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FID Overview . 113

FID Overview

Flame Ionization Detectors (FID) are mass sensitive and used for the destructive analysis of organic

compounds.
As the sample enters the detector, it is mixed with hydrogen and then burned in air, thereby 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 voltage (

+50

V) to the jet tip. The detector sensitivity is affected primarily by the hydrogen 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.

Setting Up a PPC FID

To set up a FID that uses PPC modules, first read the FID setup summary, then follow these procedures.

FID Setup Summary

To set up the PPC version of the FID:

•

Set the air and hydrogen flows.

•

Automatically ignite the flame.

•

Manually ignite the flame.

Содержание CLARUS 590 GC

Страница 1: ...CLARUS 590 GC User s Guide GAS CHROMATOGRAPHY ...

Страница 2: ...gard 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 rig...

Страница 3: ...ual Injection 27 Signal Button 28 Ignite Button 28 AutoZero Button 28 Signal Plot 28 Signal Display and Scaling 29 Zero Display Button 29 Heated Zones 29 Injector and Detector Buttons 30 Oven Button 31 Aux Zone Buttons 31 Navigation Bar 32 Injectors 33 Program Buttons 33 Display Text 33 PSSI 34 Configuration Options 34 Temperature Program 34 Isothermal Program 36 Carrier Gas Program 36 Split Flow ...

Страница 4: ... 65 Setting Up an Isothermal Program 65 Setting Up a One Ramp Temperature Program 66 Holding an Oven Temperature 67 Setting Injector Temperatures 69 Displaying Injector Temperature Screens 69 Turning Injector Heaters On or Off 70 Changing Injector Temperatures 70 Oven Temperature Programming Mode 71 Inlet Temperature Programming Mode 71 Setting Up a One Ramp Injector Program 72 Viewing Setting Car...

Страница 5: ...rs 106 Configuration Button 106 Auto Resume 106 Running Viscous Samples 106 Using Solvent Pre Washes 107 Priority Button 107 About Waste and Wash Vials 107 Multi Program Mode 107 Waste Vials 107 Wash vials 108 About Sample Vials 108 Using a TCD with the Autosampler 108 Available syringes 108 4 Setting Up the Detectors 109 Overview 111 FID Overview 113 Setting Up a PPC FID 113 FID Setup Summary 113...

Страница 6: ...tor Heaters 144 Adjust the Make up Gas 145 Set the Make Up Gas in the PPC Version 146 Turn on the UV lamp 148 Optimize the Lamp Intensity 149 NPD Overview 150 Setting Up a PPC NPD 151 Set the Hydrogen Flow and Air Flow for PPC 151 Setting Up a Manual Pneumatics NPD 153 NPD Setup Summary 154 Disconnect the Hydrogen and Air Lines at the NPD Bulkhead 154 Adjust the Hydrogen Flow 155 Adjust the Air Fl...

Страница 7: ...93 Matching Detector Signals with Your Integrator 194 Autozeroing a Detector 196 5 Using the Method Editor 197 Method Editor 199 Method Edit Mode 200 Oven Settings 201 Managing Methods 202 File Menu 202 New Method 202 Open Method 203 Save 203 Save As 204 Activate 206 Delete 206 Exit Editor 206 6 Using the Tools Menu 207 Using the Tools Menu 209 Method Editor 209 Event Log 209 Maintenance 210 Confi...

Страница 8: ...brating the Oven Temperature 251 Calibrate the Reference Thermometer 251 Place the Thermometer Probe in the Oven 251 Equilibrate the Oven Temperature 252 Enter the Required Offset Value 254 Remove the Thermometer Probe 254 Utilities 255 Column Flow Calculator 256 Column Flow Calc Main Screen 257 Length 257 Diameter 257 Temp 257 Carrier Gas Name 257 Outlet Press 257 Suggested Velocity 257 Inlet Pre...

Страница 9: ...About This Manual 9 Flame Ionization Detector FID 270 TCD 273 Autosampler 277 Index 279 ...

Страница 10: ...10 Clarus 590 GC User s Guide ...

Страница 11: ...1 Introduction ...

Страница 12: ...12 Clarus 590 GC User s Guide ...

Страница 13: ...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 contains information on how to run a typical analysis on the Clarus GC using the most common configuration Conventions Used in this Ma...

Страница 14: ...s En recuadros éste se proporciona información sobre este tipo de circunstancias F Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci I Caution Attenzione Con il termine CAUTION ATTENZIONE vengon...

Страница 15: ...s recuadros como éste se proporciona información sobre este tipo de circunstancias F Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci I Warning Pericolo Con il termine WARNING PERICOLO vengono segna...

Страница 16: ...nization 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 injector POC Programmed On Column Capillary Injector PPC programmed pneumatic control Pre of pre injection syringe washes Psi or psig pounds per square inch gauge PSS Programmed Split Splitless Capillary I...

Страница 17: ... Mode The style of injection Fast Fast speed of the syringe during sample injection This is used to eliminate discrimination in the needle Normal Normal speed of the syringe during sample injection Slow Slow speed of the syringe during sample injection in order to inject directly into a wide bore capillary column in hot injection port Instrument Specific Terms Term Description Background compensat...

Страница 18: ... Pneumatic Control Pre run The time after equilibration during which negative time events are executed PreVent PPC version only Sample management system Range Range means amplification 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 progr...

Страница 19: ...ydrogen 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 re...

Страница 20: ...ction 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 nitrog...

Страница 21: ...2 Touch Screen Navigation ...

Страница 22: ...22 Clarus 590 GC User s Guide ...

Страница 23: ... may like to touch the active areas of the touch screen Do not use sharp pointed objects A light touch is 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 activ...

Страница 24: ...hic 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 the PPC carrier gas zone is active The icon buttons that represent the heated zones injectors detectors oven and Aux if configured include a light to indicate the ready not r...

Страница 25: ...ith a specific channel Non Configured Devices If a device is installed but not configured or configured as None the graphic and light are grayed out Touching the button prompts the following dialog box The following capture shows the drop down list on the injector configuration screen to set a device as None ...

Страница 26: ...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 When an Autosampler is enabled the Run button defaults to that screen The following scree...

Страница 27: ... 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 is disabled and the wording in instruction 3 is modified to exclude the tone The system ...

Страница 28: ...gh an attenuation and offset filters The name of the channel appears on the top left of the screen Detector controls include Ignite and Autozero Zero 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 AutoZero Button Autozeroes the selected detector Signal Plot...

Страница 29: ...doubling the current factor 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 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 ...

Страница 30: ...uching 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 alternative 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 ...

Страница 31: ...sed 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 screen that follows the same format as the injector screens and shows the current temperature ...

Страница 32: ...ion 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 with the corresponding icons on the status screen ...

Страница 33: ... 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 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 veloc...

Страница 34: ... Program The PSS temperature program can be set for Program Inlet or Oventrack Mode Description Program Inlet In the program inlet 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 Oventrack The oventrack mode is where the injector setpoint equals the oven setpoint plus 5 C The tem...

Страница 35: ...jectors 35 To modify the temperature program during a run touch the program button You can modify the temperature time or rate However if the program is currently in that step the changes will be ignored ...

Страница 36: ...locity If the option for Cap control is selected you can program the carrier gas according to one of the three values The corresponding actual values for the other units appear as read only text on the screen Touching the program button next to the field displays the associated program for the entry field value Pressure The carrier gas is configured for Pressure This option appears in the entry fi...

