USER MANUAL - Quantum Materials Group
Contents
1. Ge GO E 0 700 0 800 0 900 0 600 0 200 0 300 0 400 0 600 0 100 2400 2300 2200 2100 2000 1900 1800 1700 1600 1500 1400 1300 1200 1100 1000 lt M ez fh For Help press F1 No Active Task UE NUM RF Ej Fig 26 Constant part of the single channel sample spectrum 25 Bruker Optik GmbH 5 4 Calculation of the in phase and out of phase single channel sample spectra This calculation is done once again using the Interferogram to Spectrum function but for these signals the calibration phase spectrum is used By pressing the Ctrl button of the keyboard and using the mouse select the data blocks S_IFG the real part interferogram and S_IFG the imaginary part interferogram of the file resulting from the sample measurement Select in the Manipulate menu again the Interferogram to Spectrum function Thereupon the Interferogram to Spectrum dialog window appears See figure 27 Interferogram to Spectrum Phase Correction Mon Linearity Peak Search select Files Store Apoadization Limit Data al l PTY File s to convert ra D Stemps PP O 1 D Memp lPP 0 1 me Ip Fig 27 Appling the Interferogram to Spectrum function to the real part sample interferogram and to the imaginary part sample interferogram Also for this conversion do NOT store the phase i e deactivate the Save Phase check box on the Store page Click on th2. File name for the measurement results and specify the Path under which this file is to be stored For typical polymer stretching experiments a resolution of 4cm is appropriate but you are free to enter a different resolution value The parameter Sample scan time however MUST be set to 1 scan Otherwise the experiment will not work properly The parameter Background scan time is not relevant because the polymer stretching experiment does not require a classical background measurement In the fields Save data from to you need not enter anything as well since the Fourier transformation will be performed later by the DMA algorithm Select in the Result spectrum drop down list the option Transmittance In the group field Data blocks to be saved activate only the Sample Interferogram check box 9 Bruker Optik GmbH Chromatography GC LC TGA Path D PolymerstreckerWal Messungens Resolution d cm 1 Sample scan time Er i Scans ei Background scan time Ea Scans ei Save data from EO cm l to 370 Result spectrum Transmittance E Interferogram size 14220 Points FT size 16 K r Data blocks to be saved Transmittance Phase spectrum Single Channel Background ld Sample Interferogram Background Interferogram Exit Cancel Help Fig 6 Chromatography dialog window Advanced page Click on the Acquisition tab fig 7 This page is id
3. Strain tab in the DMA dialog window See figure 16 Enter the modulation frequency of the polymer stretcher into the Frequency field In most cases particular for experiments using the Polymer Modulator by Manning Technology the value for the parameter Phase should be 0 Only if you use a modulator of which the strain output has an electronic phase shift with respect to the physical strain this can be compensated by entering a different parameter value The remaining parameters on the Strain page are not relevant to this kind of experiment They are only useful for old fashioned step scan or multiplexing based experiments Click on the Calculate button OPUS Operator Default Administrator 3d Display MIR_Advanced ows EO File Edit view Window Measure Manipulate Evaluate Display Print Macro validation Setup Help X SS ki EI BEEN dE i a E OEE EIEZiOdDenlau MIE Advanced puz Rotation 30 140 3d Display MIR 0 70 I ECalibration 0 1 Inclination 20 fe 08 af IPP O 1 120 0 62 EKO EEREN x 4826 00 0 58 x 9614 00 e 100 aR 0 50 Z OU 0 46 zZ 196 00 w EU 0 42 E 3 is Ky 0 34 Calibration 0 60 0 30 Index 48 0 26 Select Files Strain 40 0 22 0 18 File s for demodulation i 20 0 14 Ais D Stemp Calibration 0 1 0 10 a 0 06 O 2000 4000 6000 8000 10000 1200014000 0 02 X Paints 0 02 D 0 6 a a o a E JE 2 04 2 UA ed gt
4. dei errr f i b ok bai be bei rh a EA d erd t amp Te 1 tt d 2 tiar MIR Dei E box Poe idl gress PI No Ath Task i Fig 29 Copying the entire sample measurement file with the Copy Entry function 27 Bruker Optik GmbH Select in the Manipulate menu the Spectrum Calculator function The in phase absorption change differential absorption is calculated by dividing the in phase single channel sample spectrum SSC by the constant single channel sample spectrum SSC Perform this calculation with the spectrum blocks of the original file resulting from the sample measurement In phase absorbance change SSC sample SSC sample Drag and drop the spectrum in the spectrum calculator See figure 30 Spectrum Calculator Spectrum Calculator Shit Hyp in eei i Fi UD MtempiiPP O 1 ScSm_Fl r D MtemplPF 0 1 5c5m gt g b cL one D Data Block EAEE ZK EA D br TZ Es e z E T ol TRAER w A OD Exit Cancel Help Fig 30 Spectrum Calculator Calculating the in phase absorbance change of the sample Select in the spectrum calculator the absorbance data block and click on the button The out of phase absorbance change is calculated by dividing the out of phase single channel sample spectrum SSC by the constant single channel sample spectrum SSC Perform this calculation with the spectrum blocks of
5. gt GO o gt 0 2 0 2 D 2000 4000 6000 8000 10000 12000 14000 D 20 40 60 60 100 120 140 X Points 2 Points For Help press F1 No Active Task JF NUM SI Fig 15 DMA dialog window Select files page The S_IFG data block of the 3D file resulting from the calibration measurement is included 1 8 Bruker Optik GmbH Select Files Strain Strain parameters Frequency Phase Fit parameters FFT before fit Additional phaseshitt D Data i multiplexed Strain i odd Post filtering Calculate Cancel Help Fig 16 DMA dialog window Strain page Only the parameters Frequency and the Phase are relevant to this kind of experiment The DMA algorithm calculates several new interferograms which are added as additional data blocks to the 3D file in the OPUS browser See figure 17 The data block S_IFG is that part of the infrared signal which does not depend on the different strain phases at all The data blocks S_IFG and 2 CHN result from the sample measurement which has been performed before the DMA calculation i e these data blocks contain the pure measurement results The fourth block S_IFG is the real part of the DMA demodulation It is the part of the infrared signal which is in phase with the strain signal The fifth block S IFG is the imaginary part of the DMA demodulation Its interferogram is 90 phase shifted with respect to the strain signal It
