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H User`s Manual - Agilent Technologies

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1. Figure 105 Validate instrument ID window Your GC appears to be OK but the configuration record is missing from your system Click Yes to re create the configuration record No if you are unsure about whether or not the GC is properly configured Compatibility and computer system requirements GC Verification requires that your computer meet the following specification e 80386 or better e 6 At least 2 Mb RAM e At least 2Mb free Disk Space before installation e Atleast 1Kb free disk space for new configuration records e Windows Version 3 1 or greater 158 10 Common Questions Common Questions I have a printer connected to my computer but I cannot get it to work with the EZChrom 200 400 Data System l Make sure the printer is configured on and connected to LPT1 Check Windows Control Panel Printers for setup Make sure the correct printer driver has been installed during Windows installation I can t figure out how to delete data and or method files 1 To delete Method files select the Method menu and the Open command A list of method files will appear on the screen Click the left mouse button on the file or files to be deleted They will be highlighted as evidenced by the file name being blackened Press the Delete key to remove the files To delete Data files select the Data menu and the Open command A list of data files will appear on the screen Click the left mouse butt
2. 117 Quick Reference Graphical manipulation of chromatograms Split screen This command either removes or restores the upper display 1 Select Display 2 Check Split Screen This removes the upper display 3 To regain the upper display select Split Screen again Baseline This command either removes or restores the calculated integration baselines and hashmarks 1 Select Display 2 Select Baseline No baseline will be displayed 3 To regain the baselines and hashmarks select Baseline again Cursor This command enables or disables the vertical cursors as well as the time and amplitude windows in the lower display 1 Select Display 2 Check Cursor A mobile vertical cursor will appear in the lower portion of the window 3 To disable the vertical cursor and regain the arrow cursor press the number 3 key or click the right mouse button Remember all these mouse functions can be performed with the keyboard by using the arrow keys for direction and the numeric 1 and 3 keys as the left and right mouse buttons respectively The Cursor On command must be selected will show a check mark next to the Cursor command to operate the cursor with the keyboard 118 Quick Reference Graphical manipulation of chromatograms Defining a zoom box A zoom box may be defined in the upper or lower portion of the channel A or B window The zoomed image will always appear in the lower portion of the window and th
3. For a Molecular Sieve column enter Nitrogen in the PKNO 2 name box Leave the RT Time and RT Window at default levels for the moment They will be set graphically after the air sample is analyzed 37 Sample Session Collecting data 16 Enter the symbol in the CU boxes 17 Enter values in the Level 1 Cal Amount boxes for the various compounds Air on an OV column is 100 On a HayeSep or PoraPLOT however it will be 99 967 as COs is separated from Os and Ns on this type column and makes up approximately 0 033 of the atmosphere On a Molecular Sieve the amounts of O and N will be about 21 and 78 respectively Enter values as whole numbers since the CU has already been set to percent For example 21 should be entered as 21 not 0 21 18 Leave the BP RRF and Peak boxes at default values and close the Peak Table by pressing lt Enter gt or clicking on Ok This completes the basics of building a peak table At this stage many of the commands found under the Method menu can be ignored Because certain default values have been specified during EZChrom 200 400 installation these features will function properly under normal conditions without a new user having to worry about them The one exception to this rule is the setting of optimized Timed Events The Timed Events tables contain all the parameters which control peak detection and integration of the chromatograms collected on channels A and B While it is poss
4. Parameter Remarks Name Parameter Remarks Name Parameter Remarks Name Parameter Remarks Name Parameter Remarks Name Parameter Remarks Dynamic Data Exchange DDE EZChrom DDE server Sample Sample Name Get new data from the GC using the parameter as the run id Sets the number of runs to one Ifthe parameter is not the empty string then the data is saved in the file specified by the parameter Print DIF PRN Ext and User Program are not supported with this command Calib Level Setup a calibration for the level specified by the parameter The parameter must be between 1 and 8 inclusive Note this command does not do any analysis with the GC Analyze Data file name Opens the data file specified by the parameter and analyzes it If the parameter is the empty string then the current data file is analyzed GetMethName None Get the fully qualified path to the current EZChrom 200 400 method file GetDataName None Get the fully qualified path to the current EZChrom 200 400 data file GetCycleTime None Returns the maximum of the run times for all of the channels plus the sample pump run time 171 Dynamic Data Exchange DDE EZChrom DDE server Name Parameter Remarks Name Parameter Remarks Name Parameter Remarks Name Parameter Remarks GetCalLevels None Returns the number of calibration levels GetC
5. Explanation Since the stored column head pressure zero values have been lost it is necessary to re zero the column head pressure Action Please disconnect the Helium Carrier gas supply from the back of the MTI GC and click the OK button Staus Reties Head pressure zeroed BE Figure 83 Resetting CHP offset window Click OK to continue Usually this will fix any problems and you will see the GC Verification Successful window as shown in Figure 84 MTI GC Yerification Successful Explaination The GC is functioning properly There are no outstanding error conditions and the configuration has been verified Figure 84 GC verification successful window 145 The GC Verification Tool Typical sessions What happens if your GC has problems that cannot be fixed If a problem arises that GC Verification can not solve you will see a window as shown in Figure 85 Call Technical Support Explaination our HTI GC has unresolved problems that will interfere with proper operation Please call MTI Technical Support at 510 490 0900 to get the problem resolved Subject CHECK can t clear the GC errors The error code is 1024 Figure 85 Call technical support window If you get a window as shown in Figure 85 the problem is probably not one that you can fix Call Agilent Technical Support and tell them what message is displayed in the Subject box so that t
6. Status Found MTI GC connected to COM1 Figure 75 Searching for GC window The first indication that there is a problem is that the GC name is indicated as which implies that it is empty as shown in Figure 75 Click OK and GC Verification confirms that there are problems as shown in Figure 76 Explanation i The GC has outstanding error conditions Do you want to fix them Since you want a functioning GC click Yes The next window Figure 77 advises you that the GC has forgotten its name i e serial number 140 The GC Verification Tool Typical sessions The MTI GC has forgotten its name Please enter the serial number of the GC in the box below The serial number is located on a sticker on the back of the unit Figure 77 Instrument ID window Type in the serial number which is found on a sticker on the rear panel of the GC and click OK If you have typed in the serial number correctly GC Verification will restore its configuration as shown in Figure 78 Status Restoring MTI GC Configuration Figure 78 Status window After the configuration is restored you will probably have to cycle the power to the GC GC Verification Tool automatically detects when this is the case and walks you through this process First you will have to turn the GC OFF as requested in Figure 79 141 The GC Verification Tool Typical sessions Cycle GC Power Explanation It
7. Be careful to zoom Closely on the base of a peak to determine if it has been properly integrated Ifthe peak is properly integrated the upward pointing hashmark will appear at the beginning of the peak s upward slope and the downward pointing hashmark will appear where the peak returns completely to the baseline See Figure 26 40 Sample Session Optimizing timed events If the answer to either of the questions was no then the Timed Events tables must be optimized in order for an accurate analysis to be made It may be that the default timed event parameters were sufficient to find and integrate the peaks in such a simple application In general though this will not be the case Therefore please proceed to the next chapter which describes optimizing timed event parameters graphically Optimizing timed events A Timed Event is a resetting of any of 10 calculation variables see the Events menu that are used to calculate the area under a peak Any or all of these may be adjusted at various time points along the chromatogram The purpose for setting Timed Events is to attain the best possible peak area integration In order for EZChrom 200 400 to perform an accurate analysis it is essential that the proper parameters and values are entered into the Timed Events tables Tables are provided for both channels because different columns will require different parameters to properly identify and integrate individual peaks The most accu
8. Explanation There is no record of this GC on this workstation and we can t verify the configuration without that information Figure 98 Invalid or unknown GC ID window If the serial number you enter does not match any numbers on file GC Verification will display this window asking you to double check the serial number Click Yes if you are sure it is the right one or No if you want to re enter the number 154 The GC Verification Tool Explanation of GC Verification windows GC verification MTI GC Verification Explanation e will check out your MTI GC to verify that it is OK and will perform properly If there is a problem we will guide you through the necessary procedures to restore the GC to proper operating condition Request If you have not done so please connect your MTI GC to one of the computer s serial ports T Aee GC ome Figure 99 GC verification window Figure 99 shows the first window that GC Verification displays Click Yes if your GC is connected No if it is not Quit to terminate GC Verification or About to find out which version of GC Verification Tool you are using GC verification successful MTI GC Verification Successful Explaination The GC is functioning properly There are no outstanding error conditions and the configuration has been verified Figure 100 GC verification successful window Figure 100 shows the window that wi
9. sec 0i gen 21 000 35 750 21 000 21 000 21 000 0 000 Nitrogen 79 000 42 390 79 000 79 000 79 000 0 000 Method SERIALNO MET File ch4 001 1 x Method Instrument Data Analyze Math Calib Start Help Figure 18 Crosshair cursor Graphics manipulation without a mouse While more time consuming than using a mouse all the manipulations described in the previous chapter can be made using the keyboard In this case the numeric key 1 acts as the left mouse button and the numeric key 3 acts as the right mouse button The arrow Keys on the number pad are used for moving the various cursors Each arrow allows movement in a different direction Be sure the Numbers Lock is not engaged if you use the arrow keys Text and numeric editing Occasionally it will be necessary to manually add delete or replace text and or numbers during an EZChrom 200 400 session For example you may want to add a compound to the peak identification table The general procedure to manually edit text or numbers is the same and is as follows 1 First select the Method menu and choose the Open command A series of existing Methods will appear Choose the default method Serialno met 26 Program Manager Getting Started Text and numeric editing Call up the Peak Table See Figure 19 by selecting the Method menu and then the Peak Table command RT Level 1 Pkno Peak Name Time Window CU BP CalAmount RAF i Butane 5 83
10. 1 LI Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 8 Drawing a zoom box 2 Pressand hold the left mouse button and at the same time drag the cursor to the right and down just below the baseline This should draw a rectangular box around a portion of the chromatogram 3 Release the mouse button EZChrom 200 400 will now draw the area inside the zoom box so that it fills the lower screen See Figure 9 17 Getting Started Graphic manipulation with a mouse Chan A 100 sec Attn 2048 Chan B 100 sec Attn 2048 f Reports Events Display Print Help Reports Events Display Print Help Method btu met File btu 1 Method Instrument Data Analyze Math Calib Start Help Figure 9 Zoom box display 4 Move the cursor to the top bar of the channel A window where the channel identification run time and attenuation are listed Chan A 100 sec Attn 2048 f Chan B 100 sec Attn 2048 f Reports Events Display Print Help Reports Events Display Print Help E Method btu met File btu 1 Method Instrument Data Analyze Math Calib Start Help Progam Figure 10 Moving channel A window 18 Getting Started Graphic manipulation with a mouse 5 Click and hold the left mouse button while dragging the mouse to the right This should move all of the channel A window to the right partially covering the channel B window See below When abou
11. 11 Hardware setup sonne ie E ogee T E ONTA EEEN 14 Installation troubleshooting sseesssessssssssssssssssesssessseessessseresssessseesseess 14 Chapter 3 Getting Started Selecting commands in EZChrom 200 400 ssesssssssssssssssesssesssssssssesss 16 Graphic manipulation with a mouse ssssssssesssessssssssessssesssessseessesse 16 Graphics manipulation without a mouse ee ceeeceesssceeeeeeeaeeeeees 26 Text and numeric editing iiss cod sheds orxehaa tassteuneoussatodane ta adedtaatidanleaeeadetiaak 26 Chapter 4 Sample Session Building a Method Joine aE A E EA aS 30 Collecting data sssenesessesessseesessseseesseessesersseesseserssresseserssresseseesseessesee 38 Optimizing timed events ssssessesssessesseserssressessrssressessrssressessrssressesee 41 Setting retention times graphically sesessssessesssessesssssssssessessesssesseese 46 Calibrating the Method a gqsasescscasescecivessacesetensecqeoteca Qpeasacacerestessioescayetes 48 Chapter 5 Technical Reference Data Sapling esanian tanana a aa 52 Peak detecUOn oa a E A note eich eins 52 Baseline correcti ri u ccececceecesccccccssssccccsssccecssscccssecceeescsceesesesceeeeesces 53 Peak 1G e ntiiGation 2ic2iccecedi vs sedan ds sh eden cdesaek a tetanic seeks 54 Peak q a titatioii spricar e otoda a a ia EE a AEAEE 54 Chapter 6 Menu Reference EZChrom 200 400 menus and commands sssssossssssesensssssssseseresssssseee 58 Channel A B commands ii C
12. A practical minimum value is 20 milliseconds In most cases a value of 0 to 5 milliseconds will result in no injection Each channel can have a different inject time Long injection times in conjunction with high detector sensitivity allow detection in the low ppm range parts per million Detector filament This toggles power to the GC detector which must be on for the GC to collect data A minimum column head pressure of 5 psiis required for the detectors to function If carrier gas pressure falls below 5 psi power to the detectors is turned off automatically Allow a minimum of 5 minutes equilibration time between powering on detector and the first analysis Detector autozero This compensates for detector dc voltage offset when pure carrier gas is passed over both sample and reference filaments Detector Autozero should always be left on Detector sensitivity This controls the detector output gain The low setting amplifies the detector output by a factor of 5 The medium and high settings each provide an additional factor of 10 Set these at the highest value which does not give flat topped peaks when the display is fully unzoomed 33 Sample Session Building a method 10 11 Increase the temperature settings by 10 degrees for channels A and B To do this click on channel A in the instrument setup window shown in Figure 22 Instrument settings for channel A should appear on the screen Click on the Column T
13. ESTD C NORM O BTU o Ccenca Figure 52 Print options window Caution Chromatograms generate many data points that occupy a lot of memory on your storage media If you are printing multiple chromatograms simultaneously you may overload the printer memory and lock up your system 1 Select Method 2 Select Print Options 3 Check any of the reports you wish to print at the completion of the analysis for both channels 4 Select OK 110 Quick Reference Print options Remember to check the Print box in the Start window prior to beginning a run The available options are Chromatogram full scale and or zoomed Hard copies of the chromatograms can be generated for channels A or B If the Zoomed option is selected the zoomed chromatogram shown in the lower display will be printed Reports area percent normalized percent and or external standard Any or all of the three available reports for channels A and B can be printed between autoruns Run ID sample Number of Runs 1 999 inf 5 Time Between Injections secs 350 Wait For External Start P Save C Print DIF Save LJ PRN Save LJ Extended User Program Cancel Recall Figure 53 Run window 111 Quick Reference Running the GC Running the GC Running the GC and obtaining accurate results is a simple task once a good Method has been develop
14. GC Verification Tool MTI GC Yerification Explanation e will check out your MTI GC to verify that it is OK and will perform properly If there is a problem we will guide you through the necessary procedures to restore the GC to proper operating condition If you have not done so please connect your WTI GC to one of the computer s serial ports Figure 66 Agilent verification introduction window Is the GC connected In general GC Verification windows will have three text items Explanation A short explanation of the purpose or use of a particular window Request If you are expected to do anything in particular the Request item tells you what the program wants you to do Question If GC Verification needs any information from you a Question item will pose a question which you answer by clicking a button in the window This window asks you to verify that a GC is connected to your computer Click Yes when you have connected your GC to the serial port of your computer and are ready to proceed If you click Quit GC Verification will terminate 134 The GC Verification Tool Starting GC Verification Tool Ifyou click No GC Verification Tool will tell you that it cannot proceed without a GC as shown in Figure 67 MTI GC Verification Sorry we can t do anything unless a GC is connected Figure 67 GC verification window If you click About GC Verification will tell you ab
15. Statistics or type C Comments After the next analysis the values for MIN MAX MEAN and RSD will be reset in both the External Standard and Normalization reports 60 Menu Reference EZChrom 200 400 menus and commands Conditions sub Data Purpose Displays and prints the run conditions of a stored chromatogram Syntax Select Conditions Comments The conditions window is tied to the instrument ID file which was resident in memory at the time the chromatogram was stored The ID file contains information on carrier gas and column configuration under which the sample was run Make sure that the proper instrument ID file is resident before data is collected Open sub Data Purpose Allows the retrieval of a data file by highlighting a name from a scrolled list or by entering a path and filename in the space provided Syntax 1 Select Open or type O 2 Choose a data file from the list given Use the scroll bar to access files which are not immediately visible 3 Select Open Comments Select the symbol or a drive letter to access alternate directories or drives The Open command can also be used to delete files that are no longer needed When the list of data files is shown on the screen highlight the file you wish to delete by clicking on it This should blacken the file name If 61 Menu Reference EZChrom 200 400 menus and commands you wish to delete several files in a row press the lef
16. Tangent Skim Purpose Forces a baseline tangent from the start of overlapping peaks to their tails Syntax 1 Select a region for which the tangent baseline is to be drawn 2 Click on TAN Comments If there is a peak valley that is higher than the tangent baseline a perpendicular is dropped to the baseline from the lowest point in the valley This perpendicular defines the peak start for the second peak 90 Menu Reference Channel AJB commands Help Main menu See Figure 44 Purpose To provide access to an interactive help menu EZChrom 200 Version 4 0 Copyright 1988 1994 MTI Analytical Instruments Figure 44 Help window Syntax Select Help or type H Comments Future versions of EZChrom 200 400 will have help routines similar in format to those used by Windows At the present time Help will only display a screen showing the current version of EZChrom 91 Menu Reference Channel A B commands Print Main menu See Figure 45 Purpose Allows the user to print individual reports or chromatographic displays Chan A 100 sec Attn 2048 me Reports Events Display Big Help Normalization External Standard Full Scale Chromatogram Zoomed Chromatogram Figure 45 Print menu Syntax 1 Click on Print or type lt Alt gt P 2 Click on the desired type of report or display that is to be printed Comments Multiple print jobs may be selected with the print command Disablin
