing into the oven Since in the manual pneumatics version the hydrogen pressure regulator and the air needle valve have been turned off prior to shipment first set the hydrogen and air inlet pressures to 30 psig Then measure and set the gas flows as described in this chapter NOTE The detector gas modules have been set to OFF at the factory for both manual and PPC pneumatics Clarus 600 680 User s Guide FID Setup Summary To set up the PPC FID e Set the air and hydrogen flows e Automatically ignite the flame or Manually ignite the flame Set the Air and Hydrogen Flows The FID pneumatics utilizes two PPC modules one to control the air and the other to control the hydrogen You set the PPC controlled air and hydrogen flow from the Clarus GC touch screen Each PPC module is calibrate
43. and down arrow or keypad al 333 buttons to change the value to 75 to 75 mL min 7 Touch the Air field and use the up and down arrow or keypad w 3 buttons to change the value to 90 mL min 8 To change the filter value touch the Filter field and use the up and down arrow or keypad nd aj analysis Seq Te a ad ad oo oo buttons to set the value appropriate for your The default setting is 200 milliseconds If you want to improve the signal to noise change the setting to 800 milliseconds however the noise improves but the peak shapes broaden If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase 4 65 Setting Up the Detectors EO Disable Fiter 200 J Linearize PRAT voltage OFF w Gas Flow SetPoint Actual sirf 90 7 mLitnin H2 so f 26 mLmin amp Fecorder _jlnteqrator ofset 5 Not Ready 17 01 v aj Bl OK Cancel 7 Touch OK when completed Turn On the Photomultiplier Tube 1 From the System Status screen touch the FPD button 4 66 Clarus 600 680 User s Guide 2 The FPD tab page is now visible B POCO Oven B FPD Events EO i OFF C Healer Off temp M ooo my 25 C Aten 4 Method Ecitor Ca PRIT on Event Log L haintenance Filler 200 ri PMT Voltage OFF Conhguraion Gas flow mL ilies gel Air 0
44. buttons are active with or without capillary control The options include Auto which is the default setting and Fixed When Auto is selected enter the value for the Leak Limit The Fixed option allows you to enter the split flow offset directly The field label changes from Leak Limit to Offset Program Mode Configuring the injector for the Program mode displays the following Configure Injector A Type PSSI A P Capillary Control Carrier Contal Pressure amp Program J Overtrack column Length j 25 00 mo LOL 250 um Split mode Flow Ofset Flow Ratio JAU Fixed afset 17 00 mLtnin HE Control T Vacuum Compensation a Ready 17 01 v a JE OK Cancel 6 13 Using the Tools Menu Oventrack Mode Configuring the injector for Oventrack mode means that the injector set point equals the oven set point plus 5 and the Column Length and Split Mode fields are not used Also on the Active Method screen the Program button next to the temperature field 1s deactivated as shown below A PSSI Oven AFID Events m m aaa LA i OFF Pa 25 C o ternp init Prograrn Carrier Gas 0 0 psi AA eal fee hele Configure Injector A Type PSSI J Capillary Control Carrier Control Pressure H _ Program Oventrack Flow Citset Auto ay Fixed ofset 1 00 mbLtnin HE Control e Vacuum Compensation ra aa OK cancel When using a mass spectrometer sel
45. cannot operate the injectors below the oven subambient temperature 3 20 NOTE Clarus 600 680 User s Guide Viewing Setting Carrier Gas Pressure Flow Velocity For a description of programmable pneumatics control PPC refer to PPC Fundamentals In the Hardware Guide PPC enables you to select and set the carrier gas Pressure Flow or Velocity In all three modes you can operate at a constant pressure flow or velocity or at a programmed pressure flow or velocity You can also make a pressure pulse flow pulse or velocity pulse injection In this case the initial pressure flow or velocity is quite high at the time of injection This minimizes the expansion in the injector liner as the liquid sample is vaporized and increases the transfer time onto the column This is recommended for splitless operation of wide boiling point samples In this case you would actually program the pressure flow or velocity down to the normal column pressure flow or velocity for the remainder of the chromatographic run The following terms are used in PPC analysis Zero removes the flow controller from the GC method and sets the flow to 0 Flow enables the flow controller in the GC method and sets its initial flow to 30 of the nominal maximum flow rate according to the installed flow range element and carrier gas type The operator has the option to enter a different flow rate and enter a flow program When in the flow mode the PP
46. configured is to bring a peak on scale by amplifying a weak signal or reducing an overly strong signal Attenuation in this case affects only the presentation of the signal Acceptable attenuation values are of the 2nd power for example 1 2 4 8 16 etc up to a maximum of 64 The system rounds off values to the next highest power of 2 For example if you go to the Atten field and select 1 then an attenuation of 32 appears on the screen The range of attenuation values that may be used is 1 65 536 Raising the attenuation decreases the signal to the recorder Lowering the attenuation amplifies the signal to the recorder To change an attenuation value an FID detector is used as an example 1 From the System Status screen touch the FID button a to display the FID tab screen page A FID Events A PSSI Oven iy i OFF c Healer Cf an mp 0 00 mY 25 C Aten lz g M Auloero Range fi gp Output Recorder ofset Wo Filler 200 mS Flameout 0 10 rri Gas flow imli Set Actual A Ar 0 F eH oO op Ignite 17 0 Tools nd 2 To change the attenuation touch the Atten field Use the drop down menu to select an attenuation range for the detector that is appropriate for your analysis 4 87 Setting Up the Detectors 3 After this is done you may continue with another tab page or touch the System button to return to the System Status screen A table listing attenuation vs the maximum detect
47. down arrow or keypad al z23 buttons to enter a pressure HOLD time and HOLD rate NOTE The rate for the range is 0 end to 99 A rate of 999 is a go to setting The go to mode of programming is not recommended Setting a CAUTION program rate will be more reproducible 4 Touch Close 3 26 Viewing Setting Carrier Gas Velocity You can view set carrier gas velocity using PPC To view or set the carrier gas velocity Clarus 600 680 User s Guide 1 From the System Status screen touch corresponding Injector button for which you wish to set the carrier gas velocity The page for the selected injector appears E Split total flowy ratio Feady 17 0 Tools x Ready A PSSI Oven AFID Events Heater OF A pe a 75 C temp init Prograrn i Carrier Gas Ce psi ah 0 00 mem 2 0 0 cmisec vel init Prograrn OFF mbm flowy R Tools ad In this example the Clarus GC is configured with the capillary mode on for velocity as shown by vel init displayed under the carrier gas field If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The Carrier Gas field on the injector tab screen displays the set point value The label below the field displays the current step The actual values for all the available configuration options is displayed to the
48. flow at 0 25 min 8 Touch the A Cap Injector tab The Injector status screen appears olg mia A Cap Oven AFID Events Healer Off OFF c a Carrier Gas 0 0 psi TP 0 00 mun 29 ps 00 cmsec press imit Program Split total flow 0 2 mbm 0 rato flow Ready 17 0 EFE Tools gt 9 Touch the Program button for the Carrier Gas field The Carrier Gas Pressure Program screen appears 3 44 Clarus 600 680 User s Guide Carrier Pressure Prograrn Current 20 i 0 0 00 0 00 O10 psi jaa 11 Touch the Initial time dialog box and use the up and down arrow or keypad ya E 12 Touch the Initial rate dialog box and use the up and down arrow or keypad 13 xa E down to the operating pressure in psi min Touch the step 2 dialog box for pressure and use the up and down arrow or keypad al buttons to enter the column operating pressure oo ao CE NOTE Jf you selected flow or velocity you should still follow the above procedure Just enter NOTE the appropriate flow or velocity values for your analysis If you are in the capillary mode and you set up the pressure mode first you can enter 70 psi and or 10 psi then read the appropriate flow or velocity values respectively This helps determine the values to use This technique is also recommended for the Clarus GC MS detector With mass spectrometers you must be careful not to overl
49. flowy 0 1 psi Mot Ready har 4 Mot Ready har 4 Start a Tools o aat x a Tools 2 28 Capillary Cap Injector 1 From the Configuration menu select Cap from the drop down Conhigure Injector A f Debug Type Cap Capillary Control ressure Flow Offset Jsu Fixed afset 1 00 mbithi H Control 17 01 OK Cancel Clarus 600 680 GC User s Guide 2 Exit from Configuration and display the active method screen Oven A FID Events Healer Gf A T oFF sc temp j Carrier Gas 1 C 0 1 psi E Split total Aow 100 10 0 psi press init Program flowy la Ready 17 01 eee 2 29 Touch Screen Navigation Oven The Oven Temperature Program provides fields and a graph that reflect the current temperature program as shown in the screen on the left below Pressing the Go to button invokes a dialog box that allows users to raise the temperature to a value associated with another step The last step of the current program is selected by default Radio buttons for steps that exceed the number of steps in the current program are deactivated In the example below step 2 is selected As soon as the user touches the OK button the change is implemented The graph in the capture on the right shows the immediate temperature rise and the departure from the program Touching the Go to button displays the Go to Temp dialog box to select a step to go
50. gas 6 58 CAP abbreviation 1 6 Carrier Gas PPC velocity viewing setting 3 27 Changing TCD polarity 4 80 Chromatographic terms glossary 1 10 Clarus 600 680 GC User s Guide Cmptr abbreviation 1 6 Column Flow Calculator 6 67 Column Length Calculator 6 73 Configuration 6 10 Configuring injectors 6 10 Connect PPC module socket descriptions 6 35 Conventions Notes cautions and warnings 1 4 text 1 4 Coolant cut in temperature setting 3 8 Ctrl abbreviation 1 6 D Deconfiguring injectors 6 10 Detector attenuating signal to a recorder 4 87 signal to an integrator 4 90 autozeroing 4 93 output rerouting 4 83 Detector Gas Modules calibrating 6 57 Detectors 2 32 7 11 7 16 Displaying injector temperature 3 14 E ECD abbreviation 1 6 outlet 4 23 overview 2 37 4 20 setting up 4 22 setting up PPC 4 25 setup summary 4 22 Event Log 6 5 FID Index abbreviation 1 6 auto ignition 4 9 overview 4 5 setting up PPC 4 6 File Menu 5 9 Flow Programming 1 11 Flowmeter attaching to an ECD 4 24 FPD abbreviation 1 6 cross sectional view 4 56 igniting the flame 4 69 overview 4 56 setting up PPC 4 57 G Gen abbreviation 1 6 Ghost Peaks 1 11 Glossary autosampler terms 1 7 AutoSystem specific 1 8 chromatographic terms 1 10 I Inj vial abbreviation 1 6 Injector temperature displaying 3 14 setting 3 14 Injectors 2 17 7 6 7 8 carrier gas p
51. injector POC Programmed On Column Injector PPC programmed pneumatic control Pre of preinjection syringe washes Psi or psig pounds per square inch gauge PSS Programmed Split Splitless Capillary Injector TCD Thermal Conductivity Detector 1 6 Clarus 600 680 GC User s Guide Glossary of Clarus GC Terms The glossary of Clarus GC terms are divided into two types e Autosampler Terms e Instrument Specific Terms Autosampler Terms Washing the syringe Pre Wash The number of prewashes of sample to prime the syringe no pumping Pre Inject The number of pre injection syringe washes with a solvent Post Inject The number of post injection syringe washes with a solvent The number of times the syringe draws up sample and evacuates it before acquiring the volume This is done to eliminate bubbles The style of injection Fast speed of the syringe during sample injection This is used to eliminate discrimination in the needle Normal speed of the syringe during sample injection Slow speed of the syringe during sample injection in order to inject directly into a wide bore capillary column in hot injection port 1 7 Introduction Instrument Specific Terms Attenuation The amplification of the detector output signal Background A routine that automatically subtracts a stored calibrated compensation baseline profile from the signal generated during a GC run Ballistically Changin
52. method touch the Method Name field to display the Save As dialog box Assign a name to the new method and save the changes Open Method Touching the Open Method option prompts the following warning box only if changes have been made since the last save Method Editor This method has not been saved Do you want to save the changes Yes Mo Cancel If you touch Yes the Save As dialog appears When the Open option is selected the Open dialog appears for you to select a method 5 11 Using the Method Editor Touch the method name and OK to populate the method edit screens with the values from the selected method Open Name default PN ox _Cancet mL flowy Method Name aromatics File oo If you choose Cancel or touch the OK button without selecting a method the dialog box will close and the operation will be ignored Save The Save command saves the previously opened and optionally modified method under the same name No dialog box appears if a name appears in the Method Name field If the Method Name field is empty either from generating a New Method or from entry into the Method Editor the Save As dialog box appears 5 12 Clarus 600 680 GC User s Guide Save As The Save As command saves the current method under a new or existing name Touching this option displays the Save As dialog box external OF Cancel The Name field displays the nam
53. not aware at the time that you modified certain Active Method parameters Since the conditions used then were not necessarily those required by the analyses you want to perform you should now edit the Active Method to set your operating parameters Examples of how to perform the tasks listed below are described in the sections which follow You should of course substitute your values for ours e Setting up oven temperature programs e Setting injector temperatures programs PSS and POC e Setting detector temperatures e Viewing setting carrier gas pressure programs PPC e Viewing setting carrier gas flow programs PPC e Setting up valves e Setting FID PID NPD or FPD range e Setting TCD filament current e Routing detector output e Attenuating detector signals e Autozeroing a detector e Building a timed events table 3 4 Clarus 600 680 User s Guide Getting Ready to Edit the Active Method gt Close the oven door NOTE Jf a column has been installed make sure you have carrier gas flow through the column before closing the oven door and elevating the oven temperature The Status screen icon buttons provide access to the active method parameters Mot Ready 17 01 e tas v NOTE When you change an Active Method parameter the change goes into effect immediately For example if the system is READY and you change an injector temperature setpoint the status screen displays NOT READY until the new setp
54. not display a check mark 2 Touch the Temp field and using the up and down arrow or keypad al FFF buttons increase the value to 255 C 235 temp ini 3 16 NOTE Clarus 600 680 User s Guide Oven Temperature Programming Mode In this mode the POC or PSS injector is configured as Oven The injector temperature is set to the oven temperature plus 5 C This is the default mode and the easiest mode to operate in For example if the oven program is as follows Time 1 2 min 5 Cimin 240 C Time 2 10 min The initial injector temperature will be 55 C When the GC run begins the injector will hold this temperature for 2 minutes then it will ramp up to 245 C at 5 C min and hold for 10 min T Injector 2 e Injector Time 2 m Oven 2 p e r Injector 1 a Ea Injector Time 1 t 45 C J u pa S 4 Time 1 1 2 3 Step Figure 3 3 PSS oven mode temperature program Opening the oven door turns off the oven and the injector heater Also if you reset the oven temperature during the run to the next level the injector temperature will follow 3 17 Using the Active Method Inlet Temperature Programming Mode The inlet temperature programming mode 1s used when the POC or PSS injector is configured as Inlet In this mode the injector follows the injector temperature program that you entered in the method LA Injection Time is 999 min and Inj Rate is 0 With
55. sample before it is acquired for injection The default is 6 Permissible entries are 0 to 15 Post inject 1s the number of times the syringe if filled with solvent and emptied to waste after sample injection The first half of these washes is taken from solvent vial 1 or 3 The second half from solvent vial 2 or 4 The default is 2 Permissible entries are 0 to 15 Injection Mode Fast 30 milliseconds Not available when a 50 0 syringe is installed Normal injection takes about second Slow takes about 7 5 second Auto resume provides option for autosamplers program to automatically resume where it left off should a power failure occur Autos resume should not be used if you have FID or FPD configured with PPC since flame is extinguished during a power failure 6 27 Using the Tools Menu Setup Security Enable Password Set Preferences Brightness fo o psig _ kPa Language English EN go I Key Clicks FE OK Cancel The Key Clicks check box is selected by default The Enable Password check box is deselected by default If the check box is enabled the default password is Clarus Touch the Set button to display the password dialog box Security Enable Password Set 6 28 Clarus 600 680 GC User s Guide Touch the New field The alphanumeric keypad appears for you to enter the password Passwords are limited to eight characters and are case sensitive Password
56. should recalibrate 6 57 Using the Tools Menu The TCD and PID flow module for reference gas is calibrated with helium at the factory You must recalibrate the TCD and PID flow module if you are using a reference gas other than helium CAUTION The ECD flow module for make up gas is calibrated with nitrogen at the factory You must recalibrate the ECD flow module if you are using a make up gas other than nitrogen CAUTION To calibrate a detector gas module 1 Ensure that the gases connected to the Clarus GC have been turned on and stabilized for at least 15 minutes before you begin calibration Ensure that no detector flame is lit before calibrating 2 To eliminate the column flow from the detector gas calibration disconnect the column from the detector and cap the detector fitting This is very important when you are using packed columns at high flow rates 3 From the PPC screen touch the PPC Configure button Touch OK on the Caution message 6 58 Clarus 600 680 GC User s Guide Configuration PPC Configuration PPG Caution PPO Connect A Peene coals To avoid damaging he PPC system do not modify he setings unless Manual Preurmatics he hardware configuration has changed Do you want to proceed PFC Aarm Enable sool a Reacly 17 01 OK Cancel OK Cancel Select Detector tab Touch the Calibrate button Select OK In the Calibrate screen use drop down menu to select the
57. speed also slows down during injection The more viscous the sample the higher you should set this value To optimize reproducibility you should experiment with different values The plunger speed during sample acquisition and injection will vary with the viscosity of the sample To find the optimum setting for the sample being analyzed you should experiment with various syringe settings Highlighting the Viscosity Control Field use the up and down arrow or keypad al 77 buttons to enter a value between and 15 This value is the number of seconds the plunger pauses at the top of stroke during sample acquisition You can obtain improved precision with viscous samples by using the 0 5 mL syringe and septa in the waste wash vials in place of the diffusion caps Using Solvent Pre Washes Pre washes refers to the number of solvent washes you want the system to perform prior to the pre injection sample washes Highlight the Solvent Pre Wash field and using the up and down arrow or keypad al buttons type in a value Acceptable values are 0 1 or 2 Pre washes occur only at the beginning of an autosampler program Auto Resume should not be used if you have an FID or FPD configured with PPC since the flame will have been extinguished during a power failure Priority Injection Press the Initiate button to inject a priority sample during a run Touch the Initiate button in the Tasks tab buttons to input the number of pri
58. the AutoZero check box prompts the system to zero the signal before the run and also activates the Signal button on the Signal screen The mV value next to the small signal icon that displays the current signal The read only text displays details about configuration settings The following screen shows the major components that apply to all detector screens The subsections that describe each detector type includes details about settings that are unique to that particular detector FID Selecting this checkbox turns the detector heater Method 5 ty AW Over A FID Events 100 C Healer Of Actual temperature emp C 00 mi 100 C Aten 16 e Autozera Range 20 g Output Recorder Offset amp To Filter 200 m Flarneout 0 10 mi Temperature setpoint Dynamic text displays the current signal Selecting the AutoZero checkbox zeros the signal before the run Indicator lights show the gas flow status Gas fow iL set Artal Ar 100 10 6 H 20 O ignite B Feady 9730 Me aE The FID Flame Ionization Detector uses a hydrogen and air flame to generate ions from the combustion of an organic compound The detector collects and measures the concentration of these ions to determine the amount of compound Touch the Ignite button to light the FID flame 2 32 Clarus 600 680 GC User s Guide in the sample The FID active method s
59. the GC to warm up for approximately 15 minutes before calibrating any gas 6 49 Using the Tools Menu Table 6 2 Injector Detector and Corresponding PPC Module Gas Function Injector Detector PPC Module Gas Function Packed Column and POC Injector Capillary and PSS Injector Carrier Gas and split flow FID NPD FPD Both air and hydrogen gases Makeup Gas Makeup Gas e Make sure that the gas supply to the Clarus GC 1s turned off at this time e Ensure that the pressure in the lines has completely bled down by loosening the restrictor on the rear of the PPC module that you are calibrating see the following with a 1 2 inch socket wrench or open end wrench Refer to above table for a listing of the injectors and detectors with the corresponding PPC gas module functions Restrictor __ ae PPC Modules Chimney vent
60. the PPC controller interprets stored PPC programs as the average capillary column linear velocity settings 1 12 Touch Screen Navigation 2 Touch Screen Navigation Clarus 600 680 GC User s Guide Chapter Overview You operate the Clarus GC using the touch screen on the front of the GC The touch screen 1s the interface between you and the instrument enabling you to control the Clarus GC in order for you to perform your analyses easily and conveniently The touch screen contains active areas that you touch to perform the required action You may find it more convenient to use a stylus or you may like to touch the active areas of the touch screen Do not use sharp pointed objects A light touch 1s all that is needed You do not need to press forcefully on an active area Please note that when you touch an active area various processes are started in the instrument Some of these processes may take several seconds Be patient and wait for the process to complete before touching another active area on the touch screen This chapter gives a brief overview on touch screen definitions and navigation For details on using the active method method editor and tools menu see chapters 3 4 and 5 Touch Screen Navigation Touch Screen The main display area on the touch screen is referred to as screens You use various screens to set up your Clarus GC to perform the analyses These screens contain e Entry fields wh
61. the example below This example also shows that the Heater is off 4 If you require the heater on for your analysis just touch the Heater button and it will toggle to heater on 7 11 Setting up a Typical Analysis 5 To autozero the detector baseline touch the AutoZero field for the check off to appear in this example AutoZero is used Ge ET tap A FID Events A PSSI Oven ad i OFF C temp 0 00 mv 25 C Aten 16 I Autozero Range fi H Output Recorder ofset oo Filter 200 ms Flarmeouk 0 10 mv Gas flow tnl Sel Achal Ar Si 5 He 1500 150 6 The Gas flows Output Offset Filter and Flameout are shown above as reference fields and they cannot be changed in this screen 7 Ifthe Gas flows Output Offset Filter and Flameout have to be changed touch the Tools button and then touch Configuration on the displayed menu a A PSSI Oven A FID Events a i OFF c Heater Of aee P 0 00 mi Alten 3 Method Editor Event Log Range 20 gt El hlaintenance configuration Gas flow iml Sel Actual Ar 50 He 150 0 Ready m jA 7 12 Clarus 600 680 GC User s Guide The Configuration screen appears B Injector A Injector ae ali a G coe Run selip Preumalics Relays Ready Mar 4 Close As shown in the screens below the Configuration screen allows you to modify the Filter Flameout Gas Flows and Output fields a
62. to achieve the sensitivity required for your samples For example if you have a concentrated sample such as drugs it can be analyzed with a background of 0 25 0 50 mV If you have a low level sample such as pesticides it may require a setting as high as 1 2 mV To get the maximum life from your NPD bead operate at the lowest setting to achieve your required sensitivity 4 52 NOTE NOTE Clarus 600 680 User s Guide 1 The bead will be stable after operating for several hours but it will drift in time At the start of each day adjust the background reading to the setting you are using and allow a few minutes for it to stabilize 2 Due to the loss of alkali metal with use the nature of the bead is to drift over time We strongly recommend using an internal standard for quantitative analysis 3 The bead can operate at higher background settings The higher the setting the greater the signal and noise Therefore the signal to noise ratio will not increase dramatically Operate at the lowest possible setting to achieve the required sensitivity this will also prolong the life of the bead The bead should be turned off by turning the bead potentiometer dial fully counterclockwise before you turn off the Clarus GC Remember that the bead has a finite life You can extend the bead life by turning the bead off when it is not in use for long periods of time for example over the weekend Reactivate a Used NPD Bead
63. to the ECD outlet 5 Press down and turn the metal sleeve on the end of the vent tubing to secure it to the ECD 6 Thread the vent tubing through the detector cap and insulating cover as you position them over the ECD 7 Secure the insulating cover to the Clarus GC with the two screws previously removed 8 Thread the tubing through the hole in the detector cover then close the detector cover This hole is either directly above the ECD or at the rear of the detector cover depending on the detector configuration 9 Attach a flowmeter to the vent tubing 4 24 Clarus 600 680 User s Guide Adjust the Make up Gas Flow The ECD flow module for make up gas is calibrated with nitrogen gas at the factory You must recalibrate CAUTION the ECD flow module if you are using a make up gas other than nitrogen The following procedures describe how to set the make up gas With PPC pneumatics the make up gas is set from the Clarus GC keyboard The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure To set the make up gas l 2 Set the make up line pressure to 60 90 psig In the System Status screen touch the ECD button Method B Pkd Oven B ECD Events st OFF C Heater Of o imp 0 00 mw 23 C hletnod Editor ften 4 Ej Event Log Gas flow HL gel Make Up Q Ready In the ECD Tab change the Make Up fiel