6. have to activate the Power checkbox interferogram to Spectrum Phase Correction Non Linearity Feak Search Select Files Apodization Limit Data Select frequencies for file First Last Save d Phaze Power Convert Cancel Help Fig 19 Interferogram to Spectrum dialog window Store page 21 Bruker Optik GmbH interferogram to Spectrum Phase Correction Non Linearity Peak Search Select Files Apodization Limit Data Apodization functor Blackman H aris 3 T erm erotilling factor AA Convert Cancel Help Fig 20 Interferogram to Spectrum dialog window Apodization page The parameters on the Apodization page fig 20 are identical to those on the corresponding page of the standard Measurement dialog window The parameter settings shown in fig 20 are useful for this kind of experiment however you can also try out other apodization functions and zerofilling factors On the Limit Data page fig 21 the checkboxes Limit resolution to and Limit phase resolution to usually need not to be activated Activate in the Direction group field the Forward option button and in the Datapoints group field the option button Both See figure 21 interferogram to Spectrum Phase Correction Non Linearity Peak Search Select Files Apodization Limit Data ah ETa Resolution Limit resolution to Phas
7. in the S_IFG data block of the 3D file Double clicking on the 2 don data block in the OPUS browser opens a 3D window in which the single strain traces are displayed in a 3D plot left upper subwindow See figure 13 These strain traces have been acquired simultaneously with the interferograms shown in figure 12 For the DMA algorithm which will be used for evaluation it is extremely important that there is a certain phase shift of the strain signal for consecutive interferograms To find out whether there is a phase shift have a look a the contour plot in the right upper subwindow of the 3D window that shows parallel lines minima 1 5 Bruker Optik GmbH and maxima of the strain signal See figure 13 Note If this is not the case it might be necessary to adjust the contour level color scale For detailed information about the 3D window refer to the OPUS 3D Manual If there is a phase shift between two consecutive interferograms scans the parallel lines incline as indicated by the angle q in figure13 The angle should not be too small It depends on the relation of scanner velocity resolution and modulation frequency Thus this angle can be influenced by changing one or several of these parameters Estimate the number of modulation periods along the x axis of the contour plot xz plot The number of periods along the z axis should be at least equal to the number of periods along the x axis or even larger In case of the exam
8. is also called quadrature interferogram Drag amp drop the calibration data file in the standard OPUS spectrum window See figure 17 1 9 Bruker Optik GmbH OPUS Operator Default Administrator Display MIR_Advanced ows 2 EO File Edit View Window Measure Manipulate Evaluate Display Print Macro Validation Setup Help dr E RZ Ei Eiz C8 ba AO Gb Si ZB ARS TT KE OGUI ZZ 7 x SIZ 3d Display MIR_Advanced ows 1 ZE Calibration 0 1 See db SE Sd hesi IPP 0 1 EKO LA badere SlmiDisplay MIE Advanced nuz d J Calibration 0 1 Seige be ul En cite hr 0 700 SAE 0 600 l y t 0 500 y 0 200 0 100 0 000 0 100 0 200 0 300 0 400 ae 0 300 0 400 14000 13000 12000 11000 10000 9000 8000 7000 6000 5000 4000 3000 2000 1000 0 Draw took 0 ms No Active Task Fig 17 OPUS browser with the calibration file after the DMA calculation i e several new data blocks have been added to the file Select in the OPUS browser the file resulting from the sample measurement by clicking on it with the left mouse button Then select in the Evaluate menu the DMA function Apply the DMA function to file resulting from the sample measurement with exactly the same parameter settings as for the file resulting from the calibration measurement Also in case of the sample measurement file additional interferogram blocks will be added to the
9. useful for real chromatography measurements In the group field Time base synchronization activate the option button Off Activate Maximum measurement time check box and enter the desired maximum measurement time A maximum measurement time of 5 minutes is a good starting point but depending on the results you can also test longer and or shorter measurement times In the Save Spectra drop down list it is recommended to select the option On 8 Bruker Optik GmbH Chromatography GC LC TGA li Basic Traces amp Timing a Advanced Optic Acquisition FT e Check Signal Beam Path Spectral Range Selection Timebase synchronisation Off C Manual C External start f External start and stop Traces by spectral integration iw Mau measurement tine 5 min Save spectra On Exit Cancel Help Fig 5 Chromatography dialog window Traces amp Time page Click on the Advanced tab See fig 6 This page is identical to the Advanced page of the Measurement dialog you probably know from standard FT IR experiments e g transmittance reflectance By clicking on the Load button you can load an existing XPM file that contains parameters which might turn out to be useful for your particular experiment By clicking on the Save button you can save the measurement parameters you have specified into a new XPM file for future use Furthermore you can enter a
