FTIR Talk Letter Vol. 05
Contents
1. s La a TI j T MP oh IN an MM r 75 E 5 25 Tie E a premere rore prr 4000 3500 3000 2500 2000 1750 1500 1250 1000 730 Caffeine Microscope Transmission Method Diamond Cell 1 om Fig 1 Transmission Spectra of Caffeine Powder Fig 1 shows that an interference pattern is superimposed over the sample spectrum measured using two cell plates such that the baseline exceeds 100 The interference pattern occurs due to the parallel space between the two diamond disks When measurements are conducted with two cell plates the noise increases near the 2000 cm absorption band of diamond For the reasons above after a sample is crushed between the two cell plates the sample adhered on a single cell plate is analyzed As an exception rubber and other elastic samples are measured while sandwiched between the two cell plates 2 Sample Quantity Only a trace amount of sample is required for measurement Too much sample lowers the baseline and results in a spectrum with saturated peaks Fig 2 shows an example of this using a caffeine power sample The red line shows the spectrum obtained with an appropriate sample volume the green line is the spectrum for an excess of sample 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 Caffeine Excessive Sample Microscope Transmission Method Diamond Cell 1 cm Fig 2 Transmis2. Why You Should Use Macro Programs To Simplify Routine Tasks Microscope Measurement Techniques Transmission Measurements Question 7 Up to what size can measure with an IR microscope E ae i E lt 8 a 7 ONE z EX ve las CUN Bx gt E S NN i P A AN NI In xA IA A ALD LN n p J ne_2006 Why You Should Use Macro Programs To Simplify Routine Tasks Each generation of Shimadzu FTIR workstation software offers powerful macro functions to simplify various tasks The latest IRsolution FTIR control and data processing software inherits this tradition of powerful macro functions This FTIR Talk Letter introduces the possibilities offered by macro functions tomated Measurement If measurements are required on two types of sample with the following different measuring conditions for each Sample A Resolution 2 cm wavenumber range 400 to 4000 cm Sample B Resolution 4 cmt wavenumber range 750 to 3500 cm In this case it is necessary to determine which sample is being measured and then ensure that the measurement parameters are correct This process involves the following steps 1 Set the resolution to 2 cm 2 clicks 2 Set the wavenumber range 400 to 4000 2 clicks keyboard entry Measure the background 1
3. Industry Ae E TIE TESTA LT ay Ta 4 rr Analysis Guidebook Chemical Analysis Guidebook Electronic and Semiconductor Solutions for Science To support customers engaged in the FTIR analysis Shimadzu has established a global service network incorporating h A ES m customer support training and service centers in the USA Germany China and Singapore as well as in Japan Shimadzu provides comprehensive support services including instrument maintenance training workshops and the provision of relevant information to meet customer needs regarding both software and hardware 4 Ln i SHIMADZU DO BRASIL COM RCIO LTDA Avenida Marqu s de Sao Vicente 1771 Barra Funda CEP 01139 003 S o Paulo SP Brasil Phone 55 11 3611 1688 Fax 55 11 3611 2209 SHIMADZU HONG KONG LIMITED Suite 1028 Ocean Center Harbour City Tsim Sha Tsui Kowloon HONG KONG Phone 852 2375 4979 Fax 852 2199 7438 SHIMADZU INTERNATIONAL TRADING SHANGHAI Co LTD SHANGHAI OFFICE 24th Floor Shanghai Xin Hualian Building No 755 Huaihai Zhong Lu Shanghai China Phone 86 21 6472 8442 Fax 86 21 6472 8648 Overseas Offices Istanbul Moscow URL http www shimadzu com 3295 12509 30A NS
4. click Load sample A Measure sample A 1 click Unload sample A Set the resolution to 4 cm 2 clicks Set the wavenumber range 750 to 3500 cm 2 clicks keyboard entry 9 Measure the background 1 click 10 Load sample B 11 Measure sample B 1 click and 12 Unload sample B If this process is handled by a macro the following dialog box is displayed Select the sample you want to measure Sample Sample C Click Sample A to set the measurement parameters for sample A and measure the background The following dialog box is displayed when the background measurement is complete 3 4 5 6 8 FTIR TALK LETTER vol 5 IR solution Basic j x Set Sample to the sample compartment and click Ok button Load sample A in the sample compartment and click OK to start sample measurement When sample A measurement are completed a dialog prompts whether to measure another sample Click Yes to display the sample selection dialog box again Click Sample B to measure sample B in the same way Measurement finished X Measurement has Finished Measure another sample Cancel When handled by a macro the process described above can be summarized as follows 1 Run the macro 2 Click the Sample A button 3 When the background measurement is complete Load sample A and click OK 4 Unload sample A 5 Click Yes in the measur
