A Flex Fle ible, ible, Po Po t r a t ble Inst Ins rument rumen Plat Pla fo f rm r fo FT IR Analys Analy is

Transcription

1 A Flexible, Portable Instrument Platform for FT IR Analysis Series

2 Introduction StandardlaboratoryFT IRspectrometers have many desirable qualities, but are not generally considered portable. Dedicated, portable instruments can provide quality spectra, but may not have the sampling flexibility desirable for various experiments. A new series of FT IR instruments are designed that can be used as dedicated, portable spectrometers, or, can be configured with multiple sampling techniques, thus extending the analysis capability with a minimal footprint. The series of instruments can also be utilized as a basic interferometer engine for user designed experimental stations.

3 The Portable FT IR Series Instrument (w/transmittance sample FT/IR 4000 chamber) Laboratory performance for a field analysis instrument An expandable compact FT IR Dedicated systems for analysis applications Et Extensive array of sampling accessories

4 User Friendly Operations User friendly Control Panel Instrument optics verification Sleep mode for economical operation Basic instrument operations without PC access Validation program Regulatory compliance (ASTM, JP, EP, JIS) Automated instrument validation system for reliable data.

5 Series Specifications Model name Measurement wavenumber range 7, cm -1 7, cm -1 15, cm -1 Resolution 4-16 cm cm cm -1 Detector - standard DLATGS DLATGS - option MCT (removable and replaceable / InGaAs,InSb,MCT(removable and replaceable / automatic) automatic) N-MCT,W-MCT,InGaAs (for FT-Raman) Beam splitter - standard - option Ge/KBr Ge/KBr Broad band KBr Si/CaF2 Broad band KBr Light source - standard d Ceramic Ceramic Halogen - option Halogen (automatic) Ceramic (automatic) Interferometer 45 degree incident Michelson type interferometer Aperture N/A 5 positions Purge Option A/D converter 18 bit 21 bit Drive mode DSP electromagnetic drive Mechanical bearing DSP electromagnetic drive Mechanical bearing Interferometer speed 2, 4 mm/sec 0.5, 1, 2, 3, 4 mm/sec Rapid scan N/A 40 Hz (option) Communication port USB 2.0 Dimensions and weight 270 mm(w) x mm(d) x 24 5mm(H), 12 kg (main unit only )

6 Modular Design for Custom Configurations Standard model with superior performance as compact FT IR Advanced model with excellent performance and expandability Dedicated NIR model for in situ analysis Transmission measurement chamber SMART TECH accessory Near IR reflection measurement Fiber interface Gas cell chamber Single reflection ATR, multi bounce ATR IRT 1000 FT IR microscope Auto sampler Multi ChambIR ConnectIR Optical System Universal Optical Attachment

7 Modular Configurations Single purpose measurement (Single accessory) Multiple purpose measurement (Multiple accessories) Various ATR Process Monitoring Gas Analysis Multi ChambIR ConnectIR Optical System Universal Optical Attachment and Universal Optical Attachment and dedicated system

8 Dedicated Measurements: Oil Analysis Using a Single Reflection ATR Simple qualitative analysis of various oils such as vegetable oil, animal oil, industrial oils and fats can be accomplished using an ATR by simply placing the liquid sample onto the ATR crystal without dilution of the sample Single reflection ATR Wavenumber [cm 1] ATR spectra of various oils

9 Dedicated Measurements: Polarized Single Reflection ATR Molecular Orientation of Polymers A polarized single reflection ATR accessory can be used to evaluate the molecular orientation of polymer compounds, regardless of the film thickness. The evaluation of the z axis molecular orientation is also possible. p polarization s polarization y z x Polarized Single Reflection ATR Polypropylene p-polarization (ǁ) s-polarization ( ) Ab bs x Wavenumber [cm 1] ATR IR spectra of a liquid crystal (p polarization and s polarization) y Wavenumber [cm 1] Wavenumber [cm 1] Calculation results of molecular orientation = 0.95

10 Dedicated Measurement: 65 Incident Angle ATR ATR PRO650-G Single Reflection ATR (65 incident angle) A 65 incident angle ATR can easily measure samples of high refractive index, such as carbon filled rubbers or silicon wafers, offering a lesser depth of penetration for infrared spectra of optimal quality. 0.1 ATR PRO450-S Wavenumber [cm -1 ] Measurement of a surface oxide film Si-O on Si Comparison table of 45 and 65 incident angle Incident angle Measurement limit of the prism n 1 n 2 Depth into the sample 1000cm -1 n ~ 700 cm µ 65 ~ 700 cm µ N : index of refraction of the prism N 1 : index of refraction of the prism N 2 : index of refraction of the sample