10. 71500 C ADC Count 72000 72500 Exit Cancel Help Fig 10 Check Signal page displaying the correctly adjusted strain signal using the 2 ADC channel The signal is maximized and neither the top nor the bottom of the sinusoidal signal is clipped Note It is normal that the strain signal moves along the X axis when it is displayed on the Check Signal page Chromatography GC LC TGA E Basic Traces d Timing Li Advanced Optic Acquisition FT Background Check Signal Beam Path Spectral A ange Selection Full Scan Amplitude 1280 Position 69367 Save Peak Position Scale Display Scan range gt Show Store mode i nterterogram Spectrum ggg g500 Foooo FOS00 71000 71500 ADC Count 72000 72500 Exit Cancel Help Fig 11 Check signal page displaying the stress signal using the 2 ADC channel This signal is more noisy and weaker in intensity compared to the strain signal but it is still sinusoidal 1 4 Bruker Optik GmbH 4 2 Sample measurement Plug the cable of the 2 ADC channel into the STRAIN output of the controlling unit again Click on the Optic tab and select the detector option LN MCT MID plus External Sig Internal Pos 2 i e the MCT detector option that allows measurements with both ADC channels Finally start the measurement by clicking on the Basic tab and afterwards on the Start Chromatography Measurement
11. 9002 90 Dynamic FT IR Analysis of Polymers using continuous scan dual channel data acquisition USER MANUAL IES Ga 1 edition 2006 publication date September 2006 2006 BRUKER OPTIK GmbH Rudolf Plank Str 27 D 76275 Ettlingen www brukeroptics de All rights reserved No part of this manual may be reproduced or transmitted in any form or by any means including printing photocopying electronic systems etc without our prior written permission Brand names registered trademarks etc used in this manual even if not explicitly marked as such are not to be considered unprotected by trademarks law They are the property of their respective owner The following publication has been worked out with utmost care However Bruker Optik GmbH does not accept any liability for the correctness of the information Bruker Optik GmbH reserves the right to make changes to the products described in this manual without notice Table of Contents de 2 3 Ta sale V POV eie 3 MVE OGG eia E 4 Technical Requirements Sample Preparation and Installation assa 5 3 1 Sede dele ezla AGEN 5 3 2 Eide ezda baizue la 5 dedi Sampie DEDALO EE 6 3 4 AVS EAN AION AEE 6 Parameter Setting and NGO assa 8 4 1 Measurement parameters ccsscrncia 8 4 2 Sample mease MIS GA 15 4 3 Calibration meas rem Nt issevi an ieee tabilveiean 16 Alar FOCCSSING KAE 18 5 1 Applying the DMA algorithm to the calibration and sample GGe 18 5 2 Extraction of the calibrati
12. Signal tab fig 9 in order to check the infrared signal Depending on the displayed signal level you can increase or decrease the Aperture Setting on the Optics page In principle a higher signal level will always result in a better signal noise ratio S N but avoid to get too close to detector saturation 1 O Bruker Optik GmbH Chromatography GC LC TGA H Basic Traces Timing B Advanced Optic Acquisition FT Background Check Signal Beam Path Spectral Range Selection Full Scan Amplitude 25995 Position 7074r Save Peak Position C Scan range gt GA Shor Store mode C Interterogram Spectrum 3000 2500 2000 1500 C ADC Count Exit Cancel Help Fig 9 Chromatography dialog window Check Signal page showing the infrared signal spectrum or interferogram detected by the MCT detector with first ADC channel Select the option LN MCT Mid External Sig Internal Pos 2 i e MCT detector with GIE activated ADC channel and click on the Check Signal tab in order to check the strain signal stretching amplitude of the polymer stretcher See fig 10 Slowly increase the GAIN of the polymer stretcher controlling unit by turning the knob to the right until the strain signal of the stretcher is sinusoidal While the GAIN knob controls the amplitude of the Strain signal the BIAS knob controls the offset By using these two controlling knobs maximize the s
13. b See fig 8 This page is identical to the Optic page of the standard Measurement dialog window The parameters on this page are in both cases the same For detailed information about these parameters refer to the OPUS Reference Manual Set the following parameter values External synchronization Off Optical Filter setting Open Source setting MIR in most cases Beamsplitter KBr in most cases Measurement channel Sample compartment Sample signal gain x1 Background signal gain x1 Preamp gain Ref Scanner velocities Recommended values are 5 10 or 20kHz The list Detector settings includes 3 options for the MCT detector with the activated 2 channel See fig 8 Each detector channel can be accessed separately or both of them simultaneously The syntax of these entries is as follows detector type channel information detector position The detector with the activated 2 channel is LN MCT Mid See fig 8 This detector is mounted in the internal detector position no 2 of the spectrometer Therefore each of the 3 entries ends with Internal Pos 2 1 1 Bruker Optik GmbH 1 ADC channel The option for the detector with the first activated ADC channel does not include any channel information This channel records the standard infrared signal interferogram For this case it is the option LN MCT Mid Internal Pos 2 OE ADC channel The option for the detector with the second act