17. entry is used to reference the RRF discussed above to a particular peak in the Peak Table Choose a compound which has a similar thermal conductivity to the uncalibrated peak Print sub Method Purpose Prints the current Method Syntax 1 Click on Print or type P Comments A method printout includes the following items for both channels Instrument Setup Peak Table Calibration Setup Peak Calibration Tables Timed Events Print Options Display Options Print Options sub Method Purpose Allows the user to choose which reports and chromatograms will be printed after a single run or during the time between runs in an autorun The Print option under the Start window mustalso be selected for this option to be active 75 Menu Reference EZChrom 200 400 menus and commands Syntax Select Print Options or type R Comments The following choices are available Full scale chromatogram Zoomed chromatogram Area Report Normalization Report External Standard Report Check or uncheck any or all entries to get the desired set of printed reports Be aware that printing large datasets such as full scale chromatograms is time consuming If printing must be done between runs in an autorun sufficient time must be allotted for printing to be completed A standard IBM dot matrix printer will require approximately 3 minutes to print a single 100 second chromatogram Save sub Method Purpose Saves the current Method un
18. feature 1 Select Method 2 Select Calibration Setup 3 Check Update Retention Time After Run The retention time can also be updated after each calibration by checking the appropriate box Peak quantitation The external standard calculations are performed by multiplying the raw area of an identified peak by its response factor Component area x Response factor External standard amount The response factor is usually generated from a calibration plot The calibration plots are displayed in the Peak Calibration portion of the Method The type of calibration plot which is to be used point to point or linear is determined in the Calibration Setup portion of the Method 54 Technical Reference Peak quantitation Point to point calibration plots A point to point calibration plot uses calibration gas standard amounts y axis and their raw peak areas x axis as Cartesian coordinate pairs These pairs are used as points on a calibration plot In the simplest case a one level calibration a line is drawn from the origin through the single point The slope of the line is equal to the Response Factor Real sample amounts are then calculated by multiplying the area of the sample components by the slope of the line response factor in the calibration plot For a multi level point to point calibration there are several lines which define the calibration plot Each response factor corresponds to the slope of asegment on the cali
19. forces the integration baseline to be drawn to the lowest point in the valley between two peaks Syntax 1 Choose the two peaks whose baseline is to be identified 2 Place the vertical cursors around this region 3 Select BLV or type V Comments Two peaks that are separated by a valley must be selected The baseline will be drawn from the start of the first peak to the valley between the peaks Then it will continue from the valley between the two peaks to the end of the second peak 86 Menu Reference Channel A B commands FINE SLPSEN sub Event Fine Slope Sensitivity Purpose Defines a threshold value for the second derivative of the detector voltage The second derivative is used in peak processing to determine peak start and stop Syntax 1 Choose a 2 second segment of the baseline with no peaks 2 Select FINE SLPSEN or type F 3 Review adjust the event values and choose OK Comments Generally you should adjust the time for FINE SLPSEN to zero seconds This starts the peak search with the correct FINE SLPSEN value from time zero When the change in the slope between three data bunches is greater than the threshold FINE SLPSEN value a peak start is defined When the change in slope falls below the threshold FINE SLPSEN value a peak end is defined INTG OFF sub Event Integration Off Purpose Turns integration off for a specified period of time Syntax 1 Choose a region of the chromatogram as de
20. hashmarks drawn under integrated peaks 58 Calib Menu Reference EZChrom 200 400 menus and commands Main menu Purpose Sets up EZChrom for a two channel calibration It also provides the capability of selecting a calibration level from 1 8 for users who desire a multilevel calibration Syntax 1 Select Calib or type lt Alt gt C 2 Enter a number between 1 and 8 to select a calibration level 3 Select OK To stop a calibration prior to analysis select Cancel 4 Select Analyze This will take the calculated peak areas and assign them to the appropriate peak name and amount value Comments Calibration does not begin until data is actually collected or stored data is analyzed Level 1 is all that is required for normal use Higher levels are used to construct linear or nonlinear point to point calibration plots Method Instrument WELES Analyze Math Calib Start Help Open Clear Statistics Tamas es Figure 38 Data menu 59 Menu Reference EZChrom 200 400 menus and commands Data Main menu See Figure 38 Purpose Allows raw chromatograms to be accessed or stored Also allows the statistical records of the External Standard or Normalization reports to be cleared Syntax Select Data or type lt Alt gt D Clear Statistics sub Data Purpose Resets the statistics MIN MAX MEAN RSD in the External Standard and Normalization reports Syntax Click on Clear
21. not read from the hardware before the next character arrived The character was lost 4 Hardware detected a parity error 8 Hardware detected a framing condition 16 Hardware detected a break condition 32 CTS clear to send timeout 64 DSR data set ready timeout 164 Error Number Description 128 RLSD receive line signal detect timeout 256 Transmission queue was full when afunction attempted to queue a character 165 Error Number Description 166 Appendix B Dynamic Data Exchange DDE Dynamic Data Exchange DDE EZChrom is now extensible through the use of Microsoft s Visual Basic You can write a program in Visual Basic that can control EZChrom 200 400 This gives you the ability to generate custom reports from analyzed data or to create something as complex as on on line process monitoring system Agilent Technologies does not provide programmable applications but the framework on which to build them Overview Features Asmall but powerful set of commands are available to the Visual Basic programmer EZChrom 200 400 will perform the following functions at the request of a Visual Basic program Acquire a new data file from the GC and return the results of the analysis Perform a calibration Recall a run from disk and return the results of the analysis 1 2 3 4 Recall a method from a disk 5 Return the status of the GC 6 Return the conditions under which the current sampl
22. peaks in conjunction with slope sensitivity Baseline correction Up to this point only peak detection has been discussed Besides finding the beginning and end of a peak the peak s baseline needs to be defined so that a peak area can be calculated The area is calculated by subtracting the trapezoid under the baseline correction from the raw uncorrected baseline EZChrom 200 400 constructs separate baseline segments from the beginning of the first peak to each of several successive valleys The baseline that has the least positive slope is selected to correct the peaks included in that baseline This method works well for almost all cases of baseline drift 53 Technical Reference Peak identification Peak identification The next step in the process is peak identification The peaks are identified by using the retention time and retention time window specified in the Peak Table EZChrom 200 400 tries to match the retention times of peaks it has found with retention times listed in the Peak Table If a matching retention time is found the peak is given the name specified for that window If more than one peak is found within a given window the retention time of the largest peak in the window is used in the Normalization or External Standard reports Retention times can be updated at the end of each run as long as the peaks are detected and identified This is particularly handy if the retention times are shifting To activate this
23. the GC module about 5 minutes over any temperature range A large steady baseline drift indicates the system is not at equilibrium Remember the higher the column temperature the faster the elution Therefore analysis time can be reduced by increasing the column temperature A balance must be struck however as peak separation decreases with an increase in temperature and this can make accurate integration difficult The allowed range is ambient to 180 C 160 C for modules equipped with a HayeSep column Columns in the two modules may have different temperature settings Run time seconds The amount of time that data is collected from the detector Initially this should be set to the maximum value of 160 seconds Later it should be set to a value slightly greater 10 s than the time at which the tail of the last sample peak has eluted This parameter may be different for the two modules 32 Sample Session Building a method Sample time seconds The time that the built in vacuum pump is run prior to sample injection The pump should be run long enough that the injector sample loop is flushed with sample The maximum sample time is 255 seconds but 15 to 20 seconds is usually sufficient This parameter is the same for both channels Inject time milliseconds variable loop only The amount of time the inject valve is open and sample is flushed onto the column from the sample loop The range of values is 0 255 milliseconds
24. values other than the defaults may be appropriate To access and alter the Calibration Setup table 1 Select Method 2 Select Calibration Setup 3 Make any necessary changes in the table 4 Select OK to close the table The features available in the Calibration Setup table See Figure 50 and their default values are described below 103 Quick Reference Multi level calibration Peak Attribute Area or Height Determines whether the calibration and quantitation are to be based on peak height or peak area The default is Area Calibration Setup Update Calibration C Yes C No Peak Attribute Area C Height Calibration fit Point C Linear Number of Runs A amp B Begin Calibration at Run Uncalibrated Peaks RF 0 00000000 Multiplication Factor ii Update Retention Time After I Calib Run x Figure 50 Calibration setup table Calibration Fit Point or Linear Determines whether the calibration plot is to be based on a point to point plot or a linear plot The default is Point Number of Runs A amp B This corresponds to the number of calibration runs that will be performed at each calibration level The integrated areas for each peak are then averaged and an average response factor is generated The default is One Begin Calibration at Run This allows the instrument to stabilize before calibration The default is One 104 Quick Reference Multi level calibration Unca
25. within a defined region of time even though the retention time of the peak may not match the retention time listed it will be identified as the compound defined by the preset retention time window Concentration Unit CU This is a text entry which identifies the concentration units of the various compounds Any three character text entries are allowed The unit is not a conversion factor and has no mathematical significance Each component may have a different concentration unit The concentration units are only used for external standard reports Level 1 Cal Amount This is the amount of a compound that the level one external calibration standard contains When a Level 1 calibration is run the entered amounts are assigned to the areas of any integrated peaks which elute in the appropriate retention time windows Obviously accurate calibration standards must be used and retention time windows must be properly set for EZChrom 200 400 to accurately quantitate real samples EZChrom 200 400 can use up to eight levels of calibration but for routine analysis one level is usually sufficient Each level corresponds to a gas standard concentration and a point on a calibration plot 74 Menu Reference EZChrom 200 400 menus and commands Relative Response Factor RRF When an external standard is unavailable an estimated response factor may be specified Enter a number which will be multiplied by a calibrated response factor Peak This
26. 0 400 or Windows 1 Place the single headed cursor on a vertical border of any window displayed on the screen When the cursor rests on the border it will change from a single headed to a double headed arrow See Figure 13 This may take a bit of practice as the borders are narrow and easy to overshoot 20 Getting Started Graphic manipulation with a mouse Chan A 100 sec Attn 2048 f Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help g H Method SERIALNO MET File SERIALNO 1 z BE Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 13 Using double headed arrow 2 Click and hold the left mouse button and drag the mouse to the left or right and release Ifa horizontal border was chosen drag the mouse up or down Place the cursor on any corner of a window border 4 Click and hold the left mouse button and drag the mouse in any direction and then release The corner border allows two dimensional growth or shrinkage of any window See Figure 14 5 Practice placing the cursor on the borders of the various windows until it is routine 21 Getting Started Graphic manipulation with a mouse Chan B 100 sec Attn 2048 l Reports Events Display Print Help SERRO Reports Events Display Print i Help Method btu met File btu 1 Method Instrument Data A
27. 0720 0 397 0 000 Method SERIALNO MET File SERIALNO 1 Method Instrument Data Analyze Math Calib Start Help Figure 19 Peak table Select Channel A then place the single headed arrow cursor in the first empty box under the heading Peak Name and click the left mouse button The flashing cursor which appears may be moved to the left or right up or down using the arrow keys Type the word Example then place the cursor at the end of Example Press the backspace key repeatedly until the entry is completely deleted To delete more easily place the arrow cursor at the beginning or end of the entry Then click and hold the left mouse button while dragging the mouse so that the whole entry is blackened Now press the delete key to remove the entry All text and numbers surrounded by a box other then the values in the instrument status window may be edited in this way 27 Getting Started Text and numeric editing 28 Sample Session Sample Session Once you have mastered a few skills running an Agilent gas chromatograph with EZChrom 200 400 is relatively simple The system has been designed so that a wide variety of analyses can be handled quickly and easily The purpose of the Sample Session is to provide you with the basic skills needed in a typical session with EZChrom While it does not cover all the capabilities and features of EZChrom 200 400 all of the nece
28. 123 The GC Module Change Tool Starting GC Module Change Tool Program Manager HA a Options Window Help New Open MS Move E E Copy t Manager Clipboard Viewed S DOS Prompt Delete Del Properties Alt Enter A Figure 58 Program manager window When you select Run you will see a window like Figure 59 me Command Line c mti utility change C Run Minimized Browse Figure 59 Run window 124 The GC Module Change Tool Starting GC Module Change Tool Type in the complete path and file name of the Module Change Tool as shown in Figure 59 and click OK If you ve typed in the correct name the Module Change Tool will search your serial ports for a connected GC and then display a window similar to Figure 60 showing the current module configuration record MTI GC 18 Module Change Module A Column Temperature Offset Column Temperature Scale Maximum Column Temperature Fixed Loop Injector Module B Column Temperature Offset Column Temperature Scale is Maximum Column Temperature _ Fixed Loop Injector Figure 60 Agilent GC 18 Module change window The path shown C HP UTILITY assumes that you have installed the GC Tools diskette in the standard directory C HP If you have installed the Tools program in any directory other than C HP you will have to enter lt dir gt UTILITY CHANGE where lt dir gt is the directory into which you have ins
29. 3 Installation Hardware setup Hardware setup Setup your Micro GC as specified in your instrument manual e g M200 M200H P200 P200H To connect your Micro GC to your computer do the following 1 Connect the serial port of the computer COM 1 when using a bus or no mouse COM 2 when using a serial mouse to the serial port of the instrument back panel for M and Q series front or back panel for P series using the RS 232 serial cable provided See Figure 7 for mouse connections 2 Plug the mouse and printer if you are using one into the computer see your computer owners manual This completes the installation of the EZChrom 200 400 data system Serial port Bus port OO0O00O e da o o Figure 7 Mouse connections Installation troubleshooting See description of installation troubleshooting in the chapter addressing the GC Verification program found in the addendum of the instrument manual Getting Started Getting Started Selecting commands in EZChrom 200 400 Any command in EZChrom 200 400 may be selected via the keyboard or with a mouse controlled cursor To select a command with the keyboard 1 Hold down the lt ALT gt key while at the same time pressing the underlined letter of the Menu you wish to select A pull down menu will be displayed Now all that is necessary is to press the underlined letter of any command listed in the pull down menu To select a command with a mouse 1 Place the singl
30. 400 is designed for beginning chromatographers and experts alike and when interfaced with an Agilent gas chromatograph performs routine gas analysis with minimal user input For complex samples a variety of commands are provided to simplify the quantitation and identification of gaseous fractions A personal computer is used as a sophisticated chromatography data analysis station and storage device With EZChrom 200 400 running on a personal computer you can Set up modify catalog recall and print Instrument settings Peak identification tables Calibration tables Integration parameters Start and stop the instrument to upload and download experimental conditions and to monitor instrument status Catalog and recall chromatographic data Introduction General description Integrate and identify observed peaks Set up and run automated sequences Perform calibration sequences Graphically manipulate data displays via zooming functions scroll bars and mouse or keyboard controlled zoom boxes and cursors Graphically specify Timed Integration Events Calculate display and print Area Normalization and External Standard reports Store integrated results in DIF or PRN format for direct input to spreadsheet applications such as Lotus 1 2 3 and Microsoft Excel Introduction How to use this manual How to use this manual This manual covers the installation and operation of the EZChrom 200 and EZChrom 400 Chr
31. Agilent EZChrom Chromatography Data System User s Manual Agilent G2890 G2891 Micro GC Agilent EZChrom Chromatography Data System Agilent Technologies 2000 Microsoft Windows Lotus 123 and MS DOS are registered trademarks and Windows and Excel are trademarks of Microsoft Corporation All rights reserved Reproduction adaptation or translation without permission is prohibited except as allowed under the copyright laws Part No G2890 90327 Replaces DOC 2049 First edition APR 2000 Printed in USA Safety Symbols This manual contains safety information that should be followed by the user to ensure safe operation WARNING A warning calls attention to a condition or possible situation that could cause injury to the user CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the user s work Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19808 1610 USA Contents Chapter 1 Introduction General GESCrIDTION creeeren a ea eA Aaaa A aE EE e 2 How to use this manual sossseeseeesseseesssseesssssrssssrresssereesseseesssseesssseessss 5 Chapter 2 Installation Requirements ernennen a E E eee ans 8 EZChrom 200 400 installation cccccecsseccsscecssscecseececsseceeeseceesseeeeeees 9 Getting started 526d to cus tdacteoatetncacdetasg pancaeds ebuncastsesabdednenunas menage ebuentine
32. B commands Baseline sub Display Purpose Draws or removes the baseline on the lower display Syntax Select Baseline or type B Comments Removing the baseline from the display also removes it from a printout of the chromatogram Cursor sub Display Purpose Turns the vertical cursors time and amplitude readouts on or off Syntax Select Cursor or type C Comments This option is most useful when operating without a mouse or when the cursors and orreadouts overlap an interesting portion of the chromatogram A check will appear next to the Cursor command when the cursor is activated Simply click on the command bar to activate or deactivate 82 Menu Reference Channel A B commands Full Unzoom sub Display Purpose Unzooms the lower portion of the window to a full scale chromatogram Syntax Select Full Unzoom or type F Comments The fully unzoomed chromatogram is displayed at the attenuation setting shown at the top of the channel A or B window Split Screen sub Display Purpose Splits unsplits the screen An unsplit screen will display only the lower or zoom portion of a channel window Syntax Select Split Screen or type S 83 Menu Reference Channel A B commands Comments Removing the upper display can give better vertical resolution of high amplitude peaks Chan A 100 sec Attn 2048 Reports Sawai INTG Off SLPSEN FINE SLPSEN PKWD BL at BLY BLH TAN M
