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Threeway analysis

Threeway analysis. Batch organic synthesis. Paul Geladi. Head of Research NIR CE Chairperson NIR Nord Unit of Biomass Technology and Chemistry Swedish University of Agricultural Sciences Umeå Technobothnia Vasa paul.geladi @ btk.slu.se paul.geladi @ syh.fi. THREE-WAY ARRAY. K.

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Threeway analysis

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  1. Threeway analysis Batch organic synthesis

  2. Paul Geladi Head of Research NIRCE Chairperson NIR Nord Unit of Biomass Technology and Chemistry Swedish University of Agricultural Sciences Umeå Technobothnia Vasa paul.geladi @ btk.slu.se paul.geladi @ syh.fi

  3. THREE-WAY ARRAY K C = time B = variable J A = batch I

  4. Literature Geladi P. & Åberg P., Three-way modeling of a batch organic synthesis process monitored by near infrared spectroscopy, Journal of Near Infrared Spectroscopy, 9, 1-9, 2001 Geladi P. & Forsström J., Monitoring of a batch organic synthesis by infrared spectroscopy: modeling and interpretation of three-way data, Journal of Chemometrics, 16, 329-338, 2002.

  5. Three-way arrays • GC-MS • LC-UV • Fluorescence • Batch processing • many others

  6. Properties • Components / pseudorank • 3 types, not 2 • No orthogonality • Parsimonious model

  7. BATCH REACTION • ester synthesis by refluxing alcohol and acid • many batches as experimental design • measure NIR spectrum with transflectance fiberoptic probe at regular intervals • 400-2500 nm every 2 nm, 32 scans average • reference = air

  8. REACTION

  9. REACTION C5H11OH + CH3COOH -> C5H11OCOCH3 + H2O -acid catalysis H+ -remove water to shift equilibrium

  10. Parsimony = not using too many model parameters = no overfitting 10 Stations x 13 Variables x 22 Times 2 Components MODEL PARAMETERS PCA1 10x286 20 + 572 = 592 PCA2 13x220 26 + 440 = 466 PCA3 22x130 44 + 260 = 304 PARAFAC 20 + 26 + 44 = 92

  11. IMPORTANT QUESTIONS - can we learn something about reaction kinetics? - can we see difference between batches? - can we interpret the spectra? - how does it all fit together?

  12. REACTION 1 14 x 701 x 13 array. Source of SS % explained Rank 3 model 97.1 Residual 2.9 Total 100 Component 1 48.0 Component 2 15.3 Component 3 4.0

  13. REACTION 2 6 x 40 x 776 array number %SS SS 1 62 2.73 2 18 0.78 3 16 0.71 4 3.2 0.14 Model 99.2 4.38 Residual 0.8 0.038 Total 100 4.42

  14. a1 block effect Batch # Fig 10.51

  15. Component size 6 5 4 3 2 1 0 3 5 1 2 4 0 Pseudorank Fig 10.55

  16. Bias Wavelength

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