Страница 37: ...in the entry field Touching the Program button in the Active Method displays the Carrier Flow Program Velocity The carrier gas is configured for Velocity This option appears in the entry field Touching the Program button in the Active Method displays the Carrier Velocity Program ...

Страница 38: ...tpoint 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 Capillary Control Off Cap Injector PSSI Injector ...

Страница 39: ...ure field The carrier gas can be programmed by Pressure or Flow as shown in the following screens The following procedure shows how to navigate through the screens to configure PPC for a packed column injector 1 Select Configuration from the Tools menu 2 Touch the Pneumatics button ...

Страница 40: ...Touch the OK button 5 Touch Carrier B to Configure your injector for PPC 6 Select Pres Read from the drop down menu Then touch the OK button 7 Touch Close to close the Connect PPC Device screen 8 Touch OK on the Configuration PPC screen 9 Touch the B Injector button on the Configuration screen ...

Страница 41: ...r B screen appears 11 Select Pressure or Flow from the drop down menu 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 ...

Страница 42: ...be programmed by Inlet POCI or Oven POCO The POC injector is configured and controlled according to the same parameters as the PSS injector Capillary Cap Packed On Column Inlet Packed On Column Oven 1 From the Configuration menu select Cap from the drop down list 2 Exit from Configuration and display the active method screen ...

Страница 43: ... in the current program are deactivated In the example below step 4 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 Graph and status bar show the oven is ready to run a program Touching the Go to button displays the Go to Temp dialog box to select a step to ...

Страница 44: ...arus 590 GC User s Guide Aux Zone If the GC is 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 ...

Страница 45: ... describes the screen components for each type of configuration The Ignite button allows you to light the FID flame About Auto Ignition The PPC version of the FIDW 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...

Страница 46: ...urs 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 1 When auto ignite begins the Clarus GC equilibrates 2 Once the two minutes of equilibration expire PRE RUN begins and the GC detects that the flame is not lit and i...

Страница 47: ...tector 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 is set up with the same amount of carrier gas flowing through both channels The presence of a sample component in the carri...

Страница 48: ...48 Clarus 590 GC User s Guide PPC Active Method Configuration Screen Manual Pneumatics ...

Страница 49: ...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 handli...

Страница 50: ...50 Clarus 590 GC User s Guide PPC Active Method Configuration Screen Manual Pneumatics ...

Страница 51: ...ization 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 PPC Active Method Configuration Screen Manual Pneumatics ...

Страница 52: ...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 The following screens sho...

Страница 53: ...be 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 PPC Active Method Configuration Screen Manual ...

Страница 54: ...Clear button Always 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 lis...

Страница 55: ...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 is accepted do not occur until the next run The following error message may appear Delete Touching this button deletes an event The following messages may appear ...

Страница 56: ...box and retains the contents of the Events table If the table is empty the following Error message appears Event 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 The PreVent ProTect MS Vent valves are never operated during a run and are not required in the Timed E...

Страница 57: ...pear as set in the configuration screen A User can turn on the initial and or current settings by touching the check box 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 Aux Zones Heated Au...

Страница 58: ...rol When one or more of the aux zones is configured the following button appears on the status screen The same button also appears on the Events screen Touching this button displays the following screen Aux Zones that have been set 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 show...

Страница 59: ...3 Using the Active Method ...

Страница 60: ...60 Clarus 590 GC User s Guide ...

Страница 61: ... 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 out...

Страница 62: ...nt 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 Setting up oven temperature programs Setting injector temperatures programs PSS and POC Setting detector temperatures Viewing setting carrier gas pressure programs PPC V...

Страница 63: ...column before closing the oven door and elevating the oven temperature The Status screen icon buttons provide access to the active method parameters 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 RDY until the new setpoint is reached ...

Страница 64: ... button to activate the next row The following figure shows a typical temperature step program Before you actually set up an oven temperature program you should decide on the Equilibration Time you need and change the default value 2 minutes 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 set...

Страница 65: ...ant 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 below which the coolant starts to cool the oven The default temperature is 60 C The allowable cut in temperature range is 30 C 110 C We recommend that for every C above a room temperature...

Страница 66: ...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 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 ...

Страница 67: ...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 Parameter Value RATE 2 4 C min TEMP 3 100 C TIME 3 5 min RATE 3 0 C 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 Wh...

Страница 68: ...u want to hold Touch OK Modify the temperature on the oven tab screen using the up and down arrow or keypad buttons When completed return to the system status screen The oven heats ballistically to the temperature value for oven Temp 2 and holds instead of executing the time associated with oven Temp 2 To hold the oven program at a specific time during or before a run use an oven HOLD timed event ...

Страница 69: ...cked injector installed and configured in position B rear This section contains examples of how to 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 From the System Status screen touch the injector icon this will bring you to the injector t...

Страница 70: ...e 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 not display a check mark 2 Touch the Temp field and using the up and down arrow or keypad raise the value to 255 ºC ...

Страница 71: ...and hold for 10 min NOTE 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 Inlet Temperature Programming Mode The inlet temperature programming mode is used when the POC or PSS injector is configured as Inlet In this mode the injector follows the injector temperature program ...

Страница 72: ...initial to the final injector temperature Initial Rate Final injector temperature Temp 2 Isothermal time for the final temperature Time 2 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 The parameter values used in the example are shown below Parameter Value Initial Temp ...

Страница 73: ...reen NOTE You can enter Rate 2 Temp 3 and Time 3 to set up a second ramp An entry of 999 for Rate 1 or 2 will cause the injector to ballistically heat up NOTE If 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...

Страница 74: ...e 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 in the PPC Version for information on...

Страница 75: ... the set limit for more than one minute a warning message appears Setting PPC Carrier Gas Pressure in the PPC Version To view or set the carrier pressure 1 From the System Status screen touch the Injector icon for which you want to set the carrier pressure The screen for the selected injector appears In this example the Clarus GC is configured with the capillary mode on for pressure If the option ...

Страница 76: ...pas recommandé La définition d un taux de programme sera plus reproductible 4 Touch Close to return to the injector screen Viewing or Adjusting Carrier Gas Pressure Using Manual Pneumatics To view and or adjust carrier gas pressure 1 From the System Status screen touch the Injector icon The tab page for the selected injector appears 1 In the screen above the set point value for Carrier Gas field i...

Страница 77: ...GC is configured with the capillary mode on for flow If the option for capillary control has been selected during configuration the user 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 of the available con...

Страница 78: ...mming is not recommended Setting a program rate will be more reproducible Le mode balistique de programmation n est pas recommandé La définition d un taux de programme sera plus reproductible 4 Touch Close Viewing Adjusting Carrier Gas Flow Using Manual Pneumatics To view the display 1 From the System Status screen touch the Injector icon The tab page for the selected injector appears In this exam...

Страница 79: ... can set the carrier gas velocity only if you have the PPC version To view or set the carrier gas velocity 1 From the System Status screen touch Injector icon for which you wish to set the carrier gas velocity The tab page for the selected injector appears In this example the Clarus GC is configured with the capillary mode on for velocity If the option for capillary control has been selected durin...

Страница 80: ...ld ranging from the Initial field to the step 4 field and use the plus minus 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 ballistic setting CAUTION ATTENTION The ballistic mode of programming is not recommended Setting a program rate will be more reproducible Le mode balistique de programmation n est pas recommandé La définit...

Страница 81: ...um purge and offset 1 Touch the Tools button and select Configuration from the drop down menu The Configuration screen appears 2 Touch the button for the injector you want to modify A Injector or B Injector The Configure Injector screen appears 3 From the Carrier Control drop down menu select Pressure ...

