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1、布鲁克红外光谱培训布鲁克红外光谱培训傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍电磁波Gamma RayX-RayUVInfraredMicro WaveShort WaveRadio WavesEnergyeVWavenumbercm-1WavelengthmVisible傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红
2、外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍如何得到一张图如何得到一张图色散型红外光谱仪色散型红外光谱仪傅立叶变换红外光谱仪傅立叶变换红外光谱仪傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍色散型红外光谱仪DetectorDetector优点:-不需要计算机缺点:-速度慢-光通量低=灵敏度低(S/N ratio)傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅利叶变换红外光谱仪原理
3、光源动镜定镜x分束器LL+xx=0傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍sourceDetectorfixedmirror M1xBeam splitterLL+L+x xx=0例 1:x=0,相长干涉结果1.Beam part(定镜)2.Beam part(动镜)傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍sourceDetectorfixedmirror M1xBeam splitterLL+L+x xx=1/2例 2:x=1/2,相消性干涉0结果1.Beam part(定镜)2.Beam part(动镜)傅立叶红外光谱介绍傅立
4、叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍sourceDetectorfixedmirror M1xBeam splitterLL+L+x xexample 3:x=,constructive Interference0Resulting signal1.Beam part(fixed)2.Beam part(movable)x=傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍sourceDetectorfixedmirror M1xBeam splitterLL+L+x xx=3/2example 4:x=3/2,destructive Interferenc
5、e0Resulting signal1.Beam part(fixed)2.Beam part(movable)傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Mirror motionIntensity监测器信号监测器信号FrequenceIntensity光源光源单色光源单色光源的调制信号傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Entstehung des InterferogrammsMirror motionIntensityResultingdetectorsignalFrequenceIntensity9条单一频率的光源条单一
6、频率的光源Mirror motionIntensity总和总和:傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍检测器信号检测器信号FrequencyIntensity红外光源红外光源 X,movingmirrorIntensity干涉图的来源傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍透射光谱1.)In the empty sample compartment an Interferogram is detected.The result of the FOURIER transformation is R().Fourier-Transf
7、ormationFourier-Transformation5001000150020002500300035004000wavenumber cm-10.100.200.300.40Single channel intensity X,movingmirrorDetector intensity傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍2.)A second interferogram is detected with the sample placed in the sample compartment.The result of the FOURIER tr
8、ansformation is S().S()shows similarities to the reference spectrum R(v),but has lower intensities at the regions the sample absorbs radiation.Fourier-TransformationFourier-Transformation5001000150020002500300035004000wavenumber cm-10.100.200.300.40Single channel intensity X,movingmirrorDetector int
9、ensity透射光谱傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍The transmission spectrum T()is calculated as the ratio of the sample and reference single channel spectra:T()=S()/R().5001000150020002500300035004000wavenumber cm-10.100.200.300.40Single channel intensity5001000150020002500300035004000wavenumber cm-1406
10、080100Transmission%20ratioratio透射光谱傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Absorbance Transmission-Why?100020003000400050006000Wavenumber cm-1020406080100Transmittance%100020003000400050006000Wavenumber cm-10.00.20.40.60.81.0Absorbance UnitsTransmissionAbsorbanceT()=S()/R()Lambert-Beerslaw:AB=-log(S()/R
11、()AB=cb傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Principle layout of FT-IR spectrometerSourceMovingmirrorFixed mirrorxBeamsplitterLL+xx=0傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Layout of an FT-IR spectrometer(TENSOR series)ElectronicSourcecompartmentSamplecompartmentSamplepositionDetectorInterferometercompart
12、mentAperturewheelFilterwheel傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍NIR:Source:tungsten lampOptical material:QuartzDetector:Ge,InGaAsMIR:Source:GlobarOptical material:KBr,ZnSeDetector:DTGS,MCTFIR:Source:Globar,Hg lampOptical material:PE,CsIDetector:DTGS,BolometerDifferences between NIR,MIR,FIROptical co
13、mponents:傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍FourierTransformation(FT)傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Data acquisition results in a digitized interferogram,I(x),which is converted into a spectrum by means of the mathematical operation called a Fourier Transform(FT).The general equation for the F
14、ourier Transform is applicable to a continuous signal.If the signal(interferogram)is digitized,however,and consists of N discrete,equidistant points,then the discrete version of the FT(DFT)must be used:S(k.)=I(n x)exp(i2k n/N)The continuous variables x and have been replaced with n x and k ,represen
15、ting the n discrete interferogram points and the k discrete spectrum points.The fact that we now have a discrete,rather than continuous,function,and that it is only calculated for a limited range of n(i.e.the measured interferogram has a finite length)leads to important effects known as the picket-f
16、ence effect and leakage.The Fourier Transform傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍sourcedetectormovablemirror M2fixedmirror M1xBeam splitterLL+xx=0高光谱分辨低光谱分辨傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍添零The picket-fence effect occurs if the interferogram contains frequency components which do not exactly coi
17、ncide with the data point positions,k.,in the spectrum.The effect can be thought of as viewing the spectrum through a picket fence,thereby hiding those frequencies that are behind the pickets,i.e.between the data point positions k.In the worst case,if a frequency component is exactly between two sam
18、pling positions,a signal reduction of 36%can occur.The picket-fence effect can be reduced by adding zeros to the end of the interferogram(zerofilling)before the DFT is performed.This interpolates the spectrum,increasing the number of points per wavenumber.The increased number of frequency sampling p