14. button The measurement result is stored in a dual channel 3D file The 3D block named S_IFG contains all the single interferograms and the 3D block named 2 Gin contains all the single strain traces Double clicking on the TZ IE data block in the OPUS browser opens a 3D window in which the single interferograms are displayed in a 3D plot left upper subwindow See figure 12 The file containing the measurement results is called OU because the sample is isotactic polypropylene OPUS Operator Default Administrator 3d Display mir_advanced ows 2 EO File Edit view Window Measure Manipulate Evaluate Display Print Macro Validation Setup Help 8X rT UGI F BO BA cs et EZO Z HEe dt Display mir_adyvanced ows 1 Ec A m Eunduistors Draw took 0 ms ta SATE SES o s Rotation IA Inclination 23 x 4826 00 x 9614 00 2 48 00 Z 96 00 IPP 0 Index 48 Z Points X Pons 0 0 2000 4000 6000 8000 10000 12000 14000 X Paints 0 6 0 6 0 4 E t 0 2 E nN Y No Y unit defined No Y unit defined A Se 0 2000 4000 6000 000 10000 12000 14000 0 20 40 60 80 100 120 140 x Points 2 Paints Ji 3d Displa adya d 15 2 No Active Task NUM O Fig 12 OPUS 3D window In the 3D plot left upper subwindow all the single interferograms acquired with the first ADC channel of the detector are displayed These interferograms are
15. clination 20 af Calibration 0 1 T 14826 00 d x 19614 00 Z 48 00 Z 96 00 e gt E GO a bl Calibration 0 Index 48 15900 d SEA O 2000 4000 6000 8000 10000 12000 14000 X Paints 0 6 0 6 a D oa a d E 304 dd DUA gt gt Oo GO gt 0 2 0 2 D 2000 4000 6000 8000 10000 12000 14000 D 20 40 60 80 100 120 140 X Points Z Paints lt j E 4 D m Display MIR_Advanced ows 1 E 3d Displa Y PIE A anced ows 2 b x Draw took 0 ms No Active Task JF NUM RF oO Fig 14 OPUS 3D window displaying the single interferograms of the calibration measurement The interferograms are in the S_IFG data block of the 3D file resulting from the calibration measurement These interferograms contain strong modulations due to the oscillating shutter aperture 1 7 Bruker Optik GmbH 5 Data Processing 5 1 Applying the DMA algorithm to the calibration and sample data Select in the OPUS browser the 3D file resulting from the calibration measurement by clicking on it with the left mouse button Then select in the Evaluate menu the DMA function Thereupon the DMA dialog window appears See figure 15 In the field File s for demodulation the data block S_IFG resulting from the calibration measurement should already be included If not just drag amp drop the data block S_IFG of the corresponding 3D file into this field Click on the
16. ct the output of the frequency generator with the BNC connector labeled INPUT of the polymer modulator controlling unit using a BNC cable Connect the controlling unit BNC output labeled STRAIN with the GIE channel Input of the detector typically labeled from LIA An adequate cable BNC plug at one end SMB plug at the other end is included in the delivery Turn on the controlling unit of the polymer stretcher 7 Bruker Optik GmbH 4 Parameter Setting and Measurement 4 1 Measurement parameters Select in the OPUS Measure menu the Chromatography function Thereupon the Chromatography GC LC TGA dialog window appears See fig 4 Chromatography GC LC TGA Basic Traces amp Timing Advanced H Optic Acquisition FT Background Check Signal Experiment Load DEFAULT Operator name beai Sample name sample Sample form sample fom Path C ProgrammeSOPUS6 JUEZ 43AMEAS File name WORE Background Single Channel Exit Cancel Help Fig 4 Chromatography dialog window Basic page On the Basic page you can store additional information such as sample name sample form etc On this page you also start the measurement after having entered all relevant parameters Click on the Traces amp Timing tab See fig 5 Make sure that the check boxes Compute Gram Schmid and Traces by spectral integration are not activated because they are only
17. e Phase correction tab This time select in the Phase correction mode drop down list the option Mertz Stored Phase Drag amp drop the data block SPH calibration phase spectrum in the Stored phase field See figure 28 All the other parameter settings have to be identical to the previous Interferogram to Spectrum conversions Click on the Convert button As a result two additional data blocks are added to the file resulting from the sample measurement The spectra of these data blocks are usually much smaller in intensity than the constant single channel sample spectrum The data block SSC contains the in phase single channel sample spectrum and the data block SSC contains the out of phase single channel sample spectrum 26 Bruker Optik GmbH interferogram to Spectrum Select Files store Apodization Limit Data Phase Correction Non Linearity Peak Search Phase correction mode Mertz Stored Phase Stored phase EF D Mtemp Calibration 0 1 Convert Cancel Help Fig 28 Calibration phase spectrum in the Stored phase field 5 5 Calculation of the in phase and out of phase absorbance change spectra Click in the OPUS browser with the right mouse button on the file resulting from the sample measurement and copy the original file See figure 29 be GEUZ w ee d bei ed Gide ME Bi erd QO Kre E
18. e resolution Limit phase resolution to i Direction Forward f Backward Datapoints 0 Even f Odd Convert Cancel Help Fig 21 Interferogram to Spectrum dialog window Limit Data page OO Bruker Optik GmbH On the Peak search page the peak search mode Absolute largest value and Automatic for the symmetry of the interferogram usually works fine as indicated in fig 22 However you can also fix the peak position ZPD to a particular value or optimize the position by entering a number larger than 0 Interferogram to Spectrum Select Files Shore Apodizatior Limit Data Phase Correction Non Linearity Peak Search eke ETI Do not search Use Optimize position Number of positions to test 0 Symmetry of interferogram C Symmetric O Asymmetric f Automatic Fig 22 Interferogram to Spectrum dialog window Peak Search page We recommend to do NO non linearity correction as shown in fig 23 Interferogram to Spectrum Select Files Apodization Limit Data Phase Correction Non Linearity Peak Search Detector cutoff 100 Modulation efficiency 08 Convert Cancel Help Fig 23 Interferogram to Spectrum dialog window Non Linearity page 93 Bruker Optik GmbH On the Phase Correction page we recommend to choose the Mertz phase correction fig 24 interferogram to Spectrum Select Files Store Apodi