Страница 82: ...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 which is equal to the septum purge flow plus the column flow at the time of injection Since the system controls...

Страница 83: ...ty you must enter your column dimensions as described in the following steps However if you select the Oventrack mode from the Carrier Control drop down menu you do not need to enter column dimensions and you can skip to step 12 8 Select either Program or Oventrack The following screen shows Program selected However if you select the Oventrack mode you do not need to enter column dimensions and yo...

Страница 84: ...low 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 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 If you select Flow yo...

Страница 85: ...ute 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 sa...

Страница 86: ...se the up and down arrow or keypad 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 ...

Страница 87: ...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 The Configuration screen appears 2 Touch the Injector icon for which you which to configure the split mode The Configure Injector screen appears 3 Touch the Capillary Control check box ...

Страница 88: ...Configuration screen appears 5 Touch Close 6 On the System Status screen touch the Injector icon The active method screen appear The screen above displays the Split mode configured for Ratio 7 Touch the r ratio field to modify the value OR If you configured the split mode for Flow the following screen appears ...

Страница 89: ...e O ring seal column connector etc See the Clarus Hardware Guide Chapter 8 for further information NOTE It should be noted that if the displayed value is much greater than the total flow split flow and septum purge column flow this indicates a leak in the pneumatics Setting the Split Mode Using Manual Pneumatics Set the Solenoid Valve for Split Operation 1 From the System Status screen touch the I...

Страница 90: ...s the split vent open NOTE If you are using the Clarus GC for the first time valves 1 and 2 will be OFF Valves that are off are shown as unchecked NOTE Modifications to the valve settings become part of the Active Method and are automatically saved Measure and Adjust the Split Vent Flow To measure and adjust the split vent flow 1 Open the detector cover indicated below ...

Страница 91: ... split vent 3 Attach a flowmeter to the split vent 4 Turn the outer knob of the split flow knob fully counterclockwise see below 5 Measure the flow 6 Remove the cap from the split flow knob thereby exposing the split flow needle valve ...

Страница 92: ... suggested starting point is 100 mL min 8 Remove the flowmeter 9 Replace the cap on the split flow knob 10 Set up the detector to be used with this column NOTE If the inlet pressure is changed the split flow will also change NOTE Recheck the inlet pressure with the vent open when using high vent flows The inlet pressure may have dropped slightly ...

Страница 93: ...l 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 Clarus 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 experimentall...

Страница 94: ...94 Clarus 590 GC User s Guide 2 Touch the Events tab 3 Touch Add The Add Timed Event screen appears 4 Select Split A from the Event drop down menu ...

Страница 95: ...lues 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 flow at 0 25 min 8 Touch the A Cap Injector tab The Injector status screen appears 9 Touch the Program button for the Carrier Gas field The Carrier Gas Pressure Program screen appears 10 Touch the Initial pressure dialog box and use the up and dow...

Страница 96: ... Clarus GC MS detector 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 sa...

Страница 97: ... 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 up and down arrow or keypad buttons to enter a negative Time for example 1 00 min for the event to occur prior to the Clarus GC coming ready Then press Enter The cursor moves to Event 5 Touch the Value dialog box and use up and down arrow or keypad buttons to enter a value...

Страница 98: ...he Time dialog box and use the up and down arrow or keypad 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 in...

Страница 99: ...lit flow on just prior to when the inlet pressure begins to drop to the operating setpoint 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 Si vous utilisez une injection d impulsion de pression vous devez régler le flux divisé juste avant que la pression d entrée commence à tomber à la consigne de fonctionne...

Страница 100: ...le from syringe to syringe The autosampler contains three basic parts a syringe tower a carousel and a sample tray see the following two figures The syringe tower can contain either a 0 5 5 0 or 50 0 µL syringe Autosampler Trays and Carousel The Clarus 590 GC is designed to use the large capacity 108 vial tray for standard vials There is also an 82 vial Thermostatting Tray Kit available for use wi...

Страница 101: ...Number of 4 mL Wash Vials Number of 4 mL Waste Vials Number of 2 mL Priority Vials 590 580 108 Standard 4 4 1 500 82 Standard 4 4 1 Autosampler Touch Screen 1 You can access the Autosampler by selecting the Run icon from the System Status Screen See screens below 2 In the next screen touch the Autosampler button next to the Run Type heading ...

Страница 102: ...e 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 If the system is under external control e g from TotalChrom and a method has not yet been set up the Start Button is inactive In all other instances even though the GC is not Ready the Start Button will start a run When the ...

Страница 103: ...any further injections until resumed by the user When the system is paused the Stop button turns to Resume on all top level screens Go to a temp program step Displays radio buttons that allow the user to ballistically raise the oven 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 a...

Страница 104: ...ode 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 Whi...

Страница 105: ...ither Injector A or B 5 Touch Start when you are ready to begin the autosampler run Autosampler Tasks Tab The Autosampler Tasks tab includes buttons to execute tasks such as Park and Clean Touch the Park button to park the autosampler tower NOTE If 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 was...

Страница 106: ...GC Plungers are not interchangeable from syringe to syringe Configuration Button From the Tasks tab touch the Config button The Config button provides a quick link to the configuration settings Auto Resume Check the Auto Resume checkbox to allow the autosampler program to automatically resume where it left off should a power failure occur NOTE Auto Resume should not be used if you have an FID or F...

Страница 107: ...injection field use up and down arrow or keypad buttons to input the number of priority injections Touch Start 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 acco...

Страница 108: ...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 autosa...

Страница 109: ...4 Setting Up the Detectors ...

Страница 110: ...110 Clarus 590 GC User s Guide ...

Страница 111: ...s different from the gas used to calibrate the PPC module you must recalibrate the PPC module with the gas Dans un Clarus GC équipé de modules PPC les modules sont étalonnés en usine avec le gaz correspondant Cependant il existe des exceptions Le module PPC qui contrôle le L ECD est calibré avec de l azote Le TCD est calibré avec de l hélium Le PID est calibré avec de l hélium Si vous avez l inten...

Страница 112: ...ng Au moment où le Clarus GC est allumé le four l injecteur s et le s détecteur s commencent à chauffer rapidement Pour éviter toute blessure éteignez tous les appareils de chauffage et laissez leurs zones respectives refroidir avant de toucher les détecteurs les injecteurs et leurs raccords correspondants Les procédures détaillées pour éteindre ou éteindre les radiateurs sont dans le Guide du mat...

Страница 113: ... 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...

Страница 114: ... flow simply follow this procedure Turn on the air at the source and adjust the line pressure to 70 90 psig 1 Turn on the hydrogen at the source and adjust the line pressure to 60 90 psig 2 Press the Tools button and select Configuration The Configuration screen similar to the one below appears 3 Touch the detector button labeled FIDW NOTE FIDW indicates the wide range FID is installed The configu...

Страница 115: ...ons to enter a flameout detection level in mV for example 0 1 mV 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 are used If the 0 3 mV threshold level is exceeded the flame is considered lit...

Страница 116: ...operation make sure your column is positioned in the FIDW 3 74 inches 95 mm from the back of the column nut The flame may not auto ignite if your carrier gas flow is 60mL min or higher Pour assurer un fonctionnement correct de l auto inflammation FID assurez vous que votre colonne est positionnée dans le FID à 3 74 pouces 95 mm à l arrière de l écrou de la colonne La flamme peut ne pas s allumer a...

Страница 117: ...tion is attempted with the FIDW 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 30 mL min flowrates To 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 c...