11 Dedicated Measurement: Heated Single Reflection ATR Oil Oxidation Analysis Heated Single Reflection ATR A heated ATR accessory provides the ability to monitor structural changes with temperature. The analysis of the oxidation of unsaturated fatty acid components while heating an oil to 180 C is displayed. cis trans Spectral changes with air atmosphere cis air N 2 air N 2 trans Peak area change (cis 3010 cm 1 ) Peak area change (trans 966 cm 1 ) Spectral changes with N 2 purge

12 Dedicated Measurement: Process Monitoring Quantitative Analysis of Water in Organic Solvents Using a Sipper System 1.2 Water contamination of organic solvents can be a critical control factor for solvent 1 washes of manufactured products. A sipper system minimizes sample contact 0.8 with atmospheric contamination, providing accurate quantitative analysis of the water content. Xylene Xylene (100 ppm water) Wavenumber [cm 1] Overlay of xylene and 100 ppm water contamination. One measurement requires less than 60 seconds so atmospheric contamination is minimized due to use of the sipper system. 100 Flow cell (CaF 2 Window) 2 Sipper system Quantitative program Sipper system Create calibration curve program

13 Dedicated Measurement: Process Monitoring Analysis of UV Cured Resin by Rapid Scan System 1 With a high speed scan system, the analysis of rapid reaction processes are possible. This slide shows the curing process of a UV cured resin with in situ monitoring while the sample is simultaneously irradiated with UV light After UV irradiation of the sample 0.2 Before UV irradiation of the sample UV irradiation system Resolution: 4 cm -1 Accumulation: 1 Time: 50 seconds Detector: MCT Wavenumber [cm 1] IR spectrum The C=O peak decreases after the polymerization process is initiated by UV exposure. Utilizing a rapid scanft IRand and a UV light it is possible to evaluate the various materials by changing the component ratio and types of compounds Time [msec] Monitoring (peak1637 cm -1 )

14 Dedicated Measurement: Simultaneous Monitoring of Greenhouse Gases Using a Long Path Gas Cell FT IR can rapidly measure multiple gas components in concentrations as low as a few ppm. A dedicated FT IR gas analysis system can be used for gas monitoring applications utilizing three different types of gas cells: glass, stainlesssteel or full vacuum and a gas monitoring program CO SO 2 NO 2 Greenhouse gases (PFC) N 2 O CH Wavenumber [cm-1] IR spectra of gases 2 Long path gas cell 1 PFC 116 PFC PFC 14 PFC Simultaneous monitor program for gas concentration 0 PFC Wavenumber [cm 1] Glass Stainless steel Full vacuum

15 Multi Purpose Measurements Multiple l purpose measurement (Multiple accessories) Multi ChambIR Multi Tech Optical Rail Universal Optical Attachment

16 Multi Technique System: Multi ChambIR Multi ChambIR is a compact accessory system that includes optics for simple transmission/reflection accessories, a single bounce ATR and a dff diffuse reflection accessory to provide multiple sampling techniques in the same system without the need to change accessories. Accessory selection using the Multi ChambIR is accomplished either by the PC or the integrated instrument Control Panel for measurements that are quick without complicated dlight path changes or the exchange/alignment of accessories. NIR measurement capability is also available by adding optional components to the instrument. ATR Transmission (Reflection) DR

17 Multi-Tech Optical Rail System A maximum of three different accessories can be configured, available as parallel sampling techniques, depending on the measurement purpose. The desired accessory is accessed using PC control or the instrument Control Panel without needing to swap out accessories and align them. Multi tech Optical Rail Accessory 1 Accessory 2 Accessory 3

18 Multi Tech Evaluation System: Quantitative Analysis of Trans fatty Acid with Heated ATR trans peak cis peak FT IR analysis of trans ftt fatty acid content tis easily performed without complicated preparation of the samples. The quantitative measurement of fatty acid content based on the AOAC method is obtained while controlling the temperature of the sample with a heated ATR accessory Wavenumber [cm -1 ] Quantitative results for trans fat content Sample Trans fat content [%] Multi Tech Optical Rail Area margarine 3.1 cooking oil sesame oil 0.7 Heated ATR Heated Transmission Cell NIR DRIFTS Comprehensive evaluation system Concentration of trans fat [%] olive oil 0.8 chili oil 1.2 A calibration curve based on the 966 cm 1 of the trans peak was created using standard materials outlined by the AOAC method. Quantitative analysis of the trans fatty acid content of commercial dairy products was executed with the defined calibration curve.