33. C Verification Tool Typical sessions Connect your GC and click Yes GC Verification checks each serial port on your computer system for an M200 During this time a window like Figure 70 is displayed Searching for an MTI GC e re checking out each serial port to locate your MTI GC e ll use the first one we find Figure 70 Searching for a GC window If no GC is found an error message is displayed in the status box as shown in Figure 71 When you click OK GC Verification returns to the Introduction Window Searching for an MTI GC Explanation e re checking out each serial port to locate your WTI GC e ll use the first one we find Status No MTI GC appears to be connected Figure 71 Searching for a GC window 137 The GC Verification Tool Typical sessions If a GC is found the window displays its serial number in the Status box and when you click OK GC Verification proceeds with checking the GC In Figure 72 the 18 represents the serial number of the GC Your Status box should display the serial number of your particular GC Searching for an MTI GC Explanation e re checking out each serial port to locate your WTI GC e ll use the first one we find Status Found MTI GC 18 connected to COM1 Figure 72 Searching for a GC window If your GC is OK the next and final window you will see is as shown in Figure 73 MTI GC Yerification Successful Expl
34. D starting each ata cuca Time 0 000 SLPSEN and FINE SLPSEN values depend on detector sensitivity settings Start with Low Med High SLPSEN 10 50 100 FINE SLPSEN 5 30 75 INTG OFF Start with a value of 1 5 Increase value if necessary PKWD Start with a value of 1 Add additional pkwds if necessary To name integrated peaks choose Peak Table from the Method menu Lock Unlock Instrument Setup F1 Peak Table Peak Calibration Calibration Setu v Timed Events Display Options Print Options 182 Dynamic Data Exchange DDE Developing a method Peak Table Peak Table Channel RT RT Level 1 Pkno Peak Name Time Window CU BP CalAmount ARF Peak C fs fireman Te a epenn 4 Enter Peak Names RT Times RT Windows CU and BP for each channel manually or with vertical cursors If setting RT Time and RT Windows with vertical cursors continue to steps 5 and 6 Click OK Then Save the method under the Method menu 183 Dynamic Data Exchange DDE Developing a method Peak RT and RT Window menu Time sec 001 980 Amp uV 546 INTG Off SLPSEN FINE SLPSEN PKWD BL t BLY BLH IAN Min Area Invert Peak RT and RT Window 5 Toset RT Times and RT Windows graphically set vertical cursors on either side of the peak of interest Then choose Peak RT and RT Window from the Events
35. Fill out the Peak Table 3 Run the GC 4 Set up the Timed Events Table 5 Adjust the instrument parameters and rerun the GC This step is optional and frequently unnecessary 96 Quick Reference Quick and easy method development 6 Optimize the Timed Events Table 7 Set the peak retention times and retention time windows graphically 8 Calibrate and save the method The details of each of these steps are reviewed below To exit EZChrom 200 400 at any time double click on the box above Method in the main menu Steps for the method construction procedure 1 Open the Instrument Setup window See Figure 47 and set the column temperature run time inject time and detector sensitivity to appropriate values For most applications columns temperatures of between 50 and 80 degrees will give acceptable peak resolution Instrument Setup x Channel G A CB Column Temperature 46 Run Time sec 100 Sample Time sec 10 Inject Time msec 50 Detector Filament Cot On Detector Autozero C Off On e c Detector Sensitivity CLow Med High Cancel Figure 47 Instrument setup window Start with the maximum run time 160 seconds and later reset it to 10 seconds longer than the tail of the last eluting peak Use a value of 50 milliseconds for the inject time unless sample gas concentrations are in the high range in which case use 20 milliseconds or low ppm range i
36. If you make a mistake here you can always click the Swap button again to get things back to their original configuration parameters If you are using a Quad GC you may only swap modules A and B or modules C and D and use the Swap button You cannot swap any other combination of modules and use the Swap button However if you choose to swap any other combination of modules other than A and B or C and D youshould write down the current configuration parameters for the two modules on anotepad and enter each module s configuration record to the other s record 130 The GC Verification Tool The GC Verification Tool Your GC was shipped with a GC Tool diskette which contains a record of the proper instrument configuration operational parameters for your particular GC and two GC Tools programs GC Verification and GC Module Change The GC Verification Tool is used to verify and or restore your instrument configuration record You can use GC Verification at any time to verify that your GC firmware is in proper working order to restore its configuration parameters clear error conditions or recover a lost configuration record You should run GC Verification whenever any of the following conditions pertain 1 You have just unpacked a new chromatograph and want to verify that it is in good condition 2 EZChrom or other software reports that the GC has an error condition 3 The main controller board is change
37. Method Select Lock Enter a password maximum of eight characters AG I A E Save the Method entering your password at the prompt To Unlock a Locked Method 1 Open the Method that is locked 2 Select Unlock in the Method menu 3 Enter the password 4 Changes in Method parameters will now be accepted 102 Quick Reference Multi level calibration Multi level calibration EZChrom 200 400 will handle calibrations with up to eight gas standard concentration levels Each calibration level corresponds to a point on a calibration plot Each component for a particular channel must be calibrated with the same type of calibration method i e point to point or linear That means that if a point to point calibration is used for one component the same must be used for all of the other components However the number of calibration levels may be different for each component The procedure for initiating a multi level calibration or single level for that matter begins with e Calibration setup In addition to allowing up to eight levels of calibration EZChrom 200 400 software can calibrate either on peak height or peak area Also the calibration plot can be either point to point or linear For a linear plot at least two levels of calibration are required When a new method is being built EZChrom defaults to a set of values for the Calibration Setup In most cases the default values will suffice In certain cases however
38. aced The Module Change program can also be used to assist in changing the configuration record for modulesina Quad GC but the procedure outlined below should be followed 1 Terminate all software e g EZChrom that is using the GC and disconnect all serial cables between the GC and your computer 2 Determine which module you will have replace d i e A B C or D 3 If module A or B is replaced find the RS232 DB 9 connector labeled A and B on the right hand side of the GC on your left if you re looking at the back panel If module C or D find the RS232 DB 9 connector labeled C and D on the left hand side of the GC on your right if you re looking at the back panel 4 Connect aserial cable from the connector that you located in step 2 to your computer s serial port it does not matter which serial port but make sure that no other GCs are connected and that there is no other connection to 128 The GC Module Change Tool GC Module Change Tool for a Quad instrument your Quad If there is only one serial cable connected to your computer you re OK 5 Runthe Module Change Tool To change module A or C select Module A in the Module Changer to change module B or D select Module B in the Module Changer You will then see a window that allows you to edit the GC s module configuration record See Figure 62 Click on Cancel if you want to quit without making changes Caution It s a g
39. aination The GC is functioning properly There are no outstanding error conditions and the configuration has been verified Figure 73 GC verification successful window If you get to this window the GC has been verified and is ready for use Click OK to terminate GC Verification 138 The GC Verification Tool Typical sessions What happens if your GC has problems If your GC has problems there are several possible scenarios but they all lead to one of two outcomes either GC Verification will be successful or it will not be successful What happens if your GC has problems that can be fixed Here is what a successful error fixing session would look like First you get the introduction as shown in Figure 74 MTI GC Verification e will check out your MTI GC to verify that it is OK and will perform properly If there is a problem we will guide you through the necessary procedures to restore the GC to proper operating condition Request If you have not done so please connect your MTI GC to one of the computer s serial ports Question O Is the GC connected es About Figure 74 GC verification window Click Yes and GC Verification establishes a connection to the GC as shown in Figure 75 139 The GC Verification Tool Typical sessions Searching for an MTI GC Explanation e re checking out each serial port to locate your WTI GC e ll use the first one we find
40. ak Table under the Method menu Channel Prev Next Pkno 1 Level Area Amount Cancel Plot New Open Save Save As Print Lock Unlock Instrument Setup F1 Peak Table F2 Calibration Setup F4 TimedEvents F5 Display Options F6 Print Options F7 SARE Instrument Data An Calibration Type Point 9 18 27 35 Area x 1000000 Area will automatically be inserted at Step 7 186 Data menu 5 Dynamic Data Exchange DDE Calibrating a method Open To begin calibration choose Clear Save As Statistics in the Data menu to erase MIN MAX MEAN and RSD Conditions Clear Statistics Click OK BEET Analyze Math Cali Calibration menu and window Calib 6 Choose Calib Enter the calibration level Click OK Calibration Level m Calibration L ok cance Analyze and Start menus T If calibrating with stored data click Analyze If calibrating with data to be collected click Start to E begin run 187 Dynamic Data Exchange DDE Calibrating a method 188 Manual Part No DOC 2049 Printed on recycled paper This product is recyclable Hewlett Packard Company Printed in USA 5 98
41. alRuns None Returns the number of calibration runs per calibration level GetInstStatus x Returns the current instrument status for channel x GetRunCond x Returns the run conditions for channel x 172 Dynamic Data Exchange DDE EZChrom DDE server Return value formats All of the following commands return their data via the DDE link DDE uses text strings to pass data therefore the data from some of these commands will need to be decoded The format of the data that is returned is described below Name Format Name Format Name Format Name Format Name Format GetMethName The path to the current method is returned For example C HP EZCHROM 200 200 METHODS EXAMPLE MET GetDataName The path to the current data file is returned For example C HP EZCHROM 200 200 CHROM EXAMPLE 1 GetCycleTime The cycle time is returned as a string For example if 120 is the cycle time 120 will be returned Note the return value will have to be converted to a number before it can be used GetCalLevels The number of calibration levels are returned as a string For example if there are 4 calibration levels 4 will be returned Note the return value will have to be converted to a number before it can be used GetCalRuns The number of calibration runs per levels is returned as a string For example if there are 5 calibration runs per levels 5 will be returned Note the return value will ha
42. ally or with the keyboard In the Calibration Setup table there is an option to update the retention time at the end of arun If this is selected and the retention time changes then the retention time and the window will be updated 35 Sample Session Building a method Seconds Figure 24 Retention time amp retention time window Retention time window Retention Time Window is asectioned length of time around the peak apex If a peak apex falls within the defined window even though the retention times of the peak width at its base may not exactly match the retention time window inthe table that peak will still be identified as the peak name listed See Figure 24 for a graphic representation of retention time and retention time window Concentration unit This is a text entry which identifies the concentration units of the various compounds All text entries are allowed up to a maximum of three characters The unit is not a conversion factor and has no mathematical significance Each component may have a different concentration unit The concentration units are only used for external standard reports BP bunched peaks Allows all peaks within a RT Window to be recognized as one component Therefore the peak area reported for the component will be the sum of all peaks found in the RT Window Type Y for Yes to activate BP 36 13 14 15 Sample Session Building a method When PP is actuated no Re
43. and B A run clock is provided at the top of the channel A and B windows This clock displays the real time of the chromatographic analysis that has progressed through arun Itshould count up to the run time specified in the Instrument Settings window When the run is completed the data is first stored on the hard drive in the default directory c HP ezchrom 200 chrom under the run ID which you provided The data set is then automatically analyzed using the default timed events provided with the NEW method At this point take the opportunity to carefully examine the analyzed chromatograms using the zooming and unzooming techniques you practiced in Chapter 3 During your examination keep in mind the following questions 39 Sample Session Collecting data Have all of the peaks been detected This is indicated by a baseline set off by vertical hashmarks drawn under each peak See Figure 26 Hashmarks which point upward indicate the start of integration while downward pointing hashmarks define the end of integration Method SERIALNO MET File SERIALNO 1 Eza Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 26 Integrated peaks Are the peaks correctly integrated Even though a peak has been detected perhaps only a small portion of the peak was actually integrated Conversely an integrated region may include areas on either side of a peak which should not be integrated
44. ard Comments Amounts are calculated relative to the calibrated External Standard Min Max Mean and RSD are a record of the repeatability of sample analysis over a Set of runs 94 Quick Reference Quick Reference This chapter of the manual provides greater detail concerning the features available in EZChrom 200 400 It is geared to those users who are already familiar with basic EZChrom operation and should not be used until prior chapters are fully mastered Due to the presumed sophistication of the user certain procedures are presented in other than strict chronological order of operation In certain cases the reader will be asked to refer to other chapters of the manual for further explanation or for review This chapter also presumes an extensive knowledge of EZChrom menus You should be thoroughly familiar with Chapters 4 5 and 6 before attempting the procedures described in this chapter Refer to Appendix C for several quick reference flowcharts describing the following Setting Up a Run Developing a Method Calibrating a Method Quick and easy method development The first step in optimizing the performance of EZChrom is to build a good Method This chapter provides a step by step sequence which simplifies the Method construction procedure outlinedin Chapter 4 The followingis an outline of the procedure that should be followed whenever anew application is to be run 1 Set up the instrument parameters 2
45. as an integration baseline drawn underneath it the retention time has been incorrectly set Repeat steps 1 3 fA Channel B EXTERNAL STANDARD Report x Name Amount Units RT Min Max Mean SD Nitrogen 2 558 2 320 2 558 2 558 2 558 0 000 Methane 88 112 2 760 88 112 88 112 88 112 0 000 co2 0 000 0 000 0 000 3 000 2 000 77 460 Ethane 3 501 14 240 3 501 3 501 3 501 0 000 H2S 0 000 0 000 0 000 0 000 0 000 0 000 Propane 0 000 0 000 0 000 1 011 0 843 48 990 Figure 35 External standard report with incorrect retention time 9 When all the names you have added to the Peak Table are present in the External Standard report with a non zero value proceed to the next chapter Calibrating the method The last step in building an optimized application Method is calibration This step is necessary when creating a Method in order to generate a response factor on a known sample so you can at a later time perform quantitative analysis on an unknown sample EZChrom allows a Method to contain up to eight calibration levels eight different calibration gas concentrations at one time In the great majority of cases however only a level one calibration is required Peak area 0 concentration 0 is the assumed second value of the peak 1 Select the Calib menu on the EZChrom command bar 2 A window will appear which says Calibration Level and has a number highlighted See Figure 36 Enter 1 and click on Ok 48 Sample Sessio
46. bration plot Linear calibration plots If the linear option is selected a single line is calculated using a least squares approximation The points used to generate the fit are the same amount area pairs as those in the point to point plots The slope of this line is used as the response factor for subsequent quantitations 55 Technical Reference Peak quantitation 56 Menu Reference Menu Reference This chapter of the manual describes the menus and commands available in EZChrom 200 400 They are categorized in levels according to the screen menus in which they appear Within a menu they are alphabetized for ease of reference EZChrom 200 400 menus and commands The EZChrom 200 400 Data System main menu contains all of the commands necessary to set up run calibrate and analyze data collected on an Agilent gas chromatograph as well as store and catalog all Methods and data files This menu is located in the menu bar at the lower right of the screen Analyze Main menu Purpose Analyzes the current data file using the current analysis Method i e timed events retention times and calibration tables Reports and baselines are updated accordingly Syntax Select Analyze or type lt Alt gt A Comments During analysis a series of messages are displayed in the menu bar starting with Analyzing Channel A Chromatogram Upon completion of the analysis the chromatograms will be displayed with baselines and
47. cal cursor to set integration off Chan 100 sec Attn 2048 j Events INTG Off SLPSEN EINE SLPSEN PKWD BL At BL BLH TAN Min Area Invert Peak RT and AT Window Figure 28 Events menu 42 Sample Session Optimizing timed events 3 Select the Events menu located in the channel A menu bar See Figure 28 4 Select the INTG Off command This will place an integration off event in the channel A Timed Events Table It will also set the time of the event to zero and the value to the time where the vertical cursor was frozen Chan 100 sec Attn 2048 f Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help Time sec 020 Amp uV 336 Time sec 002 040 Amp u 2018 Method SERIALNO MET File SERIALNO 1 Heat od Instrument Data Analyze Math Calib Start Help Figure 29 Using vertical cursors to determine noise level 5 Again using the vertical cursors select a small region about 2 seconds on the baseline of the channel A chromatogram which does not contain any portion of a peak See Figure 29 This region will be used to determine the noise level in the chromatogram 43 Sample Session Optimizing timed events SLPSEN Event Time 0 000 Value 16 000 Margin 9 0 000 Figure 30 SLPSEN Event window 6 Select the SLPSEN command under the Events menu A window will appear which
48. can be accessed through function calls made by the client program The GetPeak function is used to access the data for the current peak in the DLL The current peak is referred to by an index number which the DLL keeps track of Each time the GetPeak function is called this index is incremented by the DLL The SetPeakIndex function allows the client program to change the index number in the DLL The GetPeakIndex function will return the current peak index number The DLL also serves as a place to place command parameters for commands that are sent to EZChrom 200 400 via DDE The SetCmdParam function is used to place a parameter into the DLL for retrieval by EZChrom 200 400 The command parameter is stored as a string Peak Data Format The following datum are stored for each peak Peak name peak area concentration retention time peak number and channel The proceeding are stored in a string with the fields delimited by tabs Functions Name GetPeak Prototype int FAR PASCAL GetPeak LPSTR Description This function is used to access the peak data that is stored in the DLL The data is stored in the strings that is passed as a parameter to this function This function increments the peak index as aside effect The function returns TRUE if the peak index is less than 50 FALSE otherwise 175 Dynamic Data Exchange DDE EZChrom 200 400 VBE DLL Name Prototype Description Name Prototype Description Name Pro