5. 900 0 800 0 700 0 1 cm Fig 2 Magnified View of Fig 1 FTIR TALK LETTER vol 5 Application Guide Books available from Shimadzu ee e Access lo your success E SHIMADZU Analysis Guidebook Pharmaceutical Analysis Analysis Guidebook Food Analysis Guidebook Pharmaceutical Shimadzu Overseas Customer Support OVERSEAS SUBSIDIARIES OVERSEAS OFFICES J V CUSTOMER SUPPORT CENTERS 17 SHIMADZU SHIMADZU CORPORATION International Marketing Division 3 Kanda Nishikicho 1 chome Chiyoda ku Tokyo 101 8448 Japan Phone 81 3 3219 5641 Fax 81 3 3219 5710 Cable Add SHIMADZU TOKYO SHIMADZU SCIENTIFIC INSTRUMENTS INC 7102 Riverwood Drive Columbia Maryland 21046 U S A Phone 1 410 381 1227 Fax 1 410 381 1222 Toll Free 1 800 477 1227 SHIMADZU EUROPA GmbH Albert Hahn Strasse 6 10 47269 Duisburg F R Germany Phone 49 203 7687 0 Fax 49 203 766625 SHIMADZU ASIA PACIFIC PTE LTD 16 Science Park Drive 01 01 Singapore Science Park Singapore 118227 Republic of Singapore Phone 65 6778 6280 Fax 65 6779 2935 SHIMADZU SCIENTIFIC INSTRUMENTS OCEANIA PTY LTD Units F 10 16 South Street Rydalmere N S W 2116 Australia Phone 61 2 9684 4200 Fax 61 2 9684 4055 ee e Access to your success E SHIMADZU amp SHIMADZU Bolittions for Science Analysis Guidebook Chemical Industry Analyses Analysis Guidebook Electronic and Semiconductor
6. ement complete dialog box 6 Click the Sample B button 7 When the background measurement is complete Load sample B 8 Click OK and 9 Unload sample B to complete the measurements Comparing the required number of mouse clicks and keyboard entries shows Manual operation 13 mouse clicks several numeric entries from the keyboard Macro operation 6 mouse clicks Using the macro reduces the number of mouse operations required No numeric entry is required which eliminates the chance of careless errors cation of input IRsolution macro has more freedom of designing user interface than previous software Many of parts to receive user input these are called control can be available on IRsolution You can build in useful user interface bycombining these controls Available controls are shown below Fruit Selection Which Fruit do you like Cancel Radio buttons to select a single item from multiple options Fruit Selection x Which Fruit do like v Apple Grape Check boxes to select multiple items from multiple options Fruit Selection x Input your Favairte fruit from apple orange and grape L ancel Edit box for keyboard entry Fruit Selection Select your fayoirbe fruit from the list Orange Grape Fruit Selection Select your Favoirte fruit from the list Apple Grape Cancel Combo box to select from preset cha
7. he right We hope that this information assists customers who are considering introducing macro programs to enhance working efficiency 4 mU 4 li FTIR TALK LETTER vol 5 Microscope Measurement Techniques Transmission Measurements Kyoto Customer Support Center Analytical Applications Department Analytical amp Measuring Instruments Division Sachio Murakami This FTIR Talk Letter Vol 3 and 4 introduced the accessories used for IR microscope measurements and how to use them This FTIR Talk Letter introduces analytical techniques using IR microscope transmission methods Diamond cells or a KBr or BaF2 window material are often used for transmission measurements However great care is needed to obtain good quality spectra with such cells Four important precautions when conducting measurements with a diamond cell are described below 1 Using a Diamond Cell A diamond cell incorporates two cell plates which compress the sample Subsequently measurements are conducted on the sample adhered on a single cell plate If measurements are conducted with both cell plates an interference pattern is superimposed over the sample spectrum Fig 1 shows the example of caffeine powder analyzed using a diamond cell The red line shows the spectrum of the sample on a single cell plate the blue line shows the spectrum measured with the sample sandwiched between two cell plates
8. ing 100 Consequently position the sample in the center of the diamond cell and measure the background as close to the sample as possible If the sample is not in the center of the diamond cell the background must also be measured near the actual sample position away from the center of the cell An interference pattern may appear on the baseline if it is measured on a smooth part of the sample surface Fig 4 shows examples of polypropylene PP measurements The insert shows a photograph of the actual measured positions 4x0 350 3X0 250 1750 150 1250 100 7 Polypropylene PP Microscope Transmission Method Diamond Cell Tem Fig 4 Transmission Spectra of Polypropylene PP Care is required if an interference pattern appears on the baseline as the interference pattern may hide small peaks 4 Using the Aperture If the foreign matter sample is relatively large do not increase the aperture It is more effective to set the aperture to approximately 50 and measure the spectra at a variety of positions than to increase the aperture Constant results at each measurement position indicate that the foreign matter is a single component or a uniform mixture Sample identification and analysis by spectrum searching are possible on a spectrum not affected by peak saturation or an interference pattern FTIR TALK LETTER vol 5 However differences apparent between the spectra indicate a non uniform mixture of foreign matte