Страница 118: ...r est de 60 mL min ou plus 1 Touch the FID FIDW icon from the System Status screen The FID tab page appears NOTE For proper ignition to occur the FID must be heated to at least 100 C 2 Touch the temp field and use the up and down arrow or keypad 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 temperatur...

Страница 119: ...et is hot To prevent injury never place your hand over the FID outlet La sortie FID est chaude Pour éviter toute blessure ne placez jamais votre main sur la prise FID 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 prepares for the next run it checks for a flame by running the Flameout...

Страница 120: ...o the FID outlet Adjust the hydrogen flow Adjust the air flow Ignite the flame Connect a Flowmeter to the FID Collector 1 Open the Detector Cover shown in the following figure This exposes the detector outlets The following figure shows a top view of the FID outlet 2 Insert the end of the flowmeter tubing into the FID adapter P N N6103119 supplied in the shipping kit Then insert the adapter into t...

Страница 121: ...combustion gases the manual pneumatics consist of an on off needle valve for air and on off regulator for hydrogen mounted on the pneumatics control panel NOTE Do not overtighten the inner flow adjustment screw in the on off needle valve or the on off regulator Overtightening damages the mechanical device ...

Страница 122: ...ing the outer ring of the air control valve completely clockwise 2 Turn on the hydrogen at the tank Adjust the line pressure to 30 psig 3 Start the hydrogen flowing by turning the outer ring of the hydrogen pressure regulator completely counterclockwise see the previous figure NOTE The outer knob is the on off knob and it must be turned fully on for complete flow In the case of the pressure regula...

Страница 123: ...red flow 9 Repeatedly adjust the hydrogen flow and measure the flow until you obtain a flow rate of about 30 mL min NOTE Both the carrier gas and hydrogen gas exit through the FID For satisfactory operation of the FID a flow rate of 30 mL min of hydrogen is required If a column is connected to the FID and the carrier gas is set and flowing you should add the carrier gas flow rate to the required h...

Страница 124: ...flow For example if the carrier gas flow is 30 mL min adjust the air flow until the measured total flow rate combined carrier gas and air is about 480 mL min 7 Turn off the air flow by turning the outer ring of the air control valve completely clockwise 8 Replace the air control valve protective cap remove the flowmeter and replace the FID cap 9 From the Stopwatch screen touch OK when this procedu...

Страница 125: ...nsation will appear on the object if ignition has occurred WARNING AVERTISSEMENT The FID outlet is hot To prevent injury never place your hand over the FID outlet La sortie FID est chaude Pour éviter toute blessure ne placez jamais votre main sur la prise FID 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 inval...

Страница 126: ...gnite 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 WARNING AVERTISSEMENT The FID outlet is hot To prevent injury never place your hand over the FID outlet La sortie FID est chaude Pour éviter toute blessure ne placez jamais votre main sur la prise FID 2 L...

Страница 127: ...utomatically 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...

Страница 128: ...eps WARNING AVERTISSEMENT 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 the ECD is Wipe Tested at least once every six months and a record of the results are maintained for NRC inspection Please refer to the Hardware Guide Maintenance chapter for the Wipe Test procedure Pour s...

Страница 129: ... 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 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...

Страница 130: ...s 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 WARNING AVERTISSEMENT The ECD cell may only be removed for repair from the chromatograph if a specific license has been obtained THE CELL SHOULD NEVER BE DISMANTLED La cellule ECD ne peut être retirée que pour la répar...

Страница 131: ...l Vent the ECD Outlet NOTE 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 2 Remove the two screws that secure the insulating cover to the Clarus GC 3 Remove the insulating cover and detector c...

Страница 132: ...ecalibrate the ECD flow module if you are using a make up gas other than nitrogen Le module de débit ECD pour les gaz de maquillage est étalonné avec de l azote gazeux en usine Vous devez recalibrer le module de flux ECD si vous utilisez un gaz de maquillage autre que l azote Set the Make Up Gas in the PPC Version With PPC pneumatics the make up gas is set from the Clarus GC keyboard The PPC modul...

Страница 133: ...however the noise level may increase 5 In this Configuration screen use the up and down arrow or keypad buttons to set the Make up gas flow 6 Touch OK when finished Adjust the Make Up Gas in the Manual Pneumatics Version To adjust the make up gas in the manual pneumatics version use the on off needle valve mounted on the pneumatics control panel CAUTION Do not overtighten the inner flow adjustment...

Страница 134: ...ow or clockwise to decrease the flow You should only adjust make up gas flow after a column has been installed and the carrier gas flow or pressure has been set to the value required for the analysis Make up gas need not be added when using packed columns where the carrier gas flow is 30 mL min or higher To adjust the make up gas 1 Turn the outer ring of the make up valve fully clockwise 2 From th...

Страница 135: ...ke up gas turn the needle valve using the screwdriver P N 09907273 counterclockwise to increase the flow clockwise to decrease the flow Adjust the total flow until it equals 30 mL min or higher NOTE The lower the total flow the better the sensitivity provided that peak shape is maintained 8 Replace the cap on the make up gas valve and disconnect the flowmeter ...

Страница 136: ...gnal proportional to the amount of sample 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 ...

Страница 137: ...emperature appropriate for the analysis to be run 4 If you require the heater on for your analysis just touch the heater button and it will toggle to heater on Equalize the Makeup and Reference Gas Flows The following procedures describe how to adjust the makeup and reference gas in a PPC version of the Clarus GC Follow the procedure that corresponds to your instrument ...

Страница 138: ... modules are calibrated at the factory therefore to set the flows for an analysis simply follow this procedure TCD Active Method TCD Configuration Screen 1 To set the make up and reference gases touch the button in TCD tab screen then touch Configuration from the drop down menu This will bring you to the TCD Configuration screen page see screens above 2 In the TCD Configuration screen set the make...

Страница 139: ...ten the inner flow adjustment screw in the on off needle valve or the on off regulator Overtightening damages the mechanical device The make up gas control valve consists of an outer ring used to turn the make up gas completely off or on a protective cap and an inner needle valve used to adjust the flow of make up gas Removing the cap exposes the needle valve adjustment screw To set flow use a sma...

Страница 140: ...ke up valve 7 Repeatedly adjust the make up gas turn the needle valve using the screwdriver P N 09907273 counterclockwise to increase the flow clockwise to decrease the flow Adjust the total flow until it equals 30 mL min or higher NOTE The lower the total flow the better the sensitivity provided that peak shape is maintained 8 Replace the cap on the make up gas valve and disconnect the flowmeter ...

Страница 141: ...Up to 350 C 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 Off 0 40 1 80 2 120 3 160 4 NOTE Entering a negative number reverses the detector polarity For examples of reversing the polarity see the Clarus GC Hardware Guide Maintenance Chapter section Practical Hints Balance the Bridge 1 In the Sys...

Страница 142: ...he display 5 Reset the potentiometer to produce a reading between 0 0 and 20 0 mV Using a TCD with the Autosampler or GSV When using a TCD with the 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 bring the signal back before peaks of interest elute Initiate a test r...

Страница 143: ...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 A cross section view of a PID is shown in the following figure NOTE The optimum operating temperature for a photoionization detector is 250 ºC PIDs may be operated at 350 C for short periods of time with a subsequent loss in lamp life The PID ...

Страница 144: ... on the oven and the detector heaters Adjust the make up gas Adjust the make up gas flow if using a capillary column at flows of 10 mL min Turn on the UV lamp 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 icon ...