19、ositions reduces the error caused by the picket-fence effect.Generally,the original interferogram size should always be at least doubled by zero filling,i.e.zero filling factor(ZFF)of two is chosen.Zero-filling interpolates using the instrument line-shape,and in most cases is therefore superior to p
20、olynominal or spline interpolation methods that are applied in the spectral domain.1,7961,7981,8001,8021,8041,8061,808Wavenumber,cm-10.350.400.450.500.55Single channel1,7961,7981,8001,8021,8041,8061,808Wavenumber,cm-10.350.400.450.500.55Single channelZero-filling factor 2Zero-filling factor 8傅立叶红外光谱
21、介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍截趾函数In a real measurement,the interferogram can only be measured for a finite distance of mirror travel.The resulting interferogram can be thought of as an infinite length interferogram multiplied by a boxcar function that is equal to 1 in the range of measurement and 0
22、elsewhere.This sudden truncation of the interferogram leads to a sinc()(i.e.sin()/)instrumental lineshape.For an infinitely narrow spectral line,the peak shape is shown at the top of the figure on the right.The oscillations around the base of the peak are referred to as“ringing”,or“leakage”.The solu
23、tion to the leakage problem is to truncate the interferogram less abruptly.This can be achieved by multiplying the interferogram by a function that is 1 at the centerburst and close to 0 at the end of the interferogram.This is called apodization,and the simplest such function is a ramp,or“triangular
24、 apodization”.The choice of a particular apodization function depends on the objectives of the measurement.If the maximum resolution of 0.61/L is required,then boxcar apodization(i.e no apodization)is used.If a resolution loss of 50%(compared to the maximum resolution of 0.61/L)can be tolerated,the
25、HAPP-GENZEL or,even better,3-Term BLACKMAN-HARRIS function is recommended.ABOXCAR(noapodization)BTriangularCTrapezoidalDHAPP-GENZELE3-TERMBLACKMAN-HARRIS傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍EvaluationofIRspectra傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍定性分析：1.鉴定未知物2.核对已知物定量分析 光谱评价傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介
26、绍傅立叶红外光谱介绍未知物的鉴定a)通过光谱解析推出分子结构5001,0001,5002,0002,5003,0003,5004,000Wavenumber/cm-1406080100Transmission%20傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍不同有几类分子的红外吸收 烷烃烯烃芳香烃内酯卤化物羧酸盐酸酐傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍b.)与标准谱库比较e.g.by using OPUS/Search未知物的鉴定傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍identicalmateri
27、al=identicalIRspectrum-What you have:sample-What you need:reference library-What you do:comparison with reference library-What you get:identification验证已知物傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍2.)Calculateaveragespectrum&thresholdvalues3.)Librarystructure&validation1.)MeasurereferencesampleWavenumber/c
28、m-1AbsorbanceWavenumber/cm-1AbsorbanceReference library structure傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍 Identified sample:material X1.)Measurenewsamples2.)ComparewithlibraryIdentifying new samples3.)Identifymaterial傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍-What you have:sample-What you need:calibration set
29、-What you do:comparison with calibration set-What you get:concentration valueThere are two different forms of calibration:Univariatecalibration(OPUS)-Correlates just one piece of spectral information(e.g.peak height or peak area)with the reference values of the calibration set.Multivariatecalibratio
30、n(OPUS/QUANT)-Correlates considerably more spectral information-higher degree of precision-reduced chance of errorOPUS/QUANT uses the Partial Least Squares(PLS)Method.XAnalysis1234AbsorbanceConcentrationX1324AbsorbanceWavelengthCalibrationQuantitative evaluation of spectra傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍
31、傅立叶红外光谱介绍2.)Buildcalibrationset(QuantMethod)3.)Validatecalibrationset1.)MeasurecalibrationspectraWavenumber/cm-1AbsorbanceSetup of a Quant Method1234AbsorbanceConcentration傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍 Concentration:58 vol.%1.)Measuresample2.)ComparewithcalibrationsetDetermine quantitative re
32、sults(e.g.concentration values)3.)Result傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍FT-IRmeasurements傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Enter sample nameStart the background and sample measurement傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Sampling bandwidth in interferogram dom
33、ain傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍The FT of a measured interferogram yields a complex spectrum.The aim of the phase correction is to calculate the real spectrum.Interpolation of the spectrum by adding zeros to the end of the interferogram傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Defines the separatio
34、n of adjacent peaks傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍Acquisition modesingle sideddouble sidedfast backwardforward and backward傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍傅立叶红外光谱介绍IfyouhaveanyfurtherquestionsaboutIRspectroscopy,pleasecontacttheapplicationteamofBrukerOptics:Europe:BrukerOptikGmbHRudolf-Plank-Str.277
35、6275 Ettlingen,GermanyPhone:+49 7243 504 600Fax:+49 7243 504 698infobrukeroptics.deNorthAmerica:BrukerOpticsInc19 Fortune DriveBillerica,MA 01821,USAPhone:+1 978 439 9899Fax:+1 978 663 Asia:BrukerOptikAsiaPacificLtd.Unit 601,6/F,Tower 1Enterprise SquareNo.9,Sheung Yuet Road,Hong KongPhone:+852 27966100Fax:+852 结束语结束语谢谢大家聆听！谢谢大家聆听！50