Crystal growth rates and secondary nucleation threshold for γ-dl-methionine in aqueous solution

Wantha, Lek; Flood, Adrian E.

doi:10.1016/j.jcrysgro.2010.11.046

Cited by 21 publications

(38 citation statements)

References 14 publications

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“…In pharmaceutical and fine chemicals crystallisation, uniform, well-shaped crystals are commonly produced which shows what can be achieved empirically, or with computer control, for generally this must have been achieved without the knowledge 15 of the underlying reasons described here. What is being advocated in this paper is the desirability of measuring both the seeded and the unseeded determination of the crystallisation, in order to have a complete understanding of basis of the solution crystallisation behaviour.…”

Section: Large Scale Considerationsmentioning

confidence: 98%

“…In each case the curvetrajectory of the crystallisation, e,g. the turbidimetric value, will appear to slope upwards at an increasing incline, but 10 whether this is due in any particular case to several overlapping primary crystallisation events followed by varying intervals to the secondary nucleation, or to single or simultaneous nucleation events followed by crystal growth and continuously increasing proliferation, is impossible to determine merely by 15 the shape. So careful analysis of the crystallisation curves of the kind carried out by Dugua and Simon will be necessary to establish the true course of the crystallisation events 6768 .…”

Section: The Course Of the Crystallisationmentioning

confidence: 99%

“…These initial seeds however failed to proliferate, as has been discussed in detail in Strickland-Constable 13 refers to a region in which only crystal growth can occur, but fails to elaborate on the implications of such a region. Flood and co-workers 14 have identified a 'secondary nucleation threshold' in the crystallisation of carbohydrates and 5 have extended the concept to the crystallisation of methionine 15 . The earliest use of the term secondary nucleation threshold appears to have been by White.…”

Section: Introductionmentioning

confidence: 99%

“…Khaddour and Rocha 18 have investigated 'secondary nucleation within the metastable zone', which is presumably the same phenomenon, but have not considered it in relation to product formation. The terms 'surface secondary nucleation', 'activated 15 secondary nucleation' and 'surface-activated secondary nucleation' have been used by Puel, Veesler and co-workers [19][20][21] to describe what appears to be the onset of the same boundary. Agrawal 23 and 'nuclei first detection curve' 25 .…”

Section: Introductionmentioning

confidence: 99%

“…It had been expected that halving the gap would halve the sensitivity, but the resulting charts suggested that the sensitivity may have decreased by a factor of a hundred-fold. Consequently the 15 metastable width was much enlarged, even at the slowest temperature ramps. The dependence of the metastable zone width on the sensitivity of instrumental detection appears not to have been discussed in detail in the literature.…”

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confidence: 99%

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A perspective on the growth-only zone, the secondary nucleation threshold and crystal size distribution in solution crystallisation

Threlfall

Coles

2016

CrystEngComm

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The metastable zone between the solubility curve and the crystallisation curve can be divided into two regions, separated by the secondary nucleation threshold. At a supersaturation less than that of the secondary nucleation threshold seeds will grow but not proliferate. At greater supersaturations, they will proliferate. Although this concept has been known in connection with the commercial crystallisation of sucrose and of lactose for almost a century it is virtually unrecognised beyond the sugar and dairy 10 industries. The consequences are explored of the existence of such a boundary on the crystallisation process and the influence on crystal size distribution. It is recognised that the secondary nucleation threshold is the 'seeded metastable limit', but there are important consequences of avoiding the latter term. Mullin's 'Latent Period' is shown to be closely related to the 'growth only' zone within the metastable zone.15

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Section: Large Scale Considerationsmentioning

confidence: 98%

Section: The Course Of the Crystallisationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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A perspective on the growth-only zone, the secondary nucleation threshold and crystal size distribution in solution crystallisation

Threlfall

Coles

2016

CrystEngComm

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Nucleation Kinetics of the γ‐Polymorph of DL‐Methionine

Wantha

Flood

2012

Chem Eng & Technol

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The heterogeneous nucleation kinetics of γ‐DL‐methionine (γ‐DL‐met) in aqueous solution was measured using direct determination of the rate of nucleation based on measurements of particle (crystal) counts appearing in a microdroplet as a function of nucleation time. The nucleation rates increase with increasing temperature when the supersaturation ratio is used as a measure of the driving force, but the dependence is less clear when the nucleation rates are plotted against the absolute supersaturation. The nucleation rates were found to exponentially increase with respect to the supersaturation ratio of DL‐met. The measured nucleation kinetics follow trends expected from the classical nucleation theory (CNT), allowing approximate interfacial energies to be estimated by fitting the measured data to the CNT. The predicted interfacial energies and nucleation rates are consistent with results of similar species given in the literature.

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Population Balance Modeling of the Solution‐Mediated Transformation of DL‐Methionine Polymorphs

Wantha¹,

Flood²

2013

Chem Eng & Technol

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Experimental measurements of the solution‐mediated transformation (SMT) of the metastable polymorph of DL‐methionine (α‐DL‐met) into the stable polymorph (γ‐DL‐met) in water were performed at 25 °C. These results were compared to models of the crystallization and the SMT of α‐DL‐met into γ‐DL‐met that were developed using the concept of the population balance equation (PBE) applied to both of the polymorphs. The growth, dissolution, and nucleation kinetic expressions obtained in a previous work were used in the models. It was found that the PBE models did not satisfactorily describe the SMT process of DL‐met when the measured crystallization and dissolution kinetics were used. There were large mismatches between the simulation and the experimental results. Modifying the model of the dissolution kinetics of α‐DL‐met enabled these mismatches to be lowered. The results showed that the SMT of DL‐met is controlled by the rate of dissolution of α‐DL‐met.

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Crystal growth rates and secondary nucleation threshold for γ-dl-methionine in aqueous solution

Cited by 21 publications

References 14 publications

A perspective on the growth-only zone, the secondary nucleation threshold and crystal size distribution in solution crystallisation

A perspective on the growth-only zone, the secondary nucleation threshold and crystal size distribution in solution crystallisation

Nucleation Kinetics of the γ‐Polymorph of DL‐Methionine

Population Balance Modeling of the Solution‐Mediated Transformation of DL‐Methionine Polymorphs

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