Страница 145: ...ill toggle to heater on 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 NOTE Use make up gas only if you are using a capillary column at flows of 10 mL min The following procedures describe how to adjust the ma...

Страница 146: ...eypad buttons 4 As shown in the example above use the up and down arrow or keypad buttons to set the filter to 200 and the output to 5 When all the settings are appropriate for your analysis touch OK The TCD tab screen will be now visible and the changes you made in the configuration screen will be shown The default setting for the filter is 200 milliseconds If you want to improve the signal to no...

Страница 147: ...ired for the analysis Make up gas need not be added when using packed columns where the carrier gas flow is typically 20 mL min or higher To adjust the PID make up gas 1 Attach a flowmeter to the PID exit 2 Turn off the make up gas by turning the outer ring of the make up valve fully clockwise 3 From the System Status window touch Tools From the Tools drop down menu touch Utilities 4 In the Utilit...

Страница 148: ...ust the total flow until it is 10 mL min The lower the total flow the better the sensitivity provided peak shape is maintained 9 Replace the make up valve protective cap 10 Disconnect the flowmeter Turn on the UV lamp 1 Lift the detector cover to expose the PID Turn the lamp intensity control knob fully counterclockwise 3 Turn the UV lamp switch ON 4 From the PID Tab make sure that Auto Zero box i...

Страница 149: ...wly turn it clockwise increasing the signal until the background signal on your integrator or recorder whichever is configured suddenly decreases 4 Repeat steps 2 through 4 at different attenuations using the highest lamp intensity that corresponds to the lowest background signal NOTE If optimizing the lamp intensity cannot be done easily using the above procedure increase the lamp intensity until...

Страница 150: ... WARNING AVERTISSEMENT Turn off the hydrogen gas before disconnecting a column from the NPD When two NPDs are installed but only one NPD has a column connected to it plug the inlet of the NPD without a column with a 1 8 inch stainless steel plug P N N9300061 to prevent hydrogen from back diffusing into the oven Éteignez le gaz hydrogène avant de débrancher une colonne du NPD Lorsque deux NPD sont ...

Страница 151: ... 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 reduce bead performance and life Although these solvents may still be used they should be avoided whenever possible Setting Up a PPC NPD To set up a NPD usi...

Страница 152: ...o set the make up and reference gases touch the button in NPD tab screen then touch Configuration from the drop down menu This will bring you to the NPD Configuration screen page This will bring you to the NPD Configuration screen page ...

Страница 153: ... by a needle valve and on off regulator on the pneumatics control panel The needle valve controls the amount of air and the on off regulator controls the hydrogen flow NOTE Do not overtighten the inner flow adjustment screw in the needle valve or the on off regulator Overtightening damages the mechanical device Each pneumatic control consists of an outer knob which is used to turn the hydrogen or ...

Страница 154: ...hydrogen and air lines Disconnect the Hydrogen and Air Lines at the NPD Bulkhead 1 Open the detector cover This exposes the NPD bulkhead fittings shown in the following figure NOTE The hydrogen line is marked with a red sticker The air line is unmarked 2 Disconnect the hydrogen line by loosening the nut that connects the hydrogen line to the bulkhead fitting with a 7 16 inch wrench ...

Страница 155: ...e outer knob is the on off knob and it must be turned fully on for complete flow In the case of the pressure regulator if this knob is only partially opened the flow will be less than the setting made when the knob was fully opened 4 To expose the adjustment screw remove the protective cap from the hydrogen pressure regulator 5 Insert the hex wrench in the adjustment screw and turn it clockwise to...

Страница 156: ...Start the air flowing by turning the outer ring of the air control valve fully counterclockwise 4 Remove the protective cap from the air control valve The stopwatch screen should still be displayed 5 Measure the flow rate For best accuracy use a soap bubble flowmeter volume that gives a reading of at least 30 seconds 6 Adjust the air flow by turning the needle valve with the screwdriver Continue t...

Страница 157: ...5 mL min or less but not 0 or preferred disconnect the column and cap the oven end of the detector 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 1 Obtain a stopwatch or use the stopw...

Страница 158: ...in 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 NOTE 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 resu...

Страница 159: ...otentiometer to 850 6 After 1 minute move the potentiometer to 900 7 After 1 minute reduce the potentiometer to 850 8 After 1 minute reduce the potentiometer to 800 9 After 1 minute reduce the potentiometer to 750 10 After 1 minute reduce the potentiometer down to 700 11 For Capillary columns Wait 10 minutes go to the NPD detector screen then adjust the potentiometer so that the NPD baseline respo...

Страница 160: ...sing intervals of 0 25 mV are recommended Adjust the background setting 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 sett...

Страница 161: ... 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 sho...

Страница 162: ...lessures NE PAS ALLUMER SUR L HYDROGENE à moins qu une colonne ne soit fixée aux raccords du détecteur à l intérieur du four et que tous les raccords aient fait l objet d un test de fuite Avant de déconnecter une colonne assurez vous que l HYDROGENE A ÉTÉ DÉMONTRÉ Si deux FPD sont installés et qu un seul FPD possède une colonne qui lui est connectée assurez vous que vous branchez le raccord d entr...

Страница 163: ...C Turn on the photomultiplier tube 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 NOTE If Linear...

Страница 164: ...4 If Linearization is set to OFF set the Clarus GC integrator attenuation to x8 1 From the System Status screen touch the FPD icon The FPD tab page is now visible 2 For Linearizer the default value is Off To change the value to ON touch the button in FPD tab screen then touch Configuration from the drop down menu ...

Страница 165: ...erview 165 This will bring you to the Configuration screen page 3 Touch the FPD button to display the NPD configuration screen 4 In this screen touch the Linearizer field and touch On from the drop down menu ...

Страница 166: ...l 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 will be shown Set the FPD Temperature NOTE 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 icon 2 The FPD tab page is now visible NOTE For pr...

Страница 167: ... where the hydrogen and air gases are 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 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 60 90 psig 3 From the System Status screen touch the FPD icon The FPD tab ...

Страница 168: ...168 Clarus 590 GC User s Guide This displays the Configuration screen page 5 On this page touch the FPD button to get to the FPD Configuration screen ...

Страница 169: ...eld and use the up and down arrow or keypad buttons to get the value appropriate for your analysis 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 9 Touch OK...

Страница 170: ...urn on the photomultiplier tube touch the button in FPD tab screen then touch Configuration from the drop down menu This will bring you to the Configuration screen page 3 On this page touch the FPD icon to get to the FPD Configuration page ...

Страница 171: ...asing 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 GC Hardware Guide Maintenance chapter for this procedure NOTE The photomultiplier tube can be damaged if it is exposed to light while voltage is ON Never rem...

Страница 172: ...at the FPD outlet faces the front or left side of the instrument 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 W...

Страница 173: ...zer is turned on the software calculates the square root of the signal and sends that value to the integrator or recorder NOTE If Linearization is set to ON the Autozero function must be set checked off in the FPD tab screen NOTE 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 Sys...

Страница 174: ...ly eluting peaks 800 msec may be too slow thereby producing a smaller response to your peak of interest Before using this setting test it with your standard Set the FPD Temperature NOTE 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 icon The FPD tab page is now visible NOTE For proper igni...

Страница 175: ...the FPD outlet Adjust the Hydrogen Flow Combustion gases are controlled by an on off regulator and needle valve that are located on the pneumatics control panel The on off regulator controls the air flow and the needle valve controls the hydrogen flow NOTE Do not overtighten the inner flow adjustment screw in the needle valve or the on off regulator Overtightening damages the mechanical device ...