19. echnology using so called amplitude modulation the dual channel acquisition technique described in this manual is clearly superior In an amplitude modulated Step Scan experiment a considerable fraction of the total measurement duration is used for accelerating stopping and repositioning of the interferometer mirror During this time no data is acquired making the Step Scan approach a rather inefficient one By contrast the dual channel technique uses the measurement time much more efficiently Furthermore the dual channel acquisition technique is also superior to the so called multiplexing technique which for example reduces the accessible spectral bandwidth and in some cases might degrade the signal quality Modern Bruker Optics research FT IR spectrometers are equipped with a 2 channel 24bit ADC Analog to Digital Converter which is integrated in the detector socket so called Digitect technology allowing for acquisition of all DMA relevant data while the interferometer mirror is continuously moving One channel of the ADC is used for recording and digitizing the repeated interferograms which are separated by constant time intervals Simultaneously the second ADC channel records and digitizes the time dependent strain data of the polymer stretcher As soon as such a measurement is finished the in phase and the out of phase spectra can be extracted using a smart software algorithm which is part of the OPUS software version 6 0 or
20. ed using the micrometer screw Turn off the controlling unit of the polymer stretcher Remove the sample and mount the shutter aperture which is included in the delivery into the moving jaw of the polymer stretcher Mount it in such a way that roughly half of the 1 6 Bruker Optik GmbH light is blocked Because without the sample the light intensity reaching the detector is higher than with sample so it might be necessary to select in OPUS a smaller aperture setting Change the file name in such a way that the file can easily be recognized as the file containing the calibration measurement results All the other parameter settings should be identical to the ones of the sample measurement Turn the controlling unit on again Then start a dual channel measurement i e with both ADC channels of the detector as already described in section 4 2 Sample Measurement Because the light intensity has been modulated during the calibration measurement the inclined lines can now easily be seen in the 3D plot See figure 14 The strain traces of the calibration measurement will look identical to the ones of the sample measurement C OPUS Operator Default Administrator 3d Display MIR_Advanced ows 2 EO Eile Edit Yiew Window Measure Manipulate Evaluate Display Print Macro Validation Setup Help A 38x dA eT oe 08 SA At ed tS E AS HEE pe i BX i Display MIR_Advanced ows 1 Rotation 30 E S 3d Display MIR_ Advanced ows 2 In
21. entical to the Acquisition page of the standard Measurement dialog window For detailed information about this dialog window refer to the OPUS Reference Manual Set the Wanted high frequency limit to 15000cm and the Wanted low frequency limit to Dg The High Pass Filter must always be set to open For the Low Pass Filter depending on the chosen scanner velocity see Optic page other settings might be useful as well For the parameter Correlation mode select the option Off and for the parameter External analog signals always select the option No Analog Value Incase of a polymer stretching experiment the parameters on the pages FT Background Beam Path and Spectral Range Selection need not to be specified 1 0 Bruker Optik GmbH Chromatography GC LC TGA H Basic Traces Timing a Advanced Optic Acquisition FT EEE Check Signal Beam Path Spectral Range Selection Wanted high frequency limit OGUI 15800 32 cm l Wanted low frequency limit D 0 00 cm 1 Laser wavenumber 15800 32 Interterogram size 14220 Points FT size 16 K High Pass filter Open MO Low Pass filter 10 KHz ze 15800 Gu Acquisition mode Double sided Ea Correlation mode OFF External analog signals Ho Analog Value E E xil Cancel Help Fig 7 Chromatography dialog window Acquisition page Click on the Optic ta
22. ety Manual 1984 by WHO World Health Organisation Caution Radioactive Material This warning symbol indicates the possible existence of radioactivity When working with radioactive material always observe the safety regulations and take necessary protective measures Wear protective clothing e g masks and gloves Non observance may cause severe personal injury or even death Caution Corrosive Substance This warning symbol indicates the possible existence of corrosive substances When working with corrosive substances always observe the laboratory safety regulations and take protective measures e g wear protective masks and gloves Non observance may Cause severe personal injury or even death 6 2 Waste disposal Dispose all waste produced chemical infectious and radioactively contaminated substances etc according to the prevailing laboratory regulations Detergents and cleaning agents must be disposed according to the special waste regulations 39 Bruker Optik GmbH 7 Appendix B Service Addresses Bruker Optik has an international network of branch offices and representations to ensure a competent customer service throughout the world The following list includes the addresses of Bruker headquarters For a complete list with the addresses and telephone numbers of the Bruker branch offices and representations worldwide refer to the internet http www brukeroptics com contacts worldwide html Nort