64. use the up and down arrow or keypad al Z22 buttons to enter a flameout detection level in mV for example 0 3 mV A FID Disable Fiter 200 SetPoint Actual Flamecut i Tn 0 00 my Gas Flow SetPoint Actual Air ae 0 mLinin He ad mbtnin amp Recorder _ Intbegrabor oket 5 uput 17 01 EEH OK Cancel NOTE You must set a Flameout value in millivolts mV for the FID auto ignition feature to work For example 0 3 mV Flameout detection occurs 0 5 minutes into the PRE RUN time and measures the user entered baseline threshold level in mV In this example 0 3 mV is used If the 0 3 mV threshold level is exceeded the flame is considered lit otherwise the auto ignite sequence begins to automatically ignite the flame 6 Touch the Set Point dialog box for the Air flow and use the plus and minus buttons to set the FID Air flow to 450 mL min 4 9 Setting Up the Detectors A column must be installed on the base of the detector and capped CAUTION with a stainless steel Swagelok Plug before attempting to ignite the flame Digable Filer 200 SetPoint Actual Flameout 010 ooa my nas Flow me oe ad SetPoint Actual Alr 12 m Linin He a g0 mLimin Recorder _ lntegrator Orset 5 En 17 01 OK pancel 7 Touch the Set Point dialog box for the H2 flow and use the numeric keypad or the up and down arrow buttons to set the Hydrogen flow
65. with helium e PID is calibrated with helium If you intend to use a gas that is different from the gas used to calibrate the PPC module you must recalibrate the PPC module with the gas The instructional procedures in this chapter are written with the assumption that e You know how to measure gas flows using a flowmeter or with the Clarus GC s built in stopwatch and a soap bubble flowmeter If you are not familiar prior to continuing please read Using the Built in Stopwatch in Chapter 4 Before You Install a Column e All heaters are turned OFF and cool to the touch 4 3 Setting Up the Detectors The instant the Clarus GC is turned on the oven injector s and detector s begin to heat up rapidly To avoid injury turn off all heaters and allow their respective zones to become cool to the touch before you touch detectors injectors and their corresponding fittings Detailed procedures for turning heaters off and on are in the Hardware Guide WARNING Before you Install a Column If you have not read this chapter please do so before proceeding e A column has been installed carrier gas flow or pressure has been set and all connections have been leak tested The PPC modules have been calibrated at the factory 4 4 Clarus 600 680 User s Guide FID Overview Flame Ionization Detectors FID are mass sensitive and used for the destructive analysis of organic compounds As the sample enters the
66. you set the split flow to zero the flow display shows column flow plus septum purge Common places for leaks would be the septum cap the O ring seal column connector etc See the Clarus Hardware Guide Chapter 8 for further information in the pneumatics NOTE NOTE Clarus 600 680 User s Guide Set up the Splitless Mode for a CAP or PSS Injector The Splitless Mode is used for trace analyses Most of the sample is transferred onto the column then the split vent is opened thereby venting any sample remaining in the injector liner This step describes how to set the split mode for PPC modules In the Splitless Mode the split vent must be opened after the sample has transferred to the head of the column i e 0 5 2 0 minutes after the run has started The procedure which follows assumes that the carrier gas pressure has been set see Step C in this chapter The injector is shipped with a wide bore injector liner You may want to install a narrow bore liner Both liners must be packed with quartz wool before running your analysis Refer to Step B Connect the Column to the Injector in this chapter for procedural details Splitless Injection with Pressure Pulse Flow Pulse Velocity Pulse Technique Pressure flow or velocity pulse injection is recommended for splitless operation especially when analyzing wide boiling point mixtures and or large volume injections This technique increases the pressure flow vel
67. 0 90 psig 3 From the System Status screen touch the FPD button 4 62 Clarus 600 680 User s Guide Method 1701 Method 5 B Poco Oven B FPD Events EO i OFF C Healer Off p temp y GOU mi 25 C Aten 4 Bi Ie AutoZero w PMT On amp Linearizer On Filler 200 ma QuUBUE Recorder PRT volage OFF Offset ri Gas fow inL gel Actual Ar 450 45 He 460 45 i 17 01 a Ready i l ee 4 63 Setting Up the Detectors 5 To change the gas flow values touch the Tools button in FPD tab screen and 4 64 touch Configuration from the displayed menu g m i B POCO Oven B FPD Events EO i OFF C Healer Of temp OOD mw 25 Aten 4 a Method Editor a PAIT On Event Log Li hiaintenance Filter 200 mS PMT Voltage OFF Coniquraton Gas flow inL Lblities Configuraton B Injector A lnjector ae FE roe F Ery A S at Run Selip Prieurraics Relays Read 17 01 Close This displays the FPD Configuration screen Clarus 600 680 User s Guide 6 On this page touch the FPD button a to get to the FPD Configuration screen Disable Filler 200 J Linearize FMT voltage OFF oo Gas Flow SetPoint Actual Alr 0 i mLimin me O 0 o4 mLinin Recorder _ jy lntegrator Ofset D oo 17 0 Ok cancel 6 Touch the Hydrogen field and use the up
68. 0 User s Guide Setting Carrier Gas Flow using PPC To view or set the carrier flow L 2 From the System Status screen touch the Injector button for example Pkd or Cap corresponding to the injector you wish to set the carrier gas flow The tab for the selected injector appears A FID Events Heater of op temp init Over fs C Prograrri Carrier Gas 0 0 psi 0 00 mLM 20 psi O10 crvsec press init Prograrri E Split total fow J OFF mbm rato 0 flowy Ready 17 01 EE val In this example the Clarus GC is configured with the PSS capillary mode on for flow If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The carrier gas field on the injector tab screen displays the set point value The label below the field displays the current step The actual values for all the available configuration options are displayed to the left as read only text on the screen Touch the program button E for Carrier Gas 3 25 Using the Active Method The Carrier Pressure Program window appears carrier Fressure Progra Current 0 OO 00 0 0 psi i j rate pressure lime psi minubes psiinin nit O00 pmi Erd 1 67 m Close 3 Touch to highlight each individual field ranging from the Initial field to the step 4 field and use up and
69. 1 Following are summaries of its requirements Labels Do not remove any of the labels attached to the ECD cell or any of the labels attached to your Clarus GC that refer to the ECD cell Follow all instructions and abide by all precautions provided by the labels and in user instruction manuals referred to by the labels Leak Testing You are obligated under federal and state regulations to make certain that the ECD cell is wipe tested for leakage of radioactive materials at intervals of no longer than six months and that the analysis of these wipe tests is conducted by a person specifically licensed to do so either by the U S Nuclear Regulatory Commission or by an Agreement State The analyses can be performed by the firm listed below National Leak Test Center P O Box 486 North Tonawanda New York 14120 4 18 Clarus 600 680 User s Guide Cell Failure or Damage If a leak test detects more than 0 005 mCi of removable radioactive material on the surface of an ECD cell or if the cell itself is damaged in such a way as to indicate that it may no longer adequately shield the radioactive material inside you must immediately suspend operation of your chromatograph until the cell has been repaired or disposed of by a person specifically licensed to do so Any such incident must be reported by you to the Regional Office Inspection and Enforcement U S Nuclear Regulatory Commission Reporting Radiation Incidents Theft or Loss
70. 11 Detector 1 Detector 1 Detector 1 Air or TCD Ref HYD or Make Up 3 J12 4 J13 Detector 2 Detector 2 Detector 2 Air or TCD Ref HYD or Make Up 5 J14 6 J15 ow ow ooo 11 J20 12 J21 Split Vent for CAP amp PSS injectors or Pressure Readout for PKD amp POC injectors 6 35 Using the Tools Menu A flow or pressure module can be connected to positions 1 8 Split vent modules or pressure modules can only connect to positions 9 12 The PPC modules for injectors and 2 carrier gas connections are connected to sockets 1 J10 and 2 J11 respectively on the PPC board The PPC modules for the split splitless capillary Cap injector or PSS injector split vent connections that correspond to injectors 1 and 2 or the pressure readout that corresponds to a packed column injector Pkd or POC injector installed in socket 1 and 2 are connected to sockets 11 J20 and 12 J21 respectively on the PPC board The PPC modules for detectors 1 and 2 are connected to sockets 3 J12 through 6 J15 on the board Detector 1 uses sockets 3 and 4 6 36 Clarus 600 680 GC User s Guide PPC Control Board HN NANN PPC Control Board Note Disconnect the grounding wire inside panel to remove this right side panel a h BSB tse ya Phillips Screws 3 Right Side Panel Figure 6 1 The PPC board installed in the Clarus GC Your Clarus
71. 6 B FPD Gas Flow SetPoint Achal arf s 9 mLtmin H2 75 0 TE mLtmin dupu Recorder Integrator Offset ED rr Equilbrating 0 04 min v a Bl OK Cancel Output Configured B OUTPUT id M Disable Filer 200 Define Gas Sources SetPoint Actual Reference 0 0 m Linin Makeup oo oo mLtnin uput Gas Flow Recorder J Integrator Offset D ri a Ready 17 01 OK Cancel m gt Clarus 600 680 GC User s Guide 6 25 Using the Tools Menu External Configuration If an external amplifier is installed a screen similar to the following appears Disable Fiter so Heat detector Gas Flow SetPoint Actual Af o o mim QU Recorder _ 3 Integrator Orset E Yo Ready 12 01 v 4 FE OK Cancel Run AutoSampler Configuraton Injechon I Enable Autosampler Recycling Auto Resume Volume 5 0 Slut Mode n Colu ayringe Wash Viscosity Control o Solvent Pre Wwash o Pre Inject 2 Post Inject 2 Furmp a Sample Finse Before Ready Ready 1 2 01 HIS JE OK Cancel 6 26 Clarus 600 680 GC User s Guide Pre wash is number of times the syringe is filled with the sample and emptied to a waste vial before a sample is acquired for injection The default 1s 2 Permissible entries are 0 to 15 Pump is the number of times the syringe 1s filled with the
72. 6 0 8 bs Figure 4 39 An example of integrator noise 2 Gradually decrease the attenuation for example to 16 or until the noise level increases 4 90 Clarus 600 680 User s Guide VIEW C SCALE NOISE_05 C01 zZ attn x 16 50 457 50 40 50 35 5 90 30 minutes 0 0 0 2 0 4 0 6 0 8 1 Figure 4 40 An example of detector noise A table listing attenuation vs the maximum detector signal producing a 1 V output to an integrator is provided in the Clarus 600 680 GC Customer Hardware and Service Guide Maintenance chapter section Practical Hints To change an attenuation value From the System Status screen touch the TCD button 2 Inthe TCD tab page touch the Atten field m and use drop down menu to change the value OG ma B TCD Events B Pkd Oven EI OFF 0 Heater Of temp 0 00 mv M26 C Aten EI e AutoZero al Current mA Qulput Recorder Offset To Filler 200 ms aas flowy 2 Yi Acual Fe 0 W Make Wp 0 0 0 0 Ready 17 01 4 91 Setting Up the Detectors NOTE Attenuation of detector signals may be changed during a GC run with a timed event At the end of the GC run the initial attenuation value is automatically restored 4 92 Clarus 600 680 User s Guide Autozeroing a Detector Each configured detector 1s equipped with digital autozeroing capability As long as
73. 65 18 SU bhi e AAN ere ER Sera A te nee Pa nce rer E rere te fOr E A AE ene reek ett AO Sere er T 6 66 Column Plow alc Ulaton cdots cternnpeiaisasteidlerdics aa aa 6 67 Split Flow CalCulanOns SC Cen hese chant ncaa bet ded teas deta ciel ant teed ates dati 6 71 Column Teneth Calculator s514cindcin dice aininiiGacimieiacnie atabadaieensaietan 6 73 Backeround Compensation 3 sssini pn n a p 6 74 SOPA a to re et ete ee eee een ee Peete ne Pepe ese es eee Peete 6 76 Program Max Ovem Prostam Rates cicaciecciad cnn ean dae ee 6 77 Rolas oraaa cede Rat aceasta nalcstaarhd tran E Seas palatial auto uaale 6 78 PSO OU eee n A E ache thea een E ates 6 79 POOUL sasniancatabauenanucssassinkutaaabstaan ania O T ENS 6 80 vi Setting up a Typical Amal ysis viiceseisscessscocececcictsseassccesesectosenssancwsssacsssewescececasactacesssescssauss 7 1 DVS CEM SATUS 5 CUE E P E E E E O E N E E 7 4 Mjecior Setin Sieen n anes onan E ee es ee 7 6 Packed Column PK in ECO crane OTE ne wicecace 7 6 Programmed Split Splitless PSS Injector ccc ccccccccceeeeceeeeeeeeeeeeeeeeeeeeeeeeeeeees 7 8 DECORS E S ee Re eee Rc AON eR A Ce RR 7 11 Flame lonization Detector FID sssscsccxnacssnsccwnewnssseeaseaasysesnas oaesteaceoteoniveesasacsveedeates 7 11 PSUS CLOT sooty sureetens tsi huawewierawat E E E atau dunmeie 7 16 Thermal Conductivity Detector TCD 4 6eesuin eee ee ee ee 7 16 Autosprint EOE A a 7 22 Index vii viii Introduction 1 Intr
74. 9 Setting Up the Detectors Changing TCD Polarity During a Run TCD Range timed events are restricted to changing TCD polarity For example if an initial range is four then an event can only be entered for 4 or 4 Examples for using polarity changes are given in Clarus 600 680 GC Customer Hardware and Service Guide Maintenance chapter Practical Hints section To automatically change the range from 2 to 2 after 3 minutes into the run 1 From the System Status screen touch the TCD button val Read 17 01 m ors v 2 Inthe TCD tab page touch the Events tab 4 80 Clarus 600 680 User s Guide B Pkd Oven E CFF C Heater of temp 0 00 mY 26 C tae EJ Je AuloZera Current 40 mA Quiput Recorder ofset ri Filter 200 ms Gas flow gril gel Actual Ref 0 Q hake Up 00 0 0 Ready 17 01 MS 4 B mew 3 Inthe Events tab touch the Add button Method A B Pkd Oven B TCD Events Time Evert Value ese r z22 buttons enter a time 4 Using the up and down arrow or keypad al EEE of three minutes into the Time field 4 81 Setting Up the Detectors Event Range A e Ready 17 01 Tools ad 5 Using the drop down menu in the Value field select a value of 2 6 When completed touch OK to close this screen When a run is started the system uses the initial range of 2 for 3 minutes then reverses the polarity for the duration of
75. C system also monitors the column inlet pressure If the inlet pressure falls outside a selectable range a leak check fault occurs Pressure controls the column inlet pressure and reads the flow rate from the flow sensor in the flow controller The initial pressure in the method defaults to 5 psig The operator has the option to enter a different initial pressure and optionally enter a pressure program Carrier Gas Mass Flow Controller Operation Once the carrier gas operation mode has been selected see the next section Setting Carrier Gas Pressure you can also modify the default setpoints in the active GC method edit the carrier gas setpoints in stored methods or generate a new method and enter carrier gas setpoints The following parameters control the carrier gas 3 21 Using the Active Method Initial Carrier Gas Setpoint The carrier gas mass flow controller receives set points of flow or pressure depending on the configured carrier gas mode The program calculates the initial set point from the active GC method The initial set point 1s established upon setting up a method ending a run or resetting the GC The flow rate is held constant at the initial value if no additional carrier flow entries are made in the GC method The controller receives pressure set points when operating in the pressure control mode Carrier Gas Program The GC method accommodates up to three additional carrier gas program steps ea
76. Configure button Touch OK on the Caution message Configuration PPG Configuration PPC Caution PPG Connect A A To avoid damaging he FFG sysler do not modify he setings unless Ktanual Preurmatics ne hardware conhquraion has changed Do vou want bo proceed PFE Alarm Enable 2D Ready 17 01 OK Cancel OK Cancel 2 Select the channel you need in this example Channel A tab is selected Touch the Calibrate button Select OK 6 55 Using the Tools Menu Configure PPC Devices Carrier Detector ANU Channel 4 Channel B PPO 1 Garr Flow nas He EI Zero Calibrate B ero PPG 11 Split Chl Ready 2 00 OK Cancel 3 Inthe Calibrate screen use drop down menu to select the proper carrier gas and use the plus minus buttons to input the other values needed In this example the injector is a capillary split splitless and the restrictor installed is a number 6 The restrictor frit number has been entered in the software at the factory Do not change this number unless you have replaced the restrictor with a different one The number is stamped into the restrictor If you are performing this calibration procedure and you do not have a column connected to the detector you must plug the detector fitting in the oven with an Swagelok 1 S inch cap before proceeding This will ensure that all the gas flows up through the detector and not into the oven CAUTI
77. GAS CHROMATOGRAPHY CLARUS 600 680 GC User s Guide PerkinElmer For the Better Clarus 600 680 GC User s Guide Release History Part Number Publication Date 09936780 February 2010 Any comments about the documentation for this product should be addressed to User Assistance PerkinElmer Inc 710 Bridgeport Avenue Shelton Connecticut 06484 4794 U S A Or emailed to info perkinelmer com Notices The information contained in this document is subject to change without notice Except as specifically set forth in its terms and conditions of sale PerkinElmer makes no warranty of any kind with regard to this document including but not limited to the implied warranties of merchantability and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of PerkinElmer Inc Copyright 2010 PerkinElmer Inc Trademarks Registered names trademarks etc used in this document even when not specifically marked as such are protected by law PerkinElmer is a registered trademark of PerkinElmer Inc ii Ta
78. GC has been properly configured connected at the factory However you can check the configuration to become familiar with the procedure in the event that you need to reconfigure reconnect 6 37 Using the Tools Menu For example if a capillary injector 1s installed split splitless CAP or programmed split splitless PSS then Split is configured to notify the Clarus GC software that a capillary PPC module is installed If a packed injector Pkd or programmed on column POC injector is installed Flow is configured to notify the software that a PPC flow module is installed PPC Connect Press the PPC Connect button The following message appears to caution users that modifying the settings can have a negative impact on the operation of the PPC system Coniguraton PPC Caution To avoid damaging he PPC system do not modify he setings unless he hardware coniquraton has changed Do vou want to proceed Press OK and the main Connect PPC Devices screen appears 6 38 Clarus 600 680 GC User s Guide Connect PPC Device as T B Carrier A Detector A A a A A AUK 1 ALK 2 ALK AUK 4 Carrier B Read 17 01 Close The screen includes icon buttons to identify the logical PPC devices The displayed carrier icons are taken from the currently configured injector for the corresponding channel The detector icons are taken from the currently configured detectors In the above screen Carrier A and B bu
79. Gas Add Edi Relays Delete Clear Ready 17 01 EE e Tools gt The Events tab displays the timed events table and buttons valves and Aux gas controls 2 42 Clarus 600 680 GC User s Guide Timed Events Table The timed events table displays the time name and value of each event Timed events may be added and removed while the GC is running The next event to be executed is automatically selected Up to 32 events can be specified The configured hardware determines which events are available Events that are not applicable should not be available The following table lists the available events The time range 1s 99 to 999 minutes Events occurring after the temperature program is complete are ignored Add The Add button displays settings that allow you to specify an event to add to the table ogma A PSSI Oven A FPD Events Add Timed Evert Tawi Tools 2 43 Touch Screen Navigation Error Messages Error Event list 15 full Error Edit Touching this button displays the active method page for editing timed events If the GC is running then edited events at times before the run time at which the edited list 1s accepted do not occur until the next run OG m D APSSI Owen AFPD Events Edit Timed Ewent 3 Ready har 4 Start a FE Tools hd Error Ho event to edit h 2 44 Clarus 600 680 GC User s Guide Del
80. I LU oe Baas olga see Pace ae ea ae ne e ee ate ee oe 4 17 United States Government Regulations for ECDS cccccccccccccceseeeeeeeeeeeeeeeeeeeeees 4 17 Special Instructions for ECD Cell Purchasers ccccseeseeseesseeeessssessesseseeeens 4 18 United Kivedo Reoulavonsc da eine ete E ees 4 20 ECD OVENI CW acne aS 4 20 ECD SO UDe recat ean E TN A teat teers 4 22 SE a E D a E E E A ETE nieaenateeatendls 4 28 RODS a O E 4 29 ECOS UP SUNN yana A A 4 29 Using a TCD with the Autosampler or GSV 0 ccccccccccccccseceeeeeeeeeeeeeeeeeeeeeeeeeeeeeees 4 35 Senne up ARID aspan r r R 4 36 PIV OVYEINIE W eria N die celdabatudenedmeswiacehaatanaceteas 4 36 PID SOU Pee E E a A a a nee ancin 4 37 Serene Up a NPD rrin a a ad 4 43 ANEDOTA 4 44 Senne Ura NPD eases caress ee 4 45 NPD Bead Activation Proced r ssi sern a Geecweahs tausioeiaeund soreness 4 48 SE E D e A E ee ee eee 4 55 FPD OVVIE W en 4 55 Senne Up the PPD craen a a a eee 4 57 FPD Setur sunma y oa a tomaeton Creme si eeiasanetoeeise 4 57 Configure the Linearizer and Signal Filter 00 0 ccccccccccccccceeceeeeeeeeeeeeeeeeeeeeeeees 4 57 Ser sooo eal Tempera Ue in ee en nn ne oe 4 61 Detector Tempor dir S wsakcvic asia atiensteancetnateicesienutermemadtndbenlancteadepide a n 4 72 SC VELA SIR ANOS reg i e a a ae a aa 4 74 Setine the FID PID or NPD RANCE apii AAT 4 74 Changing the FID PID or NPD Range During a Run sssosooossseseeesssssssssssssssserrrreese 4 75 Setting
81. If you enter the same name as the active method the following message appears A A method vith that name already exists Do vou want to replace t Tes Ho Cancel File Menu The pop up File menu includes options to create modify store and delete methods The Exit Editor option closes the Method Edit screen and displays the view that appeared when the user invoked the Method Editor Tools option During a run the Activate menu option is grayed out since you cannot activate a different method during a run New Method When you need to develop a new method select New Method from the pop up File menu If your current method has not been saved touching New Method displays the following dialog box Warning Method not sawed If you select Yes the Save As dialog box appears Using the Method Editor You can either assign a Name to the current method by touching the Name field and use the displayed Data Entry keypad Data Entry File Name When done typing a name in this example I typed name then touch the OK button The Save As dialog reappears 5 10 Clarus 600 680 GC User s Guide OK Cancel To save it touch OK or touch Cancel to close the Save As dialog box When the dialog box closes the GC is in the New Method mode and the fields are populated with default values The Method Name field is activated and displays the name untitled After defining the values for the new
82. Kiar 4 Tools ad User can turn on the initial and or current settings by touching the check box BEE BEE BEE If GC is Ready changing the initial setting will change the current setting The initial settings are stored in the method and are only changed if the user modifies them The current settings are changed via Timed Events Any settings may be changed during a run 2 48 Clarus 600 680 GC User s Guide Aux Zones Heated Aux Zone If the GC 1s configured with an auxiliary zone the activated button appears on the status screen Aux al Touching the Aux button displays a dialog box with the setpoint and actual temperature Run A Signal T Auxiliary Zone Aux Zone Hester Ort Ea Lee Lit eres Aux 4 hMot Ready 14 5552 Tools To modify the temperature press the minus or plus button Touch OK to implement the value and close the dialog box Pneumatic Auxiliary Zones Up to four pneumatic zones can be set for PPC carrier gas control When one or more of the aux zones is configured the following button appears on the status screen dur al The same button also appears on the Events screen Touching the button displays the following screen 2 49 Touch Screen Navigation Aux Preumalics AUS Zones inital Current a None OFF op gt None OFF oo 3 Pressure ipsi OFF 0 0 a 4 None OFF oo a Close Start Tools Aux Zones that have been s
83. Method with a capillary injector installed and configured in position A front and a packed injector installed and configured in position B rear This section contains examples of how to gt Vv Vv VV V WV Display injector temperature screens Change injector temperatures Turn injector heaters off Turn injector heaters on Set oven programming mode Set inlet programming mode Displaying Injector Temperature Screens 3 14 gt From the System Status screen touch the injector button Ht this will display the injector tab page Clarus 600 680 User s Guide ij Aur J Aus Ready 17 01 n Tae A PSSI Oven AFID Events Heater Of 4A i 255 op B 286 C tetnp init Prograrri Carrier Gas O11 psi 0 00 mun ps O10 crisec press inil Pragram Split total fow 100 mhin ratio fow Ready Mar 4 eee 3 15 Using the Active Method Turning Injector Heaters On or Off gt To turn the Heater Off touch the check box OFF B IFE temp init Program f Carrier Gas 0 1 psi 100 l 0 00 mhm I e psi 0A crvsec press init Program Split total flowy 1 100 mlt ralio 0 Ready Ten Tools ad As the injector cools off the injector temperature is displayed on the above screen Changing Injector Temperatures 1 To turn the heaters on and modify temperatures make sure the Heater Off check box does
84. ON All carrier gas modules are calibrated with helium gas at the factory If you are using a gas other than helium you must select the correct gas for your application We also recommend recalibrating the carrier gas module CAUTION 6 56 Clarus 600 680 GC User s Guide The Set value displayed on the screen 1s 60 of the flow range available at the current gas supply pressure The value displayed is from a lookup table based on the restrictor installed the type of carrier gas the ambient temperature and the gas supply pressure The measured flow will be different from this value The Actual measured flow should be within 20 of the setpoint value without calibration If the inlet gas pressure from the tank is less than 60 psig or if the restrictor installed is not the same as the restrictor number entered then the actual measured flow will not match 20 of the setpoint value This indicates that there is a problem The number displayed next to Hi on the screen 1s the value that the software interprets as the actual flow This number will always equal the setpoint if control is possible If you set the flow higher than what 1s possible for a particular restrictor frit then the numbers will not agree 4 Touch OK to complete Calibrating the Detector Gas Modules Before you begin to calibrate you must first Zero the Gas CAUTION This calibration procedure is specific to the gas used If you change CAUTION the gas you
85. Post Inject 2 Furg a Sample Rinse Before Ready Program 1 Program Vial 0 Injection Q of Q hiar 4 Tools hd Ready 17 01 aa OK Cancel Clarus 600 680 GC User s Guide When the GC is ready touch the Start button to begin the run If you touch Start before the system is ready the run will start when the system reaches the ready Status When the Autosampler is disabled touching the Run button displays the Manual inject screen When the instrument is ready touch the Start button to begin the analysis The countdown enable check box is selected by default You can stop the countdown by pressing the Cancel button Type J Aulosampler hanual het Method E 1 Select Method Wait until Ready 2 Touch he Start bubon 2 njectwhen you hear he inal bne Injecton Counbdown I Enable Ready 17 01 sot E r Manual Injection If no Autosampler is installed or configured the Run button displays the Manual injection screen The enable check box is selected by default Touching the start button initiates the countdown starting from 5 seconds When the countdown reaches 0 an audible beep prompts you to inject the sample The GC will then start to program the oven and collect data If the enable check box is deselected the timer and tone are disabled The system starts as soon as the Start Button is pressed and you make an injection simultaneously Touch Screen Navigation