Страница 176: ... valve adjustment screw counterclockwise to increase the flow and clockwise to decrease the flow To adjust the hydrogen flow 1 Turn the air off at the source 2 Turn on the hydrogen at the tank Adjust the hydrogen line pressure to 30 psig 3 Start the hydrogen flowing by turning the outer ring of the hydrogen control valve fully counterclockwise 4 Remove the cap from the hydrogen control valve This ...

Страница 177: ... exit through the FPD For satisfactory operation of the FPD a flow rate of 75 mL min of hydrogen is required If a column is attached to the FPD and the carrier gas is flowing the carrier gas flow rate should be added to the required hydrogen flow For example if the carrier gas flow is 30 mL min adjust the hydrogen flow until the measured total flow rate combined carrier gas and hydrogen is 105 mL ...

Страница 178: ...ob It must be turned fully on for complete flow In the case of the pressure regulator if this knob is only partially opened the flow will be less than the setting made when the knob was fully opened 4 To expose the adjustment screw remove the protective cap from the pressure regulator 5 Insert the hex wrench in the adjustment screw and turn it clockwise to increase the flow NOTE For safety reasons...

Страница 179: ...atisfactory operation of the FPD a flow rate of 90 mL min of air is required If a column is attached to the FPD and the carrier gas is flowing the carrier gas flow rate should be added to the required air flow For example if the carrier gas flow is 30 mL min adjust the air flow until the measured total flow rate combined carrier gas and air is about 120 mL min 11 Remove the flowmeter 12 Touch OK o...

Страница 180: ...ltiplier 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 590 GC Hardware Guide Maintenan...

Страница 181: ...flow In the case of the pressure regulator if this knob is only partially opened the flow will be less than the setting made when the knob was fully opened 8 Position the hole in the side of the metal part of the ignitor against the FPD outlet on the cap Hold the ignitor firmly against the FPD outlet to make the proper contact Proper contact is made when the end of the ignitor glows and ignites th...

Страница 182: ...uide WARNING ADVERTISSEMENT The FPD outlet is HOT To prevent injury do not place your hand over the FPD outlet on the cap La sortie FPD est HOT Pour éviter les blessures ne placez pas votre main sur la prise FPD sur le capuchon ...

Страница 183: ... Status screen touch the ECD icon 2 In the ECD tab locate the Make Up field To change the setting touch Tools and touch Configuration from the drop down menu 3 In the ECD tab page touch the temp field and use the up and down arrow or keypad buttons to add an ECD temperature appropriate for the analysis to be run 4 To turn the heater On or Off just touch the Heater button The message on the button ...

Страница 184: ...wn menu to select a range for the detector PID and NPD range options are 1 or 20 where 1 is the most sensitive setting and 20 is 20 times less sensitive The value that you enter will always be used unless you change it in the Event tab page For certain analyses such as those for trace or concentrated components you may wish to change the Range during a GC run The following example illustrates this...

Страница 185: ...eed to change the Event touch the down arrow in the Event field to view the other ranges Select the one you need by touching it 5 Enter a value for the AutoZero A by touching the Value field Then using the up and down arrow buttons enter On or Off 6 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 is ...

Страница 186: ... est pas utilisé la température et le courant doivent être éteints 1 From the System Status screen touch the TCD icon 2 In the TCD tab page touch the Current field and use drop down menu to change the value TCD range options are 0 Off 1 2 3 4 maximum sensitivity and 1 2 3 or 4 A negative value reverses the polarity The TCD range values corresponding to bridge current are shown below ...

Страница 187: ... 187 Table 4 3 Correlation Between Bridge Current and Range Bridge Current mA Range Entry Off 0 40 1 80 2 120 3 160 4 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 ...

Страница 188: ...les for using polarity changes are given in Clarus GC Hardware 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 icon 2 In the TCD tab page touch the Events tab 3 In the Events tab touch the Add button 4 Using the up and down arrow or keypad buttons enter a time of three minutes...

Страница 189: ...d 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 the run When the run is completed the system switches back to the initial value in this case 2 ...

Страница 190: ...rator in this example the integrator is output A 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 icon for the FID Detector 2 The FID tab page will appear Touch the Events tab 3 In the Events screen touch the Add button The Timed Events screen will appear In the drop down ...

Страница 191: ...B 10 Touch the time field and use the plus minus buttons to input a time that TCD s output will go to the recorder 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 tab page 13 Once in the TCD tab page touch the System icon to return to the System Status screen NOTE Detector routing remains in ef...

Страница 192: ...on 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 NPD detector is used as an example 1 From the System Status screen touch the NPD button this will bring you to the NPD tab screen page 2 To change the attenuation touch the Atten field Use the drop down m...

Страница 193: ...e Attenuation setting is used to scale the peak sizes so that both big and small peaks can be seen and processed using the same method A few runs of typical samples may be needed to establish the Attenuation setting As a general rule set the Attenuation to a value that makes the height of the largest peak between 40 and 80 of the level at which it will saturate the signal normally 1000mV A saturat...

Страница 194: ...ttenuation be carried out under actual operating conditions prior to running your first sample 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 2 Gradually decrease the attenuation for example to 16 or until the noise level increases A table...

Страница 195: ... Detector Signals with Your Integrator 195 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 ...

Страница 196: ... 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 In the System Status screen touch the ECD icon 2 In the ECD Tab you will see the AutoZero field 3 To turn on the AutoZero touch the field and a check mark will appear NOTE When Autozero is Off the output signal i...

Страница 197: ...5 Using the Method Editor ...

Страница 198: ...198 Clarus 590 GC User s Guide ...

Страница 199: ...ctive Method screens The differences are noted in this section You can access and edit the first five methods The fifth method is reserved for TotalChrom and may be overwritten If you attempt to overwrite the method it will retain the name External to remind you that this is a possibility You cannot access the Default method This method is used by the system to populate a method with default value...

Страница 200: ...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 The run and signal icons on the top navigation bar are deactivated No configuration information appears No ignite button on the FID screen No status bar or current information The Start and Tools button in the bottom bar...

Страница 201: ... that follows shows the screen in Method Edit mode Active Method Screen Method Edit Mode Oven Settings Touching the oven icon displays the oven screen in method edit mode Touch the File button to display the pop up File menu that provides options to create modify and save methods The Method Name field is not active until you select an option from the File menu ...

Страница 202: ...s 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 1 Touching New Method displays the following dialog box 2 If you select Yes the Save As dialog box appears 3 You can as...

Страница 203: ...ching the Open Method option prompts the following warning box indicating that the current method is not saved 2 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 3 Touch the method name and OK to populate the method edit screens with the values from the selected method 4 If you choose Cancel or touch the OK button witho...

Страница 204: ...thod from the list clicking OK prompts the dialog box to confirm that the existing method will be overwritten 3 Clicking Yes overwrites the stored method with the new method with the same name 4 To assign a new method name touch the name field to invoke the alpha numeric keypad Although a new method name field displays the name untitled the field to enter the new name is blank The Method Name fiel...

Страница 205: ... 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 Pressing Continue returns control to the previous screen You can select a name or cancel out of the process 6 If five methods are already stored entering a new name will prompt the following dialog box 7 If you press Yes the method list appears 8 When you se...

Страница 206: ... method 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 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 clo...

Страница 207: ...6 Using the Tools Menu ...

Страница 208: ...208 Clarus 590 GC User s Guide ...