23. file in the OPUS browser These blocks have the same meaning as described above for the calibration measurement Drag amp drop the file resulting from the sample measurement in the standard OPUS spectrum window not in a OPUS 3D window 5 2 Extraction of the calibration phase spectrum Select the data block S_IFG containing the real part interferogram of file resulting from the calibration measurement Then select in the Manipulate menu the Interferogram to Spectrum function Thereupon the dialog window shown in figure 18 appears 20 Bruker Optik GmbH interferogram to Spectrum Phase Correction Non Linearity Peak Search Select Files Store Apodization Limit Data PT File s to convert E ek SE D temp Calibration 0 1 Convert Cancel Help Fig 18 Interferogram to Spectrum dialog window Select files page Click on the Store On this page you can choose the spectral range of the result spectrum See figure 19 For polymer experiments this is usually the fingerprint region To be on the safe side you can specify a somewhat broader spectral range as indicated in figure 19 It is extremely important that you activate the Save phase checkbox on the Store page The resulting calibration phase spectrum of this Interferogram to Spectrum conversion will later be needed to evaluate the sample data The power spectrum will not be needed thus you do not
24. gorithm is essential Therefore OPUS version 6 or higher is required For data acquisition and data visualization the packages OPUS CHROM and OPUS S3D are absolutely necessary 5 Bruker Optik GmbH 3 3 Sample preparation The foil you intended to analyze should be rectangular in shape with a width of approximately 25mm and a height of 10 to 45mm Experience shows that a roughly quadratic shape 25x25mm is preferable In order to avoid undesired multiple beam interferences roughen one side of the foil with abrasive paper The two edges of the foil which are to be clamped into the polymer stretcher should be masked from both sides with paper or carton etc This measure ensures a uniformly oscillating strain of the foil during the experiment and prevents the sample edges from slipping out of the mount A convenient way for preparing the sample is for example masking the sample edges with approximately 5mm wide stripes of so called post it paper used in many offices which has an adhesive area on one side fig 2 Fig 2 Prepared polymer sample isotactic polypropylene with its edges covered by so called post it paper The squares in the background have a side length of 5mm 3 4 Installation This manual describes only the installation using the Polymer Modulator by Manning technology Cool the detector by filling liquid nitrogen into the detector dewar Start the OPUS software Mount
25. h America Bruker Optics Inc 19 Fortune Drive Manning Park Billerica MA 01821 3991 USA Phone 1 978 439 9899 ext 5227 Fax 1 978 663 9177 www brukeroptics com info brukeroptics com Europe Bruker Optik GmbH Rudolf Plank Str 27 76275 Ettlingen Germany Phone 49 7243 504 619 600 Fax 49 7243 504 698 www brukeroptics de info brukeroptics de Asia Bruker Optik Asia Pacific Ltd Unit 601 6 F Tower 1 Enterprise Square No 9 Sheung Yuet Road Hong Kong Phone 852 2796 6100 Fax 852 2796 6109 asiapacific brukeroptics com hk No responsibility can be taken for the correctness of this information Subject to changes 33 Bruker Optik GmbH
26. he following warning labels indicate different dangerous situations which may be caused by improper use of the equipment Caution General Hazard the precautions described to avoid personal injury and or property damage Caution Electric Shock This warning symbol indicates electrical hazard This symbol is located near live parts or on enclosures behind which are live parts that represent an accidental contact hazard Never touch these parts Before removing the corresponding compartment covers and beginning any maintenance or repair work first turn off the main power switch and unplug the main power cable Ensure that all live parts do not come into contact with a conductive substance or liquid Non observance of these safety instructions can cause severe personal injury and or property damage gt Caution Hot Surface This warning symbol refers to components and surfaces which can become very hot during operation Do not touch these components and surfaces Risk of skin burn Be careful when operating near hot components and or surfaces gt Caution Frostbite This warning symbol indicates the existence of cryogenic materials e g liquid nitrogen required to operate the module e g cooling detector Skin contact with these liquids or cooled components causes severe frostbite Always handle the liquids with utmost care Observe the safety instructions for handling of cryogenic liquids Caution Harmful or Irrita
27. higher For a given measurement duration the S N Signal to Noise ratio of the dual channel technique will be distinctly superior compared with a Step Scan measurement 4 Bruker Optik GmbH 3 Technical Requirements Sample Preparation and Installation 3 1 Required hardware FT IR spectrometer with highly sensitive Digitect detector e g MCT or InSb including a 2 channel ADC with activated second channel A detector prepared for using the 2 channel is easily recognized by the two cables coming out at the rear side of the detector socket fig 1 Fig 1 Rear side of a Digitect detector with activated 2 channel in this example an MCT detector The dual channel ability is indicated by the two additional cables led out from the detector socket Polymer stretcher with controller installed in the sample compartment Frequency generator with frequency range of approx 0 70Hz and sinusoidal output voltage of 5V peak to peak in order to reach the full amplitude of the polymer stretcher Recommended polarizer for polarization dependent measurements Remark Using an additional optical band pass or low pass filter can distinctly improve the signal to noise ratio In this manner parts of the irrelevant spectral range can be blocked allowing the usage of a larger spectrometer aperture which in turn increases the S N in the spectral range of interest 3 2 Required software For data evaluation the DMA al