49. cs Wait For External Start Save Print DIF Save PRN Save Extended User Program Figure 41 Run window Syntax 1 Select Start or type S 2 Fill in the Run Setup screen See Figure 41 3 Select Start to run the GC or Recall to reanalyze a stored dataset Comments The Print or Save functions can be turned on or off globally but the items that are to be printed must be activated in the Print Options menu Cancel Cancels any alterations made to the Start window and returns the user to the EZChrom 200 400 menu DIF PRN Save Saves the peak name amount and run number from the External Standard Report to ASCII files read by Excel or Lotus respectively File extensions will be DIF Excel or PRN Lotus 78 Menu Reference EZChrom 200 400 menus and commands Extended Causes the peak areas and retention times to be added to DIF and PRN files Number of Runs Enter the number of runs you wish EZChrom 200 400 to collect during an autorun Entering 0 999 or INF will cause EZChrom 200 400 to run continuously If the Save option has been selected while EZChrom is running continuously the thousandth saved file will overwrite file number one and so on OK Allows the Start window to be altered without actually starting a run Print Will cause all selections in the Print Options menu to be printed in the time between the end of a r
50. d 4 The EPROM U32 is changed 5 The GC configuration record is changed 6 The GC battery backed RAM is zeroed or otherwise compromised GC Verification requires no specialized knowledge of a GC beyond its serial number It will walk you through whatever procedures you can perform to establish and or restore a proper configuration GC Verification only verifies that the embedded computer system firmware in the GC is OK It does not check the columns or other chromatography apparatus nor does it perform any special hardware checks 132 The GC Verification Tool Installing GC Verification Tool Installing GC Verification Tool GC Verification is automatically installed when you run SETUP EXE from a GC Tools diskette At this time the configuration record for your GC is also installed in your PC Since GC Verification relies upon the existence of the configuration record you should run SETUP EXE on each computer that you will want to use with a given GC You may install GC Verification on as many computers as you will use with your GC Starting GC Verification Tool To start GC Verification double click upon the GC Verification icon the one with a green check mark on it in the HP Program Group Window as shown in Figure 65 MTI GC Verification Figure 65 HP program group window The first window you will see is the Introduction Window as shown in Figure 66 133 The GC Verification Tool Starting
51. d Current Method Send Current Method Receive Method Instrument ID Hardware Setup Math Calib FEIT Help j 180 Dynamic Data Exchange DDE Developing a method a ydow iia a 7 Name the data file and define run Run iD test parameters to begin analysis Number of Runs 1 999 inf 1 Time Between Injections secs 0 To save settings without starting a Wait For Ext I Start run click OK Beran i O Print To begin run click on Start O DIF Save C PRN Save C Extended Repeat steps 1 through 7 altering User Program instrument parameters until cancer Becan optimal peak separation is Id achieved Developing a method Method menu New 1 After optimization of instrument settings set Open p s A Save integration parameters by choosing Timed Save As Events in the Method menu Print Lock Unlock Instrument Setup F1 Peak Table F2 Peak Calibration F3 Calibration Setup F4 Iimed Events F5 Display Options F6 Print Options F7 SAGE Instrument Data Al 181 Dynamic Data Exchange DDE Developing a method Timed Events window 2 Method menu 3 annel a OB Time Value Begin with 4 basic events per 1 BRWD 0 000 1 000 Events channel 3 FINE SLPSEN 0 000 30 000 O Spike OBLAt OINTGof OBLY OSLPSEN OBL SLPSEN FINE SLPSEN INTG EINE SLPSEN TAN is PKWD Inve OFF and PKW
52. d Peaks RF Assigns a single user defined response factor to all unidentified peaks in the concentration reports Multiplication Factor Multiplies the external standard amounts by a user defined value Allows compensation for preconcentrators or diluters Update Retention Time After This allows EZChrom 200 400 to update the peak retention times contained in the peak table after a calibration or after each data analysis 68 Menu Reference EZChrom 200 400 menus and commands Display Options sub Method Purpose Allows the user to select a boot up set of display criteria Every time the system restarts the screen will appear in the configuration that was specified Syntax Select Display Options or type D Comments The menu items are defined as follows Channel Selects the module for which the display will be altered Attenuation Sets the display magnification The range of values is 1 to 2048 with 1 being the greatest magnification Start Time The time in seconds of the first displayed data point Stop Time The time in seconds of the last displayed data point Start Amp The minimum voltage in microvolts which will be displayed Stop Amp The maximum voltage in microvolts which will be displayed The absolute maximum value is 12 000 000 microvolts 69 Menu Reference EZChrom 200 400 menus and commands Display Allows the user to choose which window will be displayed when EZChrom 200 400 is s
53. der the current Method filename Syntax Select Save or type S Comments If the current Method is locked the method password must be entered before this action can be completed 76 Menu Reference EZChrom 200 400 menus and commands Save As sub Method Purpose Saves the current Method under a user defined filename Syntax 1 Select Save As or type A 2 Enter the new filename for the current method using a maximum of eight characters in DOS format 3 Click on OK Timed Events sub Method Purpose Establishes integration parameters for each data analysis Syntax Select Timed Events or type T Comments Other than the Spike event Timed Events are described in this chapter under Events Spike is a filtering mechanism Specify the time that filtering should start and the smallest absolute spikes that should be filtered as the time and value respectively Spike will continue to smooth the data each time the data is analyzed Reports may change when data that has a Spike Timed Event is reanalyzed Spike is not available via graphics as a timed event All the other timed events are available via graphics 71 Menu Reference EZChrom 200 400 menus and commands Start Main menu Purpose Opens the run sequence window from which the GC can be started and various run time options specified Run ID E Number of Runs 1 9399 inf E Time Between Injections se
54. displays a calculated value for the SLPSEN event See Figure 30 Change the Event Time to 0 000 7 Click on Ok to add the SLPSEN event to the timed event table 8 Using thesame region of baseline as was defined in Step 5 select the Events menu again but this time add a FINE SLPSEN event to the timed events table for channel A Change the Event Time to 0 000 44 Program Manager Sample Session Optimizing timed events 001 090 Amp u 469284 Time sec 000 510 Amp uV 53026 Mins Method Instrument Data Analyze Math Calib Start Help Method SERIALNO MET File SERIALNO 1 Figure 31 Using vertical cursors to set peak width 10 11 12 13 14 Next place the vertical cursors on either side of the first peak See Figure 31 Be sure that the cursors are frozen at the very beginning and end of the peak zooming may be required to get the clearest view Select the PKWD event under the Events menu A window with a calculated peak width value for the selected peak will be displayed Click on Ok Repeat steps 9 and 10 for any remaining peaks in channel A Open the Timed Events table for channel A and confirm that all of the timed events you selected INTG Off SLPSEN FINE SLPSEN and PKWD are present in the table Select Ok or press lt Enter gt to close the Timed Events table Construct an optimized Timed Events table for channel B by repeating ste
55. e headed arrow cursor on the desired menu The types and functions of the various cursors will be discussed in the next chapter 2 Click the left mouse button once When the pull down menu appears place the arrow on the desired command and once again click the left button one time Graphic manipulation with a mouse EZChrom 200 400 allows the selection of commands the adjustment of zoom boxes and window sizes and the setting and manipulation of reference cursors through use of the mouse To perform these functions four types of cursors are used asingle headed arrow mentioned above adouble headed arrow two vertical lines only active in the channel A or B Windows and a crosshair This chapter describes the functions of each cursor and provides ashort tutorial Single headed arrow Use this cursor to select commands draw and select zoom boxes move whole windows in two dimensions or to activate a window To become familiar with this cursor and its functions start EZChrom 200 400 Getting Started Graphic manipulation with a mouse 1 When EZChrom 200 400 is started the cursor that is visible and active is the single headed arrow cursor Place this arrow just to the left and near the top of a peak of the chromatogram in the channel A window Chan A 100 sec Attn 2048 Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help ae Method btu met File btu
56. e was acquired 168 Dynamic Data Exchange DDE Overview Example program An example program is included with the EZChrom 200 400 data system in the form of a normalized report generator It demonstrates how to use of some of the features described above It is intended to be a simple example that can be used as a Starting point for application development Normalized Report gt File Help Component Name Normalized Unnormalized Nitrogen 2 575 2 558 Methane 88 683 88 112 c02 3 019 3 000 Ethane 3 524 3 501 H2S 0 000 0 000 Propane 1 018 1 011 i Butane 0 401 0 398 n Butane 0 400 0 397 i Pentane 0 150 0 149 n Pentane 0 151 0 150 Hexanes 0 050 0 050 Heptanes 0 020 0 020 Octanes 0 010 0 010 Nonanes 0 000 0 000 Figure 106Normalized report window The window above shows a typical output from the example program After the program is started it looks for the EZChrom 200 400 DDE server If it finds the server it establishes a DDE conversation Note that this implies EZChrom 200 400 must be loaded before the example program in order for it to work properly Once the conversation is established the example program will wait for a message from EZChrom 200 400 When EZChrom 200 400 has finished analyzing data it sends a message to the example program to let it know that there is new data When there is new data the example program will copy the data into private storage and then perform a normalization on the data The normaliz
57. e zoom box will appear on the full scale chromatogram displayed in the upper window See Figure 56 To draw a zoom box 1 2 Place the cursor at the top left of the desired zoom area Hold the left mouse button down and at the same time drag the mouse down and to the right until the displayed box encompasses the portion of the chromatogram to be enlarged Release the left mouse button Defining a reference cursor Once the Cursor On has been selected it is possible to freeze the first vertical cursor This first cursor can then be used as a reference point for asecond vertical cursor 1 Check Cursor and move the cursor to the desired reference point 2 Click once on the left mouse button Notice that the cursor becomes frozen and that the values for time and amplitude are both zero Thisis the reference cursor 3 Move the mouse a second cursor will appear Note that the time and amplitude values change relative to the reference cursor 4 Clickonce on the right mouse button to freeze the second cursor and regain the arrow cursor 119 Quick Reference Graphical manipulation of chromatograms Chan 100 sec Attn 2046 Reports Events Display Print Help Attenuation scroll bar Method SERIALNO MET File SERIALNO 1 HA Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 57 Attenuation scroll bar Adjusting the attenuation The full sca
58. ed 1 2 Select Start Arun window will appear which prompts for information regarding the automated run sequence See Figure 53 In the Run ID space enter a name for the data which is to be collected and stored This may be a maximum of eight characters and DOS illegal characters are forbidden See page 162 for a list Specify the Number of Runs If the number of runs is greater than one the run number is appended to the Run ID as a data file extension for example run 1 run 2 etc Specify the Time Between Injections in seconds Note what the delay interval is between injections make sure this interval is long enough to accommodate the run time time between runs and any necessary printing time Check if the data is to be Saved and or Printed after each run Make sure that printing selections have been made in Print Options before selecting Print here Check if the data is to be output in a DIF or PRN format The DIF format saves external standard report peak name and amount information as ASCII characters delimited by tabs EXCEL format The filename used is the Run ID followed by the extension DIF The PRN format saves the peak name and amount report information as ASCII characters delimited with quotes and numbers delimited by commas Lotus format The filename used is the Run ID followed by the extension PRN Check Extended if you would like to include the area and retention time in the information saved t
59. ed and unnormalized data is then displayed on the screen The example program then goes back to waiting for a message from EZChrom 200 400 169 Dynamic Data Exchange DDE EZChrom DDE server EZChrom DDE server The EZChrom 200 400 control interface is comprised of a Dynamic Data Exchange DDE server and acompanion Dynamic Link Library DLL EZChrom 200 400 accepts commands from the DDE client and returns analysis results through the DLL Commands Responses Parameters EZChrom e Figure 107 Server support The DDE server supports a single item The application name is EZChrom the topic name is Execute and the item name is Run All communication takes place over this single link Commands are poked to the server by the client The server responds to the command by sending the response back to the client Command parameters are passed through the DLL Furthermore the results of the chromatographic analysis are stored in the DLL for retrieval by the client The DLL contains all the functions necessary to access the results Functions also exist for setting command parameters Commands Name OpenMethod Parameter Method name Remarks This command will cause EZChrom 200 400 to open the method file that is passed as the parameter The method name can be either a fully qualified path to a method file or if only the name is given the file is assumed to reside in the current method directory 170 Name
60. emperature box and enter a value 10 degrees higher than that shown The settings for channel B are displayed by clicking the cursor in the small circle labeled B at the top of the instrument status window Change the run times for the two channels to 50 seconds Air elutes quickly on all columns so a long run time is unnecessary Change the sample time to 10 seconds This needs to be done in only one channel the other channel is automatically updated Reduce the injection times for both modules to 20 milliseconds variable loop injectors only The main components in air Og No are so concentrated that very little sample is needed to produce a large signal Using a short inject time also reduces the risk of column overload Make sure the detector filaments and autozero are ON for both channels Set the sensitivity on both channels to Low Again No and O are present in such large amounts amplifier overload is a concern Close the Instrument Setup window by clicking on OK or pressing lt Enter gt Send the revised instrument settings to your GC by selecting the Send Current Method command which resides under the Instrument menu Click on Ok when the confirmation window appears If an error message appears click on Ok or press lt Enter gt Then refer to Installation Troubleshooting resetting the COM port using the GC Verification program found in the addendum to the instrument manual Check to see that the increase in c
61. es will then be displayed 3 Double click on the appropriate peak name on the list or single click on a peak name and select OK Comments The popup window automatically highlights the last peak chosen Asymmetric retention time windows can be created by placing the vertical cursors asymmetrically about the selected peak PKWD sub Events Peak Width Purpose Used to set the data bunching rate Syntax 1 Select a peak with the vertical cursors 2 Select PKWD or type P 3 Review adjust the event values and choose OK Comments Peak width adjusts the bunching of data points to optimize peak detection This mechanism combined with slope sensitivity and fine slope sensitivity acts as a noise filter 89 Menu Reference Channel AJB commands SLPSEN sub Events Slope Sensitivity Purpose Defines the average slope of the baseline in microvolts per unit of time Syntax 1 Choose a segment of the baseline with no peaks 2 Select SLPSEN or type S 3 Review adjust the event values and choose OK Comments Generally you should adjust the time for the first SLPSEN event to zero seconds so that the peak search starts with the correct SLPSEN value from time zero When the slope between two data bunches is greater than the threshold SLPSEN value a peak start is defined When the absolute value of the slope between two data bunches falls below the threshold SLPSEN value a peak end is defined TAN sub Events
62. essure transducers Disconnect the helium carrier at the fitting on the rear panel of the GC do not just turn it off at a valve and click the OK button If the number of retries becomes excessive more than 10 click Cancel Searching for a GC Resetting CHP Offset Explanation Since the stored column head pressure zero values have been lost it is necessary to re zero the column head pressure Action Please disconnect the Helium Carrier gas supply from the back of the MTI GC and click the OK button Status Retries Figure 103 Searching for a GC window GC Verification automatically locates the first GC connected to your computer by checking each serial port in turn for a device that behaves like a GC The window shown in Figure 103 is displayed to let you monitor that process Click OK to continue Status Restoring GC configuration Status Restoring MTI GC Configuration Figure 104 Status window 157 The GC Verification Tool Compatibility and computer system requirements If the GC s configuration needs to be restored from the saved configuration record the message shown in Figure 104 will be displayed Validate Instrument ID Validate Instrument ID The GC appears to be working correctly but there is no record of it in this system If you re sure the GC is properly setup we can create a record for it l Question Serial Number
63. evel overlapping peaks 66 Menu Reference EZChrom 200 400 menus and commands Method Main menu See Figure 40 Purpose Allows access to the tables and settings which control GC operation and data analysis Lock Unlock Instrument Setup F1 Peak Table F2 Peak Calibration F3 Calibration Setup F4 Timed Events F5 Display Options F6 Print Options F7 Method SERIAL MET File SERIAL 1 SAUE Instrument Data Analyze Math Calib Start Help Figure 40 Method menu Syntax Select Method or type lt Alt gt M Calibration Setup sub Method Purpose Allows customization of the calibration sequence Syntax Select Calibration Setup or type C 67 Menu Reference EZChrom 200 400 menus and commands Comments The following options are available Channel Selects the module whose calibration sequence is to be modified The module chosen will be indicated by a bullet in the circle Peak Attribute The choices are Area and Height This parameter forces EZChrom 200 400 to calibrate on either peak area or maximum peak amplitude Calibration Fit The choices are Point and Linear This allows point to point or linear extrapolations between different calibration levels Number of Runs A amp B Allows the user to specify the number of runs for each calibration level For multi run calibrations an average value for the peak area or amplitude is calculated and entered into the peak calibration table Uncalibrate
64. fication windows Cycle GC power Cycle GC Power a s It is necessary to cycle the GC s power once or twice to re enable it DCO Figure 95 Cycle GC power window When it is necessary to cycle the GC s power i e turn it on and off the window in Figure 95 will be displayed First perform the requested action turn power on or off then click OK Click Quit to terminate GC Verification Pay close attention to the text in the Request box Have HP GC setup disk Have MTI GC Setup Disk 4 Figure 96 Have GC setup disk Window If a configuration record for a GC cannot be located on your computer GC Verification will ask if you still have the setup disk Click Yes if you do No if you don t or Don t Know if you are unsure GC Verification will tell you what you should do next 153 The GC Verification Tool Explanation of GC Verification windows Instrument ID Instrument ID Explanation The MTI GC has forgotten its name Please enter the serial number of the GC in the box below The serial number is located on a sticker on the back of the unit Figure 97 Instrument ID window If the GC has lost its serial number GC Verification will display this window Type in the serial number as it appears on the label on the back of your GC and click OK Click Quit to terminate GC Verification Invalid or unknown GC ID Invalid or Uknown MTI GC ID
