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The application of MID-IR for Process Analysis

The application of MID-IR for Process Analysis. David Baines SpectraProbe Ltd APACT 03, York. The application of MID-IR for Process Analysis. Benefits of MID-IR Considerations for implementation in a process application Practical applications. MID IR peaks “intuitive” Acetone in IPA.

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The application of MID-IR for Process Analysis

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  1. The application of MID-IR for Process Analysis David Baines SpectraProbe Ltd APACT 03, York

  2. The application of MID-IR for Process Analysis • Benefits of MID-IR • Considerations for implementation in a process application • Practical applications

  3. MID IR peaks “intuitive”Acetone in IPA 100% Acetone 50% Acetone

  4. MID IR enables peak height analysis Impurities in Peroxide Chemistry Peak Height

  5. MID IR enables peak height analysis Impurities in Peroxide Chemistry

  6. Small number of samples to build accurate models

  7. Small number of samples to build accurate models

  8. In summary the benefits of Mid-IR • “Fundamental frequencies of the molecules give clearer peaks to interpret.” • Colin McGill, CPACT • “Peak heights can be intuitively interpreted without models in seconds.” • Kay Saunders, Syngenta • “Instrument set up and calibration is quick. It requires minimal line modification to install and no lengthy fibre optical cables.” • Ewan Polwart, Avecia

  9. Considerations in using MID-IR Process Control instruments • Probe principle • Sample preparation • Sample conditioning • Maintaining the probe in the process

  10. ATR Principle for MID-IR • Extremely sensitive • High absorbance possible with multi-bounces. • ATR means no interference from bubbles and particles. • Many crystal types possible for wide range of chemistry at low cost. • May suffer from films forming

  11. Process Insertion probe No sample preparation required. Reduces installation costs and complex temperature regulation sample streams.

  12. Temperature effects need to be modelled

  13. Temperature effects need to be modelled.

  14. SpectraProbe • Process Control unit • with retractable probe holder • and cleaning system

  15. Automatic Cleaning system Remote operation Pneumatic operation to remove from process Pre-programmed cleaning cycles Optional fluid controls and pressure vessels. Full auto checking of operational status. Auto-background Crystal check.

  16. Process Development and Process Monitoring Instrumentsfrom Spectraprobe • Process Applications:- • Crystallisation • Fermentation • Distillation control • Reaction monitoring

  17. Fibre input lens Detector Spectrometer Fibre ATR crystal (sample interface Source at end - 2 bounces) Fibre Source/Fibre Coupler Collimating lens Optical Arrangement

  18. Technical features Low cost MID-IR spectrometer for Reaction Monitoring & Process Control Compact size 3 & 10Kg Certified EEx d II CT5 ATEX ExII2gD Room temperature detector Process temperature ranges:- -10 to 90C -20 to 180C Crystal types AMTIR, ZnSe, Silicon, Diamond Pressure –1 to 10 Bar Integrated PLS modelling quick to set up and calibrate. Outputs 4-20mA prediction of concentration plus process temperature.

  19. Alcohol in Aldehyde at below 1% A group of 7 samples were scanned by the Spectraprobe Diamond ATR Process control instrument. A background of 5 minutes was taken.

  20. Sample Model 1 Model 2 Model 3 Sample 1 √ √ √ Sample 2 Predict Predict √ Sample 5 √ √ Predict Sample 7 √ √ √ Sample 8 √ √ Predict Sample 10 Predict √ √ Sample 13 √ √ √ Sample 11 √ √ √ Sample 11 √ √ √ Sample 11 √ √ √ Sample 15 √ √ √ Sample 15 √ Predict √ Sample 11 Predict √ √ PLS Settings LV6 LV5 LV7 Regression No scaling No scaling No scaling Simpls Simpls Simpls Venetian blind Venetian blind Venetian blind Alcohol in Aldehyde at below 1% Three models were built with certain samples randomly left out of the model and used to later validate the models

  21. Results of model predictions Alcohol in Aldehyde at below 1% Model predictions well within the 0.2% required for the application.

  22. Crystallisation out of Propanol Figure 1 Overlaid spectra of 0.05-0.5% weight by volume samples

  23. Crystallisation reaction over 80-20 Degrees

  24. IR Spectra from the Methionine Fermentation process Amino acid production

  25. Calibration of the SpectraProbe with 27 process samples Laboratory calibration of Water in Acroline

  26. Calibration of the SpectraProbe with 27 process samples Validation of model with further process samples of Water in Acroline

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