28. ing from the sample measurement See figure 26 This file contains the constant part of the single channel sample spectrum which is independent from modulation OA Bruker Optik GmbH isplay MIR_R amp D ows 1 Display Print Macro Validation Setup Help Agi Mak a i EO A TT d e Te d b bei lt gt JI ZO B Ss GRA SEO BU b B d E Calibration 0 1 a SO e faaiu S Sei hc S g PP o 1 4 2 SR S I G D IFG IFG RC HISTORY SZ 3d Display MIR_RD ows 2 ZE Calibration 0 1 8 GL frie BaL BE 2 g PP 0 1 Aia dies d iA iE it HISTORY Q F o Interferogram to Spectrum x 3 Phase Correction Non Linearity Peak Search Select Files Store Apodization Limit Data S File s to convert 5 D temp IPP 0 1 Q 2 a GA E Q GO 2 9 Convert Cancel Help 8 N 9 GA GA a Q GO F 9 14000 13000 12000 11000 10000 a000 s000 7000 6000 5000 4000 3000 2000 1000 SS gt 4 amamak x Draw took 0 ms No Active Task UE NUM RF a Fig 25 Appling the Interferogram to Spectrum function to the constant interferogram of the sample measurement Display MIR_R amp D ows 1 e ate Display Print Macro Validation Setup Help E bel ad i A ZZ ea eg bo T ZZ a TT 4 Eg Calibration 0 1 SE SEN fe SE TIEEO 1 its lire wii re J 3d Display MIR_RD ows 2 SE Calibration 0 1 Vain i Eun Bizk Edi eke SG ASEA B e a E Fa ehre ket
29. inusoidal signal but avoid in any case that the top or the bottom of the signal are clipped flattened This procedure is described more detailed in the Polymer Modulator manual provided by Manning Applied Technology Also check whether the stress of the sample is correctly adjusted To do this remove the cable of the 2 ADC channel from the STRAIN BNC output of the controlling unit and plug it into the STRESS BNC output On the Check signal page once again a sinusoidal signal is displayed which usually contains more noise and is weaker in intensity compared to the strain signal See fig 11 To optimize the stress signal carefully adjust the micrometer screw of the polymer stretcher The sample stress is one of the most crucial parameters in the whole experiment too low as well as too high stress may lead to bad results Therefore it is recommended to run the experiment with different stresses and find out the best adjustment for your particular sample Note The STRAIN and the STRESS signal can be alternatively checked with an oscilloscope 1 3 Bruker Optik GmbH Chromatography GC LC TGA a Basic Traces amp Timing a Advanced Optic Acquisition FT Background Check Signal Beam Path Spectral Range Selection Full Scan Amplitude 9526 Position 71140 Save Peak Position lt Scan range gt Show Store mode interferogram C Spectrum 69000 69500 70000 70500 71000
30. ivated ADC channel includes as additional channel information External Sig in some cases demodulated This channel records the strain signal of the polymer stretcher For this case it is the option LN MCT Mid External Sig Internal Pos 2 Dual channel acquisition For a measurement with both channels select the option which contains plus as additional channel information Chromatography GC LC TGA EE Basic Traces amp Timing E Advanced Optic Acquisition FT Background Check Signal Beam Path Spectral Range Selection External synchronisation OF Y bd Source setting MIF bd Bearmeplitter KBr OpticalFiterseting Open o8 ei Apetture setting 25mm Measurement channel Sample Compartment E Background meas channel Sample Compartment e Detector setting JUNM Mid Internal Pos 2 Preamp gain Ref AT OLalGs riena II Scanner velocity INMA Midlotermel Pazzi UN MU Mid External Sig Internal Pos 2 LA MCT MID plus External Sig Internal Pos 2 ua Classic Style Chl External Sample signal gain Ga Background signal gain Delay after device change Delay before measurement Optical bench ready Exit Cancel Help Fig 8 Chromatography dialog window Optic page showing the available detector options Select the option LN MCT Mid Internal Pos 2 i e MCT detector with 1 activated ADC channel and click on the Check
31. nt Material This warning label indicates the existence of harmful or irritant material e g ZnSe window material Observe the safety instructions on the packaging and the safety data sheets attached Non observance may cause severe personal injury or even death Caution Toxic Material This warning label indicates the existence of toxic material e g KRS 5 material Observe the safety instructions on the packaging and the safety data sheet attached Non observance may cause severe personal injury or even death Beside the dangers described above there can also be hazards caused by the sample material Depending on the type of hazardous substances used you have to observe the specific substance relevant safety instructions Put on the specific warning label on the corresponding module position The label must be legible and permanently discernible The following list exemplifies types of hazardous substances 31 Bruker Optik GmbH Caution Infectious Material This warning symbol indicates the possible existence of biologically dangerous and infectious material When working with this kind of material always observe the prevailing laboratory safety regulations and take necessary precautions and disinfection measures e g wearing protective clothing masks gloves etc Non observance may cause severe personal injury or even death For information on how to use dilute and efficiently apply disinfectants refer to the Laboratory Biosaf
32. on phase GOGOETA 20 5 3 Extraction of the constant part of the single channel sample spectrum 24 5 4 Calculation of the in phase and out of phase single channel sample spectra 26 5 5 Calculation of the in phase and out of phase absorbance change spectra 27 Appendix A Safety NfOMalON s aenean G 31 6 1 Waning ziaz eNA 31 6 2 Waste GIS DOS all AEA 32 Appendix B Service Addresses ss 33 1 Bruker Optik GmbH Bruker Optik GmbH 1 Safety Advice If the Polymer Modulator by Manning Applied Technology was part of your delivery please follow the safety warnings and instructions given in the related manual from Manning Applied technology If you use a polymer stretcher of an other manufacturer please consult the respective manual for safety advice In the appendix of this document the most important warning labels and the adequate precautions are listed 3 Bruker Optik GmbH 2 introduction Applying dynamic strain on polymers or related materials combined with phase sensitive FT IR spectroscopy provides insight into the dynamic behavior and flexibility of these materials Besides the general interest in the in phase and out of phase spectra measurement series e g with different modulation frequencies or polarization angles can be of further help to gain access to relevant data concerning the dynamic behavior of the investigated molecules Compared to earlier approaches based on the Step Scan t
