碩一化工制藥過程分析

ProcessAnalyticalTechnologyfortheChemicalandPharmaceuticalIndustry——CalibrationPLSmodelapplyingATRFTIRtocrystallisationofL-glutamicacidLiyangMonday,May30,2016Include:TheprincipleofATRFTIRCalibrationmodeldevelopment

spectraanalysispreprocessmethodspectraselectionConclusionTheprincipleofATRFTIRWhatisATRFTIR?AttenuatedTotalReflectionFourierTransformInfraredSpectroscopyWhatistheATRtechnologyWhenthelightenteronemedium(β)fromanothermedium(α)(nα>nβ),thereappearrefractionandreflectionatthesametime.Asangle

of

incidenceincreases,

angle

of

refractionincreasesWhentheangle

of

incidenceincreasestoathreshold,therefractiondisappears,thenitistotalreflection.Butthelighthasenteredthemediumβasmalldistance,severalμm,beforereflectsWedefinethedistanceastransmissiondepth(dp)Theenergyoflightattenuatesinthemediumβ(specimen)Toincreasetheenergyattenuation,weincreasethetimesofreflectionlauncherreceiverCalibrationmodeldevelopmentCon(g/L)\temp(oC)10203040506070803

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Calibrationmodeldevelopmentspectraanalysiswholespectrumwavenumber1300-1500cm-1excludeSpectrausedtocalibratenoiseWecangetThecharacteristicpeakisnotobviousTheremaybeseveralspectra(3g/L,10℃;18g/L,70℃)existnoiseOnespectrum(18g/L,50℃)isstrayThedatamaybeintwogropeCalibrationmodeldevelopment

preprocessmethodAutoscaleexclude1stDerivative+Smoothing1st

Derivative+Smoothing+Autoscale1stDerivative+Smoothing+AutoscaleDerivativefilterwidthSmoothingfilterwidthR2CalR2CV550.9950.927570.9940.942590.9850.942750.9830.937770.9940.963790.9940.967950.9970.978970.9970.978990.9970.9781170.9940.9741190.9940.97411110.9940.975Wecanget:15spectrumismaywellstrayThepreprocessofautoscaleand1stDerivative+Smoothing+AutoscaleisbetteTheaffectofsmoothingfilterwidthissmallwhenthewidthismorethan7Calibrationmodeldevelopment

spectrasegmentselection1350-1450cm-1wholespectraspectradeleted1000-1150;2300-2400cm-1Calibrationmodeldevelopment

spectrumsegmentselection1350-1450cm-1Autoscale1stDerivative+Smoothing+AutoscaleThesummaryDerivativefilterwidthSmoothingfilterwidthR2CalR2CVR2Pred770.9590.9460.88790.9580.9460.8887110.9870.9780.981970.9540.9470.907990.9530.9460.9379110.9480.9360.9741170.9850.9770.9751190.9580.9500.97611110.9580.9490.970autoscale0.8920.8840.686Wholespectrum

autoscale1stDerivative+Smoothing+AutoscaleThesummaryDerivativefilterwidthSmoothingfilterwidthR2CalR2CVR2Pred770.9950.9680.973790.9950.9710.9737110.9950.9740.969970.9950.9740.972990.9950.9750.9749110.9950.9770.9761170.9950.9760.9771190.9950.9770.97811110.9950.9760.980Autoscale0.8950.8220.751Spectradeleted1000-1150;2300-2400cm-1autoscale1stDerivative+Smoothing+AutoscaleThesummaryDerivativefilterwidthSmoothingfilterwidthR2CalR2CVR2Pred770.9940.9630.965790.9950.9660.9727110.9950.9690.973970.9940.9700.971990.9940.9710.9729110.9960.9790.9801170.9960.9780.9791190.9960.9790.98011110.9960.9800.981Autoscale0.9810.9480.944ConclusionTurevaluePredictvalue1300-1500cm-1Error%WholespectraError%PartialspectraError%61.81803769.70

5.8910281.826.2365443.9495.84016135.118.5215395.328.302674-7.751210.1606515.3311.468864.4311.17878-6.841515.94497-6.3015.62905-4.1915.901146.011514.689742.0714.176835.4914.2136-5.241516.13159-7.5414.894390.7014.56911-2.872123.99812-14.2821.41052-1.9519.17628-8.682124.45058-16.4321.2515-1.2019.19968-8.572124.84244-18.3021.35056-1.6719.94164-5.042121.19733-0.9421.76673-3.6522.065015.072424.87772-3.6627.47424-14.48

27.7064915.44

2730.69203-13.6727.54295-2.0127.472871.752731.13543-15.3228.70643-6.3228.933617.163030.7785-2.6031.55614-5.1931.707865.693032.48396-8.2828.747944.1728.10302-6.324040.21083-0.5338.23314.4238.47769-3