19 Multi Tech Evaluation System: Iodine in Fat Measurement with FT NIR Using a Peltier Thermostatted Transmission Cell Iodine value can provide an index of the degree of unsaturation of lipids in oils. The combination of a Peltier controlled transmission cell and the accuracy of an FT NIR measurement improves measurement accuracy because temperature changes in the NIR spectrum are minimized. NIR spectra of 24 oil samples Sample Measurement Results (n=30) PLS model (r=0.9996) Multi Tech Optical Rail A(102.6) B(115.7) C(56.3) D(123.8) E(116.7) Average SD Heated Heated Transmission NIR DRIFTS ATR Cell Comprehensive evaluation system Represents the measurement result of Wijs Cyclohexane Method A PLS calibration curve was created using the NIR spectra of various oil samples, the iodine values acquired for the oils by the conventional Wijs Cyclohexane Method.

20 Multi Tech Evaluation System: Quantitative Analysis of the Soy Bean Nutrients Using NIR A PLS calibration model is created by using NIR spectra and values measured by another analysis method. The subsequent PLS models can be used to easily obtain a non destructive quantitative analysis of food ingredients PLS analysis results for soy bean nutrients Wavenumber [cm-1] Water Multi Tech Optical Rail Heated ATR Heated Transmission Cell NIR DRIFTS Comprehensive evaluation system Carbohydrate Fat Protein

21 Multi Tech Evaluation System: Quantitative Analysis of FAME Using an Autosampler The amount of fatty acid methyl ester (FAME) in di deisel lfuel lis controlled dby ASTM and EN standards. Commercial biodiesel consists of some percentage of FAME or can be mixed with standard diesel fuel. The guidelines for the ratio of FAME in diesel oil are different for each country. The EN method utilizes a transmission method with a liquid cell and a simple quantitative analysis method. Multi Tech Optical Rail 1 Rectangular cell Liquid cell Autosampler Automatic quantitative analysis program A PC controlled auto sampler is integrated with a quantitative analysis program for automated QC/QA analysis of products. A standard quartz cuvette can be utilized with the FT NIR instrument for the analysis of liquid samples. FAME 10% Auto Sampler Single reflection ATR FAME 0% Wavenumber [cm-1] % Fame

22 Multi Tech Evaluation System: Quantitative Analysis of FAME Using ATR The amount of fatty acid methyl ester (FAME) in deisel fuel is controlled by ASTM 8 and EN standards. Commercial biodiesel 6 consists of some percentage of FAME or can be mixed with standard diesel fuel. 4 The guidelines for the ratio of FAME in diesel 2 oil are different for each country. The ASTM method utilizes the ATR method with a PLS 0 quantitative prediction of concentration. ion value predicti R= Real value PLS model of FAME 0.1 FAME100% FAME 30% Diesel Fuel 70% Diesel Fuel 100% Wavenumber [cm-1] IR spectra of biodiesel (ATR method: ZnSe prism) Auto Sampler Multi Tech Optical Rail Single reflection ATR A PLS model dlfor ATR analysis of FAME content in Diesel oil is controlled by ASTM, mandating a concentration of FAME 0 10% in bio diesel. The PLS calibration method did not require a dilution of samples and requires little l sample preparation.

23 Multi Tech Evaluation System: In situ Analysis of Protein Secondary Structure with a Variable Temperature ATR Accessory The denaturation ti process of DNA/protein solutions can be obtained with the temperature control of a single bounce ATR and the JASCO SSE analysis program. The SSE program can also provide the analysis of the component distribution ib ti in a cross section of a protein sample when analyzed using the PCA multivariate program. An ATR accessory was heated from room temperature to 75 deg C and the secondary structure of a lysozyme solution analyzed using the SSE program. With the temperature change, the α Helix content rose, and the β Sheet content decreased. As the temperature was decreased, the protein re folding process could also be followed. IRT 5000/7000 Heated ATR Temp. IR spectra of a lysozyme solution

24 Multi Tech Evaluation System: SSE Imaging of a Rabbit Blood Vessel Cross Section A combination of infrared imaging and SSE mapping analysis of a cross section of an arteriosclerotic blood vessel of a rabbit provides images of the secondary structure of the blood vessel components. Infrared imaging with the SSE mapping program can be used to probe other types of protein structures and biological samples. Reflection method Points: Area: 5 mm 4 mm Resolution: 8 cm 1 Scans: 1 Time: ~17 sec. IR Imaging program IRT-5000/7000 Heated ATR Overlaid image of blood vessel (red: lipid green: protein) α helix image β sheet image The overlaid image (left) of the 1,650 cm 1 peak (Amide1) and the 1,730 cm 11 peak (lipid C=O) is displayed alongside the calculated α helix (middle) and β sheet (right) distribution.