33. ple shown in figure 13 there are approximately 2 times more periods along the z axis than along the x axis OPUS Operator Default Administrator 3d Display mir_advanced ows 2 BA TO Eile Edit View Window Measure Manipulate Evaluate Display Print Macro Validation Setup Help 8X Seo ki ZE EO Be ee AX ws Rotation b e Ga Display mir_advanced o i 13d Display avanca beteta 25 E ed Q x 4826 00 b 9614 00 EEE isplay mir_advar Z 48 00 b Z 96 00 IPP 0 Index 48 Z Points LA Fi TIK W Du Gu Tu 4 Mi AD A 7 k la W Yi Wy 2000 4000 6000 8000 10000 12000 14000 X Points a E b Y No Y unit defined GO Oo 0 2000 4000 6000 8000 10000 12000 14000 0 20 40 60 80 100 120 140 X Points Z Points bx No Active Task O Fig 13 OPUS 3D window In the 3D plot left upper subwindow all the single strain traces acquired with the second ADC channel of the detector are displayed The strain traces are in the 2_chn data block of the 3D file On the basis of the contour plot in the right upper subwindow you can assess the phase shift of the strain signal by the inclination of the parallel lines indicated by the angle a 4 3 Calibration measurement Hint Before you remove the sample in order to start the calibration measurement it is recommended to repeat the sample measurement with slightly different stresses The stress can be adjust
34. the copied file See figure 31 Out of phase absorption change SSC sample SSC sample 28 Bruker Optik GmbH Spectrum Calculator Spectrum Calculator sin cos ban Pi O Mtemp lPP O GEG I b Os tempylPP O 25cm E ic E TI Data Block BRA AE ZA E EZ A e EA E E ol fag oN a ZA Za KEA PD p E xit Cancel Help Fig 31 Spectrum Calculator Calculating the in phase absorbance change of the sample After both types of absorbance changes have been calculated the evaluation is finished Save the result spectra Figure 32 shows the result OO Bruker Optik GmbH i OPUS Operalor Diari Administrator Display MEK HOE ows 1 bebe Display Bih Hen dda ue bek EZ A ZN Ek E day MIH EO E Me d AZT Ma T d FPI Z ETO a EIF Iiia MIP FD oe ZZ Caon 1 fa ol EH Hl A SP Late Serer T d d OE Ee Hele press Fl Fig 32 In phase red and out of phase blue absorbance change of the polymer sample Bruker Optik GmbH 30 6 Appendix A Safety Information 6 1 Warning labels When operating the equipment you have to observe a number of safety instructions which are highlighted by various warning labels This section describes the warning labels and explains their meaning All warning labels on the equipment must always be kept legible Immediately replace worn or damaged labels T
35. the sample into the clamping jaws of the polymer stretcher Ensure that the sample is mounted symmetrically See fig 3 Slightly stretch the sample using the micrometer screw The sample is correctly mounted if it has no crinkles Put the polymer stretcher into the sample compartment of the spectrometer If you want to measure with a polarizer and or an optical filter put it into the mount on right hand side of the polymer stretcher 6 Bruker Optik GmbH Connect the controlling unit of the Polymer Modulator to power supply but still keep it turned off Turn the bias and the gain control knobs fully to the left minimum position Connect the polymer stretcher and the controlling unit panel location labeled HEAD using the thick cable which is included in the Polymer Modulator package Fig 3 Polymer stretcher with correctly mounted polymer sample Connect the frequency generator to the power supply and turn it on Choose a sinusoidal output and adjust the voltage amplitude to a value below but close to 5V peak to peak Then adjust the generator to the desired modulation frequency A commonly used frequency is 18Hz however other frequencies can be of interest as well In the first few minutes after adjusting the frequency many frequency generators tend to drift slightly typically in the OI decimal place Before starting a real measurement always make sure that the displayed frequency does not change anymore Conne
36. zation Limit Data Phase Correction Non Linearity Peak Search Phase correction mode Stored phase Convert Cancel Help Fig 24 Interferogram to Spectrum dialog window Non Linearity page Click on the Convert button As a result two additional data blocks are added to the file resulting from the calibration measurement The first data block SSC is the part of the single channel calibration spectrum which is in phase with the modulation The second data block SPH is the phase spectrum which has been created by calculating the SSC spectrum The phase spectrum SPH will be needed later in order to calculate the correct sample spectra 5 3 Extraction of the constant part of the single channel sample spectrum Select the data block IFG of the file resulting from the sample measurement This data block contains the part of the sample infrared signal which is independent from the modulation Select in the Manipulate menu the Interferogram to Spectrum function Thereupon the Interferogram to Spectrum dialog window appears See figure 25 This time deactivate you Save Phase check box on the Store page For the other parameters use exactly the same settings as done before in case of the file resulting from the calibration measurement Click on the Convert button As a result an additional data block SSC will be added to the file result
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