Страница 209: ...us Screen 2 Touch the button shown above When you release this button a list of options appears You are now able to select any of the options displayed in the menu Method Editor To access Method Editor touch Tools menu and press the first option Method Editor For detailed information on the Method Editor see Chapter 4 Using the Method Editor in this guide Event Log To access Event Log from the Sys...

Страница 210: ...specifies the condition that prompts the reminder When the criteria are met a dialog box displays the message 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 ...

Страница 211: ...ad buttons 3 Enter a message by touching the Message field This displays the alphanumeric keypad for you to enter a message Type the message For example Change Septum 4 Click OK to save the message If a maintenance task has already been assigned to the selected number a dialog box will ask if you want to overwrite it ...

Страница 212: ... to the task a dialog box displays the reminder 6 Touch OK to close the reminder Configuration To access Configuration from the System Status screen touch Tools menu then touch Configuration The Configuration screen appears This section describes how to configure and then shows the various GC configuration screens ...

Страница 213: ...fic 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 routed to both output channels Both detectors should not be deconfigured at the same time Deconfiguring the detectors also deconfigures the detector s PPC control You must reconfi...

Страница 214: ...r 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 pr...

Страница 215: ...he 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 is deactivated as shown below When using a mass spectrometer select the Vacuum Compensation checkbox ...

Страница 216: ... 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 the capillary control check box is not selected...

Страница 217: ...een 2 Make your settings then touch the OK button 3 Then touch the Close button to exit configuration POC Programmable On Column Injector This example shows that POCO a programmable on column injector is selected as the Type on the Configuration screen Make your settings then touch the OK button Then touch the Close button to exit configuration ...

Страница 218: ... as the Type on the Configuration screen Make your settings then touch the OK button Then touch the Close button to exit configuration GSV Gas Valve This example shows that GSV a gas sampling valve is selected as the Type on the Configuration screen Make your settings then touch the OK button Then touch the Close button to exit configuration ...

Страница 219: ... active and the GC Tune drop down field is inactive Single Point is the default setting The default value is 0 The Offset range is 10 to 10 C If the GC is not GC enabled then the GC Tune radio button is deactivated 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 a...

Страница 220: ...een assigned to the FID If no flow module has been assigned a dialog box appears 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 2 When the PPC gas source is defined touch the OK button to validate the settings and the FID detector configuration screen appears ...

Страница 221: ...h the OK button to close this screen then touch the pneumatics button 4 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 ...

Страница 222: ...following series of screens show the configuration screen for each detector FID TCD 1 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 TCD If no flow module has been assigned a dialog box appears ...

Страница 223: ...g box closes If Yes is selected the PPC connect screen appears and the user configures an available flow module When the flow module is configured you touch the OK button to validate the settings and the TCD detector configuration screen appears ...

Страница 224: ...224 Clarus 590 GC User s Guide ECD PID NPD FPD ...

Страница 225: ...Detectors 225 Output Configured ...

Страница 226: ... Permissible entries are 0 to 15 Post inject is 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 millesectonds Not available when a 50 0 syringe is installed Normal injecti...

Страница 227: ...ey 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 Touch the New field The alphanumeric keypad appears to enter the password Passwords are limited to eight characters and are case sensitive ...

Страница 228: ...ypad and continue setup Language drop down menu Touch the language option The list box closes and the selected language is immediately displayed throughout the application Brightness field The field is selected Use the plus and minus keys to increment values up or down Settings takes effect immediately Date Time Set ...

Страница 229: ...rrow or keypad buttons to enter the values 4 Select whether you want these start up settings to Repeat Once or Always Sleep 1 Touch the Sleep button to display the Sleep screen 2 Select the Method field then using the arrow button select your desired method This now enables the displayed fields for edit Value range is 6 999 3 Select the After field then set the time after which sleep will by use u...

Страница 230: ...y is blank this means that the parameter is currently unconnected to the GC The logic descriptions cover special case handling performed within the user interface to hide or disable certain options change units or limit the available ranges for parameters The extra status bar at the bottom of each bitmap and status text above the bottom row of buttons should be ignored To access the PPC Settings p...

Страница 231: ...Injector and Detector Socket Descriptions Injector 1 1 J10 Injector 2 2 J11 Injectors Carriers Detector 1 Air or TCD Ref 3 J12 Detector 1 HYD or Make Up 4 J13 Detector 1 Detector 2 Air or TCD Ref 5 J14 Detector 2 HYD or Make Up 6 J15 Detector 2 7 J16 8 J17 Aux 9 J18 10 J19 11 J20 12 J21 Split Vent for CAP PSS injectors or Pressure Readout for PKD POC injectors A flow or pressure module can be conn...

Страница 232: ...that you need to reconfigure reconnect For example if a capillary injector is 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 ...

Страница 233: ...how the logical PPC devices The 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 buttons show the packed column injector and the unconfigured injector icon respectively while the Detector A and B buttons show FID and TCD icons respectively 3 Pressing ...

Страница 234: ...owing dialog box Since the PPC has yet to be configured the primary module is undefined and the secondary module entry is disabled The primary entry is expected to be the module function The following screen shows the full potential range available for the primary module function ...

Страница 235: ...rier 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 The secondary module is now enabled This will only be the case if the primary module is set to Carrier flow or Split control The following screen shows that the second module can ...

Страница 236: ...er an option 6 Select Split control The secondary module for Carrier B is now enabled but inspection shows that there are no suitable modules available for assignment 7 Press OK to close the dialog box and implement the changes The Connect PPC Device screen appears ...

Страница 237: ...D 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 to 6 as possible options Once Position 3 is assigned to the primary module however this location is no longer available for use with the secondary module 1...

Страница 238: ...ectors a more complete list is offered as shown in the screen on the right 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 ...

Страница 239: ...as 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 Zeroing the PPC gas modules Gas turned off Setting the reference temperature and pressure Calibrating the PPC carrie...

Страница 240: ...as Make sure that the gas supply to the Clarus GC is turned off at this time 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 functi...

Страница 241: ...nieur de service local PerkinElmer CAUTION ATTENTION 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 controller has two pressure transducers per module whereas the other modules only have one In the carrier flow module pressure transducer A reads the differential pressur...

Страница 242: ...affichage 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 C and 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...

Страница 243: ... 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 Ki...

Страница 244: ...unless you have replaced the restrictor with a different one The number is stamped into the restrictor CAUTION ATTENTION 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 8 inch cap before proceeding This will ensure that all the gas flows up through the detector and not into the...

Страница 245: ...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 is possible for a particular restrictor frit then the numbers will not agree 4 Touch OK to complete Calibrating the Detector Gas Modules CAUTION ATTENTION Before you begin to calibrate you must first Zero the Gas Avant de commencer à étalonner vous devez d a...

Страница 246: ...4 Select Detector tab Touch the Calibrate button Select OK 5 In the Calibrate screen use drop down menu to select the 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 6 Enter Zero 0 for the detector gas setpoints If you are using a FID...

Страница 247: ...e turned off and their respective zones allowed to cool before touching the injector septum caps or any of the fittings inside the oven Before proceeding determine whether the packed column is in position 1 or 2 using the procedure previously described 1 Open the oven door 2 Turn on the Clarus GC if it is not already on and wait for the System Status Screen 3 Notice that as the oven cools down the...

Страница 248: ...h Utilities 9 In the Utilities screen touch Stopwatch icon Ideally the flow should be zero but some flow controllers may produce a small flow when turned off 10 Touch Time field to and make sure the time is set to 0 00 Use the plus minus keys to make any adjustments Touch OK when completed and close the screen ...