25 Multi Tech Evaluation System: Incoming Inspection of Pharmaceutical Raw Materials The ATR method does not require the amount of sample preparation like other analysis methods and can analyze a sample size ofonly only a few mg. The QCCompare Compare program provides a rapid analysis ofan incoming component versus a standard spectrum, confirming the identification and quality of the raw material. Using an ATR and the QC Compare program, quality checks of the raw ingredients, additives/excipients and even packaging materials can be rapidly executed with minimal sample preparation. Multi Tech Optical Rail ATR Fiber Probe NIR DRIFTS QC Compare Program

26 Multi Tech Evaluation System: Correlation of Skin and Age Using a NIR Fiber Interface NIR analysis can be used as a non destructive and non contact measurement for the in vivo measurement of live tissue. The measurement of human skin by a NIR probe was used to create a PLS calibration curve correlating the NIR spectrum and the age ofthe subject. Similar applications could be used for topical applications of lotions or other drug effects. Multi Tech Optical Rail NIR spectra of human skin Wavenumber [cm-1] edicted Pr Instrument : Detector: InGaAs Sample: Skin (18 samples from different ages) Method: DR probe Accumulations: 50 times Resolution: 4 cm -1 Actual ATR Fiber Probe NIR DRIFTS

27 Multi Tech Evaluation System: NIR Quantitative Analysis of Tablet Coatings NIR measurement is a nondestructive method for the analysis of tablets and tablet formulations. The use of a chemometrics method for analysis of the coating ratios for a formulated acetominophen tablet provides an accurate evaluation of the coating and component ratio Coating rate 30% acetaminophen Coating rate 0% ATR Fiber Probe Multi Tech Optical Rail NIR DRIFTS Peak ratio Coating value(%) Least squares plot of peak ratio Wavenumber [cm-1] Coating materials: Wavenumber [cm-1] Sodium lauryl sulfate, Mg stearate 7500 Spectral range of coating components

28 Universal Optical System for Dedicated Applications Optical elements including mirrors and detectors can be mounted on a PC controlled optical base, providing custom configurations for desired applications. 10 cm gas cell Gas cell Long path gas cell Chamber Multi component gas analysis system Optimized gas analysis system for quantitative analysis combining both a 10 cm and long path gas cell Process monitoring system In situ analysis for CVD film processing

29 Dedicated Analysis System: Analysis of Kidney/Gall Stones Using thesmarttech DRIFTS Measure Data processing Urological type Classification Gallstone type Calcium stone Ui Uric acid Struvite stone Cholesterol Pigment stone stone stone

30 Dedicated Analysis System: Gas Analysis aysssyste System for First Response se Vehicles ces 5000 data IR database 120 data calibration curve!

31 Dedicated Analysis System: Open Path Monitoring for Environmental Measurements Multi channel CCM ~ 500m target CH 4, N 2O, CO, CO 2, NOx, SO 2 etc CO : 4.5 ppm CH 4 : 5.4 ppm CO 2 : 240 ppm Wavenumber[cm-1] Exhaust gas analysis using open path method

32 Dedicated Analysis System: Film thickness Measurements The thickness of the epitaxial layer, substrate, FFT -1 etching residual layer, liquid crystal gap, and other semiconductor layers dramatically impacts semiconductor device performance. JASCO s film thickness measurement system provides a non destructive, non contact interference spectrum analysis using the latest spectrometric technology to provide rapid film thickness measurements. IRT 5000/7000 or Auto cassette system interference spectrum Film thickness result Reproducibility of SiN film thickness No. Film thickness information Measurement area

33 Dedicated Analysis System: Near Field Infrared Spectroscopy pysystem PS 2μ substrate Wavenumber [cm 1] Measurement result of PS (2µm) particle

34 Applications Semiconductor/materials Silicon wafer evaluation system Orientation evaluation system Solar reflectance/transmission evaluation system for glass Semiconductor gas evaluation system In situ film formation evaluation system UV cured resin evaluation system Jewelry examination system Film thickness measurement system Environment Open Path system Paper recycling evaluation system Phthalic acid ester evaluation system Bio - PAT evaluation system - Food additive evaluation system - Three nutrient evaluation system - Protein / nucleic acid heat denaturation evaluation system - Freshness evaluation system - Texture evaluation system - Alcohol concentration evaluation system - Calculus diagnosis system General Impurity analysis system Complex analysis Rheometer + IR system SFE/SFC + IR system Heat analysis + IR system

35 Conclusion Three models: 100, 200, 300 Compact size Enhanced DSP control High speed rapid scan capability Broad band KBr BS for mid to near IR measurements Wide range of accessories and optical systems Integrated control panel operations Universal optics system Compact FTIR with the high performance and expandability of a laboratory instrument: covers the range from the field to the lab