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Related Concept Videos

Recrystallization: Solid–Solution Equilibria01:10

Recrystallization: Solid–Solution Equilibria

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Recrystallization is a purification technique used to separate impurities from solid compounds. In this technique, no chemical reactions occur. Instead, it exploits physical properties only, specifically, the solubility differences between the desired compound and impurities, either at a single temperature or at different temperatures, and under other selected conditions. The solid-solution equilibrium (solubility equilibrium) of each component in the solution represents a binary phase...
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Crystal Growth: Principles of Crystallization01:25

Crystal Growth: Principles of Crystallization

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Crystallization is a phase transformation process in which crystals are precipitated from a supersaturated solution or formed from other sources. During crystallization, atoms or molecules arrange themselves into a well-defined, rigid crystal lattice to minimize energy.
Initiating crystallization involves manipulating the concentration of the solute and the temperature of the solution. Since crystal growth occurs when the ratio of concentration and solubility of the solute in the solvent...
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Precipitation Processes01:12

Precipitation Processes

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The experimental conditions in a gravimetric analysis should be optimized to maximize the particle size and purity of the obtained precipitate. Ideally, the concentration of the precipitating reagent should be low with effective stirring to maintain low relative supersaturation for the growth of large crystals. In homogeneous precipitation, the precipitant is slowly generated by a chemical reaction in the solution to avoid local reagent excesses. For example, urea decomposes gradually to...
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Washing, Drying, and Ignition of Precipitates00:52

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After filtration, the precipitate is washed to remove coprecipitated impurities and any remaining mother liquor. Colloidal precipitates, such as silver chloride, are washed with an electrolyte (such as dilute nitric acid) to prevent the peptization of the precipitate. In the case of slightly soluble precipitates, the wash solution contains a common ion to reduce solubility. Lead sulfate, which is slightly soluble in water, is washed with dilute sulfuric acid. Similarly, wash solutions may be...
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Precipitate Formation and Particle Size Control01:16

Precipitate Formation and Particle Size Control

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In precipitation gravimetry, the precipitating agent should react specifically or selectively with the analyte. While a specific reagent reacts with the analyte alone, a selective reagent can react with a limited number of chemical species.
The obtained precipitate should be either a pure substance of known composition or easily converted to one by a simple process, such as ignition or drying. In addition, the precipitate should be insoluble and easily filterable. In general, filterability...
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Colloidal precipitates01:09

Colloidal precipitates

3.7K
The high insolubility of some precipitates can result in an unfavorable relative supersaturation. This can lead to colloidal particles with a large surface-to-mass ratio, where adsorption is promoted. For instance, in the precipitation of silver chloride, silver ions are adsorbed on the surface of the colloidal particles, forming a primary layer. This layer attracts ions of opposite charge (such as nitrate ions), forming a diffuse secondary layer of adsorbed ions. This electric double layer...
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Updated: Dec 9, 2025

Optimization of Crystal Growth for Neutron Macromolecular Crystallography
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A Structured Approach To Cope with Impurities during Industrial Crystallization Development.

Stephanie J Urwin1, Guillaume Levilain2, Ivan Marziano3

  • 1EPSRC Centre for Innovative Manufacturing in Continuous Manufacturing and Crystallisation, University of Strathclyde, Glasgow, G1 1RD, U.K.

Organic Process Research & Development
|September 9, 2020
PubMed
Summary

Achieving high purity in crystallization is challenging due to impurity incorporation. This study presents a workflow to rapidly identify impurity mechanisms, enabling targeted solutions for better crystal purity and reduced development costs.

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Area of Science:

  • Chemical Engineering
  • Crystallization Science
  • Process Development

Background:

  • Achieving optimal purity, yield, and productivity in crystallization processes remains a significant challenge.
  • Unwanted impurities frequently contaminate crystalline products despite the inherent selectivity of crystallization.
  • Understanding impurity incorporation mechanisms is crucial for enhancing crystal purity.

Purpose of the Study:

  • To present a general workflow for the rapid identification of impurity incorporation mechanisms in crystallization.
  • To enable a targeted problem-solving approach for managing impurities during industrial crystallization development.
  • To decrease the resources expended on process development for crystallization.

Main Methods:

  • A general workflow comprising four standard laboratory experiments was developed.
  • The workflow facilitates discrimination between different impurity incorporation mechanisms.
  • The methodology was demonstrated using four active pharmaceutical ingredients with related organic impurities.

Main Results:

  • The presented workflow effectively identifies the mechanisms responsible for poor impurity rejection during crystallization.
  • Successful discrimination between incorporation mechanisms was achieved using standard instrumentation.
  • The workflow's application led to a targeted approach for impurity management.

Conclusions:

  • This workflow provides a rapid and targeted method for identifying impurity incorporation mechanisms in crystallization.
  • It facilitates efficient process development for industrial crystallization, leading to higher purity products.
  • The approach reduces the resources and time required for developing robust crystallization processes.