65. g order This allows the software to correctly plot the calibration data Peak Table sub Method Purpose Contains compound names and elution times which allows EZChrom 200 400 to properly identify and quantify integrated peaks It also provides the option of grouping multiple peaks which elute in a user specified window User defined response factors can be defined and referenced here Syntax Select Peak Table or type E Comments In most cases the only information that needs to be entered in this table are peak names concentration units and Level 1 Cal Amounts Retention times can be entered graphically The Peak Table contains the following information Peak Name In this portion of the table the names of the compounds which are to be analyzed are entered The peak names are entered for each component by typing them in When an integrated peak falls in a defined retention time window it is assigned the name linked to that window 73 Menu Reference EZChrom 200 400 menus and commands Retention Time This is the amount of time it takes for the apex of anamed peak to elute from the column The retention time can be entered graphically or with the keyboard In the Calibration Setup table there is an option to update the retention time at the end of a run If this is selected and the retention time changes then the retention time and the retention time window will be updated Retention Time Window If a peak apex lies
66. g the Windows Print Manager will decrease the amount of time required to print however multiple print jobs cannot be selected 92 Menu Reference Channel AJB commands Reports Main menu See Figure 46 Purpose Reveals the menu of data reports available for display Chan A 100 sec Attn 2048 intaiiems Events Display Print Help Area Normalization External Standard Figure 46 Reports menu Syntax Click on Reports or type lt Alt gt R Comments To close a report double click on the top left corner of the report display or type lt Alt gt spacebar and type C Reports may be left on the screen during data collection allowing the user to monitor data analysis during an autorun Area report sub Reports Purpose Displays a report showing the number of peaks and their retention times raw areas and percent of total area Syntax Click on Area 93 Menu Reference Channel A B commands Normalization report sub Reports Purpose Displays areport of peaknames retention times normalized amounts units and the percent standard deviation Syntax Click on Normalization Comments Amounts are normalized over the channel selected Min Max Mean and RSD are arecord of the repeatability of sample analysis over a set of runs External Standard report sub Reports Purpose Displays a report of peak names retention times amounts and units Syntax Click on External Stand
67. ged for different applications When you need more information regarding operation or use of specific features in the software please refer to Chapter 6 for the menu reference 50 Technical Reference Technical Reference Data sampling The analog signal generated by the detector of the gas chromatograph is digitized by an A D converter in the GC The A D is a 24 bit precision voltage to frequency converter The detector voltage is digitized at a rate of 100 points per second Each data point requires 4 bytes of disk space if stored A 60 second run for a dual module unit will generate 12 000 data points and requires 48 000 bytes of disk space for storage 60 sec channel x 100 pts sec x 2 channels x 4 bytes pt 48 000 bytes The digital data is made available through the serial RS 232 port Data transfer occurs as it is collected Peak detection Peak width The data output rate for an Agilent micro GC is 100 points per second per channel For most peaks ina chromatogram this is far more data then is required to get an accurate integration To reduce processing time data points are therefore averaged into data bunches by using the PKWD timed event Peak detection is then performed on the bunched points In EZChrom 200 400 the number of bunched points is divided by 5 to produce a peak width value Example 4 bunched points divided by 5 equals 0 8 PKWD As a general rule sharp early eluting peaks are best detected wit
68. h PKWD values of 0 2 Late eluting broad peaks may require PKWDs of 0 4 0 8 or even 1 6 See Chapter 7 for details of properly setting PKWD values Setting a PKWD event 52 Technical Reference Baseline correction graphically may generate non integer values These non integer values are rounded down to the nearest multiplier of 0 2 when EZChrom 200 400 analyzes a chromatogram Slope sensitivity The slope of the signal the rate of change of the detector voltage is used by EZChrom 200 400 to detect peaks A slope value or first derivative is calculated one bunched point to the next The PKWD determines how frequently the slope is calculated Narrow peaks need small bunch sizes so that abrupt changes in slope can be quickly detected Wide peaks however require bunches large enough to allow small changes in amplitude to be detected Peaks are detected when the slope value between two data bunches is greater than the SLPSEN slope sensitivity value defined in the Timed Events table The optimum slope sensitivity usually occurs when it is equal to twice the background noise level Fine slope sensitivity Fine slope sensitivity FINE SLPSEN is related to slope sensitivity it is the second derivative of the chromatogram displayed The fine slope sensitivity value corresponds to the change in the slope It is therefore a threshold for the change in steepness of a chromatogram This threshold is used to determine the start and stop of
69. habetically listed by window title About GC verification A Po Copyright Figure 92 About GC verification window This window is shown when you click the About button in the GC Verification main window It displays the path name of the executable file its revision the date the program was created and the owner of the copyright 151 The GC Verification Tool Explanation of GC Verification windows Call Technical Support Call Technical Support Explaination our WTI GC has unresolved problems that will interfere with proper operation Please call MTI Technical Support at 510 490 0900 to get the problem resolved Subject MTI GC Verification Figure 93 Call technical support window A window like Figure 93 is drawn whenever GC Verification encounters a problem that it cannot fix Call Agilent Technical Support and give them verbatim the message displayed in the Subject box the message will vary with the nature of the problem Checking for error conditions Explanation The GC has outstanding error conditions Do you want to fix them Checking For Error Conditions al Figure 94 Checking for error conditions window The window shown in Figure 94 is displayed if GC Verification finds that the GC has error conditions Click Yes to attempt to fix the errors or No to terminate GC Verification 152 The GC Verification Tool Explanation of GC Veri
70. he first cal gas standard 2 Select Calib 3 Enter the Calibration Level 4 Select OK 5 Start the GC Calibration will begin immediately Prior to sampling the EZChrom menu title bar will display the following message Calibration level X Runs left Y Where X the calibration level selected under Calib Y the number of calibration runs entered in the Calibration Setup Repeat the preceding steps for each calibration gas standard It is critical to remember that the cal gases must be calibrated in order of increasing concentrations This is necessary not only to match the previously entered Calibration Amounts but also to allow the plotting algorithm to function properly the plotting routine does not automatically sort area amount pairs For multi component cal gases it may be impossible to calibrate all compounds in order of least to most concentrated In this case it will be necessary to manually sort the area counts in the Peak Calibration table 109 Quick Reference Print options Print options To print reports and or chromatograms during an autorun sequence the Print Options table See Figure 52 must be filled in By checking the Print option in the Start window the selected material will be printed during the time between runs Remember enough time must be allowed for the printing process to be completed prior to the next run F Chromatogram O Full Scale O Zoomed r Reports O Area O
71. hey will know how to help you The contents of the Subject box will vary with the precise nature of the problem so it is probably a good idea to contact Agilent Technical Support while the window is on your screen so that you can read it back verbatim What happens if your GC is OK but the configuration record is missing This can happen if you use different computers with your GC or if the setup disks that came with your GC have been lost 146 The GC Verification Tool Typical sessions The first window is the Introduction Window shown in Figure 86 MTI GC Verification Explanation e will check out your WTI GC to verify that it is OK and will perform properly If there is a problem we will guide you through the necessary procedures to restore the GC to proper operating condition Is the GC connected Request If you have not done so please connect your WTI GC to one of the computer s serial ports Figure 86 GC verification window Connect your GC and click Yes GC Verification checks each serial port on your computer system for an M200 During this time a window like Figure 87 is displayed 147 The GC Verification Tool Typical sessions MGC Explanation e re checking out each serial port to locate your MTI GC e ll use the first one we find Status Po Ifno GC is found an error message is displayed in the status box and when you click OK GC Ver
72. ible to enter timed events manually for example as we made entries in the peak table it is more accurate to graphically set these events on a real data set At this point it is time to collect an actual data set which will be stored and for which optimized Timed Events tables will be constructed Collecting data 1 Select the Start menu A run window should appear See Figure 25 2 Entera Run ID forthe air sample whichis to be run This may be a maximum of eight characters with no DOS control characters See page 162 for a list of DOS illegal characters 38 Sample Session Collecting data 3 Enter 1 for the Number of Runs Run ID Number of Runs 1 999 inf 0 Time Between Injections secs 0 O Wait For External Start Save LJ Print DIF Save PRN Save Extended User Program Cancel Recall Figure 25 Run window 4 Select the Save box by clicking on it If any other boxes are selected as evidenced by an X appearing in the box you may deselect them by clicking on them 5 Click on Start or press lt Enter gt to begin data acquisition After the RUN window disappears the vacuum pump will start and run for the amount of time you specified in the Instrument Settings window A small amount of air sample is injected onto the sample columns then EZChrom 200 400 proceeds to draw the chromatograms for channels A
73. ic operations e Setting Up a Run e Developing a Method e Calibrating a Method 178 Setting up a run Method menu 1 Inthe Method menu choose Instrument Setup to manipulate instrument settings Instrument Setup Window 2 Adjust instrument parameters for optimal peak separation for both Channel A amp B Click OK when adjustments are complete Dynamic Data Exchange DDE Setting up arun New Open Save Save As Print Lock Unlock Instrument Setup F1 Peak Table F2 Peak Calibration F3 Calibration Setup F4 TimedEvents F5 Display Options F6 Print Options F7 SETTE Instrument Data A Instrument Setup ix Channel oA CB Column Temperature 46 Run Time sec 100 Sample Time sec 10 Inject Time msec 50 Detector Filament C Off On Detector Autozero C Off On e c Detector Sensitivity Low Med High Cancel 179 Dynamic Data Exchange DDE Setting up a run Instrument menu 3 Inthe Instrument menu choose Send Current Method to implement recent changes Send current method window 4 Click OK to Send Current Method Instrument menu 5 Choose Status in the Instrument menu to observe temperature and pressure stabilization Start menu 6 Choose Start to setup a run Method iSite Data Analyze Math Status Send Current Method Receive Method Instrument ID Hardware Setup Instrument 7 Sen
74. ification returns to the Introduction Window shown in Figure 88 Searching for an MTI GC Explanation e re checking out each serial port to locate your WTI GC e ll use the first one we find Status No MTI GC appears to be connected Figure 88 Searching for a GC window 148 The GC Verification Tool Typical sessions If a GC is found the window displays its serial number in the Status box and when you click OK GC Verification proceeds with checking the GC Figure 89 Searching for an MTI GC E e re checking out each serial port to locate your MT GC e ll use the first one we find Found MTI GC 18 connected to COM1 Figure 89 Searching for a GC window oe If your GC appears to have no errors but the verification program can not locate a configuration record for the GC you will see a screen like the one in Figure 90 gt Validate Instrument ID Explanation The GC appears to be working correctly but there is no record of it in this system If you re sure the GC is properly setup we can create a record for it Question O Are you SURE that the GC is OK Figure 90 Validate instrument ID window 149 The GC Verification Tool Terminating GC Verification Tool At this point it is important to realize that the actual configuration record of the GC cannot have been verified because the configuration record is missing The GC however does appear
75. in Area Invert Peak RT and AT Window Figure 43 Events menu 84 Menu Reference Channel A B commands Events Main menu See Figure 43 Purpose Allows most Timed Events to be set graphically Syntax 1 Select a region or point of interest with the vertical cursor s 2 Select Events or type lt Alt gt E 3 Select the appropriate Event 4 Inspect the time and value given in the confirmation window and make any necessary alterations 5 Select OK to add the event to the timed events table Comments Refer to page 22 to page 25 for instructions on selecting a region of a chromatogram with the vertical cursors BL AT sub Event Baseline At Purpose Resets the peak search from a user selected point Syntax 1 Choose a start point by freezing a single vertical cursor just to the left of a peak where you wish the peak search to reset 2 Select BL AT or type A Comments For this timed event only the left cursor needs to be set BL AT only requires a start time 85 Menu Reference Channel AJB commands BLH sub Event Baseline Horizontal Purpose Forces the baseline to be drawn horizontally from the start time selected until the stop time selected Syntax 1 Choose a baseline segment with the vertical cursors 2 Select BLH or type H Comments The horizontal baseline is drawn forward only not backward BLV sub Event Baseline Valley Purpose This command
76. ingle headed cursor may now be used in any of the ways previously described 10 To remove the vertical cursor from the screen click on Display in the appropriate channel A or B window then click on CURSOR 24 Getting Started Graphic manipulation with a mouse 11 Practice selecting various portions of the chromatogram At first you may find it difficult to obtain the desired cursor in an appropriate frozen or unfrozen state Don t get frustrated after a short time the manipulation of the mouse clicks will become habit Crosshair This cursor appears when a report is displayed and the single headed cursor is moved into the report window No commands or manipulations are possible with this cursor 1 Using the procedure described on page 16 select the Reports menu in either channel A or channel B See Figure 17 2 Select any of the reports available Chan A 100 sec Attn 2048 j maues Events Display Print Help rea Normalization External Standard Figure 17 Reports menu 3 Move the double headed cursor into the report window You should see the single headed arrow change to the crosshair cursor See Figure 18 25 Getting Started Graphics manipulation without a mouse Chan A_80 sec Attn 2048 ae SS Chan B 100 sec Attn 2048 ae Reports Events Display Print Help Reports Events Display Print Help CON f lol Amount Units RT Min Max Mean SD Time
77. ions to 0 seconds a fF WN a Select the Recall command EZChrom will then begin recalling and reanalyzing the specified set of chromatograms The program always starts with the first file extension If the 1 file or any file between 1 and the number of runs you entered is missing an error message will be displayed and RECALL will abort During a RECALL all selected operations in the START window can be active i e Print Save Transferring methods Once a valid Method has been established it is important to give this information to the GC EZChrom automatically sends the current Method to the instrument when Start is selected To guarantee that the columns have reached the correct operating temperature prior to a run it is best to transfer the Method well before the next analysis To send an updated method to the GC 1 Select Instrument 2 Select Send Current Method 3 Select OK 115 Quick Reference Transferring methods In order to check the current instrument setup in the GC Methods can be received fromt he GC 1 2 3 Select Instrument Select Receive Method Select OK Column Temp CCF Pressure ps Aulo Zero mp Detector Alament Inlet Heaters Battery 100 Firmware Version 17 5 Figure 55 Instrument status window Once a Method has been sent it is a good idea to check the instrument status to determine when column temperatures have stabilized This is done with the S
78. is necessary to cycle the GC s power once or twice to re enable it Please turn the GC off Figure 79 Cycle GC power window Unplug the GC first and then click the OK button Now you need to turn the GC back ON as requested in Figure 80 Cycle GC Power Explanation It is necessary to cycle the GC s power once or twice to re enable it Please the GC back on Figure 80 Cycle GC power window Plug the GC back in and then click the OK button 142 The GC Verification Tool Typical sessions Because of the way certain options are implemented it will probably be necessary to cycle the power again GC Verification will know if this is the case and if so it will ask you to turn the GC OFF and then back ON again When the sequence is done you will see the window illustrated in Figure 81 Cycle GC Power It is necessary to cycle the GC s power once or twice to re enable it Request cco Figure 81 Cycle GC power window Click OK If there were problems with memory that might have compromised the column head pressure CHP offset data stored in the memory you will see the window displayed in Figure 82 143 The GC Verification Tool Typical sessions Resetting CHP Offset Explanation Since the stored column head pressure zero values have been lost it is necessary to re zero the column head pressure Action Please disconnect
79. l received operation open the Instrument Setup table located under the Method menu Send Current Method sub Instrument Purpose Sends the current Method to the GC Syntax Select Send Current Method or type S Comments A method is sent automatically when Start is selected Therefore the GC will always have the current Method in memory before it starts to run However if the column temperature has been changed it is important to send the Method a short time prior to arun so that the GC module can equilibrate 65 Menu Reference EZChrom 200 400 menus and commands Status sub Instrument Purpose Allows monitoring of certain instrument settings between runs Syntax Select Status or type T Comments Status can only be monitored during idle time While the GC is in a run sequence the data collection rate is too high to allow status monitoring as well as data acquisition Math Main menu Purpose Subtracts a user selected chromatogram from the currently displayed chromatogram After analyzing the reports and graphical display are updated Syntax 1 Select Math or type lt Alt gt T 2 Select Catalog or enter a path and file name to select a chromatogram This chromatogram will be subtracted from the currently displayed data set 3 Select OK to initiate the subtraction Comments This feature could allow subtraction of large solvent peaks allowing easy identification and integration of low l
80. l then ask if you want to save changes Click on Save The command Save File Name As will appear Enter any eight character name appropriate for the file DOS illegal characters not accepted See page 162 for a list of these To build a method from scratch do the following 1 Select the New command which is listed in the Method menu Figure 20 This resets the timed events peak and calibration tables If you have been practicing cursor moves and want to begin a sample session click on Method then New and the following window will appear See Figure 21 Do not save changes to the default Method Method x 2 Current method has changed Save changes 3 No Cancel Figure 21 Save method changes window 2 Select the Instrument Setup command under the Method menu A window will be displayed which lists the chromatograph instrument settings from the last stored Method See Figure 22 31 Sample Session Building a method Sample Time sec 10 Inject Time msec Detector Filament cof On Detector Autozero C Off amp On Detector Sensitivity C Low Med High c c Figure 22 Instrument setup window A description of the settings found in this window is as follows Column temp C This is the temperature at which the column and detector are kept during and after a run When this setting is changed time must be allotted for equilibration of
