User Manual
Contents
1. OPUS Spectroscopy Software User Manual CHROM gt lt BRUKER o Table of Contents 1 Introduction ASES AAA A 1 Technical Requirements oss sis 00 5 oa see ais ia a a 3 Chromatography A TA Www wos Wel Se wl 5 3 1 Set Parameters tisdale el ean eee lar aea 5 3 2 Measuring the Background Spectrum 0 00 cece eee eee 5 3 3 Number of Sample Scans ss qdo nes oak PE oe ae ES GUS SAS RUA 6 3 4 Type of Result Speci sas exe iara aii au ee atk pla Mees 6 35 Traces CC LIMITE 24 6 4a spate des dr uai aM ea hE Ae dada 6 3 6 Starting the CHROM Measurement 0 0 0 c cece cece nee 9 3 7 Real Time Display icici teeter eta tet 9 3 7 1 Chromatography Window 0 0 cece cece eens 10 3 1 2 Display Ops ss ake do Ea ia ee wade Ea DAR STS 11 Real Time Data Exchange and Control of OPUS via External Program Sia E ead ooo eae O a Su 15 1 Introduction The OPUS CHROM software package enables you to measure time dependent processes like coupled techniques e g GC IR HPLC IR or TGA IR More over you can use this software package to acquire the spectral changes during a kinetic reaction provided that the reaction does not pass off too fast Note For very fast reactions it is advisable to use methods like Rapid Scan or Step Scan TRS The result of a measurement performed with the OPUS CHROM package will be a number of spectra measured at defined constant time intervals The inten sity ch2. If you click with the right mouse button on this subwindow a pop up menu appears The functions of this menu are described in detail in following section Display Options d Scaling and Zooming Buttons Auto Scale Auto scales all displayed traces in the trace window A green button indicates that this function is activated Show All Shows all traces in the trace window A green button indicates that this function is activated Time Zoom In Out If you click on the corresponding button you can zoom the time axis in the trace window in or out Y Scroll Down Up If you click on the corresponding button you can scroll the y axis in the trace window up or down Y Zoom In Out If you click on the corresponding button you can zoom the y axis in the trace window in or out Zoom Scroll Velocity If click on the corresponding button you can increase or decrease the velocity of the zooming or scrolling actions Reset Resets the scaling of the curve s in the trace window Note If the Auto Scale button is activated i e it is green the Y Scroll Down Up buttons and the Y Zoom In Out buttons are not displayed Bruker Optik GmbH OPUS CHROM 10 Real Time Display e Line Parameter If you can click on this button you can specify the color and the line width of the curves f Graph only If you click on this button all buttons next to the trace window disap pear To undo this action double click on the trace window g Stop Clicking o
3. an for sample mea surement Bruker Optik GmbH OPUS CHROM 5 Chromatography 3 3 Number of Sample Scans To set the number of sample scans click on the Advanced tab The number of sample scans determines the time resolution of the measurement The more scans are performed the fewer points per time unit can be measured Note If the computing power of the AQP is not sufficient to calculate the required number of spectra per time unit the interferograms are added automati cally until the next spectrum can be calculated As this may lead to an uneven time spacing it is advisable to select a timing that does not exceed the AQP s capacity With the following measurement parameter resolution 8em acquisi tion mode single sided bandwidth i e difference between wanted high and low frequency limit 7900cm zerofilling 2 2 3 spectra second for the AQP 2 and 6 7 spectra second for the AQP 4 will be calculated This does not apply to spec trometers of the Matrix and the Tensor M series 3 4 Type of Result Spectrum Specify the type of result spectrum Absorbance or Transmittance on the Advanced page Then the spectra are calculated displayed and saved as absor bance spectra or transmittance spectra For maximum time resolution only activate the Sample Interferogram check box on the Advanced page for the measurement and perform the calculation in a postrun 3 5 Traces amp Timing On the Trace amp Timing pa
4. anges of the spectra as a function of time are stored as a trace These traces are generated either by integration over a defined spectrum area with a preset integration method or by direct derivation from the interferogram using the Gram Schmidt calculation In the latter case the changes in the whole spec trum are taken into account The result is a curve that can for example be directly compared to a chromatogram from a GC measurement During the whole measurement the acquired spectra and the generated traces are displayed in real time Then these spectra and traces are saved automati cally in one file a so called 3D file To view or process this kind of file another optional software package OPUS 3D is required Bruker Optik GmbH OPUS CHROM 1 2 Technical Requirements Before starting a measurement with the OPUS CHROM package make sure that the following requirements are met Provide for sufficient hard disk space Store the CHROM files only on the hard disk not on removable media to ensure a high data transfer rate during measurement Spectrometers of the Matrix or the Tensor series or AQP 2 or AQP 4 Data acquisition and spectrum calculation can only be car ried out simultaneously if the acquisition processor is equipped with an AQP 2 or AQP 4 If only the standard AQP is available the data acquisition is stopped for the duration of the spectrum calculation Bruker Optik GmbH OPUS CHROM 3 Se