86. Stopwatch The Stopwatch computes the flow rate that corresponds to the entered volume flowing during the timed interval The start button resets the timer to zero and starts timing While timing the start button caption changes to Stop 3 Touch the Stopwatch icon button s pwatch 4 The following screen appears Time 6 00 min VWolurrie 100 riL Flow mLitnin Start Pause Ready Cet 13 nd 37 Close 6 76 Clarus 600 680 GC User s Guide Program Max Oven Program Rates 1 Touch the Program icon button eat Programi 2 The following screen appears Temp abd Power Range 0 Rate Einin 50 70 0 7O 115 G 115 175 45 175 300 20 200 450 20 Max Oven Program Rates High Power Rate Einin 140 105 6 55 36 NOTE These maximum oven programming rates represent expected typical values and are for guidance only Refer to user manual for further details Ready 6 77 Using the Tools Menu Release To access Release from the System Status screen touch Tools menu and press the Release The following screen will appear select either Yes or No If you select Yes the instrument will be released from its external control If you select No the screen will close Release the instrument tram external control 6 78 Clarus 600 680 GC User s Guide Logout To access Logout from the System Status screen touch Tools menu
87. The method editor mode retains control If the method is not named the Save As dialog box opens for you to select a method from the list Delete Touching the delete option prompts the Delete dialog box Delete X Name default rs OF Cancel 5 16 Clarus 600 680 GC User s Guide Select a name from the list The selected name appears in the Method Name field Touch the OK button to delete the selected method and close the dialog box Exit Editor The Exit Editor option closes the Method Edit screens and restores the Active Method Touching Exit Editor invokes the following dialog box This method i not saved Do you want to exit without saving changes Yes MHo Lancel Pressing the Yes button closes the dialog box and displays the active method screens Pressing the No button closes the dialog box and retains the Method Editor mode 5 17 Using the Method Editor 5 18 Using the Tools Menu 6 Using the Tools Menu Clarus 600 680 GC User s Guide Tools Menu The Tools pop up menu provides options to a number of Clarus GC features and settings such as Method Editor Configuration Maintenance and Utilities To display the menu touch the Tools button 1 To access the Tools menu display the System Status screen as shown below Method Editor o gt Event Log A hlaintenance Conhqurabon Whlibes 2 Touch the Tools button shown above and the Tools menu appears
88. When the oven reaches the new setpoint the system equilibrates for the Equilibration time Init specified in Oven Configuration screen and then becomes Ready For an isothermal run Init TIME 1 is equivalent to the total run time At the end of the time TIME 1 the system changes to Not Ready it equilibrates and then goes Ready To change the hold time gt Go to the Oven tab and enter a Time appropriate for your analysis for example 25 min Since a constant oven temperature is maintained for isothermal operation the rate of temperature increase must be set to If the Active Method you are editing is already isothermal the RATE parameter will have been properly set at 0 and is indicated on the screen by the word End NOTE Using the Active Method You can set the rate to 0 but whenever a RATE is set to 0 any subsequent program steps if present are deleted from the Active Method Setting Up a One Ramp Temperature Program Setting up a one ramp program requires entering the following information in the sequence shown Initial oven temperature Init 1 Hold Time for the initial temperature Init 1 Rate of temperature increase from the initial to the final oven temperature Init Rate 1 Final oven temperature Init 2 Isothermal time for the final temperature Init 2 Temperature increase of 0 C min which signifies the end of the RATE 2 step The following example shows how to convert an i
89. ach a value close to 100 00 C Coolant If you have an optional coolant select the type installed its target temperature and a timeout time 6 18 Clarus 600 680 GC User s Guide Soft Cooling Soft cooling is a technique whereby the cooling rate of the GC oven is initially limited by throttling the intake of the ambient cold air used to cool the oven This is done by limiting the rate of cooling Press the Soft Cooling button to display the Soft Cooling screen Configuration Oven Lirit Eguilibraton e Enable Sot Cooling Fale ae EE K Cancel hlar 4 OK Cancel Enable Soft Cooling Selecting this check box allows you to enable or disable the Soft Cooling function Checking or un checking this check box will not lose the previous settings Rate This user entered value limits the cool down rate Note that this is not a negative temperature program rate but just a means of ensuring that the rate does not exceed the entered value once cooling is initiated Limit This user entered value sets the range over which the soft cooling is applied Once the oven temperature cools to this value normal fast cooling is applied 6 19 Using the Tools Menu Detectors FID FID Disabled A FID T Disable I Disable Filr 200 Filer 200 SetPoint Artal SetPoint Actual Flameout 0 10 0 00 mil Flameout 010 ooo mV Gas Flor AAA nag Flow SetPoint Actual SetPoint Actual Air 0 0
90. aj T buttons to enter the values 4 Select whether you want these start up settings to Repeat Once or Always 6 31 Using the Tools Menu Sleep 1 Touch the Sleep button to display the Sleep screen 2 Select the Method field then using the arrow button B select your desired method This now enables the displayed fields for edit Value range is 6 999 After aa Min Alter aa mi Method on g Method Method 1 B Fo Turn FID gases off while sleeping Ready o a Ready l 17 01 a JE K Cancel a E K Cancel 3 Select the After field then set the time after which sleep will by using the up and down arrow or keypad al buttons 6 32 Clarus 600 680 GC User s Guide Pneumatics The parameter tables show the connection between the values shown on the screen and the underlying parameter interface that communicates to the GC The dependency column summarizes major issues such as if a parameter is not available or hidden when PPC is not fitted Conhigurabton selip Preurmalics Relays gep 3 Tools ad Cose To access the PPC Settings press the pneumatics icon button on the Configuration screen The pneumatic configuration screen appears and displays a number of buttons to represent different types of settings 6 33 Using the Tools Menu PPC Configure Configuration PPC To avoid damaging he PPO syster
91. alue of 0 A Cap Oven A FID Even Add Timed Evert Event Split Bi Time 1 00 Value OK Cancel Read blar 4 o aat Tools 6 Touch OK The split flow will now turn off before the GC becomes ready so that at the time of injection the split flow is off 7 Touch Add The Add Timed Events screen appears 3 48 Clarus 600 680 User s Guide 8 From the Event drop down menu select Split A if you have the injector configured for position A or Split B if you have the injector configured for position B 9 Touch the Time dialog box and use the up and down arrow or keypad al 22 buttons to enter a positive time for the event for example 2 00 NOTE The Time refers to the time in minutes into the GC run that you want to automatically turn the valve on The time depends on your sample solvent column etc Typical time values are between 0 25 and 2 0 minutes An optimum Time is the time that provides maximum area counts indicated by your data handling device with minimum solvent effect tailing 10 Touch the Value dialog box and use the up and down arrow or keypad A Cap Owen A FID Events Add Timed Event Event Split A e Time 2 00 Valle 50 OK Cancel 17 01 Tools At the end of a run the split flow resets to the original setting Setting a Value of 50 mL min minimizes contamination by keeping the splitter on during cool down
92. and press the Logout Touching Logout displays the splash screen for the Clarus 600 or Clarus 680 Clarus 600 sas Chromatograph a lt lt Copyright 2006 PerkinElmer Inc Rey 3 0 25 Language PerkinElmer precisei 6 79 Using the Tools Menu About Touch About to display version information Clarus 600 GC Neeo 2002 REVE 0 28 AUTOS TS TEM Neeo e00 REWE Gro ASOC PPC N61 0 026 REW 66 ASOC AUTOSAMP NeTO 801 3 REW 2 24 Serial Number BTONBOFOT G4 Oven Heater Line Vollaqe NOME a Ready 12 01 Close To access About from the System Status screen touch Tools menu and then touch About 6 80 Setting up a 7 Typical Analysis Setting up a Typical Analysis Clarus 600 680 GC User s Guide This chapter gives you a brief overview on how to run a typical analysis on your Clarus GC For more detailed information on the different screens and parameters discussed in this chapter see the earlier chapters in this guide on the Active Method Method Editor and Tools Menu The Clarus GC can have many configurations For the purpose of this chapter we are assuming the following configuration Injector B 1s packed Pkd Injector A is programmed split splitless capillary injector PSS One detector is a thermal conductivity detector TCD The other detector is a flame ionization detector FID An autosampler is used Setting up a Typical Analysis System Status Screen Everything starts
93. and two will be taken from vial 2 Program 2 splits between solvent wash vials 3 and 4 For example if five washes are required three will be taken from vial 3 and two will be taken from vial 4 3 62 NOTE Clarus 600 680 User s Guide About Sample Vials Use 2 mL vials with the autosampler P N N9301385 144 per box These are crimp top vials The vials and crimp caps with septa P N 00092205 1000 per box are available through PerkinElmer s catalog service in the U S call 1 800 762 4000 or online at www perkinelmer com The minimum volume of sample required in the 2 mL vial is 0 35 mL or 350 uL You should fill the vial when running multiple injections per vial A mini vial insert is available for laboratories with small sample volume requirements This insert fits into the standard 2 mL vial and requires a minimum volume of 5 uL of sample These inserts are available through PerkinElmer s Catalog service or visit us on line at www perkinelmer com When using mini vials it is not recommended to use pumps to acquire samples This assures that the sample will not be diluted by residual solvent in the syringe Only PerkinElmer vials should be used with the Clarus GC Adjust the crimper so that it does not deform the vial cap and septum but crimps the vial cap tight enough so that you cannot turn the cap An improper adjusted crimper can cause the autosampler to malfunction Using a TCD with the Autosampler W
94. and use the up and down arrow or keypad al z buttons to enter a setpoint of at least 100 C or enter a value 50 C higher than the highest temperature of your oven program 3 Wait for the FID temperature to become READY When the temperature is ready a green light appears next to the temperature display 100 C 4 Touch the Ignite button A Note the signal level in mV before the flame ignites 5 Upon pressing the Ignite button the air flow turns off for 15 seconds Flame Ignition 1 appears in the status bar and the glow plug begins to glow A Se Glow Plug Ignitor Figure 4 2 Location of the FID glow plug ignitor 6 When you hear a POP observe the Signal level in mV as it increases on the screen and remains greater than the previously noted value After the flame 1s lit a screen will appear that shows the signal level at the range that you set If you have set a range of 20 the signal will be 20 times smaller 4 14 Clarus 600 680 User s Guide You can also confirm that the flame is lit by holding a shiny object such as a mirror or small wrench over the FID outlet Condensation forms on the object if flame ignition has occurred The FID outlet is hot To prevent injury never place your hand over the FID outlet WARNING If the Flame Goes Out During a Run If the flame goes out during a run the run continues until completion however the data collected is invalid When the Clarus GC prep
95. ange the attenuation to produce a reasonable size peak When using a thermal conductivity detector TCD the range or current setting also affects the output signal Therefore start at attenuation x64 As long as the signal does not exceed 1 V you can amplify the signal by changing the attenuation 4 89 Setting Up the Detectors Matching Detector Signals with Your Integrator The following procedure should be followed if you are operating your detector near the minimal detectable quantity level This will ensure that the integrator is not filtering the signal coming from the Clarus GC The purpose of attenuation when an integrator is attached and configured is to assure that the GC output is above the noise level of the integrator Normally attenuation for an integrator need only be performed once To obtain the most satisfactory results it is recommended that attenuation be carried out under actual operating conditions prior to running your first sample Valid attenuation values when an integrator is configured are 1 2 4 8 16 32 and 64 The greater the attenuation the smaller the degree of detector signal amplification Attenuation of an integrator can be thought of as a two step process 1 Observe the integrator noise at an attenuation of 64 File System Display Options VIEW C SCALE NOISE_01 C01 2 attn x 64 50 45 gt 50 40 50 35 50 30 minutes 0 0 0 2 0 4 0
96. ares for the next run it checks for a flame by running the Flameout test If the GC detects that the flame is out it will automatically attempt to ignite it If you have the manual pneumatics version you must manually ignite the flame NOTE To prevent condensation from forming on the FID always turn off the flame both NOTE the hydrogen and air before cooling the detector or turning off the Clarus GC Using the FID in Corrosive Environments If you are analyzing samples such as chloroform methylene chloride etc that produce corrosive by products we recommend installing the piece of vent tubing P N 0250 6490 supplied in the Clarus GC Shipping Kit P N N610 0348 and setting the FID temperature greater than 250 C to minimize condensation Corrosive by products will attack the top of the FID collector assembly including the ignitor we strongly recommend venting the FID into a vent hood The flame will not ignite with this vent tubing installed To ignite the flame you must first remove the vent tubing ignite the flame and then replace the vent tubing To install the vent tubing 1 Ignite the FID flame 4 15 Setting Up the Detectors The FID outlet is hot To prevent injury never place your hand over the FID outlet WARNING 2 Lift open the detector cover 3 Cut the piece of tubing P N 0250 6490 to a length of 4 inches and firmly insert one end of the tubing into the top of the FID 4 Route the end
97. arrow buttons or the numeric keypad As shown in the example above use the up and down buttons or the numeric keypad to set the filter to 200 and the Output to 5 When all the settings are appropriate for your analysis touch OK The TCD screen will now show the changes you made in the configuration settings for the TCD detector The default setting for the filter is 200 milliseconds If you want to improve the signal to noise change the setting to 800 milliseconds however the noise improves but the peak shapes broaden If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase To protect the TCD filaments from errors associated with the sample and reference gas channels you must select the necessary detector gas sources As shipped from the factory the sample channel is Carrier 2 and the reference gas channel is the detector Reference Gas In some cases with Arnel configurations for example the TCD could be sourced with both a Carrier gas as well as an Aux gas in GSV applications half the run could look at the Carrier and half could look at an Aux source In other cases the reference gas could be replaced by a second channel of carrier gas in a dual column TCD setup Enter the TCD Bridge Current Range gt Select a bridge current range using the criteria in the following table NOTE Operating at too high a temperature can have an adverse effect on filament life Table 4
98. ary column wall coated open tubular column A small internal diameter column whose inside wall is coated with a liquid phase Carrier gas The mobile phase of the separation system An inert gas which transports the sample from the injector through the column to the detector This gas is usually helium hydrogen or nitrogen Column conditioning A process for producing a stable column by heating the column with carrier gas flowing to remove volatile impurities from the stationary phase Detectors Hardware that responds to sample components producing an electrical signal that can be measured to quantitate the amount of each component present Flow programming The stored PPC program is interpreted as real column mass flow settings or capillary column flow settings from which the inlet x Reference Denney R C A Dictionary of Chromatography 1 10 Clarus 600 680 GC User s Guide pressure is calculated This is dependent on the capillary control mode and installed pressure or split control option Flow rate The mass flow of carrier gas or detector gas in milliliters per minute Ghost peaks Peaks that are not due to sample components for example peaks produced by carrier gas impurities septum or components from previous analyses Injection port The hardware through which the sample is introduced to the column by injection Linearity Quantitatively all detectors will produce a linear response
99. ble of Contents PEACE OCU CONORN uid cces saved teases a ies emmusceususal copsassausaet sas sueavecestuculessustivonsueds 1 1 ADOT THS Mantal sosire ENE o r E oi 1 3 Conventions Used in this Viana i csacceein seeks dc een ara EE EE E ee neee ti 1 4 Notes CANONS and Walihhhie S eicces titan ais os atc a AEO 1 4 Wartnine Stenson the TSUEN tesiri aati easter aes 1 5 SCEECH ADDE VIAND S arpei hacia iea ili be ieee na 8 aeabe eae ti Wd a iets 82 1 6 Gilossairy Of Clans GC Renin oirra ET E ET 1 7 PAULO SAI Plel I Cts 2 05575 aisca cdacnesbeadiatwatdncnt a n a ani e 1 7 Instrument SCC 1G Term cases aaa cease AE A aa 1 8 Glossary of Chromatographic Terms ox cesseceeidiadesiccnieceactinttecasnattee ATEA 1 10 Touch Screen Navi Gato ny oesistisssesscecdascscassecascueendbesaasissscecdnuecsedsasseuueendsebansascocasaussctnccnvent 2 1 CHAPE OVENI O OE ee ne ee en a ee nnn UE Nee ea ee ene Pe 2 3 TOUS CHC CMe sper oa ct e a Sah cat eet de ole dal Morac Sah cea ce NS te Sak Race RR a ct 2 4 MAS enei E a a r a Ea a 2 6 Non Coni eured Devices sirenes Tna eae atc ee ee oe 2 6 Nom installed DEVICES eron E em 2 7 R n BUTON asara E A 2 8 OPM a A ceienatnatancantisons sue tab ed anmeeatnataecomauias 2 11 Sena BUON ee ee ee ee ee 2 11 Heated ZOMG S esne a a a EN 2 13 Naiva on BaT eor 2 16 TECTO S i E E a aes E a a ln E E ER 2 17 Propran BUNON Suoraan E O E A AT idclinieys 2 18 Display TEx anan aaa eae 2 18 EE EEA E ELA AE AAA E ANE E E E AAA EEE sleet 2 18 Packed
100. cates that the flame is lit NOTE Jf you find it difficult to light the flame rotate the FPD cap so that the FPD outlet faces the front or left side of the instrument ignitor Figure 4 33 Ignitor assembly positioned on the FPD outlet 8 Remove the ignitor assembly from the FPD outlet If the flame is lit the signal on the Autozero screen should increase and remain greater than the noted amount Confirm that the flame is lit by holding a shiny object such as a mirror or small wrench over the FPD outlet Condensation will appear on the object if ignition has occurred 4 70 Clarus 600 680 User s Guide The FPD outlet is hot To prevent injury never place your hand over the FPD outlet WARNING NOTE To prevent condensation on the FPD always turn off the flame hydrogen and air gases before cooling the detector or turning off the Clarus GC 4 71 Setting Up the Detectors Detector Temperatures To display or change detector temperatures and turn the detector heaters on or off can be done from one screen in the Clarus GC The example shown below assumes that the Clarus GC has an ECD detector 1 Inthe System Status screen touch the ECD button Not Ready ie lv 2 Inthe ECD screen you will see the Make Up field to change the setting touch Tools and touch Configuration from the drop down menu 4 72 Clarus 600 680 User s Guide A PSSI Oven AECD Events irs i CFF 7 Healer Off
101. ch consisting of a hold time ramp rate and plateau set point Sequential set points may be greater than or less than the preceding set point The PPC system programs the carrier gas controller with a positive or negative ramp as required At the end of the GC oven program the carrier gas resets to the initial set point value in the method even if a carrier gas program 1s 1n progress The carrier gas also resets if the end of the carrier gas program occurs before the end of the oven program Carrier Gas Timed Events You can also use timed events to produce step changes in the set point Carrier gas events can occur before or after a run starts A carrier gas event supersedes the method set point value at the time the event occurs However if the carrier gas program in the method advances to a new step after a carrier gas event the new program step or ramp takes control Leak Checking The Clarus GC monitors the inlet pressure with a carrier gas mass flow controller in use After selecting the carrier gas Flow mode in configuration you can enter the maximum inlet pressure value If the inlet pressure drops below or rises above the set limit for more than one minute a warning message appears 3 22 Clarus 600 680 User s Guide Setting Carrier Gas Pressure To view or set the carrier pressure l From the System Status screen touch the corresponding Injector button A or B for which you want to set the carrier pressure T
102. creen varies depending on whether the detector is configured with manual or programmable pneumatics This section describes the screen components for each type of configuration Touching the Ignite button allows you to light the FID flame A FID Events i i 100 C Heater OF A PSSI Oven temp 00H my 190 C Aten fie g J AutoZero Range 20 e uput Recorder Offset Yo Filler 200 mS Flameout O 10 mv Gas fow rl sel Artal Ar 100 10 a H 20 02 ignite Ready Oct 11 Auto Ignition The PPC controlled FID has flameout detection and an auto ignite feature Flameout detection occurs 0 5 minutes into the PRE RUN time and it measures the user entered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignite automatically lights the flame before the start of a run With the FID temperature set the air and hydrogen flows set and auto ignition activated by setting a positive mV value for the flame offset the FID attempts auto ignition at 0 5 min before the system becomes ready At this Pre run time the status bar flashes Flame Ignition as the air flow is shut off hydrogen purges the FID for about 10 seconds and the ignitor energizes for ignition followed by a return of the air flow to the detector to sustain the flame 2 33 Touch Screen Navigation After the flame igni
103. d at the factory with the gas air and hydrogen that it controls therefore to set the gas flow simply follow this procedure Turn on the air at the source and adjust the line pressure to 70 90 psig source and adjust the line pressure to 70 90 psig 2 Press the Tools button and select d Configuration B Injector a The Configuration screen similar _ to the one to the right appears P i 3 Touch the button labeled as an A Injector A FID FID detector Pneumatics Relays 17 01 Close The configuration screen for the A FID detector appears Setting Up the Detectors in I Disable Filter 200 SetPoint Actual Flamecut O10 Gas Flow SetPoint Achal NOTE The screen above shows that an FID is installed in Channel A 4 Select a filter value from the Filter drop down menu Disable Filter E H Flameout Gas Flow SetPoint Actual afo o ZZ mL Hef o o o o 00 mhiin Recorder j integrator Offset G i Ready 17 01 a FE Cancel uput Clarus 600 680 User s Guide The default setting is 200 milliseconds To improve the signal to noise change the setting to 800 milliseconds This improves the noise but broadens the peak shapes If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase 5 Touch the Set Point dialog box for the FID Flameout and then
104. d to both output channels Both detectors should not be deconfigured at the same time 6 10 Clarus 600 680 GC User s Guide Deconfiguring the detectors also deconfigures the detector s PPC control You must reconfigure the PPC control when restoring the detector configuration 1 Touch the A Injector button Configuration Ay 5a B lAjechor E TCD i Over af A lnjector A FID Fun Seip Frneumaics Relays 2 00 34 Close The Configure Injector A appears Ready Configure Injector A Type EI r Capillary Control Carrier Control Off Flow Ofset Auto Fixed ofset 1 00 mLmin I HS Control Ready 11 18 a E OK Cancel 2 Select the Injector Type from the drop down list The Type options are None Packed Cap GSV PSSI and POC The example below shows None selected 6 11 Using the Tools Menu Configure Injector A Type None H D Capillary Control Flow Ofset Aut Fixed ofset 1 00 mmi 17 9 FE OK Cancel PSS Programmed Split Splitless Injector 6 12 The PSSI injector includes a Capillary Control option Capillary Control If the Capillary Control mode is selected the following additional parameters are displayed shown below in the bordered area and the Capillary Control can be configured for pressure flow and velocity When set for inlet programming the injector is first heated to the injector temperature ent
105. d touch the Tools button and touch Configuration from the drop down menu The following screen appears 4 25 Setting Up the Detectors Configuration B Injector a a i po a8 Br a A rypector 12 00 34 Close 4 In this Configuration screen touch the A ECD button The following screen appears a Disable Fiter 200 Gas Flow SetPoint Actual Make Up o o mumn uput Fecorder j Integrator Offset 5 To a Ready Mar 4 a E OK Cancel The Filter default setting is 200 milliseconds If you want to improve the signal to noise change the setting to 800 milliseconds however the noise improves 4 26 Clarus 600 680 User s Guide but the peak shapes broaden If you want a faster detector response change the setting to 50 milliseconds however the noise level may increase 5 To change the Make Up gas flow in this Configuration screen use the up and down arrow or keypad al T buttons 6 Touch OK when finished 4 27 NOTE Setting Up the Detectors Setting up a TCD The PPC pneumatics detector gas modules have been set to OFF at the factory TCD Overview The Thermal Conductivity Detector TCD is a dual channel detector that measures the difference in thermal conductivity between carrier gas flowing through a reference channel and carrier gas plus sample flowing through an analytical channel see the following figure
106. detector it is mixed with hydrogen and then burned in air generating ions The ions are collected and measured by the detector with their concentration proportional to the amount of compound present Ion collection is enhanced by a polarized electric field that is created by applying a negative voltage 200 V to the jet tip The detector sensitivity is affected primarily by the hydrogen flow The detector linearity is affected by the air flow The FID has flameout detection and an auto ignite feature Flameout detection occurs 0 5 minutes into the PRE RUN time and it measures the user entered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignite automatically lights the flame before the start of a run You can also manually light the flame at any time by pressing the Ignite button A cross section view of a FID is shown below Amplifier Connector Ignitor Polarizing Pin Collector s me IYN Flame Jet r H i T Air In ll Hydrogen In Flame Jet Extension Detector Fitting H Figure 4 1 Flame Ionization Detector FID cutaway view 4 5 Setting Up the Detectors Setting Up an FID To set up an FID that uses PPC modules first read the FID Setup Summary then follow these procedures To avoid injury Do Not turn on the hydrogen gas unless a column is connected to the FID and