81. le chromatogram displayed in the upper portion of the window may be adjusted by scrolling the display attenuation To adjust the full scale magnification 1 Move the cursor onto the scroll bar at the right side of the upper chromatogram display See Figure 57 2 Select the up or down arrow of the scroll bar to change the attenuation value The up arrow increases magnification the down arrow reduces it 3 Observe the change in the upper display 120 The GC Module Change Tool The GC Module Change Tool The GC Module Change Toolis provided to allow you to modify or correct several GC instrument configuration parameters that are specific for a particular module i e injector column and or column heater specific parameters With this program you can alter or swap GC module parameters in both the GC firmware and in the computer s configuration record i e HP INI The configuration parameters that can be modified through this Program include the following items e Column temperature offset e Column temperature scale e Maximum column temperature limit e Fixed or variable loop volume injector When shipped from our factory your GC was loaded with the GC configuration file appropriate for the particular GC modules installed in your instrument However it may be necessary to change a GC s configuration and thus use this Module Change Tool when you do any of the following 1 Install anew GC module or swap po
82. librated Peaks RF This option allows the assignment of a blanket response factor to all unidentified peaks This response factor is multiplied by the area of the unknown peaks to give an amount value The default is Zero Multiplication Factor This is a multiplication factor that is applied to all quantitated peaks both in calibration standards as well as samples This feature is useful when a concentrator or dilutor is used in the sampling system The default is One Update Retention Time After Calib and or Run This allows the user to update the retention times of the components listed in the peak table after each calibration and or run The default is No 105 Quick Reference Multi level calibration Entering calibration amounts i a e ON To enter the concentrations from your calibration standard gases into your Peak Calibration Table See Figure 51 Select Method Select Peak Calibration Select Channel A or B Enter the amount information for each level using Page Down as necessary The calibration amounts must be entered in order from least to most concentrated A level one calibration will require only one entry per compound To switch compounds click on Prev or Next The area information can also be entered now manually or later while performing a calibration on stored or newly acquired data To plot the new calibration points click on the Plot button The slope of this plot defines the response fac
83. ll be displayed when your GC is OK and either there were no problems or all problems have been fixed Click OK to terminate GC Verification 155 The GC Verification Tool Explanation of GC Verification windows Re Install the GC support software Re install the MTI GC Support Software Explanation In order to verify the configuration of an MTI GC certain support software has to be installed on each computer that you will use the GC with Please insert the MTI GC setup diskette in drive A or B and run the program named Setup EXE When you are done please re run this program to verify the installation Figure 101 Re Install the GC support software window If there is no configuration record on file but you have an GC Tools diskette for the GC GC Verification will display this window to ask you to set up the GC on the computer you are currently using Resetting CHP Offset Resetting CHP Offset Explanation Since the stored column head pressure zero values have been lost it is necessary to re zero the column head pressure Action Please disconnect the Helium Carrier gas supply from the back of the MTI GC and click the OK button l Status Retries Figure 102 Resetting CHP offset window 156 The GC Verification Tool Explanation of GC Verification windows If necessary the window in Figure 102 walks you through resetting the column head pr
84. lly the peak will be successfully integrated Repeat the above steps for both channels and all subsequent peaks which are still incorrectly integrated remembering to double the value for each successive PKWD See page 52 for additional information on the adjustment of PKWD 100 Quick Reference Quick and easy method development At this time you may also wish to extend the Intg Off event to include solvent or composite peaks which are not of interest Set the Retention Times and Retention Time Windows graphically as described in Chapter 4 for all peaks of interest in both channels If you now reanalyze the data the External Standard report should display the names and area counts for all integrated peaks in the chromatogram Select the Calib command from the lower menu bar and run the GC Data will be acquired and a calibration will be done Inspection of the External Standard reports should show all compounds which were in the calibration gas and at the correct concentrations The Method is now complete Save the Method to the hard drive and if necessary lock it 101 Quick Reference Method locking Method locking Locking a Method protects it from being inadvertently modified A locked Method may be modified during a session but these changes will not be stored at the end of the session unless a password is given To Lock a Method Select Method Select Open Select the method that is to be locked Select
85. me parameter should be zero for all these events The value for the INTG Off event in seconds should be set to 1 5 seconds This turns the integration off during the first part of the aquisition where baseline artifacts are 98 Quick Reference Quick and easy method development observed due to sample injection The valwes for the SLPSEN and FINE SLPSEN events are dictated by the detector sensitivity for a particular channel Channel a OB EVit Event Time Value E 1 SLPSEN 0 000 10 000 Events 2 INTG Off 0 000 5 500 Ogni 3 FINE SLPSEN 0 000 200 000 Spike BLA 4 FINE SLPSEN 7 500 5 000 5 PKWD 11 000 1 000 INTG Off O BLY 6 PKYYD 20 000 2 000 SLPSEN BLH 7 PKWD 42 000 4 000 8 SLPSEN 65 230 16 000 FINE SLPSEN TAN 9 PKWD 76 330 8 000 PKWD Invert Min Area Time 08 020 Value 1 Cancel Delete Change Add Figure 49 Timed events table The most accurate way of setting SLPSEN and FINE SLPSEN is graphically see Chapter 5 The following table provides suggested initial values for SLPSEN and FINE SLPSEN Sensitivity SLPSEN value FINE SLPSEN value Low 10 5 Med 50 30 High 100 75 99 Quick Reference Quick and easy method development If necessary adjust the instrument setup parameters and column pressures so all of the desired peaks are well resolved and on scale Detector saturation is evidenced by the tops of peaks rising above
86. menu for the appropriate channel Channel A 6 From a list of components darken the 1 oxygen name of the peak that has been graphically chosen Click OK Repeat steps 5 and 6 until all peaks have been named After all peaks have been identified Save the method in the Method menu 184 Dynamic Data Exchange DDE Calibrating a method Calibrating a method Method menu N ew 1 Choose Calibration Setup in the Method Open Menu Save Save s Print Lock Unlock Instrument Setup F1 Peak Table F2 Peak Calibration F3 IimedEvents F5 Display Options FE Print Options F7 SEE Instrument Data Ane Calibration Setup window 2 Define calibration parameters for each channel Specifying Update Calibration vYes Ono calibrationfitandnumberof Pek Attribute area Height runs is usually sufficient Click OK Calibration fit Point Linear Number of Runs A amp B Begin Calibration at Run Uncalibrated Peaks RF 0 00000000 Multiplication Factor ill Update Retention Time After CO Calib C Run Ca il 185 Dynamic Data Exchange DDE Calibrating a method Method menu 3 Choose Peak Calibration under the Method menu to enter calibration standard amounts Peak Calibration window 4 For each component enter calibration standard Amount in ascending order for each level of calibratiion The calibration Amountcanalso be entered in the Pe
87. n Calibrating the method Calibration Calibration Level fa Figure 36 Calibration window 3 The EZChrom bar will then display Calibration Level 1 and Number of Runs Left 1 For purposes of this sample session a level 1 calibration is all that is necessary 4 Select Analyze from the lower command bar EZChrom will perform an analysis and assign the peak areas to the amount values you entered into the Level One Cal Amount spaces in the peak table 5 Again select the Reports menu and open the External Standard reports for channels A and B They should display the peak names in order of elution time but the values should now be readable as standard numbers 6 Select the Method menu and the Save As command There will be a prompt See Figure 37 which requires you to enter aname for the method you have just constructed Remember only eight characters may be used in an ID and DOS illegal characters are forbidden Save File Name As C A MTiezchrom 200 met EXAMPLE MET Figure 37 Save file name as 49 Sample Session Calibrating the method Use the extensions met when naming method files to distinguish them from data and instrument ID files This concludes the EZChrom 200 400 sample session The examples in this sample session have been provided to illustrate the ease of use of the EZChrom 200 400 software The integration timed events used when setting up a particular Method may need to be chan
88. n which case use over 100 milliseconds 97 Quick Reference Quick and easy method development Channel A OB RT RT Level 1 Pkno Peak Name Time Window CU BP CalAmount RRF Peak 1 160 00 0 000 1 000 0 000 O For concentration levels between 10 and 100 use Low sensitivity For levels from 500 ppm to 10 use Medium sensitivity For levels less than 500 ppm use High sensitivity Set the column head pressures for the individual modules Pressures of between 15 and 20 psi are reasonable in most applications for the majority of columns Open the Peak Table See Figure 48 and enter the names of the compounds for which you wish to screen If you are unsure of which column is appropriate for analysis ofa given compound call Agilent Technical Support for assistance Peak Table Fron on oe nt Joon C foo Sooo gt 1 000 ooo fo iT 0 o foo foom fe f f ro foam 160 00 0 000 1 000 0 000 Cancel Delete PgDn Figure 48 Peak table In the Level One Cal Amount boxes enter the concentrations of each compound in your first external calibration gas standard Attach your sample or calibration gas to the sample inlet and run the GC As the datais being acquired observe the number resolution and amplitude of the peaks in the chromatogram Open the Timed Events tables See Figure 49 and add a SLPSEN FINE SLPSEN and INTG Off event to both the channel A and B tables The ti
89. nalyze Math Calib Start Help Program Manager Figure 14 Reduced channel A window Vertical lines Use these cursors as mobile reference points to observe peak amplitude and retention times They are also extremely useful in simplifying the selection and definition of integration parameters and in the peak identification routine 1 Place the single headed arrow cursor in either the channel A or B lower window 2 Click the right mouse button A single vertical line should appear See Figure 15 When the mouse is moved to the left or right the vertical cursor should move accordingly 22 Chan A 100 sec Attn 2048 f Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help Getting Started Graphic manipulation with a mouse Program Time sec 017 890 Amp uY 23284 Method btu met File btu 1 Method Instrument Data Analyze Math Calib Start Help Manager Figure 15 Using the single vertical cursor When using a laptop computer the mouse must be moved slowly for the vertical line to remain visible 3 Scan the cursor across the chromatogram and observe the string of text in the lower display window You should see the time and amplitude vary Dragging the mouse to the right should result in a larger time value This is because data is collected from time 0 left to right The value of the amplitude is the actual instrument output in micro
90. nd the computer s serial port turn the GC on start the GC Module Change Program described in Chapter 2 and click Change button A as shown in Figure 60 The program will ask you which module you have affected with the change of position as shown in Figure 63 Figure 63 shows a top view of the GC with the top cover removed displaying the position of modules A and B Which Module Which module do you want to change E lt i Figure 63 Which module Window 127 The GC Module Change Tool GC Module Change Tool for a Quad instrument Click the Module A or Module B button depending upon which module s location has altered and then click OK Use the diagram on the right hand side of the window to determine which module you have replaced and wish to update with the correct configuration file You can also click on the diagram of the GC clicking on the upper half selects module B and clicking on the lower half selects module A When using GC Module Change Tool for a Quad instrument make sure only one side of the GC is connected The program will see the GC as an M200 P200 having modules A and B If the C D side is connected module A represents module C and Module B represents module D GC Module Change Tool for a Quad instrument The GC Module Change Tool allows you to alter or swap GC Module parameters in the GC and the HP INI file configuration record when a physical GC module is repl
91. ntion times graphically 4 Repeat the procedure for each successive peak in the channel A chromatogram choosing the appropriate name from the list 5 Repeat the procedure for the channel B chromatogram 6 Select the Analyze command from the lower menu bar EZChrom will analyze the chromatogram according to the parameters just set Zoom in closely on each peak to assure that the entire peak is within its predetermined hashmarks If the peak does not have an upward hashmark at its beginning and a downward hashmark at its end it has not been integrated Chan A 100 sec Attn 2048 intiaiiems Events Display Print Help Areas Normalization External Standard Figure 33 Reports menu J Channel B EXTERNAL STANDARD Report Name Amount Units RT Min Nitrogen 25 576 2 320 25 576 Methane 88 118 2 760 88 118 co2 30 012 8 560 30 012 Ethane 35 033 14 240 35 033 H2s 0 000 0 000 0 000 Propane 10 111 71 520 10 111 Figure 34 Uncalibrated external standard report 7 Open the External Standard reports for channels A and B by clicking on Reports then on External Standard See Figure 33 They should display the peak names in the order of elution time and have large amount values for all of the peaks listed in the reports This is because the method is not yet calibrated See Figure 34 47 Sample Session Calibrating the method 8 Ifany of the peaks in the report have an amount of zero See Figure 35 and h
92. o DIF or PRN files 112 Quick Reference Analyzing the data 8 Select Start to begin a run 9 After completion of the run the chromatogram is automatically analyzed Analyzing the data All of the data collected by EZChrom 200 400 is kept in an active buffer and saved to amass storage device at the user s request All of the analysis and reporting activities are handled according to the current Method parameters The analysis process does not alter the raw chromatographic data Methods may therefore be altered and adjusted and chromatograms reanalyzed until an optimal Method is constructed An analysis is always done when achromatogram is first acquired To reanalyze a stored dataset 1 Select Data 2 Select Open 3 Double click the left mouse button on the desired datafile 4 Select Analyze Upon completion of the Analyze step the chromatograms will be displayed in the split screen labeled Channel A and Channel B All reports are updated and if specified will be printed and saved Now the graphics can be manipulated reports can be displayed the Method can be adjusted and data can be reanalyzed until the results are satisfactory 113 Quick Reference Automated sequences Automated sequences Autorun An Agilent GC can be set up to run automatically from the Start window The chromatograph can be set to run continuously i e for process control applications or for a specified number of times The p
93. olumn temperature has been received and implemented by the GC To do this select the Instrument Status command under the Instrument menu If the temperature is correct click on Ok If the temperature setting is not correct return to Instrument Setup confirm that your entries are correct and Send Current Method again 34 Sample Session Building a method RT RT Level 1 Pkno Peak Name Time Window CU BP CalAmount ARF Peak 1 160 00 0 000 1 000 0 000 O Frsn 0 0 5 rato Joo fo o foo fomo ion foon fo i 0 C fon fom fa froo fonw 160 00 0 000 1 000 0 000 12 Figure 23 Peak table for a new method Open the Peak Table which is listed under the Method menu The Peak Table See Figure 23 contains all the information on the types of compounds in a sample and the amount of time it takes for these compounds to pass through the sample column A table is provided for both channels A brief description of the peak table begins with Peak name The names of the compounds to be analyzed are entered in this portion of the table The peak names for each component are entered by typing them in maximum 20 characters When an integrated peak falls in a defined retention time window it is assigned the name linked to that window Retention time Retention Time is the amount of time it takes for the crest of the named peak to elute from the column The retention time can be entered graphic
94. om be reinstalled if the original GC COM port designation is incorrect 63 Menu Reference EZChrom 200 400 menus and commands Instrument ID sub Instrument Purpose Provides a table in which column and carrier gas information can be stored Syntax 1 Select the Instrument ID command 2 Select the Edit option 3 Enter an instrument ID along with the column types and carrier gas used in your GC 4 Select OK 5 Select the Instrument ID command again 6 Select the SAVE option 7 Enter an ID for the file just created Comments The Instrument ID file last opened will be automatically loaded when EZChrom 200 400 is restarted The Instrument ID file is tied to report and condition window printouts The Instrument ID column type and carrier gas sections of these printouts will display the information you entered into the Instrument ID file The file is also attached to all raw chromatograms stored while the file was loaded in memory 64 Menu Reference EZChrom 200 400 menus and commands Receive Method sub Instrument Purpose Loads the Method from the GC to EZChrom 200 400 and makes it the current EZChrom 200 400 Method Syntax Select Receive Method or type R Comments The current Instrument Setup parameters column temperature run time inject time etc will be written over and lost unless saved The method name displayed in the EZChrom title bar will not be changed To check for a successfu
95. omatography Data Systems Chapter 2 discusses the installation of EZChrom 200400 Chapter 3 describes how to get started with EZChrom s user interface This includes selecting commands graphic manipulation both with and without a mouse and text numeric editing Chapter 4 provides a step by step sample session that takes you through building a method collecting data optimizing integration parameters timed events and calibrating a method Chapter 5 is a technical reference describing the theory behind topics such as data sampling peak detection and peak identification Chapter 6 describes the purpose syntax and any relevant comment on each menu and command available in EZChrom 200 400 Chapter 7 focuses on more advanced skills such as method locking multilevel calibration print options and automated sequences Chapter 8 describes how to modify or correct several GC instrument configuration parameters that are specific for a particular module Chapter 9 describes how to verify that your GC firmware is in proper working order to restore its configuration parameters clear error conditions or recover a lost configuration record Chapter 10 provides answers to your most common questions Introduction How to use this manual Installation Installation Chapter 2 describes how to set up your computer to install and operate EZChrom 200 400 Requirements Computer system requirements l e wo N on Comp
96. on on the file or files to be deleted They will be highlighted as evidenced by the file name being blackened Press the Delete key to remove the files To delete EZChrom files you can also use the File Manager program provided with Windows a Open the File Manager executable located in the Main group of the Program Manager b Files are deleted by selecting File and Delete and then entering the fully qualified file name that is to be deleted I can t communicate with the GC 1 2 Press lt ESC gt if EZChrom 200 400 is hung up Make sure the proper COM port is currently attached to the instrument see Installation troubleshooting page 14 160 Common Questions One of my applications closes itself and disappears from the screen What is happening 1 This phenomenon usually occurs when there is not enough RAM available to open EZChrom s three or four program windows This can happen if you have tried to start EZChrom directly from Windows using the EZSTART icon while having other Windows applications opened These other applications require memory which your computer may not be able to spare Therefore make sure all Windows applications besides EZChrom are closed before you start EZChrom with EZSTART 2 You do not have the required 4 MB of free RAM required to run EZChrom If you are using a RAMDRIVE or a software RAM cache you may have to decrease its capacity to free up the required RAM memory I am ha