9. r In this case differential spectra are determined to obtain a spectrum for each component Fig 5 shows the measurement of foreign matter on the surface of paper The aperture is set to 0 x 0 4X0 300 2500 50 190 1250 1099 70 Foreign Matter Microscope Transmission Method Diamond Cell 1 cm Fig 5 Transmission Spectra of Foreign Matter on the Surface of Paper The diagram shows a position of strong intensity near 1500 cm 5 1 and a position of strong intensity near 1000 cm 5 2 The position near 1000 cm results from a normal component of paper cellulose Calculating the difference between the spectra from S 1 to S 2 in Fig 5 gives the spectra for just the foreign matter Fig 6 shows the resulting differential spectrum Spectrum searching of the differential spectrum in Fig 6 indicated the foreign matter to be magnesium carbonate i i i i i i i i i i i i i i i tQ A ERES e rM p E 8 i i i i i i i i i i i i i i i 4000 3500 3000 2500 200 1750 1500 1250 1000 750 Differential Spectrum 1 am Fig 6 Differential Spectrum This FTIR Talk Letter introduced four important precautions when using a diamond cell for transmission methods with an IR microscope Follow these precautions to more effectively utilize your IR microscope Analysis up to 10um x 10 is generally possible although this depends on the measuremen
10. racter strings or make a keyboard entry Fruit Selection x Select pour Favorite fruit from the list Apple m Apple Orange Grape Cancel Dropdown list box a list box to select from preset character strings W button displays the candidate items FTIR TALK LETTER vol 5 Automating multiple data processing operations in a designated sequence with a macro ensures they are conducted reliably The measured data is processed after measurements are complete and only the processed results are displayed Some special data processing which is available by combining some standard data processing can be done with easy operation by macro program In case you calculate the corrected height of a peak by selecting peak top and peak bottom you need many steps of operation to get the final result You can decrease most of the steps by macro program which can process many steps of operation automatically A macro program can call up external programs This feature uses external programs to expand the functionality of IRsolution such as accessing the RS 232C port Macro programs are introduced above As macro programs offer higher functionality it may become difficult for customers to create detailed macro programs Therefore Shimadzu handles all tasks from designing the specifications to writing the program and instruction manual The standard procedure to create a macro program is shown at t
11. sion Spectra of Caffeine Powder As an excess of sample cannot be compressed thinly enough measurements must be conducted on a thick film This results in a spectrum that is difficult to analyze due to a lower or inclined baseline and saturated peaks as shown by the green line in Fig 2 Therefore the amount of sample must be adjusted to create a thin layer on the diamond cell 3 Background BKG Measurement and Sample Measurement Positions The positions chosen for background measurement and sample measurement have an influence on the spectrum Choosing a background measurement position as close as possible to the sample measurement position achieves a good spectrum with approximately 100 baseline Fig 3 shows the spectra for cellulose fiber obtained with BKG measured in a corner of the diamond cell BKG1 and with BKG measured near the sample BKG2 FTIR TALK LETTER vol 5 125 75 aci ARSE ter 50 LES SEPSIS mss cem ROMANS ARAN ARS 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 Cellulose Microscope Transmission Method Diamond Cell 1 Fig 3 Transmission Spectra of Fibrous Foreign Matter The amount of transmitted IR light differs between the center and edges of the diamond cell The amount of IR light is lower if BKG is measured away from the center of the cell In this case sample measurements result in a spectrum with a baseline exceed
12. t method and type and form of the sample The size is related to the instrument sensitivity light intensity and the wavelength IR range 2 5 to 25um For example conducting measurements with the aperture set to 10um x 10um may result in the peak broadening or the appearance of ghost peaks in the region exceeding 10um to 1000 Fig 1 shows an example of analyzing a novolac resin film on a metal plate with different aperture sizes 05 0 0 4000 0 3000 0 2000 0 1500 0 1000 0 1 cm Fig 1 Specular Reflection Absorption Spectrum of Novolac Resin at 5 10um and 30um Aperture Up to what size can I measure with an IR microscope ABS To avoid influence of noise measurements are conducted using different numbers of accumulations for each aperture setting 3Oum x 30um Resolution 8 cm accumulations 20 approx 8 s 1Oum x lOum Resolution 8 cm accumulations 100 approx 40 s x bum Resolution 8 accumulations 400 approx 160 s Fig 2 shows a magnified view of the 1300 to 700 cm range in Fig 1 Even at 5um x 5um aperture this view reveals the sample to be novolac resin However deformation of the spectrum at the low wavenumber end is clearly apparent Fig 2 This shows that care is required with spectral distortion at the low wavenumber end if the aperture is set to 10um x 10 or less 0 8 0 6 0 4 0 2 1300 0 1200 0 1100 0 1000 0
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