107. do not modify the setings unless he hardware configuration has changed Do you want to proceed a Ready 17 01 v 4 FE OK Cancel Feslrictor 1 P Wacuurn ia PRET 6 34 conhigure PPC Devices Carrier Detector ALX Channel A Channel B PPC 1 Carr Flow Gas He gi Restrictor 4 9 Zero Calibrate PPG 11 Split Chr Zero E Ready E _ Clarus 600 680 GC User s Guide Connecting the PPC Modules The Clarus GC PPC modules have been properly installed and configured at the factory for your specific combination of injectors and detectors The configuration information is stored in a reserved area of the battery backed memory however if the memory lost the PPC module connect configuration or if you installed a new PPC module by purchasing an add on kit you must follow the procedure s listed in this section By connecting a PCC module you actually set the Clarus GC controlling software to recognize a specific PPC module that is installed at a specific location This is necessary so that the software can control the installed hardware The PPC board has 12 sockets to which various injector and detector modules are connected The socket locations and descriptions are listed in the following table and shown in the following figure Table 6 1 Injector and Detector Socket Descriptions Injector 1 Injector 2 Injectors Carriers 4 J10 2 J
108. dure NOTE The photomultiplier tube can be damaged if it is exposed to light while voltage is ON Never remove the detector cap or Photomultiplier tube WITH the voltage on 4 68 Clarus 600 680 User s Guide Ignite the Flame 1 Open the electronics cover to access the ignitor assembly Figure 4 32 Ignitor assembly 2 From the system status screen touch the FPD button 3 The FPD tab page is now visible B POCO Oven B FPD Events EO i OFF ie Healer Off temp 00H my 25 C Aten 4 H I AutoZero w PMT On is Linearizer On Filler 200 ma QuUbuUE Recorder PRT volage OFF Offset ri Gas flow iL gel Actual Ar 450 45 He 460 45 Ready 17 01 EEE aj E s NOTE For proper ignition to occur the FPD must be heated to at least 250 C 4 Use the up and down arrow or keypad nd aj z22 buttons to enter a setpoint of at least 100 C this is the minimum entry for a FPD in the temp field 4 69 Setting Up the Detectors il ag C temp or enter a temperature that is 50 C higher than the highest temperature of your oven program 5 Close the oven door Wait for the FPD 1 temperature to become READY 6 Position the ignitor assembly on the FPD outlet see the following figure 7 You may hear a slight POP This indi
109. e Close Touch Close to close the Connect PPC Device screen Sep Pneumatics Relays Touch OK on the Configuration PPC screen 2 26 10 The Configure Injector B screen appears Configure Injector B Type EM Carrier Contral Pressure A Leak Threshold 0 00 m Limin iroi OK Cancel 12 To exit out of Configuration touch the OK button then touch the Close button 13 Display the active method and view the B Pkd injector parameters as shown on the right Clarus 600 680 GC User s Guide 11 Select Pressure or Flow from the drop down menu Configure Injector B Type Fke Carrier Control Off H Leak Threshold M 17 01 OK Cancel EN a Oven BTCD Events Healer Off OFF ie 25 C bam Carrier Gas O10 psi g a rnb JFF psi press init Program 17 01 Tools 2 27 Touch Screen Navigation POC The packed on co lumn injector can be programmed by Inlet POCI or Oven POCO The POC injector is configured and controlled according to the same parameters as the PSS injector Packed On Column Inlet Packed On Column Oven Oven A FID Seas Oven A FID Events Heater Or Heater Of me gal nl ae ee e cC lempit C tetnp init acral Progratri f Carrier Gag O H Carrier Gas 0 4 psi 10 0 pi Lat 10 0 psi press inil Program pressini Program Split A Ee oN total flowy tatal Aow 1 100 mLin
110. e Flow Ofset Flon Palio euo Fixed Leak Omit 9 0 mLtnin HE Control vacuum Compensation l l OK Select either a Flow or Ratio Split mode 3 38 Clarus 600 680 User s Guide Touch OK The Configuration screen appears Touch Close On the System Status screen touch the corresponding Injector button The active method screen appears A PSSI oven AFID Events Je Heater Of L re 25 C termp init Prograrn i Carrier Gas ao psi z 6 00 mum 20 ps O 0 crivsec press inil Program Split total Aow 0 S0 1 rato ralio Not Ready 101 E vale mew The screen above displays the Split mode configured for Ratio Touch the ratio field to modify the value OR If you configured the split mode for Flow the following screen appears 3 39 Using the Active Method NOTE Please note that if the displayed value is much greater than the total flow defined as split flow and septum purge column flow this indicates a leak 3 40 A FID Events fe Heater Of 2 C temp init Oven Prograrn j Carrier Gas 0 0 psi a l 0 00 mLin aM psi 0 0 crvsec press init E Split total Aow g zo mbm 0 ralio 17 4 FEF Tools x The Total Flow split vent septum purge column is displayed as a non editable text field The septum purge flow is factory preset to 3 0 mL min It is not user adjustable If
111. e NPD and all fitting connections have been leak tested WARNING Nitrogen Phosphorus Detectors NPD use hydrogen gas Before you turn on the hydrogen gas to the NPD ensure that a column is connected to the NPD fitting inside the oven Turning on the hydrogen gas without first connecting a column to the NPD could create the possibility of an explosion in the oven 4 43 Setting Up the Detectors Turn off the hydrogen gas before disconnecting a column from the NPD When two NPDs are installed but only one NPD has a WARNING column connected to it plug the inlet of the NPD without a column with a 1 8 inch stainless steel plug P N N930 0061 to prevent hydrogen from back diffusing into the oven NOTE NOTE NOTE The detector gas modules have been set to OFF at the factory for both manual and PPC pneumatics NPD Overview The nitrogen phosphorus detector NPD is a highly specific thermionic detector for organically bound nitrogen and phosphorus When using capillary columns with the NPD Hydrogen is NOT a recommended carrier gas The additive effect of the hydrogen carrier gas and the hydrogen detector gas affects the sensitivity and selectivity because it produces an overall higher hydrogen gas flow If you are temperature programming column flow changes may produce a negative baseline drift The detector operates by electrically heating a glass bead that contains an alkali metal to the point where it emits e
112. e analysis Injector Terniperabre Prograrn Current 20 ee i 260 C tmp rme rale ae minutes Gmin Init Time O 00m End 1 67 f Close Touch the Carrier Gas Program button This displays the Prograrn Carrier Pressure Program screen Setting up a Typical Analysis 6 Injector Ternperature Prograrn LA Current eo 0 20 00 80 00 i eel 1G temp birrie rale a minutes Cimin nial 250 60 0 2 Init Tire O00 m End 1 67 tr Close Select the Initial psi field Use the up and down arrow or keypad a 322 buttons to set the carrier gas pressure to the required pressure for your application Repeat the same procedure for the time and rate As shown in the example this analysis has been set to have an initial temperature of 255 C and it is held at this temperature for 60 minutes then going up 2 degrees 8 Touch Close when you have entered all the parameters 7 10 Clarus 600 680 GC User s Guide Detector Settings Flame lonization Detector FID 1 Touch the FID button ay on the Status Screen 2 To program the temperature in the FID tab touch the Temperature field and it will turn black Then use the up and down arrow or keypad kd aj 77 buttons to set to the required temperature for your application 3 Set the Atten attenuation and Range by touching the arrow button and selecting a value from the drop down list as shown in
113. e is no default as this field will be already filled by a previous calculation result Velocity This is a selectable field and if selected the tO field is also enabled for input The Inlet Press and Flow fields are deselected and are display only The carrier gas velocity is in units of cm s 1 to 500cm s in 0 1 cm s increments There is no default as this field will be already filled by a previous calculation result Split Flow Calculations Screen Column flow rate This field will take its initial value from the Main Screen Flow field The same range and units will apply If the value is changed in this field the entry in the Main Screen will also be updated and the input pressure velocity and t0 will be recalculated Split flow rate This field will use mL min units 0 to 500mL min range in I ml min increments The default will be 50mL min Column i d This field will take its initial value from the Main Screen Diameter field The same range and units will apply If the value is changed in this field the entry in the Main Screen will also be updated and the active input pressure flow or velocity and t0 will be recalculated Liner i d This is the internal diameter of the injector liner The input range will be 0 1 to 6 0mm in 0 1mm increments 6 71 Using the Tools Menu Split flow ratio Value displayed to nearest integer Dimensionless units Split velocity ratio Note that the split dynamics occur a
114. e of the current method The list of method names always displays External in the last position If you do not change the name or select another method from the list clicking OK prompts the dialog box to confirm that the existing method will be overwritten Method Editor This action vill overwrite the existing method Do you want to continue Yes Ho Cancel Clicking Yes overwrites the stored method with the new method pneumatics with the same name To assign a new method name touch the name field to invoke the alpha numeric keypad 5 13 Using the Method Editor Method Hame Alpha Num Accent Katakana patie Jie i ad Le e r EA ee Es ES Pm Lan Le e Lalli jis JL Ly Jv2 OK Cancel D Although a new method name field displays the name untitled the field to enter the new name is blank The Method Name field displays each character as it is touched starting from the center of the field The name can be comprised of any combination of letters and numbers and is limited to 13 characters Touching OK closes the keypad and displays the Save As dialog box with the name entered in the name field Touching Cancel closes the keypad and displays the Save As screen The name field is not modified The External method is always the last entry in the list The External method cannot be renamed but it may be overwritten Touching OK saves the edited method under the assigned name T
115. e or flow The following procedure shows how to navigate through the screens to configure PPC for a packed column injector 1 Select Configuration from the 2 Touch the Pneumatics button Tools menu Ay AA oy Configuration Gwern ae IL Events Heater Of os OFF g a 26 C mem Carrier Gas hethiod Editor 00 psi Event Log 0 0 riL haintenance press namane A Injector bli Z tt Pur Sep FPreumatics Relays Ready hlar 4 Close 2 24 3 Touch the PPC Connect button Configuration PPC PPG Connect Reference Selings Manual Phneumatcs PPC Alarm Enable Ready 17 01 a Bl OK Cancel Caublon To avoid damaging he PPO systern do not modify he setings unless he hardware coniquraton has changed Do vou want bo proceed OK 4 Touch the OK button Clarus 600 680 GC User s Guide 5 Touch Carrier B to Configure your Packed column injector for PPC Connect PPC Device Carrier B Detector B ob Detector 4 A Al A A AUX 1 AUK Z AUK Aux 4 Carrier A la Ready 1701 Close 2 25 Touch Screen Navigation 6 Select Pres Read from the drop 9 Touch the B Injector button on the down menu Then touch the OK Configuration screen button Connect PPC Device Configuration PPC Define Carrier B api B Injector _ Functor Position carr Flow H jz e secondary Position x Pres Read e fiz e A Injector har 4 har 4 Clos
116. eached full Ready status Stop Button As soon as the Start button is touched the Stop button appears on all top level screens Reach Running init E e Touching the Stop button before the system is running prompts the following dialog box Are you sure OK Cancel Touch OK to cancel the run The status bar reflects that the system is running and the Start button changes to Stop 3 55 Using the Active Method Run Type Aulosarnpler J hlanyal Program 1 Program 2 Tasks Method Aromatics Vials n Vol EZ uL Injector JA 6 njecions ial Stabs wal 10 Program 1 es Injecton 10 of 1 a Funning init 14 11 43 ET A Fi l Touching the Stop button displays the following start menu dialog box Stop at the end of this run Pause after this run Go fo a lemp program step Cancel ls Running init casa Stop Immediately The Autosampler stops and the stop buttons turns to Start Stop at the end of this run The user can allow the current run to complete and then stop the Autosampler sequence 3 56 Clarus 600 680 User s Guide Pause after this run The system may be paused to stop any further injections until resumed by the user When the system 1s paused the Stop button turns to Resume on all top level screens Paused Go to a temp program step Displays radio buttons that allow the user to ballistically raise the oven
117. ead the ECD setup summary then follow the steps ECD Setup Summary To set up an ECD e Vent the ECD outlet e Adjust the make up gas flow PPC and manual pneumatics e Make sure a column is installed 4 22 NOTE NOTE Clarus 600 680 User s Guide Because an ECD is extremely sensitive contamination from any part of the system can add to the background and noise To help assure a clean system the injector and detector should be baked out and both packed and capillary columns thoroughly conditioned before use When conditioning columns for use with an ECD DO NOT attach the column to the ECD Clean tubing and pure filtered gases should be used Whenever a column is disconnected from an ECD the ECD should first be cooled to avoid oxidation of the Nickel foil Vent the ECD Outlet If venting the ECD effluent is required attach an additional piece of tubing to the tubing that is connected to the ECD outlet This does not affect the performance of the ECD 1 Open the detector cover see the following figure to expose the top of the ECD ae Figure 4 7 Top view of an ECD 2 Remove the two screws that secure the insulating cover to the Clarus GC 3 Remove the insulating cover and detector cap This exposes the ECD outlet see the following figure 4 23 Setting Up the Detectors 4 Attach the outer metal sleeve of the vent tubing P N N610 0161 to the ECD Outlet Figure 4 8 Connecting vent tubing
118. ect the Vacuum Compensation checkbox 6 14 Clarus 600 680 GC User s Guide Packed Injector 1 This example shows that Pkd a packed column injector is selected as the Type on the Configuration screen Configure Injector B Type Pkd l Carrier Control Pressure H Leak Threshold O00 mLimin 0 04 min FFE OK Cancel 2 Make your settings then touch the OK button Then touch the Close button to exit configuration POC Programmable On Column Injector 1 This example shows that POCO a programmable on column injector is selected as the Type on the Configuration screen 6 15 Using the Tools Menu Configure Injector B Type POCO B Capillary Control Carrier Control Pressure B Flom Ofset Auto Fixed ofset 0 00 rLimin hiar 4 OK Cancel 2 Make your settings then touch the OK button Then touch the Close button to exit configuration Capillary Split Splitless Injector 1 This example shows that Cap a Capillary Split Splitless injector is selected as the Type on the Configuration screen Configure Injector A Type Cap J Capillary Control Carrier Gontral Pressure El Program J Oventrack column Length 25 00 mo LOJ 250 um Split mode Flow Ofset Flow 3 Ralio Auto Fixed Offset 7 00 mbt HE Control P Vacuum Compensation 17 01 PEE K Cancel 2 Make your settings then touch the OK button Then touch the Close button to e
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120. eees 3 27 Setting the Septum Purge Mode and Offfset cccccccccccccceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeees 3 29 Sn E ID VAI CS essa este a a A toes 3 37 setting the Split Mode Using PPC seca ersen nena ei eee ee 3 37 Set up the Splitless Mode for a CAP or PSS Injector cccccccccccccceeceeceeeeeeeeeeeeees 3 41 Splitless Injection with Pressure Pulse Flow Pulse Velocity Pulse Technique 3 41 Contolling th Aut samplersissssennnroin dereires eneoti a anai esna i iait 3 51 utosamipler Traysand Carousel scarier EAE 3 51 Autosampl r Touch Serec iien eE OOE 3 53 Sr BULON ternen a a a Gc testc tee anata aul Caen e he destie 3 54 SOP DUON aig sees occ ed acci iat baad nacre geen seat paalnals Sede cele ete abe nvoeau sea pandase A 3 55 About Waste and Wash VidlSisarse neen lias duaioncil E a a a 3 62 Miulti Proerain Mode sssrini p e EiT pEi Riia 3 62 POUG Salle NV TANS eaa E bes eae 3 63 Using a TCD with the Autosampler crsiranescnonnii A 3 63 PN VAMADIC SS VOCS na e a ld van re aca dolar le aes 3 64 Petting Up the DECOT Siaa E aE 4 1 OVON OW ea E 4 3 Iv BREE 1c eh eee eR Ena eA OED DONT EUR ORT NOT AU EER eC ER CoP SE E See AAE OnE Ter ee 4 5 Seine Upan FID oeps Ri dia ai E ERa de tarindents 4 6 Automacally Tenite Me Flame scscrsec 2 acess es outa E es esata 4 11 Manually lontte the Plame crn ena eee 4 13 Using the FID in Corrosive Environments cccccccccccccceeceeeeceeceeeeeeeeeeeeeeeeeeeeeees 4 15 BIT dl e
121. elow to drop the bead below the active level Remove the Detector Cap Nut P N N9300061 and reconnect the column to the detector Set the desired column flow for the application to be run then again increase the bead current potentiometer to give a reading around 0 5 mV on Range 1 Allow the baseline to stabilize for 30 minutes Using the potentiometer adjust the baseline between 0 4 and 0 6 mV at Range 1 and the bead ready to use After conditioning the bead remove the Swagelok plug from the detector fitting and reconnect the column 4 51 Setting Up the Detectors EAM Over A NPD Events i ag Heater Off temp Me 4 09 m ao c ae 16 AutozZero Ti Output Recorder a al Range Offset 5 Fiter 200 mS Gas Flow mL set Actual Ar 450 O He 45 O Running Rate 1 2 17 min EE toser 15 Make sure the column flow is properly set Touch the signal icon a to display the detector background produced by carrier gas flow The bead background will be less due to cooling effects 16 Turn the bead potentiometer dial clockwise until you achieve a reading of 0 25 mV above the off reading with the detector range set to x1 17 Once the system has stabilized it is ready for operation If you are unable to achieve adequate sensitivity for your standard increase the background of the NPD Increasing intervals of 0 25 mV are recommended Adjust the background setting
122. emperature PPC version only A program that specifies the rate of oven program temperature increase from one plateau to the next and the time the oven temperature is held constant at a plateau Timed Events Events that take place before or during a GC run as specified in a timed events table A heated area in the GC oven injector or detector 1 9 Introduction Glossary of Chromatographic Terms Adsorption A process that occurs at the surface of a liquid or solid as a result of the attractive forces between the adsorbent and the solute These forces may be physical or weakly chemical Analysis The complete investigation of a sample by gas chromatographic separation including identification of the sample components and quantitative measurements Anode The positively charged electrode in any electrical circuit to which charged particles and ions are attracted Band Broadening A process that occurs in the GC whereby the peak width for a component increases the longer the component travels through the column Baseline The detector signal to a recorder or integrator when only the carrier gas is passing through the detector Baseline drift Any regular change occurring in the baseline signal from the detector usually resulting from column temperature and or gas flow changes Blank run A run without the sample being injected Bleed The evaporation of the stationary phase from a column Capill
123. en and detector heaters e Equalize the makeup and reference gas flows e Enter the TCD bridge current e Balance the bridge Turn on the Oven and Detector Heaters 1 Close the oven door This turns on the oven heater 2 From the System Status screen touch the TCD button 2 l 4 29 Setting Up the Detectors a ae temp 2 Inthe TCD tab page touch the temp field and use the up and down arrow buttons or the numeric keypad to enter a TCD temperature appropriate for the analysis to be run 3 The detector heater can be turned on or off by touching the Heater On Off button B Pkd Oven B TCD Events ED i qoo C Heater Of temp 0 00 my 26 C an 256 eI P AutoZero Current 40 mA Output Recorder ofset w Filter 200 mg gas fow rL gel Achal Fef 0 Make Up 0 0 0 0 Ready 4 30 Clarus 600 680 User s Guide Equalize the Makeup and Reference Gas Flows The following procedures describe how to adjust the makeup and reference gas using PPC pneumatics in the Clarus GC The TCD flow module for reference gas is calibrated with CAUTION helium at the factory You must recalibrate the TCD flow module if you are using a reference gas other than helium For optimum performance apply a minimum flow of 5 mL min to each of the two detector channels Set the Makeup and Reference Gas With PPC pneumatics the reference gas is set from the Clarus GC touch screen Also PPC pneuma
124. ered in the method and then follows the injector temperature program The temp field does include a program settings button in this case If the Capillary Control mode is set for flow or velocity the radio buttons for Program and Oventrack are deactivated If the mode is set for pressure and the Oventrack radio button is selected the column dimension fields are deactivated In this case the pressure is entered in the method and the software maintains the column flow based on the initial oven temperature and pressure When the Oventrack mode is selected you cannot view the flow or velocity If Capillary Control is not selected the split pneumatics only controls the inlet pressure and split flow The options in the field include None and Pressure The Column Length and ID fields and Split Mode radio buttons are deactivated when capillary control 1s off Configure Injector A Type PSI H Capillary Control Carrier Control Pressure Flow Ofset JAU Fixed afset 1 00 mLmin H Control a Ready 17 01 4 gag OK Cancel v a JE OK Cancel column Length 25 00 mo LD 250 um Split mode Clarus 600 680 GC User s Guide Configure Injector A Type PSSI H M Capillary Control Carrier Control Pressure Program J Oventrack Flow Offset _ Ratio Auto ay Fixed ofset 1 00 9 mbtnin T H Control T vacuum Compensation 1701 BEB BE BEB The Flow Offset radio
125. esence of a sample component in the carrier gas flowing through the analytical channel changes the resistance of the filaments in that channel This unbalances the bridge and produces a signal proportional to the amount of sample The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configuration Screen E Disable Filer 200 B Pkd Oven B TCD Evers Ep qo C Heater Off temp 0 00 mY 100 C Aer 256 gp e Autozero Current 40 T mA citput Recorde fet T Filler 200 mS SetPoint Reference a0 hake Wp ERN Ready Oct 4 JE OK Cancel Tools hd 2 36 Clarus 600 680 GC User s Guide ECD The Electron Capture Detector ECD is the most sensitive detector available for the analysis of electrophilic compounds such as chlorinated hydrocarbons found in pesticide residues It is concentration sensitive and nondestructive The ECD cell contains a nickel foil in a cylinder through which the carrier gas flows The coating of the foil s inner surface contains the radioactive isotope Nickel 63 and has a nominal sensitivity of 15 mCi To optimize detector response make up gas is combined with column effluent Beta particles emitted from the isotope ionize the carrier gas The resultant ions and electrons travel to the collector anode assembly under the influence of a pulsed polarizing voltage applied b
126. et in PPC configuration display the configured unit type and include a status indicator light The initial values can be modified via timed events The current value is shown next to the initial value field 2 50 Using the 3 Active Method Using the Active Method Clarus 600 680 User s Guide Overview The Clarus GC 1s controlled by a collection of operating parameters called the Active Method You can prepare and save up to five methods and make any one of them the Active Method However the fifth method is reserved for TotalChrom external computer controlled software and may be overwritten The operating parameters include the an oven temperature program injector temperature or injector temperature program detector temperature or detector temperature program carrier gas pressure set for pressure flow or velocity valve settings for example the operation of a gas sampling valve or split splitless operation of capillary column a timed events table and a variety of parameters for controlling data output Active Method parameters are always saved when you turn the Clarus GC off and automatically reloaded when you turn it back on 3 3 Using the Active Method Editing the Active Method If you have read and used the chapters in this manual sequentially as recommended by now you have probably installed and conditioned one or two columns and set up one or two detectors Also you were probably
127. ete Error Cannot delete Fom an empty list Clear Touching the Clear button deletes the contents of the entire event table A dialog box confirms the action lear Events Table Are You Sure Pressing Yes clears the table Touching the No button closes the dialog box and retains the contents of the Events table If the table is empty the following Error message appears 2 45 Touch Screen Navigation A PSSI Oven A FPD Events Value Time Event Aux Gas Add Edit Relays Delete Clear 17 01 Tools x Value The value box function depends on the event For some events such as Carrier X a numeric value is required For others such as TCD polarity a choice between two options is required 2 46 Clarus 600 680 GC User s Guide The PreVent ProTect MS Vent valves are never operated during a run and are not required in the Timed Events list e No timed event should have the same time as another timed event Time resolution is 0 01 minutes e Timed Events may be entered and removed in any sequence e Pressing the Clear button prompts a dialog box This action will clear the entire table Do you want to continue Yes No e Timed Events are re ordered chronologically after each entry The capacity is 32 entries 2 47 Touch Screen Navigation Relays They appear as set in the configuration screen inital Current eRe Se EADIE 9 Ex
128. etector Cap Nut is in the 1 8 in Plug Kit P N N9300061 Capillary Column Setup With a capillary column connected adjust Carrier flow to 0 5 mL min or less but not 0 or preferred disconnect the column and cap the oven end of the detector Reactivating a Used NPD Bead Preparing to Activate the NPD Bead To activate a NPD bead NOTE Never activate a NPD bead with a column connected to the detector fitting To properly activate the NPD bead the column must be removed from the detector fitting and the detector fitting must be capped 4 48 WARNING NOTE NOTE Clarus 600 680 User s Guide Obtain a stopwatch or use the stopwatch function in the GC Utilities screen Open the oven door and allow the oven to cool Using a 7 16 inch wrench loosen and remove the column nut from the detector fitting Remove the column from the detector fitting Install a 1 8 inch Swagelok plug P N N9300061 on the detector fitting Provide a leak free seal by tightening the plug with a 7 16 inch wrench Close the oven door Maintain a carrier gas flow through the column Install the bead in the conventional manner according to the installation procedure in the GC Hardware Guide Make sure that the bead does not contact any other surfaces Set the following conditions in the following order Set the Detector temperature to 150 deg C or greater Wait for the detector temperature to stabilize If a capillary column is
129. eter 2 Place the thermometer probe in the oven 3 Equilibrate the oven temperature 4 Enter the required offset value 5 Remove the thermometer probe Calibrate the Reference Thermometer Calibrate your reference thermometer according to its instructions If the thermometer has been calibrated by an outside service there is no reason to recalibrate it yourself 6 60 Clarus 600 680 GC User s Guide Place the Thermometer Probe in the Oven The thermometer probe must be placed as close as possible to the same position in each GC oven to be calibrated Access to the CAUTION oven is provided on the left side oven wall l Turn off the power and allow the oven to cool 2 Remove the left side instrument cover Note the location of three approximately 1 inch diameter holes that correspond to the holes on the left side of the oven One or more of these holes may be occupied by gas sampling valves lt Oe tt a Holes ey ts o Figure 6 5 Left panel removed to reveal left side of the oven exterior 3 Insert t