97. ontents Chapter 7 Quick Reference Quick and easy method development cccccecsssceceessceceessraeeeeees 96 Meth Od l cking sordina ana s 102 Multi level calibration 2vcca cczcisesiacvestasiocezedh sented dheeessisrgedtaaademdideteedads 103 Print ODWONS eeri rrie Bedslavchea ene eats ad eee eae 110 R nnine the mete teense te enn E ee a 112 Analyzing the Gata senatende aia en a i i 113 Automated sequences sseesseessseesssesseesseessseesssessseesseesseessseesssessseesseess 114 Transferring methods ssssssssessseessessssssssesssessseessressesesssessseesseessressee 115 Graphical manipulation of chromatograms cccssceesseeeeseeeees 117 Chapter 8 The GC Module Change Tool Installing GC Module Change Tool ecceeeeeeceeeceeeeceenceeeeeceeeeeeeee 123 Starting GC Module Change Tool ssssssssssssssssssesesssressessesssesssessesses 123 Changing a module s configuration record sesssesssssssessssssssesesssee 127 GC Module Change Tool for a Quad instrument ceeeeeeees 128 If you are swapping module POSITIONS oo eee eceesteeeceeseeeeceeeeneees 130 Chapter 9 The GC Verification Tool Installing GC Verification Tool c cciccaaceesatseteesccochtesesescasuanetansiese tented 133 Starting GC Verification Tool gic ccciccissasdods sactediactacetemaidele sete Sacstess 133 Typical SOS SIONS naosncusnuenmmusninenrein aeia cate ca e oi 136 Terminating GC Verification Tool ssessssssessesesss
98. ood idea to write the original configuration down somewhere before changing anything That way if you make a mistake you can recover from it by clicking the Change button again selecting the same module and reentering the original configuration from your notes Change Module A Module A Column Temperature Offset Column Temperature Scale Maximum Column Temperature x Fixed Loop Injector Inject Time Figure 64 Change module A window The new module configuration parameters can be found on the label on the module cover 129 The GC Module Change Tool If you are swapping module positions Change the configuration by selecting items from the drop down lists and or checking the Fixed Loop Injector check box Be sure that you enter the data correctly from the module s label When you click OK the GC s configuration will be updated and the Change Module window will disappear Click Cancel ifyou want to quit without making changes The Inject Time selector will only be shown when the Fixed Loop injector is checked If you are swapping module positions If you have swapped modules i e you have simply moved module A to the module B position and module B to the module A position you will not need to manually enter any data Simply click the Swap button as shown in Figure 60 After asking if you re sure of this choice the program will update the GC s configuration file to reflect the swap
99. out itself as shown in Figure 68 About MTI GC Verification Path C M TINUTILITYASCHECK EXE 23 Noy 1993 09 28 56 Copyright gt S Syy Copyright 1993 Microsensor Technology Inc Figure 68 About GC verification window It does not matter which serial port you use GC Verification will automatically search the serial ports available to it for a connected GC 135 The GC Verification Tool Typical sessions Typical sessions In general there are two types of sessions you will encounter when you are using GC Verification If your GC is OK there is a simple sequence of windows which will be displayed as the condition of the GC is verified If there is a problem there are a large number of possible window display sequences depending on the type of problem which has occurred In this section we will illustrate cases when your GC is OK and when a GC is experiencing problems What happens if your GC is OK The first window is the introduction window as shown in Figure 69 MTI GC Yerification Explanation e will check out your MTI GC to verify that it is OK and will perform properly If there is a problem we will guide you through the necessary procedures to restore the GC to proper operating condition If you have not done so please connect your MTI GC to one of the computer s serial ports Question Is the GC connected Figure 69 Introduction window The G
100. ps 2 through 13 Changing the time values for SLPSEN FINE SLPSEN and PKWD to zero allows EZChrom 200 400 to begin its peak search with the proper sensitivity from time zero 45 Sample Session Setting retention times graphically Setting retention times graphically The next step in constructing a complete and optimized application specific method is to enter the retention times and retention time windows for each of the compounds in the peak table The most accurate way to do this is to graphically select each peak in a real chromatogram with the vertical cursors l Place the vertical cursors around the first peak that elutes on channel A Youmay use the vertical hashmarks as a guide in placing the vertical cursors For an explanation of vertical hashmarks see the peak detection and peak integration questions on page 40 Select the Peak RT and RT Window command which is found under the Events menu for channel A A window will appear which lists the compounds you previously entered in the channel A Peak Table See Figure 32 1 i Butane 2 n Butane 3 i Pentane 4 n Pentane 5 Hexanes 6 Heptanes 7 Octanes 8 Nonanes Cancel Figure 32 Compound list window Click on the compound name of the peak in the window The compound name will depend on the type of column you have in module A See number 13 and 14 on page 37 Click on OK or double click on the highlighted peak name 46 Sample Session Setting rete
101. r gt or use your mouse to click on OK EZChrom 400 RGA Data System Version 4 2 Copyright 1988 1995 MTI Analytical Instruments Figure 5 EZChrom 200 400 confirmation window EZChrom 200 400 will then proceed to open and draw the windows which comprise the data system Two display windows four display windows one each for Channels A B C D will appear with EZChrom 400 will appear in EZChrom 200 i e one each for Channels A and B At this time a default method and data file named after your instrument serial number will be recalled and displayed see Figure 6 When you access the window represented in Figure 6 the method and file names will be replaced by the serial number of your particular instrument i e the method EXAMPLE MET will read XXXXX MET and the file name EXAMPLE 1 will read XXXXX 1 where XXXXX respresents the serial number for your instrument Installation Getting started Beas Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help Method Instrument Data Analyze Math Calib Start Help Figure 6 EZChrom 200 400 recalls EXAMPLE MET and EXAMPLE 1 If EZChrom doesn t start l Verify that you have at least 4 Mb of RAM Also check that your processor clock speed is at least 20 MHz Refer to your owner s manual If the previous conditions have been met and EZChrom 200 400 still will not function call Agilent Technologies for assistance 1
102. rate way to build an optimized Timed Events table is to select regions of areal chromatogram with the vertical cursors and then evaluate the region with one of the four basic timed event parameters EZChrom 200 400 then calculates the correct value for the event over the selected region and if desired adds the event with the calculated value to the Timed Events table 1 If necessary review the use of vertical cursors beginning on page 22 Familiarity with vertical cursor manipulations is critical for this stage of the sample session 2 Inthe channel A window activate a single vertical cursor and freeze it about 0 5 seconds to the left of the first peak See Figure 27 Note the time where you froze the vertical cursor Be careful that only one vertical cursor is visible in the window otherwise the time and amplitude of the mobile cursor will be in reference to the frozen one Should two vertical cursors appear click the right mouse button then the left mouse button and the two 41 Sample Session Optimizing timed events cursors should merge For further information on vertical cursors see Chapter 3 Chan A 100 sec Attn 2048 fF Chan B 100 sec Attn 2048 Reports Events Display Print Help Reports Events Display Print Help Time sec 000 020 Amp u j 302 Method SERIALNO MET File SERIALNO 1 Data Analyze Math Calib Start Help Method Instrument Program Manager Figure 27 Using verti
103. rocedure for initiating an autorun is as follows 1 Select the Start menu The Run window will appear See Figure 54 2 Enter the number of times you wish the GC to run for continuous operation enter a 0 999 or INF Run ID sample Number of Runs 1 999 inf 5 Time Between Injections secs 350 Wait For External Start E Save O Print O DIF Save CI PRN Save C Extended User Program Figure 54 Run window 3 Enter a value for the time between injections in seconds This time should be long enough so that any highly retained compounds can elute from a column prior to the next run and all specified print jobs can be completed An autorun sequence can be aborted at any point by pressing the lt Esc gt key or paused by pressing the lt F1 gt key while the EZChrom command bar is active Each file saved in an autorun is given the Run ID plus a numeric extension The 114 Quick Reference Transferring methods extension of the last collected file will be the same as the number of runs you entered Batch processing EZChrom 200 400 can be instructed to reanalyze print and display sets of stored data by using the Recall command in the Start window To use this feature Select the Start menu See Figure 54 Enter the Run ID minus the extension of the series of files to be reanalyzed Enter the number of files to be reanalyzed Set the time between inject
104. scribed for Events 2 Select INTG Off Comments This event is used to prevent integration over user selected regions i e the baseline rise immediately after injection or a large solvent peak 87 Menu Reference Channel AJB commands Invert sub Events Purpose Allows the user to invert any portion of a chromatogram Syntax 1 Choose the region to be inverted with the vertical cursors as described in Chapter 3 2 Select Invert or type I Comments This event is used when a negative peak is present in a chromatogram An inversion will only occur when Invert is selected or added to the Timed Events or the first time a dataset is analyzed with a method which includes an Invert event When Invert is selected an analysis is done automatically Min Area sub Events Minimum Area Purpose Defines the smallest integrated area that should be identified as a peak Syntax 1 Select a peak with the vertical cursors 2 Select Min Area or type M 3 Confirm the time and value for the minimum area then press OK Comments Allows small peaks or baseline defects to be ignored during peak search 88 Menu Reference Channel A B commands Peak RT and RT Window sub Events Purpose Used to set retention times and retention time windows for peaks listed in the Peak Table Syntax 1 Select a peak with the vertical cursors 2 Select Peak RT and RT Window or type R A popup window listing valid peak nam
105. sessessssseessessrsseessesse 150 Explanation of GC Verification windows ccsssceesseceesteeeessees 151 Compatibility and computer system requirements c0c008 158 Chapter 10 Common Questions Appendix A Error Number Description 163 Appendix B Dynamic Data Exchange DDE 167 Appendix C Dynamic Data Exchange DDE 177 Introduction Introduction General description Welcome to the EZChrom Chromatography Data System a complete gas chromatography GC data system designed to control Agilent Technologies micro gas chromatographs EZChrom s compatibility with Microsoft Windows 3 1 makes the data system extremely user friendly With a simple click of a mouse button you can initiate data collection save or retrieve data or begin data analysis of your chromatogram This manual covers the operation of both EZChrom 200 which controls the operation of the M P series of GCs and EZChrom 400 which controls the Quad series of GCs Whether you are using the EZChrom 200 or the EZChrom 400 Chromatography Data System you will be able to reference this manual for operation and explanation of either software package For this reason the EZChrom Chromatography Data System will be referred to as EZChrom 200 400 throughout this manual Instructions given in the manual will apply to either software package with the following understanding of the differences between the two data sy
106. sitions of existing modules whose configuration record is known 2 Need to correct an error resulting from installing a GC module 3 Are asked to alter the GC module configuration by Agilent Technical Support You will use the GC Module Change Tool whenever any of the above situations occur and there is aneed to update or correct the GC s configuration parameters Although these instructions are written for an M P200 instrument Quad instrument specific instructions can be found in Chapter 3 of this manual 122 The GC Module Change Tool Installing GC Module Change Tool Installing GC Module Change Tool GC Module Change Tool is automatically installed when you run SETUP EXE from the GC Tools diskette shipped with your instrument At the time of installation the configuration record for your GC is also installed in your PC as the HP INI file Since the GC Module Change Tool relies upon the existence of the configuration record you should run SETUP EXE on each computer that you will want to use with a given GC You may install GC Module Change Tool on as many computers as you will use with your GC No icon is created in the HP Program Group Window for the Module Change Tool but the file is installed as C HP UTILITY Change EXE on your computer system Starting GC Module Change Tool The easiest way to start the GC Module Change is via the Windows Program Manager From program Manager select File Run See Figure 58
107. ssary steps required for data acquisition analysis and storage are discussed This sample session run on ambient air is meant to be followed in sequence so please start at the beginning If the chromatograph option you have purchased is unable to separate the N and O in air the single composite peak you observe is sufficient to demonstrate the operating procedure First start EZChrom 200 400 Building a method The first step in using EZChrom 200 400 is to construct the proper Method This is important because the Method not only controls the GC but also controls all the calculations and peak detection performed by EZChrom 200 400 When EZChrom 200 400 is first started the last saved Method is automatically loaded initially Serialno met This default Method is created using your column configurations The method may or may not be appropriate for your sample analysis The following instructions illustrate how to build and save a Method which is optimized for the analysis of air Once mastered constructing an optimized Method for your specific application s will be easy If at any point you wish to terminate the sample session double click on the square above Methad 30 Sample Session Building a method EZ Method example met File example 1 Method Instrument Data Analyze Math Calib Start Help Figure 20 EZChrom 200 400 menu A screen will appear asking if you wish to terminate EZChrom Click on OK The screen wil
108. stems There are several operational and display differences between EZChrom 200 and EZChrom 400 however these differences are subtle and thus EZChrom 400 does notrequire aseparate manual With an understanding of the differences between the two software packages you will be able to use this manual for operation of either EZChrom 200 in conjunction with an M P series Gas Chromatograph or EZChrom 400 in conjunction with a Quad series Gas Chromatograph Introduction General description The differences between the EZChrom 400 and EZChrom 200 Chromatography Data Systems are as follows Four channel display EZChrom 400 software has a four channel display window Channels A B C and D rather than atwo channel display window Channels A and B only as found in EZChrom 200 EZChrom 400 collects displays and reports data for up to four 4 GC modules whereas EZChrom 200 does so for up to two 2 GC modules only As a result where there is reference to Channels A and B in this manual regarding the operation of EZChrom 200 the same instructions will apply for the operation of Channels C and D in EZChrom 400 Real time display EZChrom 400 does not have real time display of data during a chromatographic analysis Chromatogram displays go blank during an analysis and only an hour glass is displayed Once data acquisition is complete EZChrom 400 displays four chromatograms one in each of the four window displays EZChrom 200
109. t 50 of the channel B window is covered release the mouse button Movement in two dimensions is not restricted to channel windows Any and all windows or icons in either EZChrom 200 400 or Windows may be moved in this way Chan 100 sec Attn 2048 fec Attn 2048 Reports Events Display Print isplay Print Help Help a Method btu met File btu 1 HH Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 11 Channel A overlay 6 Nowtrytodrawazoom box inthe channel B window To do this the channel B window must first be activated Place the cursor in an uncovered portion of the channel B window 7 Click the left mouse button This will cause the channel B window to be redrawn above the channel A window See Figure 12 Zoom boxes may now be drawn as previously described 8 Take afew minutes to become familiar with the single headed arrow and its functions When you are comfortable move to the next chapter 19 Getting Started Graphic manipulation with a mouse Chan A 100 sec Attn 204 Chan B 100 sec Attn 2048 i l Reports Events Display Prig Reports Events Display Print Help ol Method SERIALNO MET File SERIALNO 1 z Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 12 Channel B overlay Double headed arrow Use this cursor to enlarge or shrink any of the windows in EZChrom 20
110. t mouse button over the first file and hold it down while scrolling down the list Release the mouse button when you reach the last file to be deleted The entire list of files to be deleted should be blackened Now press the lt Delete gt key Save As sub Data Purpose Allows raw chromatograms to be saved under user specified names Syntax 1 Click on Save As or type A 2 Enter a filename Comments The file will be stored in the directory listed at the top of the popup window unless another directory is specified in the filename dialog box The specified name must be eight characters or less and may not contain any spaces or illegal DOS characters Send Current Method Receive Method Instrument ID b Hardware Setup EEA Data Analyze Math Calib Start Help Figure 39 Instrument menu 62 Menu Reference EZChrom 200 400 menus and commands Instrument Main menu See Figure 39 Purpose Allows the current state of the M200 or P200 to be monitored and updated Commands for method sending receiving and status monitoring are located here Syntax Select Instrument or type lt Alt gt I Hardware Setup sub Instrument Purpose Allows changes to be made to the COM port designation for the GC Syntax 1 Select Hardware Setup or type H 2 Click on the down arrow until the desired COM port number is in the highlighted box 3 Click on OK Comments With this capability no longer must EZChr
111. t the CALIB menu and then the proper calibration level prior to analyzing the data My data and or method files are not saved or can not be copied with the File Manager What is happening 1 The hard disk or storage device is full 2 Youhave put illegal characters or spaces in your filename Illegal characters are lt gt 5 3 162 Appendix A Error Number Description Error Number Description EZChrom 200 400 checks for communication errors while transferring data to and from the gas chromatograph If an error occurs you are prompted with a dialog box that displays the error number Refer to the list below for a description of each possible error number Note that more than one of these errors can occur at one time In such a case the error number reported will be the sum of the numbers of the errors that occurred For example if error 1 and 2 both occurred then the error number reported would be their sum or 3 Errors 1 and 2 usually occur when the computer is not fast enough to keep up the communication at the required speed Running other programs in the background can cause these error to occur All of the other errors are usually caused by some sort of communications failure in the hardware either at the computer or at the chromatograph 1 Receiving queue overflowed There was either no room in the input queue or a character was received after the end of file character was received 2 Character was
112. talled this tool You can use the BROWSE button from the Run window Figure 59 to search your disk for this directory see Figure 61 125 The GC Module Change Tool Starting GC Module Change Tool Browse File Name Directories _exe pif com bat aj setup exe List Files of Type Drives Porm H E Figure 61 Browse window from run window If there is no available GC you will see an error message as shown in Figure 62 CHANGE There appears to be no GC connected to this computer Figure 62 Change window A GC may be unavailable if another program is using it Windows does not allow programs to share serial ports If you see the window shown in Figure 62 click OK and check the following 1 Check that the GC is connected and that it is ON 2 Ifthe GC has a front panel check that the GC is in Remote mode 3 Check that there are no other programs running in your computer that are trying to use the GC The safest policy is to make sure that no other GC programs are running e g EZChrom 200 400 If you are still unable to communicate with the GC after checking all the above conditions contact Agilent Technical Support for assistance 126 The GC Module Change Tool Changing a module s configuration record Changing a module s configuration record After you install the new module as described in the instrument User s Manual connect the GC to both electrical power a