Страница 249: ...sing Manual Pneumatics 249 11 For the channels that you are using select Flow from the Carrier Device drop down menu From the Gas drop down menu select the gas you are using 12 Touch the Calibrate button The following screen appears ...

Страница 250: ...urn the flow control knob counter clockwise to start the carrier gas flowing 16 Measure and adjust the flow to one of the following If a 0 to 100 mL min flow element is installed 100 10 mL min If a 0 to 20 mL min flow element is installed 20 2 mL min 17 Repeat steps 11 through 18 18 Touch the dialog box for High Flow and use the plus and minus buttons to enter the flow you just measured ...

Страница 251: ... 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 Place the Thermometer Probe in the Oven CAUTION ATTENTION The thermometer pro...

Страница 252: ... of the oven cavity The figure below shows the holes on the left side of the oven interior 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 Equilibrate the Oven Temperature 1 Close the oven door then turn the GC and thermometer on From the System Status screen press the oven icon ...

Страница 253: ...ct Tools and press on Configuration in the drop down menu 3 In the oven configuration screen press on the Oven icon 4 From the window shown below set the oven temperature of 100 C or use another temperature if desired by using the up and down arrow or keypad buttons ...

Страница 254: ... 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 1 After the temperature has stabilized subtract the thermometer reading from the actual oven temperature shown on the previous screen 2 Usi...

Страница 255: ...Utilities screen of the Tools Menu go to the System Status screen and select Utilities from the tools menu 2 Touch the following icon on the Utilities screen to access the Column Flow Calculator the Column Length Calculator or the Stopwatch ...

Страница 256: ...and outlet pressure 3 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 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 ke...

Страница 257: ...velocities as shown in the Table Screen Name Gas ref η Pa s x Suggested Velocity cm s He Helium 0 000018662 0 646 20 to 40 H2 Hydrogen 0 000008399 0 725 30 to 55 N2 Nitrogen 0 000016736 0 680 8 to 16 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 accordi...

Страница 258: ...led 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 ...

Страница 259: ...e the injecor and so they would be cancelled out in this equation Close Press the Close button on to bring you back to the Column Carrier Gas Calculator screen Column Length Calculator The capillary column gas flow rate calculator allows you to automatically calculate the correct gas flow rate Touch the Column Length Calc icon The following screen appears Stopwatch The Stopwatch computes the flow ...

Страница 260: ... The following screen appears 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 ...

Страница 261: ...ect Yes the instrument will be reset and data will be lost If you select No the screen will close Logout 1 To access Logout from the System Status screen touch Tools menu and press the Logout 2 Touching Logout displays the splash screen About 1 To access About from the System Status screen touch Tools menu and press the About 2 Touch About to display version information ...

Страница 262: ...262 Clarus 590 GC User s Guide ...

Страница 263: ...7 Setting up a Typical Analysis ...

Страница 264: ...264 Clarus 590 GC User s Guide ...

Страница 265: ... 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 is 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 a...

Страница 266: ...am the oven temperatures touch the temperature field and it will go black 3 the up and down arrow or keypad buttons to get 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 ºC and it is held at this temperature for 1 minute then going up 10 degrees ...

Страница 267: ...e 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 buttons to enter the proper initial temperature for your application 2 Next set the carrier gas by touching the Program button to display the Carrier Pressure Program screen ...

Страница 268: ...atus screen Once you touch the PSSI icon the following screen appears 2 Touch the Temperature Program button to the right of the 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 the analysis ...

Страница 269: ...se the up and down arrow or keypad buttons to set the carrier gas pressure to the required pressure for your application 6 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 ºC and it is held at this temperature for 60 minutes then going up 2 degrees 7 Touch Close when you have entered all the parameters ...

Страница 270: ...d temperature for your application Repeat the same procedure for the Atten attenuation As shown in the example below this analysis has the heater off 3 If you require the heater on for your analysis just touch the heater button and it will toggle to heater on 4 To have the detector autozero the baseline to a fixed amount touch the AutoZero field for the check mark to appear 5 The Gas flows Offset ...

Страница 271: ... filter flameout gas flows and output fields as your application requires Once you have modified the Configuration screen touch OK and the new values will now be visible on the FID tab screen 8 If timed 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 even...

Страница 272: ...to input the amount of time for this event in the time field 11 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 13 Once all the fields have been set as required by your application touch the ignite button on the FID tab screen to ignite the ...

Страница 273: ...d temperature for your application 3 Repeat the same procedure for the Filter attenuation and Current As shown in the example below this analysis has the heater off 4 If you require the heater on for your analysis just touch the Heater button and it will toggle to heater on 5 To have the detector autozero the baseline to a fixed amount touch the AutoZero field for the check off to appear in this e...

Страница 274: ...set and filter are shown above as reference fields and they cannot be changed in this screen 7 If the gas flows output offset and filter have to be changed touch the Tools button and touch Configuration from the drop down menu The Configuration screen appears ...

Страница 275: ...ion requires 9 Once you have modified the Configuration screen touch OK and the new values will now be visible on the FID tab screen 10 If timed 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 ...

Страница 276: ...ttons to input the amount of time for this event in the time field 13 In the Value field use the drop down menu to insert the correct value 14 When completed touch OK to return to the Event tab Repeat this procedure until you have added all the timed events for your procedure 15 Once all the fields have been set as required by your application for the TCD touch the Autosampler icon on the screen ...

Страница 277: ...utosampler run touch the Stop button 2 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 3 Touch the Run button on the Configuration screen The following screen displays 4 In the AutoSampler Configuration screen check off the Enable Autosampler field by touching it If your application requir...

Страница 278: ...ch OK on the AutoSampler Configuration screen the main autosampler screen will appear again 5 Touch Start to begin the run 6 Touch the Signal icon to get to the Signal screen 7 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 ...

Страница 279: ...Index ...

Страница 280: ...280 Clarus 590 GC User s Guide ...

Страница 281: ...mn Flow Calculator 256 Column Length Calculator 259 Combustion control valves FPD 175 needle valves FID 122 needle valves FPD 176 Configuration 212 Configuring injectors 213 Connect PPC module socket descriptions 231 Control valves combustion FPD 175 Conventions Notes cautions and warnings 13 text 13 Coolant cut in temperature setting 65 Ctrl abbreviation 16 D Deconfiguring injectors 213 Detector ...

Страница 282: ...tting up 65 K kPa abbreviation 16 L Logout 261 M Maintenance 210 Make up gas control valve 134 139 143 needle valve 134 139 143 PID needle valve 146 Method Editor 209 file menu 202 mode 200 overwriting the active method 202 Multiprogram mode 104 Multi ramp temperature program setting up 67 N Navigation Bar 32 NPD adjusting the air flow 156 adjusting the hydrogen flow 155 bead activation reactivati...

Страница 283: ... with manual pneumatics 120 FID with PPC 113 FPD with manual pneumatics 173 FPD with PPC 163 NPD with manual pneumatics 154 PID 144 TCD 136 Split mode flow knob 91 flow needle valve 91 setting up 93 split vent flow adjusting 90 measuring 90 Split vent attaching a flowmeter 91 locating 91 Split vent flow adjusting 90 measuring 90 Splitless mode setting up 93 stopwatch 259 Syringe cleaning 106 Syste...

Страница 284: ...play button 29 Typical Analysis autosampler 277 detectors 270 U Utilities 255 column flow calculator 256 column length calculator 259 logout 261 release 260 reset 261 stopwatch 259 UV lamp PID optimizing intensity 149 turning on 148 V Valves combustion FID 122 Z Zeroing PPC module 239 ...

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