Solubility Determination from Clear Points upon Solvent Addition
Solubility Determination from Clear Points upon Solvent Addition
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DOI：
10.1021/acs.oprd.5b00156
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发表时间：
2015-08-01
影响因子：
3.4
通讯作者：
ter Horst, Joop H.
中科院分区：
文献类型：
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作者：
Reus, Marloes A.;van der Heijden, Antoine E. D. M.;ter Horst, Joop H.
本文介绍了一种在恒温条件下从样品稀释后的澄清点测定多组分结晶化合物溶解度的方法。通过向已知组成的悬浮液中连续加入溶剂混合物直至出现澄清溶液来建立澄清点。为了进行验证，将该溶剂添加方法与恒温下的传统平衡浓度方法和最近的温度变化方法进行比较，其中温度变化方法在增加样品温度时测定澄清点温度。与平衡浓度法相比，使用溶剂添加法测量的二元体系（1种溶质，1种溶剂）的溶解度数据相对较快地获得。这些溶解度数据与温度变化法和平衡浓度法的数据一致。对于温度变化法，结果取决于加热速率。同样，对于溶剂添加方法，它们取决于添加速率。此外，对于涉及反溶剂或共晶的三元体系，溶解度在恒定温度下使用溶剂添加法测定。在溶剂混合物和其它复杂的多组分体系的情况下，使用溶剂添加法是特别有价值的，其中温度变化法不能容易地应用。
A method is described for determining the solubility of multicomponent crystalline compounds from clear points upon sample dilution at a constant temperature. Clear points are established by continuously adding a solvent mixture to a suspension of known composition until a clear solution appears. For validation, this solvent addition method is compared to the traditional equilibrium concentration method at constant temperature and the more recent temperature variation method with which clear point temperatures are determined upon increasing the sample temperature. Solubility data of binary systems (1 solute, 1 solvent) measured using the solvent addition method are obtained relatively quickly compared to the equilibrium concentration method. These solubility data are consistent with those of the temperature variation and the equilibrium concentration method. For the temperature variation method, the results are dependent on the heating rate. Likewise, for the solvent addition method, they are dependent on the addition rate. Additionally, for ternary systems involving antisolvent or cocrystals, solubilities are determined at a constant temperature using the solvent addition method. The use of the solvent addition method is especially valuable in the case of solvent mixtures and other complex multicomponent systems, in which the temperature variation method cannot be applied easily.