113. tarted Instrument Setup sub Method Purpose Contains the instrument conditions for data acquisition Syntax Select Instrument Setup or type I Comments Valid entries for the instrument parameters are Parameter Range Column temperature C 30 180 Run tme seconds 0 160 Sample time seconds 5 255 Injection time milliseconds 5 255 Detector filament On off Detector autozero On off Inlet heaters On off Detector sensitivity Low med high For heated inlet GCs M P 100H or 200H column temperature range is 40 180 C The increased minimum temperature results from the transfer of heat from the heated inlet and injector portions of the module to the column heater Remember to set parameters for both channels The Sample Time is set for both channels at once 70 Menu Reference EZChrom 200 400 menus and commands Lock Unlock sub Method Purpose Protects a method from alteration Syntax 1 Select Lock or type L 2 At the prompt enter a password Comments Any locked method can be temporarily modified during a session Locking prevents these changes from being stored to the hard disk i e when quitting EZChrom or opening another method unless the appropriate password is given New sub Method Purpose Creates a method called New This clears the peak timed event and calibration tables and sets the instrument setup and calibration setup tables to their default values S
114. tatus command To check the instrument status 1 2 3 Select Instrument Select Status Observe the display window See Figure 55 which lists the current temperature pressure autozero voltage detector filament status and remaining battery charge P200 only in the GC Select OK to close the Status window 116 Quick Reference Graphical manipulation of chromatograms Graphical manipulation of chromatograms Once the data has been analyzed and the chromatograms have been displayed there are a wide variety of options available for manipulating the display and setting up new analysis parameters See Figure 56 Note that the upper portion of the channel windows has a complete display of the chromatograms and the capability to adjust the display attenuation Using the mouse or keyboard a zoomed portion of the chromatogram may be displayed in the lower portion of the screen Chan A 100 sec Attn 2048 i l Chan B 100 sec Attn 64 Reports Events Display Print Help Reports Events Display Print Help a Method SERIALNO MET File SERIALNO 1 thod Instrument Data Analyze Math Calib Start Help Program hananar Figure 56 Full unzoomed and split screen windows Full unzoom This command returns the lower display to a full scale chromatogram at the current display attenuation 1 Select Display 2 Check Full Unzoom The lower portion of the window will return to a full scale chromatogram
115. tention Time will be listed in the External Standard Report Level 1 cal amount This is the amount of a compound that the level one calibration standard contains When a calibration is run EZChrom assigns the entered amounts to the areas of any integrated peaks which elute in the appropriate retention time window Obviously accurate calibration standards must be used and retention time windows must be properly set for EZChrom 200 400 to accurately quantify realsamples EZChrom 200 400 can use up to eight levels of calibration but for routine analysis one level is usually sufficient Each level corresponds to a standard concentration and a point on a calibration plot Calibration plots are discussed in Advanced Skills Chapter 7 Relative response factor peak These advanced features deal with calibrating compounds which are not present in your calibration gas standard A complete discussion is reserved for the Advanced Skills chapter of the manual In the channel A peak table activate the text cursor in the PKNO 1 peak name box Then type in Air If you have an OV HayeSep or PoraPLOT type column in module A Oxygen If you have a Molecular Sieve column in module A Proceed to fill in the peak names for channels A and B For OV type columns you are already finished since these columns will not separate any of the percent level components in air For a HayeSep or PoraPLOT column enter Carbon Dioxide in the PKNO 2 peak name box
116. the Helium Carrier gas supply from the back of the MTI GC and click the OK button Figure 82 Resetting CHP offset window Disconnect the helium carrier from the back of the GC and click the OK button GC Verification will repeatedly send a command to set the CHP zero and then check that the CHP actually is zero Each time through this process the number of retries is incremented and displayed in the Retries box The process should be complete within one to five retries if it goes longer there may be a problem with the carrier gas plumbing If the number of retries becomes excessive more than 10 or so click Cancel and call Agilent Technical Support Be sure that you actually disconnect the carrier at the fitting on the rear panel of the GC Itis not enough to simply turn off the carrier supply it must be allowed to fall to atmospheric pressure When the pressure measured at the pressure transducer remains steady for greater than one second the measured pressure value will be taken as zero psig regardless of whether it is atmospheric pressure or the pressure remaining in the attached carrier gas line If the measured pressure is anything other than atmospheric pressure this will cause an error in the pressure readings equivalent to the difference 144 The GC Verification Tool Typical sessions Ifthe CHP reset is successful the window display will read as shown in Figure 83 Resetting CHP Offset
117. the upper limits of the channel window display See page 117 through page 120 respectively for explanations of how to unzoom and how to adjust attenuation After adjusting the instrument parameters run the GC again If the analysis is still unsatisfactory repeat this step Be careful not to be fooled by the display Always set the display Attenuation to 2048 and Fully Unzoom the lower display when checking for detector saturation Once the instrument settings have been optimized the integration parameters tables should be adjusted During the course of completing Step 5 you may have noticed that some of the peaks in the chromatogram were not integrated or were integrated incorrectly To correct this deficiency PKWD events must be added to the Timed Events tables Observe the last analyzed dataset on the screen Note the first peak which is not properly integrated the calculated baseline does not extend from the true beginning of the peak to its true end Using a Vertical Cursor determine the time at which the missed peak begins to elute Now add a PKWD event with a value of 0 2 and a time slightly less approximately 0 5 seconds than the beginning of the missed peak to the appropriate Timed Events table See Figure 49 After the PKWD event has been added Reanalyze the data The peak which was previously not integrated should now be properly integrated If it is not double the PKWD value to 0 4 and reanalyze Eventua
118. to be working properly and there are no errors in the GC s memory where it has a stored copy of the configuration record If you know of no other problems with the GC and you have not performed any replacement or Swapping of modules since the configuration record was last verified click Yes The Verification Tool will create a new configuration record for the GC in your computer system and continue with the verification process If you are unsure whether your GC is properly configured you can call Agilent Technical Support to find out how to manually verify the configuration In this case click No and you will see the screen in Figure 91 Call Technical Support Explaination our MTI GC has unresolved problems that will interfere with proper operation Please call MTI Technical Support at 510 490 0900 to get the problem resolved Subject How can manually verify my GC s configuration Figure 91 Call technical support window Terminating GC Verification Tool GC Verification terminates automatically when you click OK in an GC Verification Successful Figure 9 or Call Technical Support Window Some windows such as the Introduction Window Figure 5 have Quit buttons that can also be used to terminate GC Verification Tool 150 The GC Verification Tool Explanation of GC Verification windows Explanation of GC Verification windows The display windows of the GC Verification Tool are alp
119. tor for that compound 106 Quick Reference Multi level calibration e Calibrating the instrument Once the Calibration Setup and Peak Calibration Tables have been completed the instrument is ready to be calibrated Channel oA CB Pkno 1 Prev Next Calibration Type Point Level Area Amount 0 35 Pave 0 26 PgDn Cancel Plot 9 18 27 35 Area x 1000000 Figure 51 Peak calibration table Calibration can be performed with stored data or during an acquisition sequence Follow directions for Stored Calibration or Run Calibration depending on which option is preferred Any combination of these options can also be performed 107 Quick Reference Multi level calibration Stored calibration First clear the statistics for a clean start 1 Select Data 2 Select Clear Statistics 3 Select OK Now select the stored data file to use as a calibration standard 1 Select Data 2 Select Open 3 Enter the data file name manually or double click on the data file name Now set up to calibrate 1 Select Calib 2 Enter the Calibration Level The calibration level refers to which calibration gas dataset is being analyzed first second third etc 3 Select OK To finish the calibration 1 Select Analyze 2 Repeat the preceding steps for each calibration gas standard dataset 108 Quick Reference Multi level calibration Run calibration 1 Attach t
120. totype Description GetPeakIndex int FAR PASCAL GetPeakIndex void This function is used to retrieve the current peak index in the DLL The index is returned by the function SetPeakIndex int FAR PASCAL SetPeakIndex int This function is used to set the peak index The function returns TRUE if the index is in the range 0 50 FALSE otherwise SetCmdParam int FAR PASCAL SetCmdParam LPSTR This function is used to place a command parameter in the DLL The command parameter is passed as an actual parameter to this function This function always returns TRUE 176 Appendix C Dynamic Data Exchange DDE Dynamic Data Exchange DDE Quick Reference Flowcharts This Appendix provides several simplified flowcharts on how to perform several chromatographic functions with EZChrom 200 400 The assumption made in developing these flowcharts is of an established understanding of the function and operation of the EZChrom chromatography data system The intent of this Appendix is to serve as a quick reference to allow you to quickly perform these chromatographic functions with little explanation or description of what is being done If you should find a need for further explanation as to the operation or definition of the functions referenced herein please refer to the earlier chapters of this manual which address these issues in greater detail In this Appendix you will find flowcharts describing the following chromatograph
121. tte into the appropriate floppy drive 3 Click the left mouse button on File in the top menu bar the File menu will appear Then click the left mouse button on Run Installation EZChrom 200 400 installation 4 A command box will appear In the command line Type a setup If your installation disk is in drive A b setup If your installation is in drive B Command Line C Run Minimized Figure 1 Program manager run window 5 The initializing window will appear see below EZChrom 200 400 will automatically load the software to C HP Setup is initializing Please wait Figure 2 EZChrom 200 400 initializing window Installation Getting started 6 Should you wish to use another drive or directory type the location in the space provided see below Click the left mouse button on OK or press lt Enter gt Installation Location Where shall we install EZChrom 400 Figure 3 EZChrom 200 400 installation location window 7 After all the EZChrom 200 400 files have been copied an HP Group window should appear with an EZChrom 200 400 icon Getting started Starting EZChrom In the Windows Program Manager 1 Locate the EZChrom 200 400 icon in the HP group window Double click on the EZChrom 200 400 icon Figure 4 HP group window 11 Installation Getting started 2 When EZChrom 200 400 begins a confirmation window will appear see below Press lt Ente
122. tween injections User Program Enter a path and program name to run an external program between runs in an autorun The external program must terminate prior to the next data acquisition EZChrom 200 400 is not multi tasking Attempts to multi task may cause a system crash Wait for External Start This feature allows EZChrom and an Agilent GC to be started from an external source If this box is checked when the START command is given EZChrom will pause until pin 2 on the GC ANALOG port is grounded Details of the GC IO port pin connections can be found in the M200 M200H or P200 P200H operations manuals 80 Menu Reference Channel AJB commands Channel A B commands This chapter describes the commands and features available in the display windows of EZChrom 200 400 Zooming printing and graphical selection of timed events are all controlled by selecting the appropriate command The command menus are located at the top of the channel A and B windows DISPLAY Main menu See Figure 42 Purpose Controls basic display features of zooming splitting the screen and displaying the baseline Syntax Select DISPLAY or type lt Alt gt D Comments Be sure that Channel A or Channel B windows are activated Activate a window by clicking in the window Chan A 100 sec Attn 2048 Display Full UnZoom F3 v Split Screen Baseline F5 Cursor Figure 42 Display menu 81 Menu Reference Channel AJ
123. un and the beginning of the next If a full scale chromatogram is printed the interval between runs must be at least 3 minutes as this type of printing takes a long time to complete Recall Allows batch reprocessing of data files To use this option enter the names of a sequential set of datafiles in the Run ID window Then enter the number of files which are to be reanalyzed in the Number of Runs window Selecting the Recall command will cause EZChrom 200 400 to retrieve and reanalyze as many files as you entered in the Number of Runs window Only datasets which have sequential extensions beginning with 1 can be Recalled It may be necessary to rename a data file to generate sequential extensions 1 2 3 etc The Recall function can be used with Print and or PRN and Save options in the start window Run ID Will save data files automatically under the filename specified The run number is appended to the Run ID as a file extension 79 Menu Reference EZChrom 200 400 menus and commands Caution Save Saves raw chromatograms to the hard disk or a user specified drive or directory The chromatogram is stored under the Run ID Time Between Injections The time from the beginning of one run to the beginning of the next run The interval time must be long enough to allow for run time saving data and report printing Example 100 seconds Run Time 5 seconds save data 60 seconds interval 165 seconds time be
124. uter Any Microsoft Windows 3 1 compatible system minimum 20 MHz 386 processor System memory Minimum 4 Mb of RAM Disk storage 100 megabyte hard drive and 3 5 or 5 25 inch floppy drive Ports One free serial port two serial ports if a serial mouse is used Operating System MS DOS version 5 0 or higher Video Monitor Any Microsoft Windows 3 1 100 compatible including EGA VGA or SVGA Operating environment Microsoft Windows Version 3 1 Printer Any Microsoft Windows 3 1 100 compatible GC instrument requirements Firmware version 17 4 or later Installation EZChrom 200 400 installation Windows installation Before installing the EZChrom 200 400 Data System Windows 3 1 must be properly installed and running on your computer If you are not familiar with Microsoft Windows it is recommended that you acquaint yourself with Windows 3 1 or later Windows versions being used with EZChrom 200 400 Refer to Chapter 1 of the Windows 3 1 manual for an excellent overview of basic Windows skills The HIMEM SYS driver must be present in the CONFIG SYS file for EZChrom to function properly EZChrom 200 400 installation Introduction Your Agilent GC is shipped with one diskette containing the following 1 EZChrom 200 400 This diskette contains the chromatography data system Installing EZChrom 200 400 1 Make sure the computer is running Windows and is atthe Program Manager 2 Insert the EZChrom 200 400 diske
125. ve to be converted to a number before it can be used 173 Dynamic Data Exchange DDE EZChrom DDE server Name GetInstStatus Format The current instrument status for the specified channel is returned as a tab delimited string The format is as follows Column Temperature lt TAB gt Column Head Pressure lt TAB gt Detector Auto Zero Voltage lt TAB gt Detector Status lt TAB gt Battery lt TAB gt Firmware Version For example the value returned may look like 60 lt TAB gt 15 1 lt TAB gt 27 lt TAB gt On lt TAB gt 100 lt TAB gt 17 5 Name GetRunCond Format The conditions under which the current sample was acquired for the specified channel are returned as a tab delimited string The format is as follows Acquisition Date lt TAB gt Instrument ID lt TAB gt Column Type lt TAB gt Carrier Gas lt TAB gt Column Head Pressure lt TAB gt Column Temperature lt TAB gt Detector Gain lt TAB gt Sample Time lt TAB gt Inject Time lt TAB gt Run Time For example the value returned may look like Feb 21 1994 14 54 19 lt TAB gt BTU lt TAB gt HSA lt TAB gt Helium lt TAB gt 17 383 lt TAB gt 52 lt TAB gt LOW lt TAB gt 10 lt TAB gt 50 lt TAB gt 100 174 Dynamic Data Exchange DDE EZChrom 200 400 VBE DLL EZChrom 200 400 VBE DLL DLL Format The peak data in the dynamic link library is stored in tab delimited strings There is a limit of 100 characters per string and 50 strings in the library These strings
126. ving trouble integrating peaks What do I do If the peak is not being integrated 1 Check the PKWD graphically at the base of the missed peak and make sure it corresponds in time and value to a PKWD event in the Timed Events table 2 Check the SLPSEN and FINE SLPSEN graphically on a representative section of baseline without peaks and make sure they are set correctly 3 Check to see if there are any INTG OFF periods that overlap any portion of the peak If there are delete or change them 4 Check that the baseline has not been turned off If the peak is found but the baseline is too high on the peak 1 The SLPSEN and or the FINE SLPSEN values are too high Check and reset them graphically See page 99 for suggested values 2 The PKWD is too small try doubling it If too many peaks are found 1 The SLPSEN and or FINE SLPSEN value s is too low Reset it on a region of baseline See page 99 for suggested values 161 Common Questions If peaks are identified graphically but the reports are empty 1 Reset the retention time and retention time windows graphically See page 46 for a description on how to set retention times graphically 2 Make sure the multiplier in the Calibration Setup is not equal to zero See page 67 and Figure 50 for further explanation After analysis the calibrated results in the External Standard report do not match the calibration amounts I entered 1 Make sure that you selec
127. volts at the displayed time Click the left mouse button This will freeze the first vertical cursor Drag the mouse to the right The frozen cursor should remain while a second mobile cursor will appear See Figure 16 The values for time and amplitude now displayed are in reference to the first vertical cursor That is to say the first vertical cursor now has been assigned a time and amplitude value of 0 23 Getting Started Graphic manipulation with a mouse Chan A 100 sec Attn 2048 Chan B 100 sec Attn 2048 j Reports Events Display Print Help Time sec 002 220 Amp u 696 Time sec 004 760 Amp u 252 a Method btu met File btu 1 Method Instrument Data Analyze Math Calib Start Help Program Manager Figure 16 Using two vertical cursors 6 Click the right mouse button This freezes the second vertical cursor The region between the two vertical cursors is called the selected region Being able to select specific regions in a chromatogram is essential in graphically setting up peak identification tables and integration parameters 7 Click the right mouse button again This unfreezes the second vertical cursor 8 Click the left mouse button This will cause the two vertical cursors to merge and be mobile as in step 2 9 Click the right mouse button This will freeze the single vertical cursor remaining while also reactivating the single headed cursor The s
128. yntax Select New or type N Comments This command should be selected when first using the GC or when a new application is being developed It is usually easier to modify an existing method to compensate for slight variations in sample conditions as this is much faster than starting from scratch 71 Menu Reference EZChrom 200 400 menus and commands Open sub Method Purpose Allows the user to recall any Method file and make it the current Method Syntax 1 Select Open or type O 2 Enter the filename or select one from the list 3 Select Open Comments Scroll bars on the right of the file box enable the complete list to be examined Peak Calibration sub Method Purpose The peak calibration table contains the area counts and corresponding amount values for all compounds listed in the peak table A separate page exists for each compound listed in the Peak Table Syntax 1 Select Peak Calibration or type K 2 Enter the area and amount values for each compound in ascending order Up to eight area amount pairs may be entered 3 Select Next or Previous to access the calibration tables of the other compounds to be calibrated 72 Menu Reference EZChrom 200 400 menus and commands Comments Typically this procedure is done automatically by using the Calib command Thus manual entry is usually not required If multiple levels are being used amount area pairs should be entered in ascendin

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