Raman and ATR FTIR spectroscopy in reactive crystallization: Simultaneous monitoring of solute concentration and polymorphic state of the crystals

Qu, Haiyan; Alatalo, Hannu; Hatakka, Henry; Kohonen, Jarno; Louhi-Kultanen, Marjatta; Рейникайнен, Сату-Пиа; Kallas, Juha

doi:10.1016/j.jcrysgro.2009.04.018

Cited by 53 publications

(39 citation statements)

References 35 publications

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“…Ono et al 23 and Qu et al 9 have used peak height ratio to compute the mass fraction of the a-form. Fitting of the 2nd degree polynomial (Eq.…”

Section: Analysis Methods For Solution and Product Qualitiesmentioning

confidence: 99%

“…1-8) in a neutral and acidic pH range where Glu 2À (C 5 H 7 N0 The sum of the dissociation reaction of Glu 2 and the solid-liquid equilibrium 3 is given in equation. 9 The equilibrium constant or solubility product, K sp, for reaction equation 9 is given in equation. 10 The value for the solubility product was solved from the equilibrium constant of the reaction 2 when a[…”

Section: Glutamic Acid: Solution and Crystalsmentioning

confidence: 99%

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Process control and monitoring of reactive crystallization of L‐glutamic acid

Alatalo¹,

Hatakka²,

Kohonen³

et al. 2009

AIChE Journal

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The aim of the present study was to investigate feedback control of a reactive crystallization process. The present study built up a control structure needed to control the driving force of reactive crystallization using the feed rate of added acid. The concentration of the crystallizing compound and pH was used to compute feedback in the closed-loop control of semi-batch precipitation. The concentration of L-glutamic acid was determined from measured MID-IR ATR-FTIR spectra based on a multivariate model. Dynamic change of set value was based on the mass of added sulfuric acid and pH. The studied properties of the product crystals were polymorphism and crystal size. The polymorphic composition was analyzed with a Raman spectrometer and was expressed by mass fraction of the a-polymorph. The obtained results showed that the developed feedback process control system allows effective control of forming of polymorphs.

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“…Ono et al 23 and Qu et al 9 have used peak height ratio to compute the mass fraction of the a-form. Fitting of the 2nd degree polynomial (Eq.…”

Section: Analysis Methods For Solution and Product Qualitiesmentioning

confidence: 99%

Section: Glutamic Acid: Solution and Crystalsmentioning

confidence: 99%

Process control and monitoring of reactive crystallization of L‐glutamic acid

Alatalo¹,

Hatakka²,

Kohonen³

et al. 2009

AIChE Journal

Self Cite

View full text Add to dashboard Cite

show abstract

“…ATR-FTIR is a consolidated technique in the monitoring of crystallization processes (Chen et al, 2009;Kadam et al, 2011;Pöllänen et al, 2006;Qu et al, 2009;Sheikhzadeh et al, 2008;Liotta & Sabesan, 2004). The method allows estimating the degree of supersaturation of the system by measuring the concentration of solute in the solution.…”

Section: Attenuated Total Reflectance Fourier Transform Infrared Specmentioning

confidence: 99%

Real-Time Analysis to Evaluate Crystallization Processes

Silva¹,

Silva²,

Sena³

2012

Crystallization - Science and Technology

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“…In principle, there are many different techniques such as thermo analytical methods (DSC), X-ray powder diffractometry (XRPD), solid-state NMR, NIR, IR and Raman spectroscopy can be used for identification and quantification of specific crystal forms in drug substances [8][9][10][11]. X-ray powder diffractometry (XRPD) technique is widely used for the identification and quantification of polymorphic forms of drugs since it is non-destructive and requires small amount of sample.…”

Section: Introductionmentioning

confidence: 99%

FT-Raman Spectroscopy with Chemometric Methods for Quantification of Lamivudine Form II in Lamivudine Form I

Rao¹,

Reddy²,

Sekhar³

et al. 2017

Asian J. Chem.

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Lamivudine is known to exhibit polymorphism and the needle-shaped crystals are named as Form I and the bipyramidal crystals as Form II. The FT-Raman spectrum of lamivudine Form II and I shows characteristic bands at 798, 463 cm -1 and 697 cm -1 Raman shifts, respectively. FT-Raman spectroscopy method combined with chemometrics was developed for quantitative analysis of lamivudine Form II in lamivudine Form I drug substance. Solid mixtures of Form I and Form II shows the relative intensity of the characteristic bands at 798, 463 and 697 cm -1 were proportional to the relative amounts of Form I and Form II in mixtures. A calibration was made which is linear in the range from 1.0 to 20.0 % (w/w) of Form II in Form I. The results indicate that levels down to 3.0 % (w/w) of Form II could be quantified using this non-destructive approach, with less than 1.5 % (w/w) limit of detection.

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Raman and ATR FTIR spectroscopy in reactive crystallization: Simultaneous monitoring of solute concentration and polymorphic state of the crystals

Cited by 53 publications

References 35 publications

Process control and monitoring of reactive crystallization of L‐glutamic acid

Process control and monitoring of reactive crystallization of L‐glutamic acid

Real-Time Analysis to Evaluate Crystallization Processes

FT-Raman Spectroscopy with Chemometric Methods for Quantification of Lamivudine Form II in Lamivudine Form I

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