130. etween the source and the collector The pulse frequency is varied to maintain a constant average current The presence of an electron absorbing species in the detector decreases the current as the absorbed electrons form ions which travel more slowly than electrons The pulse frequency of the polarizing supply is automatically controlled to maintain a constant current and is used to form the detector output signal The ECD works with nitrogen carrier or makeup gas or a carrier or makeup gas mixture of 95 argon 5 methane When using capillary columns at low flows 5 mL min or less helium or hydrogen may be used as the carrier gas provided nitrogen or argon methane is used as the make up gas A cross section view of an ECD is shown below The 63 Ni radioactive foil coating and requires careful handling to ensure that it does not create a safety hazard In order to prevent a Thermal Runaway risk the GC shuts down if any heated zone exceeds 470 C If this occurs the following message appears Warning Instrument Shutdown Thermal Runaway xxxxxx zone Call your PerkinElmer service representative 2 37 Touch Screen Navigation Instrument shutdown also occurs if there is a PRT Platinum Resistance Thermometer or MPU Micro Processor Unit failure In this case the following message appears Instrument Shutdown xxxx zone PRT error Call your PerkinElmer service representative The ECD works with nitrogen carrier or makeup gas or
131. ew In the Flame Photometric Detector FPD the column effluent is mixed with hydrogen and then burned in air Light emitted from the flame passes through a lens filter and to a photomultiplier tube which generates an electrical signal The Flame Photometric Detector is used for detecting sulfur phosphorus or tin compounds which produce chemiluminescent reactions with emissions at wavelengths characteristic of the S Sn and HPO species A filter that isolates sulfur emissions P N N6000637 is supplied with the detector Another filter that isolates phosphorus emissions P N N6000981 and a filter that isolates tin emissions P N L4145472 are available from PerkinElmer at www perkinelmer com 4 55 Setting Up the Detectors A cross section view of an FPD is shown below pt Optical Filter Assembly Cap it Window Filter L Assembly Airin O Ring Nall lt Hydrogen in Photomultiplier Tube Assembly A Column Connection Figure 4 31 Flame Photometric Detector FPD
132. f the NPD is detector 2 rear position the potentiometer is located on the right side of the panel NPD Detector B Mounted in the rear position Figure 4 30 Location of the Potentiometer Dial 4 50 Clarus 600 680 User s Guide Activating the NPD Bead The bead requires an activation step prior to use Do not inject a sample during Activation To Activate the bead carefully follow this procedure in sequential steps below I 2 Turn the bead potentiometer dial clockwise to apply current to the bead Slowly increase the NPD control voltage potentiometer to a setting of 700 Note The bead will gradually acquire an orange glow at this point Oe ON e ee 12 13 14 Wait for 5 minutes then increase the potentiometer to 750 After 1 minute move the potentiometer to 800 After 1 minute move the potentiometer to 850 After 1 minute move the potentiometer to 900 After 1 minute reduce the potentiometer to 850 After 1 minute reduce the potentiometer to 800 After 1 minute reduce the potentiometer to 750 After 1 minute reduce the potentiometer down to 700 For Capillary columns Wait 10 minutes go to the NPD detector screen then adjust the potentiometer so that the NPD baseline response reads around 0 5 mV on Range 1 Then set the desired column flow for the application to be run For Packed Columns Wait 10 minutes go to the NPD detector screen then adjust the potentiometer down to 500 or b
133. from the system status screen F g5 EA Aux Pre Run 0 04 min cE tats v 1 Touch the Oven button aW to display the oven information a 2 The oven information is now visible To program the oven temperatures touch the temperature field and it will turn black highlighted Then use the up and down arrow or keypad al T buttons to set to the required temperature for your application Repeat the same procedure for the time and rate As shown in the example below this analysis has been set to have an initial temperature of 75 C and it 1s held at this temperature for 1 minute then goes up 10 degrees minute 7 4 Clarus 600 680 GC User s Guide A PSS Oven A FID Events cl Temp Time Rate nit f 1 00 ioo a C a 100 100 so 4 150 100 END w 7 5 Setting up a Typical Analysis Injector Settings Packed Column PKD Injector 1 After entering the oven settings touch Injector B the Pkd tab and then touch the Temp field The field is highlighted to indicate that it is selected Use the up and down arrow or keypad al Z22 buttons to enter the proper initial temperature for your application B Pkd oven B TCD Events Heater Off i EE n Ts j Carrier Gas 0 1 psi ag milin TER 100 pressini psi aa Tools gt 2 Next set the carrier gas by touching the Program button to display the Carrier Pres
134. g the oven temperature as quickly as possible to reach a set point Soft Cooling Soft cooling is a technique whereby the cooling rate of the GC oven is initially limited by controlling throttling the intake of the ambient cold air used to cool the oven Detector The detector output signal when no components are being background eluted Equilibration The delay time after the method set points have been reached before the system becomes READY Flameout Detects if the flame is on to prevent injection into a nonfunctioning system and subsequent loss of sample Isothermal A method in which the oven temperature remains constant method throughout a GC run Method A collection of parameters that control the GC Negative time A timed event that you set to occur before the instrument event becomes READY 1 8 Clarus 600 680 GC User s Guide Parameter An independent variable used to specify a condition to be met Programmable Pneumatic Control Pre run The time after equilibration during which negative time events are executed PPC version only Sample management system Range For a Flame lonization Detector range means sensitivity of the detector output signal Ready Indicates that all method parameters have reached their set points and that you can start your analysis Run The time from sample injection to the end of the oven temperature program Sleep mode The GC can be set to a predefined method for gas savings T
135. gas 6 54 calibrating detector gas 6 58 zeroing the module 6 49 PPC Modules connecting 6 35 Pre abbreviation 1 6 Pressure Programming 1 11 Pressure Pulse Splitless Injection 3 41 Priority sample inserting 3 62 Psi abbreviation 1 6 psig abbreviation 1 6 PSS abbreviation 1 6 R Reference Pressure setting 6 53 Clarus 600 680 GC User s Guide Reference Temperature setting 6 53 Release 6 78 Rerouting detector output 4 83 S Screen abbreviations 1 6 Septum Purge Mode PPC viewing setting 3 29 Setting injector temperature 3 14 Setting up isothermal temperature program 3 8 multi ramp temperature program 3 11 one ramp temperature program 3 10 3 19 split mode 3 41 splitless mode 3 41 Setup summary ECD 4 22 FID with PPC 4 6 FPD with PPC 4 57 PID 4 38 TCD 4 29 Split mode setting up 3 41 Splitless mode setting up 3 41 stopwatch 6 76 Syringe cleaning 3 60 System Status Screen 7 4 T TCD abbreviation 1 6 balancing the bridge 4 34 polarity changing 4 80 range vs bridge current 4 78 Index setting up PPC 4 31 using with autosampler 3 63 4 35 Temperature program isothermal setting up 3 8 setting up a multi ramp 3 11 setting up a one ramp 3 10 3 19 Temperature Programming 1 12 Timed Events 2 42 Timed Events Table 2 43 Tools Menu 6 3 configuration 6 10 detector gas modules calibrating 6 57 event log 6 5 maintenance 6 6 method edito
136. gi 25 00 m LO 260 ur Split mode Flow Ofset Split riode Flow Ofset Flow 3 Ralo uo J Fixed Flow J Ratio Juo Fixed Leak mit 30 0 mLimin ofset 4 00 mitin T H Control Vacuum Compensation H Control vacuum Compensation 17 01 Ready 17 01 FEF OK Cancel a OK Cancel In the Auto mode the system performs a PreRun for one minute before it becomes READY the split vent is closed and the system measures the septum purge flow plus the column flow This is referred to as the offset The septum purge flow is controlled but not user selectable it is factory set to 3 mL min The split vent flow is restored to the value set in the method and the system stabilizes for 30 seconds This entire procedure takes one minute In the Fixed mode enter the offset value This value should be equal to the septum purge flow plus the column flow If the wrong value is entered then the difference is added to or subtracted from the split vent flow so your actual split vent flow may be slightly higher or lower than the value entered in the method In both cases the split ratio is maintained for every injection If you want to save time from run to run select Fixed mode The Auto mode is recommended to improve area precision and is required for vent flows less than 50 mL min If Auto is selected the Leak Limit appears Using the up and down arrow or keypad a buttons enter a value slightly
137. h is equal to the septum purge flow plus the column flow at the time of injection Since the system controls the total flow equal to the split vent plus septum purge plus column flow the septum purge is fixed and the column flow is controlled the difference between these two flows and the offset entered will go out the vent flow This will be consistent for each run If Fixed is selected use the up and down arrow or keypad al E to enter an offset value in mL min buttons Press OK Skip steps 9 16 if you are only programming the capillary control for pressure If you wish to program the Capillary Control for more than just pressure check the Capillary Control check box from the Injector tab Configure Injector A Type PS8 E M Capillary Control Carrier Control Pressure E Program J Overtrack column Length 25 90 mo LD 250 um Split mode Flow Offset e Flow Ratio Abo J Fixed Leak Omit 9 0 mLinin HS Control vacuum Compensation Mar 4 EEE OK Cancel 3 31 Using the Active Method From the Carrier Control drop down menu select from the following options Off Pressure Flow or Velocity 8 Select either Program or Oventrack However if you select the Oventrack The following screen shows Program mode you do not need to enter selected column dimensions and you can skip to step 12 Configure Injector A Configure Injector A Type PSSI_ F Capillary Control Type
138. h method is reserved for TotalChrom and may be overwritten If you attempt to overwrite the method it Log Out will retain the name External to remind you that this is a possibility You cannot access the Default method This method is ik J used by the system to populate a method with default values when the New Method menu option 1s selected The default settings are the same as the current or active method 5 4 Clarus 600 680 GC User s Guide Method Edit Mode gt Event Log 4 Maintenance configuration lilies Toul x When you touch Method Editor from the Tools menu a screen similar to the status screen appears Using the Method Editor Method Editor Pkd Oo Pos Aus f Aux Method Klethod File The buttons with icons provide access to the injector detector oven and aux settings associated with the Active Method in the method mode If an Aux temperature is configured an Aux button appears on the method edit screen The Method Edit screens are similar to the Active Method screens with the following differences e The run and signal icons on the top navigation bar are absent e No configuration information appears e No ignite button on the FID screen e No status bar or current information e The Start and Tools menu button in the bottom bar are replaced with the File menu button Clarus 600 680 GC User s Guide The following screens show the difference
139. hange it on the Event page For certain analyses such as those for trace or concentrated components you may wish to change the Range during a GC with a Timed Event run The following example illustrates this 4 74 Clarus 600 680 User s Guide Changing the FID PID or NPD Range During a Run To automatically change the range from 1 to 20 after 1 minutes into the run The example below uses FID but the following procedure can also be used for PID or NPD 1 Touch the Event tab to view and change a range during a run 4 75 Setting Up the Detectors Method 5 CHC AALS APSSI Oven AFID Events Add Timed Event Event AutozZero A Bi Time O00 Value Ol OK cancel a Ready 17 01 In the Add Timed Event screen enter an Event by touching the down arrow in the Event field to view the other ranges Select the one you need by touching it Evert AutozZera A biar 4 Tools x 4 76 Clarus 600 680 User s Guide 4 Enter atime by touching the Time field and using the up and down arrow or 6 7 buttons enter the time required for your analysis This will keypad a FE change the time for AutoZero A as shown Enter a value for the AutoZero A by touching the Value field Then using the up and down arrow buttons enter On or Off Method 5 G ma APSSI Oven AFID Events Add Timed Event Event AutozZera Ay Bi Time 120 Vaue M OK Cancel
140. he injector screen appears Oven 4 FID Events Heater OF 76 C ternp init Program i Carrier Gas 0 0 psi P oul psi press inil Progra E Split total fov 0 GFF mbm fow Read 17 0 Tools x In this example the Clarus GC is configured with the PSS capillary mode on for pressure psi If the option for capillary control has been selected during configuration you can program the carrier gas according to one of three values pressure velocity or flow The carrier gas field on the injector tab screen displays the set point value The label below the field displays the current step The actual values for all the available configuration options are displayed to the left as read only text on the screen Touch the program button E amp H for Carrier Gas The Carrier Pressure Program window appears 3 23 Using the Active Method Carrier Pressure Prograrn LA Current nit Tite O00 nm End 1 67 in y h Close 3 Touch the field ranging from the Initial field to the step 4 field and use up and down arrow or keypad al Z22 buttons to enter a pressure hold time and rate NOTE The rate for the range is 0 end to 99 A rate of 999 is a ballistic setting maximum The ballistic mode of programming is not recommended Setting a CAUTION program rate will be more reproducible 4 Touch Close to return to the injector screen 3 24 Clarus 600 68
141. he name is added to the list and the Save As box closes The new name appears in the Method Name field If you press the OK button before entering a method name the following error message appears 5 14 Clarus 600 680 GC User s Guide Method Name Mo method name entered Pressing Continue returns control to the previous screen You can select a name or cancel out of the process If five methods are already stored entering a new name will prompt the following dialog box Method Editor The number of methods has reached A maximum capacity a Do you want to overyrite an existing method Yes Heo Cancel If you press Yes the method list appears Delete x default rs external OE Cancel When you select a method and press OK the Save As screen appears with the new method name in the field You can now press OK to save the method in the available position 5 15 Using the Method Editor Save As Mame Pires default e OF Cancel If you press No the Save As dialog box displays the same fully populated list of methods The new method name is still in the Name field You can press Cancel to return to Method Edit mode and access the File button or OK to prompt the memory full error again Activate This command is deactivated while the system is running When the command is available the Activate option applies the currently edited method conditions and name to the active method
142. he temperature probe through the exposed white insulation covering one of the holes so that the probe tip is positioned in the center of the oven cavity 6 61 Using the Tools Menu Note which hole you used and measure the length of the probe that protrudes into the oven Use the same position for subsequent oven calibrations Figure 6 6 Holes on the left side of the oven exterior Equilibrate the Oven Temperature 1 Close the oven door then turn the GC and thermometer on From the System Status screen press the oven button 6 62 Clarus 600 680 GC User s Guide A FID Events Temp Time Rale init o foio aioe al 500 o a1 oo hiethod Editor Event Log hlaintenance Oven Off la Ready 3 Press on the Oven button on the Configuration screen 6 63 Using the Tools Menu Conhiguraton 4 From the window shown below set the oven temperature of 100 C or use another temperature if desired by using the plus and minus buttons Configuraton Oven Lirit Equilitraton I 300 ME o min Startup Heat Delay Aux Heat None Calibration Orset 00A C Actual 50 C Coolant Type a AG Enable Timeout at mir sof Cooling gwen Fan 1400 RPM a Ready oct 13 IRIE BBE OK Cancel 5 Single Point is the default setting When the Single Point Calibration radio button is selected the Offset field is active and the GC Tune drop
143. hen using a TCD at high sensitivity with a GSV or the autosampler a minor baseline upset may occur at the time of injection If the signal goes below zero incorporate a timed event Autozero to bring the signal back to zero before the peaks of interest elute Observe the initial chromatogram to determine the proper time for the timed event 3 63 Using the Active Method Available Syringes The following syringes are available for the Clarus GC 5 uL 0 63 mm O D Teflon tipped plunger Std N6101390 0 5 uL 0 63 mm O D N6101252 NOTE 4 0 47 mm needle is required for use with the POC injector and 530 um columns in the on column injection mode only You can achieve better precision in the on column injection mode when you use sample volumes of 1 0 uL or greater 3 64 Setting Up the Detectors 4 Setting Up the Detectors Clarus 600 680 User s Guide Overview This section contains procedures for setting up the following detectors FID flame ionization PID photoionization ECD electron capture NPD nitrogen phosphorus TCD thermal conductivity FPD flame photometric The instructions provided in this chapter describe how to set detector gases that are controlled by PPC modules The Clarus GC PPC modules are calibrated at the factory with their corresponding gas however there are exceptions The CAUTION PPC module that controls the e ECD is calibrated with nitrogen e TCD is calibrated
144. higher than your operating flow Ifthe system detects flows higher than this value it considers it a leak 2 os OR 3 35 Using the Active Method If Fixed is selected use the up and down arrow or keypad kd al z22 buttons to enter an offset value in mL min 15 Press OK NOTE The Clarus PPC split pneumatics adds the septum purge offset to the split vent setpoint to obtain the total split system flow rate See Chapter 7 for more details 3 36 Clarus 600 680 User s Guide Setting Up Valves The Clarus GC operates six internal solenoid valves You can initially configure valves from the Configuration screen by selecting the Relays button To change valve settings for your current method use the Timed Events screen and touch the Relays button Setting the Split Mode Using PPC To set the split mode 1 Press Tools menu button and select Configuration Tools x The Configuration screen appears 3 37 Using the Active Method Configuration B Injector E ECD A Injector A FIL Run Sep Preurmaics Relays ja Ready 17 01 Close 2 Touch the Injector button for the corresponding injector which to configure the split mode The Configure Injector screen appears 3 Touch the Capillary Control check box Configure Injector A Type P551 Hi J Capillary Control Carrier Control Pressure B Program J Oventrack column Length 25 00 mo LOJ 250 urm Split mod
145. hod 1 Vials fo eo vol 0 6 UL injector wA JE Injectionsvial Stabs wal 0 af T Injection oO Ff Ready hiar 4 ee eo The Autosampler screen contains three tabs The first two tabs display identical screens for setting Program 1 and 2 allowing you to sequence two methods The Tasks tab displays buttons to perform tasks such as Park Clean and specify a priority injection All of the screens provide status information The method field allows the user to run the GC under the control of a method other than the current active method Start Button Touch the Start button to start a run The Start button is active whether or not the system is ready Issuing the start command before the system is ready gives users the flexibility to set up and run a method without having to wait for the system to attain ready status As soon as you touch OK the Start button changes to Stop whether or not the system is ready This enables you to cancel the run before it starts e Ifthe system is under external control e g from TotalChrom and a method has not yet been set up the Start Button is inactive e In all other instances even though the GC is not Ready the Start Button will start a run 3 54 Clarus 600 680 User s Guide e When the GC oven starts to program the Start Out signal will be asserted for 1 second e The Ready Out signal will be asserted only when the GC 1s fully equilibrated and the GC has r
146. ich allow you to make entries e Buttons that you touch to start or stop actions or to display a dialog e Option Buttons that you select drop down menu options from a list e Boxes that you use to switch functions on or off and e Radio Buttons that allow you to choose one of two or more options The Clarus GC 1s controlled by a collection of operating parameters called the Active Method You can prepare and save up to five methods and make any one of them the Active Method However the fifth method is reserved for TotalChrom and may be overwritten 2 4 Clarus 600 680 GC User s Guide The following Status Screen shows the different sections of the user interface The Status Screen displays icons that provide quick access to major areas of the system The injector and detector buttons show graphic representations of the devices for each channel If a heated auxiliary zone is configured the Aux button with a thermometer appears active on the bottom of the screen The Aux zone button with the carrier gas icon indicates that the PPC carrier gas zone 1s active The icon buttons that represent the heated zones injectors detectors oven and Aux if configured include a light to indicate the ready not ready status A red blinking light indicates not ready and a steady green light indicates ready status Click here to view the Signal If The Title bar displays the name of the active method Method 5 a method is not running the The
147. ier gas is selected in order to apply the correct viscosity coefficients and suggested column carrier gas velocities as shown in the Table Screen Name Nop Pa s Suggested Velocity cm s 0 000018662 0 646 20 to 40 Hydrogen 0 000008399 0 725 30 to 55 The default will be He Outlet Press The column outlet pressure is set to Ambient or Vacuum 0 or to a user entered Other value Units will be in absolute units psi abs or kPa abs and will be set according to the units chosen in the Configuration screens for the rest of the user interaction The range for this field will be 0 to 100 psi abs in 0 1 psi increments or 0 to 689 kPa abs in 1kPa increments The default will be Ambient 14 7psi abs or 101kPa abs Suggested Velocity A display only field that shows the recommended carrier gas velocity range from the selected carrier gas name Inlet Press This is a selectable field this is the default selection and if selected the Flow and Velocity t0 fields are deselected and are display only The carrier gas input pressure is in units of psig 1 to 100psig in 0 1 ps1 increments or kPa 1to 689kPa in 1kPa increments The default is 5 0psig or 34kPa Flow Rate This is a selectable field and if selected the Inlet Press and Velocity t0 fields are deselected and are display only 6 70 Clarus 600 680 GC User s Guide The carrier gas flow rate is in units of mL min 1 to 100mL min in 0 1mL min increments Ther
148. ill be shown Set the FPD Temperature NOTE When using the FPD with Turbochrom Version 3 1 or earlier OMEGA or the Model 1020 1022 software Version 7 10 for the SX or Version 6 5 for GC Plus the FPD temperature values must be entered between 250 C and 450 C only Do not enter any value less than 250 C 1 From the System Status screen touch the FPD button 2 The FPD tab page is now visible 4 61 Setting Up the Detectors Alten 4 Bi I AutoZero he PMT On ae Linearizer Gn Filter 200 ma OuUBuUE Recorder PRT volage OFF o Offset ri Gas flow iL gel Actual Ar 450 45 He 45 0 45 Ready 17 01 BES v a Ffi Tools d NOTE For proper ignition to occur the FPD must be heated to at least 250 C 3 Touch the temp field and use the up and down arrow or keypad al 7 buttons to enter a setpoint of at least 250 C this is the minimum entry for a il so FPD in the temp field lemp or enter a temperature that is 50 C higher than the highest temperature of your oven program Set the Hydrogen Flow and Air Flow for PPC The PPC pneumatics consists of PPC modules to set the hydrogen and air gases from the Clarus GC touch screen The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure 1 Turn on the air at the source and adjust the pressure to 70 90 psig 2 Turn on the hydrogen at the source and adjust the pressure to 6
149. in When the count down goes to zero the analysis will begin If you need to stop the autosampler run touch the Stop button Type Autosampler J Manual Program 1 Program 2 Tasks Method metho 1 vials fo o vol 0 6 UL injector eA JE injectons val otalus Vial 0 af athe Injection Q of Oo Ready itt 13 7 22 3 Clarus 600 680 GC User s Guide If you need to modify the method for running the autosampler or enable the autosampler touch the Tools button and from the drop down menu touch Configuration Touch the Run button L screen displays on the Configuration screen The following Configuraton Injection I Enable Autosampler Recycling Auto Resume Volume los JUL Mode onGolu B Syringe Wash Viscosiby Control 0 solvent Pre titash 0 Pre lnject 2 PostInject 2 Purrip a Sample Rinse Before Ready 20 OK Cancel 7 23 Setting up a Typical Analysis 5 Inthe Autosampler Configuration screen check off the Enable Autosampler field by touching it If your application requires Recycling and or Auto Resume touch the field to check off Use the drop down window to set the volume and mode type For the Syringe wash use the plus minus buttons to modify the fields of Viscosity Control Solvent Pre wash Pre Inject Post Inject and Pump Configuration Injection T Enable Autosampler Recycling F Auto Resume volume 05 UL Mode on Colu H ovringe Wash
150. inil Program or velocity i Carrier Gas Te 3p NA program button Split Flow Ready Not Ready total Aow 100 rato 0 uu Split flow set owu value Mot Ready 17 0 ye E w css Tools w System Status Oven Program Step 2 17 Touch Screen Navigation Program Buttons otter The program button appears next to the temperature and Carrier Gas fields for a programmable PSS or POC injector If the program button associated with a value 1s active the entry field is grayed out You must go to the program screen to modify the settings If the programmable injector is not configured to program the setting the program button is grayed out In most cases fields with a deactivated program button are editable allowing you to modify the setting directly Display Text The text displayed next to the set point entry fields show the current values If the injector configuration allows you to display the value in other units such as velocity or flow the display text shows the actual values for all of the available options PSS This section describes the main components of the PSS active method screen and the relationship between program and configuration options 2 18 Clarus 600 680 GC User s Guide Configuration Options The following screens show the configuration choices and how they correspond to the entry fields in the active method Configuration Screen Active Method Configure Injector A
