Comparison between approaches for the experimental determination of metastable zone width: A case study of the batch cooling crystallization of ammonium oxalate in water

Gherras, Nesrine; Févotte, Gilles

doi:10.1016/j.jcrysgro.2011.06.058

Cited by 37 publications

(46 citation statements)

References 31 publications

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“…These differences are due to different mechanisms of nucleation in the two studies. For example, the value of the interfacial tension γ obtained from the data reported by Sangwal and Wójcik is twice higher than that obtained from the data of Gherras and Fevotte ; see Table . A lower value of γ from the data of Gherras and Fevotte is probably associated with the occurrence of heterogeneous or secondary 3D nucleation .…”

Section: Resultsmentioning

confidence: 64%

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On the induction period for crystallization in solute−solvent systems by polythermal method

Sangwal

Mielniczek‐Brzóska

Borc

2013

Crystal Research and Technology

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The data of induction period tin derived from the data of maximum undercooling ΔTmax at different cooling rates R for some solute−solvent systems at different saturation temperature T0 are discussed using classical and atomistic theories of three‐dimensional nucleation. In the case of potassium nitrate aqueous solutions the tin data are analyzed in terms of the maximum supersaturation ratio Smax calculated from temperature dependence of solubility and the maximum undercooling ΔTmax and the values of solid−solution interfacial energy γ and number i* of molecules in the stable critically‐sized nuclei predited from tin(lnSmax) and tin(ΔTmax) data are compared. These results revealed that: (1) the values of supersaturation calculated as lnS from solubility data are lower than the real values expected from the chemical potential difference Δμ and that the description of Δμ in terms of undercooling ΔTmax is realistic, and (2) analysis of induction period data for solute−solvent systems should be carried out using applied undercooling ΔT or maximum undercooling ΔTmax instead of the usually used lnS or lnSmax. Examination of tin(ΔTmax) data for different systems showed that: (1) the value of γ lies between 1.7 and 13.2 mJ/m2 while that of i* between 2 and 50, and (2) in several cases atomistic nucleation theory describes the tin(ΔTmax) data adequately.

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Section: Resultsmentioning

confidence: 64%

“…It should be mentioned that the cooling rates used in the two studies are 10 to 60 K/h and 2 to 30 K/h . Despite this difference in the range of R in the two studies, the values of constants K 1 and K 2 of equations and obtained from the linear fitting of the ln t in (Δ T max ) data in the two studies are comparable.…”

Section: Resultsmentioning

confidence: 90%

On the induction period for crystallization in solute−solvent systems by polythermal method

Sangwal

Mielniczek‐Brzóska

Borc

2013

Crystal Research and Technology

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“…The direct measurement of the nucleation rate is complicated, and thus, the nucleation rate is often estimated using MSZW models associated with nucleation parameters and cooling rate . In the present work, Kubota's model was adopted for the estimation of nucleation kinetics since this model well reflected the detection sensitivity of the nuclei for number density on MSZW , . Kubota assumed that the number‐based nucleation rate, J , is a power‐law function of supercooling, Δ T :

true J = k_{n} {false(Δ T false)}^{n}

…”

Section: Resultsmentioning

confidence: 99%

Formation of Spherical Agglomerates in Cooling Crystallization of Hexahydro‐1,3,5‐trinitro‐1,3,5‐triazine

Lee

Kim

et al. 2017

Chem Eng & Technol

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The production of spherical agglomerates of hexahydro‐1,3,5‐trinitro‐1,3,5‐triazine (RDX) from acetone by cooling crystallization with poly(vinylpyrrolidone) (PVP) is described. It was found that PVP suppresses the nucleation of RDX at the initial stage, but tremendous nucleation of RDX occurred abruptly after the induction period. The rapid nucleation may be associated with the primary nucleation due to the presence of PVP. It can be concluded that the addition of PVP results in the formation of RDX particles with sufficient number density for spherical agglomeration. It was found that such spherical agglomeration propagates very rapidly after nucleation within one minute and the size of spherical agglomerates is affected by the cooling rate.

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“…In fact, experiments for ATR-FTIR calibration had been mainly carried out in the undersaturated zone (USZ) [9][10][11][12][13][14][15]. A small number of calibration methods were presented in the literature to analyze ATR-FTIR spectra for in-situ measurement of the solution concentration.…”

Section: Introductionmentioning

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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Comparison between approaches for the experimental determination of metastable zone width: A case study of the batch cooling crystallization of ammonium oxalate in water

Cited by 37 publications

References 31 publications

On the induction period for crystallization in solute−solvent systems by polythermal method

On the induction period for crystallization in solute−solvent systems by polythermal method

Formation of Spherical Agglomerates in Cooling Crystallization of Hexahydro‐1,3,5‐trinitro‐1,3,5‐triazine

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

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