5. e 15 G Gram Schmidt basis interferogram 8 Gram Schmidt basis set 9 Gram Schmidt trace 10 Gram Schmidt calculation 1 Gram Schmidt Parameters 7 H History View 13 I Integration method 8 10 M Maximal Measurement time 8 Measurement 5 Measurement parameter 5 6 N Needle View 12 P Proteus TG Software 15 R Rapid Scan 1 Real Time Display 9 Reset Scaling 13 Resolution 6 S Scale Trace 10 Scaling and zooming buttons 10 Scroll View 11 Signal to noise ratio 5 Step Scan TRS 1 T Text View 12 Time resolution 6 Timebase Synchronisation 8 Trace Window 10 Trace window 11 13 Traces 1 8 9 10 12 13 15 Traces amp Timing 5 6 Traces by Spectral Integration 8 Z Zerofilling 6
6. e displayed in separate windows 0 15 a Y Absorbance Units Dau 0 05 0 00 X Wavenumber cm 1 2 0 pona 8 b e NN 2 leo c d tte ro UE cep alans sema name RE E D f eae En i FR i Ss i grees 13 56 06 g ee O h Chromatography O scans num E Figure 3 Real Time Chromatography Display Bruker Optik GmbH OPUS CHROM 9 Chromatography 3 71 Chromatography Window The chromatography window comprises two subwindows 3D window and trace window and a number of buttons e g scaling and zoom buttons a 3D Window This subwindow displays the spectra in a 3D plot and in real time If you click with the right mouse button on this subwindow a pop up menu appears The functions of this menu are described in detail in the OPUS 3D Manual b Select Trace The buttons are labelled with the names of the traces The color of the buttons corresponds to the color of the traces in the trace window below If you click on one of these buttons only the corresponding trace will be fully displayed in the trace window Note The number of buttons depends on the number of the integrations you have specified in an integration method beforehand plus the Gram Schmidt trace pro vided that you have activated the corresponding check boxes on the Traces amp Timing page figure 2 c Trace Window This subwindow displays all chromatograms traces or only the selected one in real time
7. eus TG Software Netzsch Ger tebau GmbH Apart from synchronizing the measurement this software enables a data exchange during measurement The IR data acquisition is controlled by Pro teus TG software 1 e OPUS is running in the background The TG FTIR experiment is set up and saved in OPUS Preparing for the TG measurement Proteus automatically activates the FTIR spectrometer con nects to OPUS and transfers data Data Exchange OPUS imports TG Time traces and Temperature Time traces from Proteus OPUS imports file names with numerical extensions and sample information from Proteus into the parameter block of the 3D files OPUS exports the Gram Schmidt trace if activated and up to four integration traces if the integration routines have been activated to Proteus The integra tion routines have to be activated when the OPUS experiment file is generated Preparing OPUS for data exchange For automatic activation of the data exchange and control by Proteus software go to the properties of the OPUS icon on the desk top using a right mouse click and edit the shortcut to include OPUSPIPE ON immediately after opus exe e g c opus opus exe OPUSPIPE ON Bruker Optik GmbH OPUS CHROM 15 Index Numerics 3D file 1 3D plot 10 3D Window 10 A Acquisition mode 6 AQP3 6 B Background spectrum 5 Bar View 12 C Chromatography Window 10 Coupled technique 1 D Data exchang
8. ge the CHROM specific parameters are set Bruker Optik GmbH OPUS CHROM 6 Traces amp Timing Chromatography GC LC TGA x a H Basic Traces amp Timing HA Advanced Dptic Acquisition FT Background Check Signal IY Compute Gram Schmidt r Timebase synchronisation gt gt gt Gram Schmidt Vectors 20 e off d Gram Schmidt Offset 20 f i Menda d RL PR E Extemal start Gram Schmidt Points E External start and stop JV Traces by spectral integration IV Maximum measurement time to CADPUS 6 0 METHODSSINTMETH INT 1o00 min e m Save spectra c f Figure 2 Chromatography Dialog Window Traces amp Timing a Gram Schmidt Parameters These parameters determine how the reference data are used They affect the sensitivity of the calculated Gram Schmidt trace Gram Schmidt Vectors The number of interferograms or basis vectors which is used for the calculation of the basis set This number of interferograms will be acquired before the main measurement starts Gram Schmidt Offset The difference between the interferogram centerburst and the beginning of interferogram points that are used as the basis vectors Gram Schmidt Points The number of points of each interferogram that is used for the basis vectors Recommended values are GC FTIR TG FTIR Gram Schmidt Vectors 20 4 Gram Schmidt Offset 20 20 Gram Schmidt P
9. ignal to start the measurement The system stops the measurement automatically as soon as the external signal dis appears e Maximal Measurement Time If you activate this check box you can define a maximum run time in minutes After this period the measurement stops automatically f Save Spectra The drop down list contains the following options On Off and Auto If you select On all spectra including the traces will saved If you select Off only the traces without spectra will be saved In case of the option Auto traces and spectra will be saved but the spectra will only be saved if there are changes in the Gram Schmidt trace Bruker Optik GmbH OPUS CHROM 8 Starting the CHROM Measurement 3 3 6 Starting the CHROM Measurement Start the CHROM measurement by clicking on Start Chromatography Mea surement button on the Basic dialog window First number of scans x basis vectors interferograms are acquired which are then used to calculate the Gram Schmidt basis set If you have selected the option manual timebase syn chronisation see figure 2 an information message appears Click on the OK button An audible beep 2x short 1 x long sounds When the third beep sounds start the measurement of the coupled instrument If you have activated the Off option button see figure 2 the actual measurement starts immediately Fi Real Time Display During the measurement the spectra in 3D view and the traces ar