151. injections since insolubles can build up and cause friction To clean the syringe plunger Remove the syringe using the procedure in the preceding section Remove the plunger from the syringe barrel Wipe the plunger with a tissue soaked in an appropriate solvent Replace the plunger Pull and expel the same solvent through the barrel several times oe oe ae e Replace the syringe using the procedure in the preceding section NOTE Only syringes distributed by PerkinElmer should be used with the Clarus GC Plungers are not interchangeable from syringe to syringe Config uration Button From the Tasks tab touch the Config button Conhiguraton Injechon I Enable Autosampler MA Recycling Jv Auto Resume Violume o 5 sue Model Normal B ovringe Wash viscosity Coniral 0 Solvent Pre itash 0 Pre tnject 2 Post inject 2 Purrip a Sample Finse Before Ready 17 0 FEF OK Cancel The Config button provides a quick link to the configuration settings 3 60 NOTE NOTE l 2 Inthe Number of Injections field use the up and down arrow or keypad aj Clarus 600 680 User s Guide Auto Resume Check the Auto Resume checkbox to allow the autosampler program to automatically resume where it left off should a power failure occur Running Viscous Samples The Clarus GC allows you to vary the length of time the plunger pauses at the top of stroke when acquiring samples In addition the plunger
152. is 0 the undefined state Once a function is selected for the primary module in this case Carrier flow the position list is updated to offer only those positions consistent with choice and not already assigned to another logical position In this case only position 1 is valid and the screen appears as shown below 6 41 Using the Tools Menu Connect PPC Device PPC Define Carrier A Function Position carr Fic H E H secondary Position Inne ef fo a aK cancel The secondary module is now enabled This will only be the case 1f the primary module is set to Carrier Flow or Split Control The following screen shows that the second module can be configured as either Pressure readout or Split control under these conditions Connect PPC Device PPC Define Carrier A Funcion Fositorn carr Flow e ho H secondary Fosiion 6 42 Clarus 600 680 GC User s Guide In this case the secondary module is left unconfigured None Touch OK to close the dialog box and implement the settings Touch the Carrier B button on the Connect PPC Device screen to display the associated settings Connect PPC Device PPC Define Carrier B Functor Position Mone H o 4 Secondary Position fine fo a OK Cancel Select Split Ctrl control The secondary module for Carrier B is now enabled but inspection shows that there are no suitable modules available for assignment 6
153. l Paeurmatcs PPC Alarm Enable Ready 17201 v a FE OK Cancel Touch the PPC Connect button touch OK to clear the caution screen then touch the button for the PPC device you want to connect In this example the FID Connect PPC Device PPC Define Detector A FID Position Air oa row EIN EES Hydrogen Fositon Det Flow l f l FE OK Cancel Select the Det Flow or None for Air and Hydrogen and touch OK 6 22 Clarus 600 680 GC User s Guide The following series of screens show the configuration screen for each detector TCD co Disable Filer 200 Define Gas Sources SetPoint Actual Reference a mhin MakeUp o0 oo mLitnin uput Gas Flow amp Recorder _jlnteqrator Ofset E wo Not Ready l TF a E OK Cancel ECD a T Disable Fiter 200 Gas Flor SetPoint Actual Make Up o mtn uput Recorder j Integrator Ofset 5 a Ready 17 01 ea JE K Cancel 6 23 Using the Tools Menu PID a Disable Filler 200 Gas Flow SetPoint Actual Make pf Lin dupu Recorder j Integrator Ofset E oa Ready 1701 HS EFE K Cancel Disable Filer 200 SetPoint Actual Air 450 QUEUE Ofset D oo 6 24 FPD Disable Filter 200 Unearize PMT voltage OM 2
154. lectrons A mixture of hydrogen gas and air flows around the bead to produce a hydrogen plasma Stable intermediates are formed in the hydrogen plasma which then capture the electrons emitted from the bead to produce ions A polarizing field directs these ions to the collector electrode thereby creating a current which is amplified Sensitivity is affected primarily by the air flow and selectivity is affected primarily by the hydrogen flow A cross sectional view of a NPD is shown in the following figure CHLORINATED SOLVENTS MUST NOT BE USED WITH THIS DETECTOR The life and performance of the alkali bead will be severely impaired by contact with chlorinated compounds In general any halogenated compounds will degrade bead performance therefore avoid using stationary phases containing these compounds whenever possible The use of solvents such as water methanol or ethanol will also 4 44 Clarus 600 680 User s Guide reduce bead performance and life Although these solvents may still be used they should be avoided whenever possible
155. left as read only text on the screen 2 Touch the program button for Carrier Gas 3 27 Using the Active Method The Carrier Velocity Program window appears Carrier Velocity Prograrn d 40 0 Current z204 0 0 CSE velocity irme rale criisec minubes CSEE inital E 2 40 0 3 Init O00 mo End 1 67 r y h Close 3 Touch each individual field ranging from the Initial field to the step 4 field and use up and down arrow or keypad kd aj Z22 buttons to enter a velocity equilibration time and rate NOTE The rate for the range is 0 end to 99 A rate of 999 is a go to setting The go to mode of programming is not recommended Setting a program rate will be more reproducible CAUTION 4 Touch Close 3 28 Clarus 600 680 User s Guide Setting the Septum Purge Mode and Offset To set the septum purge and offset 1 Touch Tools button and select Configuration from the drop down menu The Configuration screen appears Conliguraton 2 Touch the button corresponding to the injector you want to modify A Injector or B Injector The Configure Injector screen appears Configure Injector A Type PSSI 4 Capillary Control Carrier Control ij Flow ofset Auto Fixed Oset 1 00 mLmin HS Control hiar 4 EEE OK Cancel 3 29 Using the Active Method 3 From the Capillary Control drop down menu select Pressure
156. license by the U S Nuclear Regulatory Commission NRC and or in some states by the equivalent state agency For further information on obtaining a license contact PerkinElmer Shelton Connecticut Customer Service department or the NRC Material Branch Office of Nuclear Materials Safety and Safeguards Washington DC 20555 4 17 Setting Up the Detectors Special Instructions for ECD Cell Purchasers Who are not Specifically Licensed to Handle Radioactive Materials The PerkinElmer Electron Capture Detector P N N610 0063 120 V or N610 0134 230 V contains 15 mCi of Nickel 63 Ni 63 a radioactive material Your possession and use of this detector is governed by 10 C F R Section 31 5 which is reproduced in Appendix I Under the provisions of that regulation you are deemed a General Licensee Your possession and use of the Detector Cell may also be regulated by the state where you are located The requirements of state regulatory agencies are substantially similar to those contained in NRC regulation 10 C F R Section 31 5 but they may differ in some respects It is suggested that you procure a copy of the regulations of your particular state Supplement 2 in Appendix I contains a list of the Agreement States which have been granted authority by the U S Nuclear Regulatory Commission to regulate the possession and use of radioactive material It is required that you are familiar with regulation 10 C F R Section 31 5 Supplement
157. low is shut off and hydrogen is purged through the FID for 10 seconds The ignitor energizes the flame ignites indicated by a pop sound and air flow is returned to sustain the flame The FID output level is monitored to confirm that the flame is lit If a lighted flame is not confirmed the AutoSystem repeats the ignition process up to two more times 2 34 Clarus 600 680 GC User s Guide Configuration Settings The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method Configuration Screen A PSsl Oven A FID ay T Disable iy a 100 ec Heater of Fiter 200 temp 00O mY 100 C GAT FF AuloZero F eout 0410 0 00 my as Flow Range 20 e Oulpuk Recorder Ofset So mLinin Filler 200 mg SetPoint Actual Flarneout 0 10 mi he ri Limin uput A Recorder J lrtegrator Ofset E wo Ignite Oct 4 Ready Oct 4 OK Cancel BEE BEE BEE see E aaa Tools a 2 35 Touch Screen Navigation TCD The Thermal Conductivity Detector TCD is a dual channel detector which measures the difference in thermal conductivity between carrier gas flowing through a reference channel and carrier gas plus sample flowing through an analytical channel Four tungsten rhenium filaments are connected in a bridge circuit two in each channel The TCD 1s set up with the same amount of carrier gas flowing through both channels The pr
158. ly since this can cause backflush of the column This means that the sample can flow back into the injector and either be lost out the split vent or cause peak broadening Creating a Pressure Flow or Velocity Pulse Method 1 From the System Status screen touch the Injector button for which you wish to create a pressure flow or velocity pulse method The status screen similar to the one below for the selected injector appears Oven A FID Events Healer Off a OFF Ee 25 C temp i Carrier Gas 0 0 psi 0 00 mhm d psi 0A crvsec press init Prograrn Spit total foru 0 mbm 0 rato Alcan 17 0 Tools 2 Touch the Events tab 3 42 Clarus 600 680 User s Guide A Cap Oven AFID Events Time Event Value AUX Gas Add Edit Relays Delete Clear Ja Ready 1704 ees eee Touch the Add button The Add Timed Event screen appears A Cap Oven AFID Events Time O00 Value Off JE OK Cancel Ready 1701 eS ees Select Split A from the Event drop down menu 3 43 Using the Active Method 5 Touch the Time dialog box and use the up and down arrow or keypad buttons to enter a time of 25 minutes 222 buttons to enter a flow value NOTE Values of 20 mL min and higher provide greater accuracy than values below 20 mL min 7 Touch OK You have now created a timed event set to turn on the split
159. n should be made to any one of the following governing bodies ENGLAND Department of the Environment Queen Anne s Chambers Tothill Street London SW1H 9J4 SCOTLAND Scottish Development Department 21 Hill Street Edinburgh EH2 3J4 WALES Welsh Office Cathay s Park Cardiff CF1 3NG NORTHERN Ministry of Development IRELAND Parliament Building Storemont Belfast Northern Ireland ECD Overview The Electron Capture Detector ECD is the most sensitive detector available for the analysis of electrophilic compounds such as chlorinated hydrocarbons and pesticide residues It is concentration sensitive and nondestructive The ECD cell contains a foil in a cylinder through which the carrier gas flows The coating of the foil s inner surface contains the radioactive isotope Nickel 63 and has a nominal sensitivity of 15 mCi To optimize detector response make up gas is combined with column effluent Beta particles emitted from the isotope ionize the carrier gas The resultant ions and electrons travel to the collector anode assembly under the influence of a pulsed polarizing voltage applied between the source and the collector The pulse frequency is varied to maintain a constant average current The presence of an electron absorbing species in the detector decreases the current as the absorbed electrons form ions which travel more slowly than electrons The pulse frequency of the 4 20 Clarus 600 680 User s Guide polarizing sup
160. n touch the Tools button in FPD tab screen and touch Configuration from the displayed menu B POCO Oven ind i OFF C Heater Ort lemp 0 00 ri 25 C menja Method Edir lw PRIT On Event Log Li haintenance Filter 200 mS PAT Voltage OFF 4 Coniguration Gas flow inL Lblities Ar 0 Configuraton B Injector A Injector Run Sep EA Feady 17 01 Close 4 59 Setting Up the Detectors 5 Touch the FPD button to display the NPD configuration screen 6 Disable Filter 200 Unearize PRAT voltage OFF So Gas Flow SetPoint Actual Air 0 0 mLimin He G oo fn Litnin Recorder _ylntegrator Ofset 5 g 17 0 OK Cancel In this screen touch the Linearize check box to turn it On This is indicated by a check in the box Set the Filter to 200 The default setting is 200 msec If you want to improve the signal to noise change the setting to 800 msec Then run your standard and observe that the signal remains the same and the noise improves i a uput 4 60 Clarus 600 680 User s Guide Fiter 200 fw Linearize Gas Flow SetPoint Actual Air 450 45 minin H2 450 4 5 m Linin uput Recorder j Integrator Ofiset 5 To hlar 4 JK Cancel 8 When all the settings are appropriate for your analysis touch OK The FPD tab screen will be now visible and the changes you made in the configuration screen w
161. nal The processed signal has gone through attenuation and offset filters 2 11 Touch Screen Navigation The name of the channel appears on the top left of the screen Detector controls include Ignite and Autozero Display controls include scaling and zeroing Ignite Button Pressing the Ignite button starts the ignition sequence for a PPC enabled FID During ignition the plot and signal level are active For information on setting up manual pneumatics for the different detectors see the various detector sections in chapter 4 Setting Up the Detectors and sections in Chapter 3 on Using the Active Method and Viewing or Adjusting Carrier Gas Pressure Using Manual Pneumatics AutoZero Button Autozeroes the selected detector Signal Plot The plot graph displays the signal from the selected detector in real time The window is 2 minutes wide The signal commences at the y axis and is plotted out to start 1 75 minutes The signal then scrolls back so the start is now 1 minute the last 0 75 minutes are displayed from there and the signal then scrolls out again The signal is plotted continually before during and after a run Signal Display and Scaling The signal display at the top of the screen displays the signal level of the detector in mV The default signal scale is 0 1024mV The up down arrows will adjust the display between 1 and 1024mV by halving or doubling the current factor 2 12
162. ngs Relays The Relay settings are accessed from the Tools Menu System option screen Use the drop down screen to set the type of valve Configuration Events Ready 2 00 v OK Cancel 6 48 Clarus 600 680 GC User s Guide Zeroing and Calibrating the PPC Modules The Clarus GC gas modules have been calibrated at the factory and are ready to use For good laboratory practices and your own internal validation protocol you may wish to recalibrate at installation with your own flow measuring device All carrier gas modules have been calibrated at the factory with helium If you are using a different gas you must enter the appropriate gas and recalibrate Detector gas modules must be recalibrated if you are using a different gas in your laboratory In the factory the TCD reference gas and the PID make up gas have been calibrated with helium and the ECD make up gas with nitrogen Zeroing and calibrating PPC modules consists of the following steps e Zeroing the PPC gas modules Gas turned off e Setting the reference temperature and pressure e Calibrating the PPC carrier gas modules and or PPC detector gas modules Gas turned on The calibration information is stored in a reserved area of the battery backed memory Zeroing the PPC Gas Modules Before zeroing the PPC gas modules e Make sure that the Clarus GC has been properly installed and all gases are connected e Turn on the Clarus GC power and allow
163. nitially turn Off the appropriate split flow that 1s associated with your injector with a timed event Then with another timed event turn it On from 0 25 to 2 minutes into the GC run and leave it on When the GC run is complete the GC returns the split flow to its initial setting To set up for splitless operation gt From the Injector status screen touch the dialog box for Split flow and use the up and down arrow or keypad aj 7 buttons to enter a split flow in mL min 3 46 A Cap Oven A FID Events Heater f OFF C 25 C temp Carrier Gas 0 0 psi 0 00 mhm 49 psi Q 0 msec press init Prograrn Spit total fow 1 mLin rato fow Ready 17 01 Setting the Timed Events 1 Touch the Events tab og mle A Cap Oven A FID Events Time Evert Value Clarus 600 680 User s Guide 3 47 Using the Active Method 2 Touch Add The Add Timed Event screen appears 3 From the Event drop down menu select Split A if the injector is installed in position A or Split B if the injector is installed in position B 4 Touch the Time dialog box and use the up and down arrow or keypad a T buttons to enter a negative Time for example 1 00 min for the event to occur prior to the GC coming ready Then press Enter The cursor moves to Event 5 Touch the Value dialog box and use the up and down arrow or keypad al zaa buttons to enter a v
164. njector A Non installed Devices If a device is not installed a grayed out deactivated button with no indicator light appears in the designated position 2 Touching the button prompts the following dialog box Hon installed device ag i This device is not installed ok Touch Screen Navigation Run Button The Run button displays the Manual injection and Autosampler settings if the device is enabled The bottom bar on these screens includes the Start button When the system is running the Start button changes to the Stop button Since the Start button is only available on the Autosampler and Manual inject screens you must initiate a run from these screens However when the system is running the Stop button appears on all screens allowing you to Stop the run from anywhere in the application If the system is Paused the Resume button appears on all screens Autosampler Enabled When an Autosampler is enabled the Run button defaults to that screen The following screens show the enable check box on the configuration screen and the associated Autosampler screen in the Active Method Configuration Injection P Debug J Manual Tasks helio method 1 A Wials pa to E vol 0 6 UL injector eA JE injections Status Ie Enable Autosampler Recycling Auto Resume Volume os ful Made OnCalu o vringe Wash viscosiby Control 0 solvent Pre titash 0 Pre inject 2
165. nnect screen In the example shown in the following screen press Detector B and connect Detector flow modules for the TCD module Note the changes to the window title bar and the labels on the left hand combo boxes 6 45 Using the Tools Menu Connect PPC Device Reference Position crow BIJE hake Ue Positor None jo H OK Cancel Press OK to apply these changes Define Aux Touch Aux 1 to display the dialog box In the example shown in the following screen capture on the left since all of the available modules have been assigned no options are available If Aux 1 is pressed before setting up the carriers and detectors a more complete list is offered as shown in the screen on the right 6 46 Connect PPC Device REE Define ARA Function Position Clarus 600 680 GC User s Guide Connect PPC Device For each function position pair the same basic calculation is used to identify what modules are available and what locations are available once the module type has been selected To identify the types of module available first identify the set of available locations that contain one of the acceptable set of modules for this logical position For a carrier this means scanning through all of the locations looking for ones that the hardware test has shown to contain CARR or PRES modules and that have not been assigned to another logical location 6 47 Using the Tools Menu Reference Setti
166. non programmed injectors an entry of 0 turns the heated zone Current BOO EEF ttt off With programmed injectors a temperature of 0 is fos 0 possible Therefore when 0 is entered for the initial emp tme rae injector setpoint the following screen appears injector Temperature Program The initial default values are Initial Temp 1 is 50 C Init Time 0 06 m End 1 67 m Close 1 From the selected injector tab screen make sure that the injector heater is off 2 Set the initial temperature to 50 C Gma A PSSI Oven FID Events Heater Off LA At ie T a 4d C temp init Prograrn j Carrier Gas Q 0 psi ae 0 00 mbin psi LUT stat lifer lle Program Split total flowy 0 OFF ombin rato 0 fow Eguilibraing 0 0 min E aE we 3 18 Clarus 600 680 User s Guide Setting Up a One Ramp Injector Program To set up a one ramp injector program enter the following parameters e Initial injector temperature Init Temp e Isothermal time for the initial temperature Init Time e Rate of temperature increase from the initial to the final injector temperature Init Rate e Final injector temperature Temp 2 e Isothermal time for the final temperature Time 2 e Temperature increase of 0 C min which signifies the end of the Rate 2 step The following example shows how to build a one ramp temperature program for your POC or PSS injector
167. nt cover 6 65 Using the Tools Menu Utilities 1 To reach the Utilities screen of the Tools Menu go to the System Status screen and select Utilities from the tools menu Tools 2 Touch the following icon on the Utilities screen to access the Column Flow Calculator the Column Length Calculator the Background Compensation Stopwatch or Program Max Oven Program Rates 6 66 Clarus 600 680 GC User s Guide Y Column Flow Calc Column Lengin Calc slopivalch Prograrn Feady 2700 Close Column Flow Calculator The capillary column gas flow rate calculator allows you to automatically calculate the correct gas flow rate 1 Touch the Column Flow Calc icon button Column Flow Calc 2 The following screen appears 6 67 Using the Tools Menu Column Carrier Gas Calculator Ea Column Parameters Lengh GM in Temp 50 0 c Diameter 220 UM Carrier Gas Inlet Press 5 0 psig Gas He B J Flow Rale 9 91 mLtnin Split J velocity 176 CS ol 280 min suggested welociy 20 To 40 cms ulet Press Ambient J Vacuum _ olher 14 7 psia tg Close 3 Input the column length column diameter column temperature carrier gas name and outlet pressure 4 One of the following is selected Inlet Pressure Flow Rate and Velocity t0 A value is entered into the selected field and results are calculated and inserted into the two unselected fields For example
168. o peaks Retention time The time interval from the point of injection to the appearance of the peak maximum of a component s signal 1 11 Introduction Septum Silicone rubber material placed in the injection port through which the injection is made When the needle is withdrawn the silicone rubber reseals thus not allowing any sample or carrier gas to escape Stationary phase The liquid or solid adsorbent portion of the column that retains components passing through the GC column Subambient Below ambient temperature The oven cools down below ambient temperature with the use of either liquid nitrogen or liquid carbon dioxide Syringes Precision dispensing devices used to deliver sample to the GC Liquid and gas syringes are available Tailing When a peak is not symmetrical or Gaussian shaped but the back end is broadened it is said to be tailing Temperature programming A technique commonly used to increase the rate of elution of the components After the sample is injected into the oven at a specific temperature the temperature program increases the oven temperature to the prescribed temperature at a defined rate in C min Unretained peak A component that is not retained by the column The time taken for an unretained sample to pass through the column is the same time as the time taken for the carrier gas to pass through Velocity programming Programmed linear velocity where
169. oad the vacuum chamber In order to 3 45 Using the Active Method avoid this the setup procedure is slightly different than the above procedure When using a mass spectrometer you would not want the initial pressure to be too high because at the end of the GC run all parameters are set back to their initial values and the higher pressure could cause damage to the vacuum system For the Clarus GC MS the initial value is set to the normal operating pressure flow or velocity and a negative timed event with a high pressure flow or velocity will be added to the method This causes the pressure flow or velocity to increase prior to Ready for example prior to the injection At injection the GC method holds this pressure flow or velocity for the time necessary to transfer the sample onto the column The experimentally determined pressure flow or velocity is then programmed at a controlled rate down to the initial or normal column operating pressure flow or velocity If you are using the autosampler at the end of the last sample in the sequence the Clarus MS will go Not Ready thereby sending a signal to the GC keeping it from coming Ready The External Ready must be connected See the Clarus 600 680 GC Installation Instructions 09936779 This keeps the GC from executing the negative timed event and holds the pressure at the lower setting Setting the Split Flow for Splitless Injection To make a splitless injection i
170. ocity in the system at the time of injection to minimize the gas expansion in the injector liner and maximize the gas sample transfer onto the column Therefore you should use the highest pressure that your application will allow This provides better peak shapes better recovery and no discrimination for both low boiling and high boiling compounds This technique can be incorporated in your GC method The initial pressure flow velocity is high for example 70 psig and held at this high pressure for enough time for example 0 25 to 2 0 min to transfer your sample onto the column This time needs to be experimentally determined for your sample injector temperature and injector liner used You want a time that will allow most of your sample to transfer onto the column as well as maintain good solvent and analyte peak shape If the time 1s too short you will lose sample if the time is too long the solvent will tail and possibly obscure or affect peak shape of early analytes The split vent is off at injection Split Flow zero The pressure flow velocity is then programmed at a controlled rate down to the normal column operating pressure flow velocity At the same time the split vent is set back to normal flow to clean out any remaining sample in the liner and to release the pressure in 3 41 Using the Active Method the injector It is important not to program the pressure flow velocity down too quickly or ballistical
171. oduction 1 2 Clarus 600 680 GC User s Guide About This Manual This guide is divided into following chapters Chapter 1 Introduction This chapter contains a brief introduction to the Clarus GC the conventions and warnings used in the manual Chapter 2 Touch Screen Navigation This chapter contains information that introduces you to the look and feel of the touch screen It shows you how to turn on the GC check the status and perform fundamental operations such as changing parameters selecting options using the tools menus etc Chapter 3 Active Method This chapter contains step by step explanation of the active method Detailed information on setting up the autosampler is contained in this chapter Chapter 4 Setting Up the Detectors This chapter contains detailed information on setting up the detectors Chapter 5 Using the Method Editor This chapter describes how to modify save and use the method editor Chapter 6 Using the Tools Menu The chapter contains detailed information on the tools menu section of the touch screen Chapter 7 Setting Up a Typical Analysis This chapter describes how to run a typical analysis on the Clarus GC using the most common configuration 1 3 Introduction Conventions Used in this Manual Normal text is used to provide information and instructions Bold text refers to text that is displayed on the screen All eight digit numbers are PerkinElmer part numbers unless stated other
172. of the tubing through the hole in the detector cover as you close the detector cover 5 Connect one end of a length of vent tubing to this piece of tubing and place the other end in a vent hood 4 16 Clarus 600 680 User s Guide Setting up an ECD To assure that removable radioactive contamination on the external parts of the ECD remain at a safe level the United States Nuclear Regulatory Commission requires that WARNING e the ECD is Wipe Tested at least once every six months and e arecord of the results are maintained for NRC inspection Please refer to the Hardware Guide Maintenance chapter for the Wipe Test procedure NOTE THERMAL RUNAWAY PROTECTION The Clarus GC software shuts down the GC if any heated zone exceeds 470 C Should this occur the following error message is displayed INSTRUMENT SHUTDOWN xxxxx THERM RUNAWAY Where xxxxx IS the heated zone Call your PerkinElmer Representative Instrument shutdown also occurs if there is a PRT Platinum Resistance Thermometer or MPU Micro Processor Unit failure In these cases the following error message is displayed INSTRUMENT SHUTDOWN xxxxx PRT ERROR Where xxxxx IS the failed zone Call your PerkinElmer Representative NOTE The detector gas modules have been set to OFF at the factory for both manual and PPC pneumatics United States Government Regulations for ECDs NOTE Repairing an Electron Capture Detector cell requires a specific
