Application of ATR-MIR spectroscopy in the pilot plant—Scope and limitations using the example of Paracetamol crystallizations

Helmdach, Lydia; Feth, Martin P.; Minnich, Clemens B.; Ulrich, Joachim

doi:10.1016/j.cep.2013.04.003

Cited by 30 publications

(26 citation statements)

References 18 publications

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“…Together with the hard model for water vapor which was observed in the crystallization setup due to insufficient purge of the spectrometer 8, the above‐mentioned component hard models were merged into a mixture hard model. A fit of this mixture model to an online spectrum recorded after clogging shows how the contributions of the components are found in the mixture; see Fig.…”

Section: Resultsmentioning

confidence: 99%

“…Crystallization experiments were performed in a comparable way to the procedure described elsewhere 8, using paracetamol as a model compound in an ethanol‐water mixture (20:80 w/w). A paracetamol solution with a concentration of 11 g per 100 g ethanol‐water mixture (10 wt %) was prepared in a pilot plant setup by dissolving the appropriate amount of crystals in an ethanol‐water mixture at 55 °C.…”

Section: Methodsmentioning

confidence: 99%

“…These include supersaturated mother liquor which is prone to spontaneous nucleation, streams with a high particle loading etc. Whereas, e.g., Raman spectroscopy has shown to be capable of distinguishing between different crystal modifications of the solid 1–7, mid‐infrared (MIR) spectroscopy can be applied to selectively analyze the composition of the mother liquor if performed in attenuated total reflectance (ATR) mode 8–10. Since in ATR‐MIR measurements a maximum penetration depth of the light beam around 10 µm is achieved, the optical element of the ATR accessory needs to be representatively covered by the analyte.…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Model‐Based Recognition of Mid‐Infrared Sensor Fouling in Paracetamol Crystallization

Minnich¹,

Helmdach

Ulrich

et al. 2015

Chem Eng & Technol

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A procedure for the recognition of undesired solid deposition on the optical element of an attenuated total reflectance probe for online mid-infrared spectroscopy during crystallization processes is presented. Unlike other approaches, the method exclusively uses intelligent spectral analysis for solid recognition and does not require additional devices. Indirect hard modeling enables the separation of the solid material's contribution to the mixture spectra from those contributions of the dissolved material and the solvents, expressed through the predicted component weights. The detection of the solid component weight is promising for implementation into process monitoring or control.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Model‐Based Recognition of Mid‐Infrared Sensor Fouling in Paracetamol Crystallization

Minnich¹,

Helmdach

Ulrich

et al. 2015

Chem Eng & Technol

Self Cite

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“…Note that although advanced linear or nonlinear modelling algorithms may be explored to deal with the spectral nonlinearity, as discussed in the reference [12,28], Table 4 indicates that using a piecewise modeling strategy for USZ and MSZ can easily improve the measurement accuracy.…”

Section: Model Prediction Experimentsmentioning

confidence: 99%

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

Zhang

Liu

Wang

et al. 2017

Journal of Crystal Growth

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Abstract:In this paper calibration model building based on using an ATR-FTIR spectroscopy is investigated for in-situ measurement of the solution concentration during a cooling crystallization process. The cooling crystallization of L-glutamic Acid (LGA) as a case is studied here. It was found that using the metastable zone (MSZ) data for model calibration can contribute to the prediction accuracy, compared to the usage of undersaturated zone (USZ) spectra as traditionally practiced which may lead to undesired bias for prediction of the MSZ concentration. Calibration experiments were made for LGA solution under different concentrations. Four candidate calibration models were established using different zone data for comparison, based on a multivariate partial least-squares (PLS) regression algorithm for the collected spectra together with the corresponding temperature values. Experiments under varied concentrations and operational changes of temperature were conducted. The results indicate that using MSZ spectra for model calibration can give more accurate prediction of the solution concentration during the crystallization process. The primary reason was clarified as spectral nonlinearity for measurement between USZ and MSZ. In addition, an LGA cooling crystallization experiment was performed to verify the sensitivity of these calibration models for monitoring the crystal growth process.

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“…The attenuated total reflectance (ATR)-FTIR spectroscopy is an interesting technique that is increasingly used in recent years (Karoui et al, 2010;Wang and Rodriguez-Saona, 2012;Helmdach et al, 2013;Cozzolino et al, 2014). The above spectroscopic technique combined with multivariate analysis was used for the determination of the total antioxidant capacity of red wine samples (Versari et al, 2009).…”

Section: Introductionmentioning

confidence: 99%

Estimation of Antioxidant Activity of Different Mixed Herbal Infusions using Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy and Chemometrics

Venetsanou¹,

Anastasaki²,

Gardeli³

et al. 2017

Emir. J. Food Agric

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Application of ATR-MIR spectroscopy in the pilot plant—Scope and limitations using the example of Paracetamol crystallizations

Cited by 30 publications

References 18 publications

Model‐Based Recognition of Mid‐Infrared Sensor Fouling in Paracetamol Crystallization

Model‐Based Recognition of Mid‐Infrared Sensor Fouling in Paracetamol Crystallization

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

Estimation of Antioxidant Activity of Different Mixed Herbal Infusions using Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy and Chemometrics

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