10. n the Stop button terminates the current measurement Other wise it will not terminate before the period specified in the Maximal Measurement Time entry field has run out h Save Spectra Defines whether the spectra are saved on the hard drive or not On If selected all spectra will be saved Off If selected only traces and no spectrum will be saved Auto In case of the option Auto traces and spectra will be saved but the spec tra will only be saved if there are changes in the Gram Schmidt trace i Run Time Run displays the number of spectra acquired so far Time displays the measurement time that has passed so far 3 7 2 Display Options If you click with the right mouse button on the trace window a pop up menu figure 4 appears pas pa pa pe a ao LE e e i i Scroll view Text View Bar View Needle View History View Properties Reset Scaling Assemble Traces Scie cess Asa n 65 Time 0 02 05 Figure 4 Display Options Scroll View The scroll view is the default setting See figure 3 Using the corresponding but tons next to trace window you can scroll the y axis up or down Bruker Optik GmbH OPUS CHROM 11 Chromatography Text View If you select the Text View option the current measurement data are displayed in form of a table The first column includes the name of the traces and the second column displays the measurement values Figure 5 Text View Bar View If you select the Bar View
11. oints 150 20 Bruker Optik GmbH OPUS CHROM 7 Chromatography b Traces by Spectral Integration Chromatograms can optionally be calculated by integrating the spectra To do this activate the Traces by Spectral Integration check box c Integration Method The currently selected integration method is shown here To change the method click on The integration method needs to be set up before hand by selecting the OPUS function Integration in the Evaluate menu d Timebase Synchronisation In this area you select the method of synchronizing the measurement with the GC TGA experiment etc Off The synchronization is deactivated i e the measurement starts immedi ately after the Gram Schmidt basis interferograms have been acquired Manual After the Gram Schmidt basis interferograms have been acquired a message appears showing the Gram Schmidt quality The Gram Schmidt quality is a measure of the quality of the Gram Schmidt basis A figure close to 1 0 indicates a stable measurement and is a precondi tion for a sensitive chromatogram signal Start the CHROM measure ment by clicking on the OK button The actual measurement starts after the third beep External Start After the Gram Schmidt basis interferograms have been acquired the system waits for an external signal to start the measurement External Start and Stop After the Gram Schmidt basis interferograms have been acquired the system waits for an external s
12. option the current measurement data are displayed in form of a bar chart Each bar corresponds to one trace The name of the trace is displayed above the respective bar Figure 6 Bar View Needle View If you select the Needle View option the measurement data are displayed in real time in form of a tachometer Each needle corresponds to one trace The color of the needle indicates to which trace a needle belongs to For detailed informa tion refer to the OPUS PROCESS Manual Bruker Optik GmbH OPUS CHROM 12 Real Time Display Figure 7 Needle View History View If you select the History View option the measurement data are displayed in form a line plot This view type is similar to the scroll view except for the brown scroll bar below the line plot This scroll bar allows you scrolling the line plot along the time axis The advantage of this view type is that the curve s do not move in direction of the time axis as data acquisition proceeds and that you can zoom 4 Stop Save v Run 35 Time 0 01 03 Figure 8 History View Reset Scaling Resets the scaling of the curve s in the trace window This function is identical to the Reset button next to the trace window Assemble Traces This function is only relevant to measurements performed with the OPUS PRO CESS software Bruker Optik GmbH OPUS CHROM 13 4 Real Time Data Exchange and Control of OPUS via External Programs Prot
13. t Parameters 3 Chromatography To perform a chromatographic measurement select the Chromatography com mand from the OPUS Measure menu A dialog window with several tabs opens Most of the tabs are similar to the ones of the standard measurement dialog win dow described in the OPUS Reference Manual Only the Traces amp Timing tab is specific to CHROM measurements The parameters are described in section 3 5 Chromatography GC LC TGA x H Basic Traces te Timing H Advanced Optic Acquisition FT Background Check Signal Experiment Load DEFAULT Operator name Default Sample name sampe Sample form femletom Path CAOPUS 6 0 MEAS File name WORK Background Single Channel Start Chromatography Measurement Exit Cancel Help Figure 1 Chromatography Measurement Dialog Window 3 1 Set Parameters Before starting a CHROM measurement set all necessary measurement parame ters The procedure is identical to the one for a normal measurement The vari ous parameters are described in the OPUS Reference Manual 3 2 Measuring the Background Spectrum First acquire a background spectrum by clicking on the Background Single Channel button on the Basic dialog window This spectrum will later be used to calculate the transmission or absorption spectra during the CHROM measure ment To improve the signal to noise ratio click on the Advanced tab and set the number of scans for background measurement higher th
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