173. oint is reached Using the Active Method Setting Up Oven and Inlet Temperature Programs You can set up ramp programs they are Init 1 2 3 through 10 using the Clarus GC software l 2 3 From the System Status screen touch the oven button to display the oven program screen Once the Oven program screen appears B FSSI Oven B TCD Events Temp Time Fate W nit f 1 00 ioo a C g 100 100 so TA EA A A ee value of 0 in the Rate field to make that the last step You will then see the word END appear in the Rate field all the fields that follow are deactivated You must touch END and then touch the up arrow button to activate the next row The following figure shows a typical temperature step program NOTE NOTE Clarus 600 680 User s Guide Time 4 l Oven m Only p e r a t u r Se 4 2 3 4 Step Figure 3 1 Typical temperature program steps Before you actually set up an oven temperature program you should decide on the Equilibration Time you need and change the default value if necessary see below Configuring the Equilibration Time Init When you change the oven temperature setpoint the system heats or cools the oven to the new setpoint then equilibrates the column s for the specified Equilibration Time before the instrument becomes READY A minimum Equilibration Time of lt I minute is recommended for
174. only have one In the carrier flow module pressure transducer A reads the differential pressure across the flow measuring device restrictor and transducer B reads the input line pressure 3 Retighten all septum caps and restrictors on the rear of the instrument 4 Turn on the gases connected to the Clarus GC 6 52 Clarus 600 680 GC User s Guide Turn on the carrier gas and allow at least one minute for the CAUTION line pressure to stabilize and purge the lines before selecting Calibrate from the display Setting the Reference Temperature and Pressure The reference temperature and pressure values are set at the factory We recommend leaving these parameters set to the factory default values Temp 25 Cand Press 14 7 psi If you wish to use your own flow measuring device and know the temperature and pressure at which your flow measuring device was calibrated then enter the values as described in this procedure To set the reference temperature and pressure 1 From the Configuration PPC screen touch the Reference Settings button Touch OK on the Caution message Configuration PPC Conhguraton PPG Caution PPG connect A PoR ASAL E To avoid damaging he PPC systern do not modify ne setings unless Kanual Pneumatics Ine hardware coniiguraton has changed Do you want to proceed PPO Alarm Enable 2 00 Ready nt 13 K Cancel Il LEE aa OK Cancel 6 53 Using the Tools Men
175. or GSV When using a TCD with an autosampler or a GSV Gas Sampling Valve at high sensitivity a minor baseline upset may occur at the time of injection If the signal goes below zero create an Autozero timed event to re zero the detector back before peaks of interest elute Initiate a test run to determine the timed event setting 4 35 Setting Up the Detectors Setting up a PID NOTE The detector gas modules have been set to OFF at the factory for both manual and PPC pneumatics PID Overview The PerkinElmer Photoionization Detector PID is designed to allow the effluent from a chromatographic column to be ionized by ultraviolet light provided the ionization potential of the effluent is less than that of the UV source The current produced by the ion flow is measured by the detector and is proportional to the concentration of the ionized material Lamp Power Connection Lamp Housing gt on Source Lamp Quartz Window O Electrical Output lonization D Chamber t Polarizing Voltage SEEEN xi Column t Connection Makeup Gas Inlet Figure 4 13 Cross section view of a PID 4 36 NOTE Clarus 600 680 User s Guide A cross section view of a PID is shown in the above figure Figure 4 14 is an
176. or signal producing 100 deflection on a 1 mV recorder is provided in the Clarus 600 680 GC Customer Hardware and Service Guide Maintenance chapter section Practical Hints 4 88 Clarus 600 680 User s Guide Optimizing a Detector Signal to an Integrator for Maximum Sample Dynamic Range The Clarus GC contains improved electronics which significantly reduce amplifier noise This allows you to amplify the detector signal without getting a large increase in the noise level Therefore it provides excellent minimal detection signal to noise for all Clarus GC detectors Amplification is set on the detector page in the Atten field the attenuation button and entering an attenuation value from x1 most signal to x64 least signal The maximum signal produced by the Clarus GC amplifier is 1 V To achieve the best sensitivity and widest dynamic range the sample with the highest concentration must not exceed the 1 V signal When using a flame ionization detector FID if you operate at range x1 and attenuation x64 and the signal saturates exceeds 1 V then use range x20 and determine the appropriate attenuation value from x64 to x1 that produces a reasonable size peak When using a nitrogen phosphorus detector NPD the same will apply When using an electron capture detector ECD the only range setting 1s xl To ensure that the signal does not exceed 1 V you should run your most concentrated sample at attenuation x64 then ch
177. order Offset a Filler 200 ms Gas flow trL gel Arual bake Un 0 har 4 Tools Configuration Screen oy I Disable Filter 200 SetPoint Actual Flamecut o 10 0 00 rh Gas Flow SetPoint Actual Air 0 0 mLimin Hz 0 0 j0 mLimin Recorder j Inbegrabor Ofset 5 To biar 4 OK Cancel dupult 2 39 Touch Screen Navigation NPD The nitrogen phosphorus detector NPD is a highly specific thermionic detector for organically bound nitrogen and phosphorus The detector operates by electrically heating a glass bead that contains an alkali metal to the point where it emits electrons A mixture of hydrogen gas and air flows around the bead to produce a hydrogen plasma Stable intermediates are formed in the hydrogen plasma which then capture the electrons emitted from the bead to produce ions A polarizing field directs these 1ons to the collector electrode thereby creating a current which is amplified Sensitivity 1s affected primarily by the air flow and selectivity is affected primarily by the hydrogen flow The following screens show the Active Method screen and the corresponding settings in the Configuration screen Active Method DG we EVE B Pkd Oven B NPD pr I 100 c Heater Of o PMT 0 00 mi Aten S H Je Aubozero Range 20 Bi Ouput Recorder Offset To Filler 50 mS Gas fow fL set Actual Air 460 46 He 46 0 46 Ready 17 01
178. ority injections Touch Start 3 61 NOTE Using the Active Method This option instructs the autosampler to interrupt the vial injection sequence and inject a Priority vial that has been placed in the Priority position of the turntable The priority vial will be injected after completion of the current run After the priority vial has been injected in accordance with the current program parameters and the priority run completed the program continues with the next injection in sequence Priority can only be selected when with the above screen is visible About Waste and Wash Vials The Autosampler software has been optimized to use waste vials and solvent wash vials to minimize contamination of the syringe needle Septa are available for the waste vials and solvent wash vials by ordering P N N930 2780 We recommend using these septa in place of the diffuser caps when you are using e Very viscous samples to wipe the sample off the outside of the syringe needle e Toxic solvents and samples e Very volatile solvents Multi Program Mode Waste Vials When operating in the Multi Program Mode the sample pre washes are emptied into waste vial 1 for program and waste vial 3 for program 2 The solvent post washes are emptied into waste vial 2 for program and 4 for program 2 Wash vials Program 1 splits between solvent wash vials 1 and 2 For example if four washes are required two will be taken from vial 1
179. ow is shut off and hydrogen is purged through the FID for 10 seconds 5 The ignitor energizes the flame ignites indicated by a popping sound and the air flow is returned to sustain the flame The FID output level is monitored to 4 12 Clarus 600 680 User s Guide confirm that the flame is lit If a lighted flame is not confirmed the Clarus GC repeats the ignition process up to two more times Manually Ignite the Flame You can manually ignite the flame at any time by following this procedure Before trying to ignite the flame make sure that you have sufficient combustion gases and they are turned on at the source and make sure that the flows are set as described earlier in this section To ensure proper auto ignite FID operation make sure your column is positioned in the FID 2 75 inches 70 mm from the CAUTION back of the column nut Flame ignition may not occur if your carrier gas flow is 60 mL min or higher 1 Touch the FID button on the System Status screen The FID tab page appears og mle Eve nts APkd Oven in i 100 C Heater of On lem DDA pry 100 C P EE ai je g M Aulo ero Range i uput Recorder Ose S 0 w Filler 200 mS Flameout 0 20 mi Gas fow HiL Sel Actual l Ar 450 0 450 A He AED 45 Ignite Ready hiay 28 4 13 Setting Up the Detectors NOTE For proper ignition to occur the FID must be heated to at least 100 C LI co 6 2 Touch the temp field
180. owever if the program is currently in that step the changes will be ignored Isothermal Program If the program is isothermal the program button is grayed out and the top level field is active Changes entered in the field take effect immediately A Heater Ott Ee HE Aaa Ie temp init fi Catrier Gas 2 20 Clarus 600 680 GC User s Guide Carrier Gas Program The Carrier Gas options for PSS include flow velocity or pressure If the option for Capillary Control is selected you can program the carrier gas according to one of the three values The following example shows that Pressure was selected as shown in the following Configuration screen Conhgure Injector A Type FSS a M Capillary Control Carrier Gontal Pressure l Program f Column Length Split mode Flow Ofset Flow Ratio Auto Fixed afset 1 00 mLinin HE Control vacuum Compensation 17 01 33 OK Cancel The corresponding actual values for the other units appear as read only text on the screen as shown in the following Active Method screen 2 21 Touch Screen Navigation A PSSI Oven A FID Events Heater OF 286 C temp init Carrier Gas 0 0 psi l 0 00 mum d AS psi 0 0 crvsec press init Split total flowy 100 mL ratio 0 flow a Ready Mar 4 Tools d Touching the Program button next to the field displays the associated Carrier Pressure Program sc
181. p of the instrument and will not allow the tower to pass over it Program 1 and Program 2 Tabs Type Aulosampler _ Manual Program 1 Program Tasks Method Method 1 vials 7 to 9 vol 0 6 UL injector Injections vial Stals eA JE wal 0 Injection O Ff har 4 Tools ad These two tabs allow for multi program mode 2 Select the method from the drop down menu 3 58 Clarus 600 680 User s Guide 3 Highlight the Vials Vol and Injections Vail fields and use the plus minus buttons to input the correct amount 4 Select either Injector A or B 5 Touch Start when you are ready to begin the autosampler run Autosampler Tasks Tab Type amp Autosarmpler _ Manual Program 1 Program 2 Tasks ol bm Fark Clean Priority Injector Humber of Injectors rita imax 15 otals wal Q Injection J Q 1701 Tools d The Autosampler Tasks tab includes buttons to execute tasks such as Park and Clean Touch the Park button to park the autosampler tower NOTE f the syringe is directly over the injector you should move it by selecting Park Touch the Clean button to clean the syringe plunger with the solvent wash NOTE The Clean option is only available when the autosampler has stopped 3 59 Using the Active Method Cleaning the 5 uL and 50 uL Syringe Plungers The 5 uL and 50 uL syringe plungers should be cleaned regularly after approximately 500
182. ply is automatically controlled to maintain a constant current and is used to form the detector output signal The ECD works with nitrogen carrier or makeup gas or a carrier or makeup gas mixture of 95 argon 5 methane When using capillary columns at low flows 5 mL min or less helium or hydrogen may be used as the carrier gas provided nitrogen or argon methane is used as the make up gas A cross section view of an ECD is shown below lt el oe b Collector Anode To Amplifier erally 63 i Foil Source Makeup Gas In gt lt Column Connection Figure 4 6 Electron Capture Detector ECD If you are using the ECD with a packed column check to see whether the optional Flow Readout was calibrated with nitrogen or argon methane carrier gas If not select the appropriate carrier gas To function properly the total carrier gas flow through the detector should be 30 mL min or more Where required the total carrier gas flow is adjusted to this value with make up gas using the make up gas control valve located on the pneumatics control panel The appearance and location of the make up gas control valve is shown in Figure 4 9 4 21 NOTE NOTE
183. proper carrier gas and use the plus minus buttons to input the other values needed Remember only touch the fields that need to be changed If you do not touch the field the original value will remain and not change Enter Zero 0 for the detector gas setpoints If you are using a FID NPD or FPD enter 0 for both air and hydrogen detector gas setpoint When you have added all the appropriate values touch OK If you have an ionization detector for example FID NPD or FPD you must repeat this process for the hydrogen gas also The other detector types that have only one detector gas for example TCD ECD and PID will be complete at this Time 6 59 Using the Tools Menu Calibrating the Oven Temperature The Clarus GC oven temperature is controlled by a sophisticated software routine that permits adjustment of the actual oven temperature inside the oven up or down within a 10 C window This calibration utility is intended for applications which require precisely matching oven temperatures across several Clarus GCs such as the determination of retention indices The calibration information is stored in a reserved area of the battery backed memory Required Equipment A calibrated precision platinum resistance thermometer with 0 01 C readout and a probe capable of insertion into the GC oven The following steps summarize how to calibrate the oven temperature 1 Calibrate the reference thermom
184. r Autosampler Trays and Carousel The Clarus 600 GC can use only the 82 vial standard tray or the 82 vial tall tray The Clarus 680 GC is designed to use the large capacity 108 vial tray for standard vials or the 108 vial tray for tall vials There is also an 82 vial Thermostatting Tray Kit available for use with the Clarus 600 GC and Clarus 680 GC The Standard vials are recommended and supplied by PerkinElmer The Tall vials refer to those vials not purchased from PerkinElmer which are slightly taller than the Standard vials 3 51 Using the Active Method Carousel Tray for non PerkinElmer gt taller capped vial heights ranging from cd a dial aeg 33 5 to 35 5mm For the Better N6550017 ee a 82 Vial Standard Tray 108 Vial Standard Tray 108 Vial Tall Tray and Carousel for non PerkinEImer vials 3 52 Clarus 600 680 User s Guide Clarus GC Tray Capacity Vial Height Number of Number of Number of of 2 mL Sample 4 mL Wash 4 mL Waste 2 mL Priority Vials Vials Vials E sims ee mf fo With the Tray Thermostatting Accessory Kit Autosampler Touch Screen 1 You can access the Autosampler by selecting the Run button 3 from the System Status Screen See screens below dus Aux Ready 17 01 em als 3 53 Using the Active Method 2 Inthe next screen touch the Autosampler radio button to the right of the Type heading tem brt ou 1 Method Met
185. r 6 4 oven 6 18 PPC modules connecting 6 35 reference temperature and pressure setting 6 53 utilities 6 66 Touch Screen 0 3 2 4 autozero button 2 12 aux zone button 2 15 heated zones 2 13 ignite button 2 12 injector and detector buttons 2 13 manual injection 2 9 oven button 2 15 run button 2 8 signal button 2 11 signal display and scaling 2 12 signal plot 2 12 zero display button 2 13 Typical Analysis autosampler 7 22 detectors 7 11 7 16 injectors 7 6 7 8 U Utilities 6 66 background compensation 6 74 column flow calculator 6 67 column length calculator 6 73 logout 6 79 release 6 78 stopwatch 6 76 UV lamp PID optimizing intensity 4 42 Z Zeroing PPC module 6 49 p gt PerkinElmer For the Better PerkinElmer Life and Analytical Sciences 710 Bridgeport Avenue Shelton CT 06484 4794 U S A Internet http www perkinelmer com email info perkinelmer com PerkinElmer is a registered trademark of PerkinElmer Inc
186. reater If the NPD detector will not be in use for an extended period simply turn the potentiometer to zero To reuse the bead follow the activation procedure Loss in sensitivity the NPD bead is a consumable and will experience a loss in sensitivity over time Often adequate sensitivity can be restored by repeating the activation process 4 54 NOTE NOTE Clarus 600 680 User s Guide Setting up an FPD Flame Photometric Detectors FPD use hydrogen as fuel If the hydrogen is turned on without a column attached to the i h detector fittings inside the oven hydrogen could diffuse into the WARNING oven creating the possibility of an explosion To avoid possible injury DO NOT TURN ON THE HYDROGEN unless a column is attached to the detector fittings inside the oven and all fittings have been leak tested Before disconnecting a column make certain that the HYDROGEN HAS BEEN TURNED OFF If two FPDs are installed and only one FPD has a column connected to it make certain that you plug the unused detector inlet fitting with a 1 8 inch stainless steel plug P N N930 0061 To prevent potential damage to the FPD in the manual pneumatics version the hydrogen needle valve has been factory set to a very low setting Set both the hydrogen and air inlet pressures to 30 psig then measure and set the flows as stated in this chapter The PPC pneumatics detector gas modules have been set to OFF at the factory FPD Overvi
187. reen that follows the same format as the injector screens and shows the current temperature 2 15 Touch Screen Navigation Navigation Bar The navigation bar provides icons to allow users to seamlessly toggle between channels as well as access the same main areas of the system available from the Status screen The following diagram shows the navigation bar of an Active Method with the corresponding icons on the status screen Status Screen Active Method Navigation Bar Method amp Hh nl OG F ir Oven B TCO Events Ready 17 01 e ras v 2 16 Clarus 600 680 GC User s Guide Injectors The injector elements that appear on a particular injector screen depend on injector types as well as selected configuration options Some injector types offer a variety of options while others are more limited The labels in the following screen capture identify the main components of an Active Method injector screen This example shows a screen for a PSS injector with PPC Injector Tab for Channel A PSSI selected Active Method Name Channel B Parameters EA AA oy Temp Ready Not A FID Ee Ready Light Aster Of Temp Ready Not Ready Light A PSSI Over Temp program button Carrier Gas a4 Ready NotReady lemp init Light o Carrier Gas 0 1 psi mae i Carrier gas aAA mL M psi DPA pressure flow 0 0 crivsec press
188. reen for the entry field value lt Carrier Pressure Program Current 2 00 E aa ea aa aa aa aa aa a a 0 0 00 O00 i 0 0 psi irre rale 2 22 Clarus 600 680 GC User s Guide Capillary Control Off The following screens are examples when Capillary Control is off A PSSI Oven A FID Events a Pssl oven A FID Events A moi iy g orr c Heater OF e eo E temp 0 00 mv 282 C bomp init 25 C Prograrn ij Carrier Gas _ _ _____ Aten 16 E M Aulozero gG psi FET Poo g 0 gt i i qe uput Recorder ofset To press init Program Filter 200 mg any l Fameout 0 10 mi ia a Spit sP t4a t gas flow mi sel Actual total fon 100 min sir A R fow eH oo o Ignite Hot Ready 17 0 hlar 4 o at a Tools x Tools FF Split Flow nen Sali a total flowy 103 mAT flow 100 100 ratio 2 1 _ mLim flowy imit The PPC system adds the split flow offset to the method s split flow rate setpoint to obtain the Total split flow rate delivered to the inlet system The total value is equal to the setpoint flow rate the flow at the column entrance plus the offset flow rate The inlet system flow controller delivers the Total flow rate not the setpoint flow rate 2 23 Touch Screen Navigation Packed Pkd The packed column injector has a fixed non programmable temperature field The carrier gas can be programmed by Pressur
189. ri Linin Air 0 0 mLmin He 0 0 0 0 ri Limin He 0 0 0 90 mLinin dupu uput amp Recorder J Inbegrator amp Fecorder J Integrator Ofset 5 Wi Ofset D To 17 01 Ready 17 01 EEE OK Cancel v 4 EE ok Cancel When you touch the OK button the system launches a status query to the PPC connect module to ascertain whether a PPC flow module has been assigned to the FID If no flow module has been assigned a dialog box appears Warning Mo flow module is assigned to his detector Assign one now If No is selected the dialog box closes If Yes is selected the Define Gas Sources screen appears and you configure an available flow module In this example you will define a detector 6 20 Clarus 600 680 GC User s Guide Define Gas Sources x Carrier A Carrier E Getector F Aue 4 f Aux 2 Aux Aux 4 DK Cancel When the PPC gas source is defined touch the OK button to validate the settings and the FID detector configuration screen appears A FID Disable Filer 200 SetPoint Actual Flameout 0 10 0 00 mv sas Flow SetPoint Artal Ar 450 45 mbm Hef 4590 45 mnLitnin duput Recorder j Integrator Ofse D Ei Equilbrating 0 04 min v a El OK Cancel Touch the OK button to close this screen then touch the pneumatics button 6 21 Using the Tools Menu Configuration PPG PPG Connect Reference settings Manua
190. rogram 2 21 configuration options 2 19 configuring 6 10 isothermal program 2 20 packed 2 24 program buttons 2 18 program display text 2 18 PSS 2 18 split flow 2 23 temperature program 2 19 Inlet temperature program setting up 3 6 Int abbreviation 1 6 Integrator noise 4 90 Isothermal temperature program setting up 3 8 K kPa abbreviation 1 6 L Labels Warning Signs 1 5 Logout 6 79 M Maintenance 6 6 Method Editor 6 4 file menu 5 9 mode 5 5 overwriting the active method 5 9 Multiprogram mode 3 58 Multi ramp temperature program setting up 3 11 N Navigation Bar 2 16 NPD bead activation 4 48 reactivating a used bead 4 53 cross sectional view 4 44 overview 4 44 setting up PPC 4 45 NPD abbreviation 1 6 O One ramp temperature program setting up 3 10 3 19 Oven 2 30 6 18 calibrating the temperature 6 65 calibrating the temperature 6 60 equilibrate temperature 6 62 thermometer probe 6 61 turning on 4 29 4 38 Oven Temperature holding 3 11 Oven temperature program setting up 3 6 setting up a multi ramp 3 11 setting up a one ramp 3 10 3 19 setting up isothermal 3 8 Overview ECD 2 37 4 20 FID 4 5 FPD 4 56 NPD 4 44 PID 4 36 PID abbreviation 1 6 optimizing UV lamp intensity 4 42 overview 4 36 setting up 4 38 setting up PPC 4 40 setup summary 4 38 Pkd abbreviation 1 6 POC abbreviation 1 6 PPC abbreviation 1 6 calibrating carrier
191. s between the two modes Active Method and Method Editor The first screen below shows the PSS active method screen The second screen that follows shows the screen in Method Edit mode we Oyen 4 FID Se A PSSI Oven AFID Events Heater Of I Heater Of A i E C J LA il OFF o C mpini E temp init T Carrier Gas i Carrier Gas 0 0 psi SFE OFF Prograrn Prograrri Split Split total flowy 0 OFF OFF B Ready 17 01 Start 7 Tools d File Active Method Screen Method Edit Mode Oven Settings Touching the Oven button A displays the oven screen in Method Edit mode Method Edilor Aus Wl Aux hetnod hethod amp File T Using the Method Editor Le You can program up to 10 oven steps by e touching the field and using th d AFID Events a a a Re Temp Time Rale down arrow or keypad al T omt 50 foto 100 a buttons to enter a value A PS S Oven After entering all of your settings touch the File button This displays a pop up File menu with options to create modify and save methods Hew Melod pen Save Save As Achvale Delete Exit Editor The Method Name field is not active until you select an option from the File menu Clarus 600 680 GC User s Guide Managing Methods The name of the active method is grayed out in the file name list that appears for Delete Open Activate and Save As
192. s to input a time that the FID s output will go to the integrator 5 Touch the value field and use the drop down to select a negative value detector A is negative detector B is positive B Pkd Oven B TCL Events Edit Timed Event Evert uput A e Time 2 00 Wale y 4 33 OK Cancel har 4 Tools x 6 Touch OK to return to the Events tab page 7 Once in the FID page touch the System button to return to the System Status screen 8 Inthe System Status screen touch the TCD button The TCD page will appear Touch the Events tab 9 Inthe Events screen touch the A button The Timed Events screen will appear In the drop down menu for Events and touch Output B 10 Touch the Time field and use the plus and minus buttons to input a time that TCD output will go to the recorder 4 85 NOTE Setting Up the Detectors 11 Touch the value field and use the drop down to select a positive value detector 1 is negative detector 2 is positive 12 Touch OK to return to the TCD page 13 Once in the TCD page touch the System button to return to the System Status screen Detector routing remains in effect until changed If two detectors are installed but only one configured then the output of the configured detector is sent to both output channels 4 86 Clarus 600 680 User s Guide Attenuating Detector Signals Going to a Recorder The purpose of attenuation when a recorder is attached and
193. s your application requires Once you have modified the Configuration screen touch OK and the new values will now be visible on the FID screen A FID Disable Filter 200 al SetPoint Acal Flameout oo T owo mv Gas Flow SetPoint Actual fir 5 5 mmn Hef 1500 15 0 mLmin Recorder j Iniegrabor Ofset E ris Output a Ready 17 01 z al l OK Cancel 7 13 Setting up a Typical Analysis A PSSI Oven A FID Events a OFF C Heater OF ig Oe a 0 00 mw Bi fe E M Aubzero Fange i uput Recorder Offset Oo Filler 200 m Flameout O 10 mi Gas fon inl Sel Achal Ar 0 A He Ignite Mot Ready Q 8 Iftimed events have to be added or modified in the Active Method touch the Events tab to get to this screen The Events tab accesses the timed events table and buttons valves and Aux gas controls Timed events may be added and removed while the GC is running Method 5 CNC ma APSSI Oven AFID Events Tine Evert Value El Y ALUX Gas Acid Eciit Relays Delete Clear Ready 00 7 14 Clarus 600 680 GC User s Guide 9 Touch the Add button to add a timed event to the run In the Event field select the type of event from the drop down menu Use the up down arrows to input the amount of time for this event in the time field In the value field use the drop down menu to insert the correct value When completed touch OK to return
194. sothermal program into a one ramp program using the previous isothermal method oven temperature parameter as a starting point Init Time 5 min Init Rate 2 C min Time 2 10 min End 0 Cimin To set up a one ramp program 1 From the Oven tab for the initial temp enter 50 2 Enter 5 for initial time 3 10 Clarus 600 680 User s Guide 3 Enter a ramp initial rate 1 of 2 C min 4 For Temp 2 enter a temperature of 70 C 5 Enter atime of 10 min Setting Up a Multiramp Temperature Program The following example shows how to expand the above one ramp program to a two ramp program The parameter values used in the example are shown below Temp 3 100 C Time 3 5 min 1 From the oven tab enter a rate of 4 2 Enter a temperature of 100 3 Enter a time of 5 NOTE You can enter RATE 3 TEMP 4 and TIME 4 to set up a third ramp Holding an Oven Temperature While running a temperature program you can hold the oven temperature by setting it to the temperature of the unexecuted steps To hold an oven temperature during a temperature program 1 Inthe System Status screen touch the oven button k 3 11 Using the Active Method 2 After you touch oven button the Oven tab screen appears Next touch the go to temp button 7 to display the Go To Temp temperature screen Gma B Pkd Oven BTCD Events Ta Temp Time Fate init 75 10o 100 al s260 o
195. sure Program screen Clarus 600 680 GC User s Guide Carrier Pressure Program Current O00 0 0 00 0 00 0 0 psi pressure lme rale psi minubes psiimin ital HoD END AE el S aa Lass Init Time 00m End 1 67 rm 3 Touch the Initial psi field to select it Next use the up and down arrow or keypad al your application SSS E E E 2 aaa 4 When done touch the Close button and the following screen appears gima B Pkd Oven B TCD Events Heater Of 250 8G 260 C lamp i Carrier Gas 0 1 psi l 0 0 mhm 199 psi press init Prograrn Ready Feiss Setting up a Typical Analysis Programmed Split Splitless PSS Injector 1 To select Injector A touch the icon in the active method screen or the PSS button A on the System Status screen Oven AFID Events Heater On BF i 255 C 204 C bernip init rr i Carrier Gas 0 1 psi goo mhm 199 psi 0 0 crivsec press init Prograrn E Split total fow 0 OFF mbm rato 9 faw l Not Ready 17 01 Tools gt 3 Touch the Temperature Program Clarus 600 680 GC User s Guide button to the right of the Progratri temperature field This displays the Injector Temperature Program screen Here you can set an injector temperature program for your analysis The following example shows an analysis that uses the same injector temperature 250 C throughout th
196. t an elevated pressure p and elevated temperature injector temperature The flow rates Fa and Fs are at ambient pressure and temperature The same factors would be applied to each to convert these flows to the true values inside the injector and so they would be cancelled out in this equation 6 72 Clarus 600 680 GC User s Guide Column Length Calculator 1 The Column Length Calculator displays the correct Length of tubing that should be inserted into an injector or detector as measured from the back of the nut Touch the Column Length Calc icon button Column Length Calc 2 The following screen appears Column Length Calculator Length Detector rom back of nut FID a 70 Injector CAP a 44 io 51 amp mir Jin Ready Cel 1s Done 6 73 Using the Tools Menu Background Compensation Background compensation is a routine that automatically subtracts a stored baseline profile from the signal generated during a GC run 7 1 Touch the Background Compensation icon button Pas ground compen 2 The following screen appears Background Compensation A FID B TCD Apply Calibration a Calibrate Baseline fe a Method meras amp Once A hiuliple Run Calibration Ready acti IS a OK Cancel Background compensation is a routine that automatically subtracts a stored baseline profile from the signal generated during a GC run The Background Bakeout tool 1s always enabled Detec
197. temperature programs Longer equilibration times are recommended for initial oven temperatures of lt 50 C An equilibration time of 0 0 minutes can be used for isothermal methods Setting a Coolant Timeout Value The purpose of the coolant timeout value is to conserve coolant If you select a coolant timeout value when you configure the Clarus GC the coolant solenoid shuts off if a GC run is not started within this time period after the oven reaches the initial set temperature Once the coolant shuts off the GC remains not ready and the following message will appear Coolant Timed Out Touch OK to Continue The coolant timeout must be greater than the equilibration time When you press OK the coolant solenoid will then operate again and the oven will cool to the initial temperature NOTE NOTE Using the Active Method When using a POC or PSS injector with the subambient accessory the injector temperature must not be set below the oven temperature You can minimize coolant consumption if using the oven subambient with the PSS or POC installed but not being used by deconfiguring the PSS or POC Setting a Coolant Cut in Temperature The coolant cut in temperature is the temperature at which the coolant starts to cool the oven The default cut in temperature is 60 C The allowable cut in temperature range is 30 C 110 C We recommend that YOU NOTE THE AMBIENT TEMPERARTURE AND SET the cut in temperature 20 C above your c
198. temperature to the value specified for a particular step The last step in the current program is selected by default The buttons for steps beyond the current program are deactivated To change the temperature touch the radio button and press OK Touching cancel retains the current setting and closes the dialog box Go fo Temp Go fo Temp J nijal OK Cancel Element Enabling by mode Enabling by state 3 57 NOTE l Using the Active Method Autosampler Buttons Run options include selecting the run type method autosampler parameters and run start stop program controls The various controls contents and enabling are configuration and mode dependent Multi Program Mode In this mode the autosampler runs two programs consecutively Each program specifies the method to be used each program can use a different method if desired which injector to use the size of the injection the number of injections per vial and the starting and ending vial numbers As each program is run the system sets up the specified method as the Active Method While running in this mode the autosampler attempts at least one injection from each vial in the specified ranges The autosampler tray is keyed to fit correctly only in one direction When installed properly the tray is recessed slightly around the entire Clarus GC top If installed I 80 out of position the tray will be angled not lying flat across the to
199. tes the FID output level is monitored to confirm ignition before producing a READY signal If ignition is not confirmed the ignition process repeats up to two more times if needed If ignition is not achieved after three attempts the flame gases are set to off and a dialog box appears displays the following message Flame 1 or 2 failed to ignite Touch the OK button The status is made NOT READY and FID 1 or 2 flameout appears If auto ignition 1s attempted with the FID gases set to zero flow the message No ignition Flame gases are off appears on the screen To proceed go the PPC screen and touch Reset to the Configuration screen and reset the air and hydrogen to their 450 and 45 mL min flow rates Auto Ignite The auto ignition process only occurs before the start of each run just prior to the instrument becoming READY However the manual flame ignition process performed by touching the Ignite button can be initiated at any time Auto ignite proceeds in the following sequence When auto ignite begins the Clarus GC equilibrates Once the two minutes of equilibration expire PRE RUN begins and the AutoSystem detects that the flame is not lit and indicates this by alternately flashing Flame and Method 5 in the status bar After determining that the flame is not lit the AutoSystem switches to a not ready state and attempts to automatically ignite the flame Flame Ignition 1 appears in the status bar The air f
200. the TCD Current Filament Current icre eii EAA 4 78 Changing TCD Polarity During a Rinses A NEATE 4 80 Routine Detector OUMU arasen a N a a dats 4 83 Reroute OUT OU shenoni a a a a 4 83 Attenuating Detector Signals Going to a Recorde cccecceeeeeeessesssssessesssssseeeseeeeens 4 87 Optimizing a Detector Signal to an Integrator for Maximum Sample Dynamic Range 4 89 Matching Detector Signals with Your Integrator ccccccseeesesssssssssessessesssessseeeeens 4 90 PRULOZC TOMI a DELEC TOL ameero atauanedcdsct au ed aveacdesser aeacdontssectene auaed at aoe eacee saoedoe oe eae 4 93 Using the Method Editor asiicsais skeet edesaccaatstccct avaccateiisctecstuasccastseui tcaebaessndsebivcdss oescuduteeos 5 1 IVA E21 HS YO S A E Shi 0 EEEE E EAEE EREE E A UNOS eROR ES NO AU EOI ee ER TAD SEN T ir Sen ewe Cn 5 3 INDE EMOG EGIL Mod ic scinicn sas Sear seanhsict tatiudien Yeaanadstaamhenr usenet a i i Na oe 5 5 Oven Na a a ae a ae ee eat 5 7 Manag ino Methods a fice cc nace sak atoa a a T nsec OTT 5 9 FE MeNe a N 5 9 Wsine the Pools Mentiin aaaea AEAT 6 1 LOO WICH ern a A basaudnig obeietaeanenaatony 6 3 Meomhod Edinen E a ER 6 4 Evon EOS ernen A NON TS NEE ENN SSO EE AIS ROL Tar 6 5 IMI AITILCI ADC esseen E 6 6 COMMIT OUP O Ds ae cate A ede ete 8 a altars di cleat Ns Be ete hs ae aia Sah od alien 6 10 Injectors Deconfiguring and Configuring Injectors ccccccccccccccceeeeeeeeeeeeeeees 6 10 VC ssa ceattateentis
201. the run When the run 1s completed the system switches back to the initial value in this case 2 4 82 Clarus 600 680 User s Guide Routing Detector Output The Clarus GC contains one analog data output channel for each installed detector amplifier board You can attach an integrator or recorder to either output channel Normally the detector output would go to the device configured for that channel However if you are running complex analyses such as those requiring detector switching you may wish to route the signal to either channel Rerouting Output Assume that e Detector 1 is an FID whose output is going to an integrator in this example the integrator is output A e Detector 2 is a TCD whose output is going to a recorder in this example the recorder is output To reroute the FID output A to the integrator 1 From the System Status touch the button for the FID Detector any 2 The FID tab page will appear Touch the Events tab 4 83 Setting Up the Detectors EE B Pkd Oven B TCD Events Time Evert Value AUK Gas Edit Relays Delete Clear Ready 4701 3 Inthe Events screen touch the Add button The Timed Events screen will appear In the drop down menu for Events and touch Output A Event uput A H Ready hiar 4 Tool ad T 4 84 Clarus 600 680 User s Guide 4 Touch the Time field and use the up and down arrow or keypad al EE button
202. tics provide you with TCD filament protection by monitoring the carrier gas leak tests or monitoring the gas through the alarm feature and shutting down the TCD current if a gas leak or no gas at all is detected The PPC modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure 1 To set the make up and reference gases touch the Tools button and touch Configuration from the drop down menu e rasv 4 31 Setting Up the Detectors This displays the Configuration screen page Sep Preumaics Relays 17 01 Close 2 Touch the TCD button to display the TCD configuration screen The following example shows the TCD configuration settings and how they correspond to the TCD active method screen TCD Active Method TCD Configuration Screen B TCD Filter 200 Method 5 Gma B Pkd Oven B TCD Events E i qog C Heater Off emp 0 00 my es C as Flows atten 256 g AutoZero Define Gas Sources Current 40 ma Outout Recorder ITED a tenint Actual i N mLtnin Make up 0 0 Ff 00 riLirnin Reference Filer 204 BD Gas flow gril SUE Ref 0 0 ofset b oo Make Up Oy 00 she 17 01 Ready IFO __ A Tools 4 PEE OK Cancel 4 32 NOTE Clarus 600 680 User s Guide In the TCD Configuration screen set the Make up gas and Reference gas line flows to 30 mL min using the up and down
203. to In this example step 2 is selected Press Graph and status bar show the the OK button to immediately raise The blue line in the graph reflects oven is ready to run a program the oven temperature to the value the departure from the program specified in step 4 Gma B n ap gma A FID Ewents A Gap Oven A FID Events 3 Time Rate gt i aje i Temp Time Rate E nit 76 100 10 0 i init 75 100 i0 a C a 10 100 so Go to Temp toate a fao 100 so 3 125 100 100 A 3 12 100 100 4 150 100 END Bd z si 4 150 109 END d we 38 a4 ma ji E Cancel E 750 0 Oven Of ue 14 00 a Running Time 1 0 07 min Running Rate 2 2 70 min ECE vale mv EN Af mew 2 30 Clarus 600 680 GC User s Guide Aux Zone If the GC 1s configured with an auxiliary zone the button appears on the status screen Touching the Aux button displays a dialog box with the setpoint and actual temperature Aux Pneumatics AUX ZONES Inibal Current eo None OFF 0 0 a 2 None OFF 0 0 3 Pressure psi OFF 0 0 4 More OFF aQ a A Close Not Ready 17 01 start o Tools x 2 31 Touch Screen Navigation Detectors Detector screens provide you with a way to set and control a number of parameters during a run such as temperature range and attenuation Other active elements include a Heater Off button to turn off the detector and an AutoZero check box Selecting
204. to 45 mL min uput 4 10 Clarus 600 680 User s Guide Disable Filter 200 SetPoint Actual Flameout 0 10 000 rr S oA Gas Flow SetPoint Actual Air 450 45 mimin He 1 5 mimin uput amp Recorder _ 3 Integrator Ofset F oo Mot Ready 17 01 v 4 TE OK Cancel 8 Press OK Automatically Ignite the Flame How Auto Ilgnition Works To ensure proper auto ignite FID operation make sure your column is positioned in the FID 2 75 inches 70 mm from the CAUTION back of the column nut The flame may not auto ignite if your carrier gas flow is 60 mL min or higher The PPC version of the FID has flameout detection and an auto ignite feature Flameout detection occurs 0 5 minutes into the PRE RUN time and it measures the user entered baseline threshold level in mV If the threshold level is exceeded the flame is considered lit otherwise the Clarus GC detects that the flame is out and auto ignite automatically lights the flame before the start of a run 4 11 Setting Up the Detectors With the FID temperature set the air and hydrogen flows set and auto ignition activated by setting a positive mV value for the flame offset the FID attempts auto ignition at 0 5 min before the system becomes ready At this Pre run time the status bar flashes Flame Ignition as the air flow is shut off hydrogen purges the FID for about 10 seconds and the ignitor energizes for ignition follo
205. to the Event tab Repeat this procedure until you have added all the timed events for your procedure A PSsl Oven AFD Events Mar 4 Tools ad 10 Once all the fields have been set as required by your application touch the ignite button A on the FID tab screen to ignite the FID Ignite 7 15 Setting up a Typical Analysis Detector Thermal Conductivity Detector TCD 1 Touch the TCD button on the Status Screen to display the TCD tab 2 To program the temperature in the TCD tab touch the Temperature field and it will go black Then use the up and down arrow or keypad hl EEE application 3 Repeat the same procedure for the Attn attenuation and Current As shown in the example below this analysis has the heater off 7 16 Clarus 600 680 GC User s Guide B Pkd Oven B TCD Events eg i oFF K Heater Of temp 0 00 mi 25 C ira mo EJ I Autozero Current 40 mA Output Recorder ofset wi Filter 200 mS as fon iLi Sel Actual Ref 0 0 None Ready 2700 Tol hd If you require the heater on for your analysis just touch the Heater button and it will toggle to heater on To have the detector autozero the baseline to a fixed amount touch the AutoZero field for the check off to appear in this example AutoZero will not be used it 1s not checked off B TCD Events ED i OFF 7c Heater Of emp 0 00 mv B Pkd Oven
206. tor A and Detector B need to be labeled with the installed detector names The Calibration checkboxes are enabled if a detector is installed in that position 6 74 Clarus 600 680 GC User s Guide Type Method and Start are always enabled so that a bakeout can be performed with a mass spec or other system with zero detectors Before background compensation can be applied to a detector output signal the baseline profile must be calibrated The background function controls both calibration and compensation Calibration involves running a blank using the temperature program Once run the background profile is stored This profile is overwritten if calibration is rerun thus only the most recent profile 1s used for compensation One background profile is stored for each detector Calibration and compensation can be applied independently to each detector output signal Note Calibration run time must be greater than 2 minutes Calibration Menu Options Once The background profile will be calibrated once and stored This profile is applied automatically to all manual or autosampler runs when you subsequently turn the background compensation On Multi The system runs the calibration method over and over again until you turn off calibration in the Calibration Menu You may wish to use this option for example to condition a column overnight Off Select this option to turn calibration off 6 75 Using the Tools Menu
207. ttons show the PSS injector icon and the packed column injector icon respectively Also the Detector A and B buttons show PID and ECD icons respectively Touching a Carrier Detector or Aux icon button displays a dialog that allows this device to be defined 6 39 Using the Tools Menu Connect PPC Device a D PPC Define Aux 1 Funchon Position we BIJE a OK cancel hlar 4 Close PPC Deine Carrier A Function Position Carr Fico e a secondary Pasion far el for 3 a OK Cancel Since the PPC has yet to be configured the primary module is undefined and the secondary module entry is disabled 6 40 Clarus 600 680 GC User s Guide The primary entry is expected to be the module function The following screen shows the full potential range available for the primary module function Connect PPC Device 7 3 PPC Define Carrier A Function Position fre af fr secondary Fosiion fre Pe a OK Cancel The available range of functions is calculated by combining the set of potential functions from each of the uncommitted positions with the valid set of functions for this logical position This is explained in more detail in a later section For a Carrier a Detector flow module 1s invalid and is not offered Note that at this point the only available position for the primary module
208. u 2 In PPC Reference Conditions screen add the reference temperature and pressure using the plus minus buttons Touch OK when completed Configuration PPC E PPC conigure PPC Reference Conditions SetPoint Actual Ref Pressure t San 14 70 ial Rel Temperature 26 0 C OK Cancel PRC Alarm Enable 2700 a OK Cancel Calibrating the Carrier Gas Modules If you are performing this calibration procedure and you do not have a column connected to the detector you must plug the CAUTION detector fitting in the oven with an Swagelok 1 8 inch cap before proceeding This will ensure that all the gas flows up through the detector and not into the oven If you are using a packed injector or programmed on column injector you can disconnect the column and measure the flow at the exit of the injector If you are using a capillary injector or programmed split splitless injector you must remove the column Cap the injector exit in the oven and measure flows at the split vent exit To cap the injector exit in the oven locate the Capillary Column Shipping Kit P N N6100160 and insert the solid ferrule P N 09920511 into the 1 16 inch nut P N 09903392 and connect the nut to the exit of the injector 6 54 Clarus 600 680 GC User s Guide To obtain the correct results before you begin to calibrate you CAUTION DENOTE 4 must first Zero the Gas Modules 1 From the PPC screen touch the PPC
209. urrent ambient temperature For example A room temperature of 20 C uses a default temperature of 40 C whereas a room temperature of 25 C uses a 45 C cut in temperature Examples for setting up isothermal 1 and 2 ramp programs follow Higher cut in temperatures cause more coolant to be consumed Configuration Oven Lirnit Equilipration IE o m T Startup Heat Delay Aux Heat None H Calibration Ofset 0 00 C Actual Si SiE Coolant Type co2 e al 40 C Enable Timeout a 15 fin Sot cooling Oven Fan 1400 RPM Mot Ready 17 41 v FE OK Cancel Setting Up an Isothermal Program Setting up an isothermal program requires entering the following information in the sequence shown e Initial oven temperature Temp 1 e The total run time for the initial temperature Time 1 e A temperature rate increase of 0 Rate 1 NOTE NOTE Clarus 600 680 User s Guide To set up an isothermal program 1 From the Oven tab set the initial temperature 1 to 75 C using the up and down arrow or keypad al 22 buttons Gm tap B PSS Oven B TCD Events KA Temp Time Rate int 75 100 ioo a C 9 100 100 50 4 125 100 100 4 150 100 END Bd 2 Enter a temperature setpoint appropriate for your analysis for example 100 C The oven status changes to Not Ready The changing oven temperature is displayed under the oven icon as the oven heats up to the new setpoint
210. used and is not disconnected from the detector a high detector temperature can cause bleed at the detector junction with the column Make certain the detector temperature is lower than the maximum temperature recommended for the capillary column of your application Set the hydrogen and air flow as follows e Air to 100 mL min e Hydrogen to 2 0 mL min Hydrogen flow accuracy is critical to proper NPD bead activation Make certain that the H2 flow is within 0 5 mL min or closer to the H2 set point of 2 0 mL min Check with a calibrated flow meter at the detector bulkhead that the flow is accurate if activation problems occur Ensure that the hydrogen line is well purged of entrained air before you make the final setting of hydrogen flow Failure to purge the gas line from the hydrogen supply tank or generator will result in an incorrect flow setting for operation and can lead to poor operating performance and reduce bead life 10 Set the detector range to x1 4 49 Setting Up the Detectors 11 From the system status screen touch the signal icon a to display the detector background When the bead is off the background value should be 0 0 25 mV Write down the background value that occurs with the bead off 12 Open the detector cover see Figure 4 28 and locate the bead potentiometer dial see the following figure If the NPD is detector 1 front position the potentiometer is located on the left side of the panel I
211. vents tab to get to this screen The Events tab accesses the timed events table and buttons valves and Aux gas controls Timed events may be added and removed while the GC is running 7 19 Setting up a Typical Analysis og mle B TCD Events B Pkd Oven Tine Event Value AUX Gas Add Edit Relays Delete Clear Ready O12 h Tools HHH Touch the Add button to add a timed event to the run In the Event field 11 select the type of event from the drop down menu Use the up down arrows to input the amount of time for this event in the time field In the value field use the drop down menu to insert the correct value 12 When completed touch OK to return to the Event tab Repeat this procedure until you have added all the timed events for your procedure og miD B TCL Events B Pkd Oven Add Timed Event Evert Range amp Time 0 00 Value OK Cancel ict 1 Tools nd 7 20 Clarus 600 680 GC User s Guide 13 Once all the fields have been set as required by your application for the TCD touch the Clarus GC icon v on the screen 7 21 Setting up a Typical Analysis Autosampler 1 Touch the Run button to display the Autosampler setting screen 2 The Autsosampler screen allows you to select the method from the drop down window Once you select the method you want to use for your application the injection count down will beg
212. wed by a return of the air flow to the detector to sustain the flame After the flame ignites the FID output level is monitored to confirm ignition before producing a READY signal If ignition is not confirmed the ignition process repeats up to two more times if needed If ignition is not achieved after three attempts the flame gases are set to off and a dialog box appears displays the following message Flame 1 or 2 failed to ignite Touch the OK button The status is made NOT READY and FID 1 or 2 flameout appears If auto ignition is attempted with the FID gases set to zero flow the message No ignition Flame gases are off appears on the screen To proceed go to the Configuration screen and reset the air and hydrogen to their 450 and 45 mL min flowrates To Auto lgnite The auto ignition process only occurs before the start of each run just prior to the instrument becoming READY However the manual flame ignition process can be initiated at any time by touching the Ignite button 6 1 The auto ignite begins with equilibrating the Clarus GC 2 Once the equilibration expires Pre run begins and the GC detects that the flame is not lit and indicates this by alternately flashing Flame and the method name in the status bar 3 After determining that the flame is not lit the GC switches to a not ready state and attempts to automatically ignite the flame Flame Ignition 1 appears in the status bar 4 The air fl
213. wise Notes cautions and warnings Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE 4 note indicates additional significant information that is provided with some procedures We use the term CAUTION to inform you about situations that could result in serious damage to the instrument or other CAUTION equipment Details about these circumstances are in a box like this one We use the term WARNING to inform you about situations that could result in personal injury to yourself or other persons Details about these circumstances are in a box like this one WARNING Clarus 600 680 GC User s Guide Warning Signs on the Instrument For detailed safety information see the Safety Practices chapter in the Clarus 600 680 GC Customer Hardware and Service Guide P N 09936781 Caution hot surface Caution risk of electric shock Caution laser radiation hazard Caution refer to accompanying documents 1 5 Introduction Screen Abbreviations AUX Auxiliary zone Cap capillary split splitless injector Cmptr computer Ctrl syringe control parameters ECD Electron Capture Detector FID Flame Ionization Detector FPD Flame Photometric Detector Gen generate Inj Vial injections per vial Int integrator kPa kilopascals NPD Nitrogen Phosphorus Detector PID Photoionization Detector Pkd packed
214. with respect to solute concentration over a defined range for example the Linear Range Liquid phase The material in the column that causes the components to separate because of partitioning of the components between the mobile phase carrier gas and the stationary phase liquid phase Lowest limit of detection The smallest amount of sample that can be detected by the detector being used Usually defined as any signal that is as great as two times the noise level Also referred to as Minimal Detectable Quantity MDQ Mobile phase The gas which carries the solute sample along and over the column material This carrier gas is inert and usually helium nitrogen or hydrogen Noise Background signal fluctuations arising from a detector response This response is the result of the column installed carrier gas purity electronic components etc The response of any detector is defined by the signal to noise ratio Partition Coefficient The differential solubility of a substance in two different phases In the case of gas liquid chromatography the sample components reach an equilibrium between the gas phase mobile and the liquid phase stationary Each component has a different partition coefficient thus causing separation in the column Pressure programming Pressure control through an independent four step three ramp program for each carrier gas channel Resolution The degree of separation between tw
215. xit configuration 6 16 Clarus 600 680 GC User s Guide GSV Gas Valve l This example shows that GSV a gas sampling valve is selected as the Type on the Configuration screen Configure Injector A Type esv M Capillary Control Carrier Control Pressure A Program J Ovenkack column Lenginy 25 00 mo LD 250 um Split made Flow Offset Flow ato Auto Fixed afset 1 00 mLimin T Vacuum Compensation 17 41 OK Cancel 2 Make your settings then touch the OK button Then touch the Close button to exit configuration 6 17 Using the Tools Menu Oven Use the oven configuration screen to set up oven parameters This example shows a temperature limit of 300 C and an Equilibration rate of 1 0 mL min Configuration Oven Lirnit Equiliprator w po e io mn Startup Heat Delay Aux Heat None Calibrator Ofset 0 00 E Actual BC oe Coolant Type ae Enable Timeout at min Sot Cooling Oven Fan 1400 RFM Ready 11 14 OK Cancel EE E CEE Calibration When the Calibration Offset field is selected it turns black The default value is 0 The Offset range is 10 to 10 C Enter the Offset temperature and allow the oven temperature to equilibrate for at least 30 minutes The displayed temperature will approach 100 00 C or the oven temperature you entered and the thermometer readout will appro

Clarus 600/680 GC User's Guide

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