{"title":"用缓慢蒸发法从混合溶剂中结晶对氨基苯甲酸的 α 和 β 多晶体","authors":"Ansu Mathew, Madhumitha Madhesh, Srinivasan Karuppannan","doi":"10.1002/crat.202400216","DOIUrl":null,"url":null,"abstract":"<p>Para aminobenzoic acid (p-ABA), a well-known pharmaceutical material with a challenging polymorphic nature, is chosen for study in this paper. The material has four reported polymorphs, containing two solution forms (α and β), a vapor form, and a high-pressure form. The solution-grown forms α and β are experimentally grown using mixed solvents of water and isopropyl alcohol with nine different mixing compositions at temperatures of 298, 303, and 308 K. The solubility of the commercially available p-ABA is calculated gravimetrically, and the polymorphic crystals are grown using the slow solvent evaporation method for all the mixing ratios at different temperatures. A ternary diagram constructed on the solubility of p-ABA in mixed solvents gives an insight into the nucleation nature of two polymorphs. To understand the nature of nucleation and growth of two forms of p-ABA, an in situ microscopic study is carried out, and the grown crystals are characterized using powder X-ray diffraction analysis and differential scanning calorimetry. This also confirmed that the grown crystals are two solutions grown polymorphs of para aminobenzoic acid, both belonging to monoclinic systems with P2<sub>1</sub>/n space group.</p>","PeriodicalId":48935,"journal":{"name":"Crystal Research and Technology","volume":"60 2","pages":""},"PeriodicalIF":1.5000,"publicationDate":"2024-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Crystallization of α and β Polymorphs of Para Aminobenzoic Acid from Mixed Solvents by Slow Evaporation Method\",\"authors\":\"Ansu Mathew, Madhumitha Madhesh, Srinivasan Karuppannan\",\"doi\":\"10.1002/crat.202400216\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>Para aminobenzoic acid (p-ABA), a well-known pharmaceutical material with a challenging polymorphic nature, is chosen for study in this paper. The material has four reported polymorphs, containing two solution forms (α and β), a vapor form, and a high-pressure form. The solution-grown forms α and β are experimentally grown using mixed solvents of water and isopropyl alcohol with nine different mixing compositions at temperatures of 298, 303, and 308 K. The solubility of the commercially available p-ABA is calculated gravimetrically, and the polymorphic crystals are grown using the slow solvent evaporation method for all the mixing ratios at different temperatures. A ternary diagram constructed on the solubility of p-ABA in mixed solvents gives an insight into the nucleation nature of two polymorphs. To understand the nature of nucleation and growth of two forms of p-ABA, an in situ microscopic study is carried out, and the grown crystals are characterized using powder X-ray diffraction analysis and differential scanning calorimetry. This also confirmed that the grown crystals are two solutions grown polymorphs of para aminobenzoic acid, both belonging to monoclinic systems with P2<sub>1</sub>/n space group.</p>\",\"PeriodicalId\":48935,\"journal\":{\"name\":\"Crystal Research and Technology\",\"volume\":\"60 2\",\"pages\":\"\"},\"PeriodicalIF\":1.5000,\"publicationDate\":\"2024-12-31\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Crystal Research and Technology\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/crat.202400216\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"Chemistry\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Crystal Research and Technology","FirstCategoryId":"88","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/crat.202400216","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"Chemistry","Score":null,"Total":0}
Crystallization of α and β Polymorphs of Para Aminobenzoic Acid from Mixed Solvents by Slow Evaporation Method
Para aminobenzoic acid (p-ABA), a well-known pharmaceutical material with a challenging polymorphic nature, is chosen for study in this paper. The material has four reported polymorphs, containing two solution forms (α and β), a vapor form, and a high-pressure form. The solution-grown forms α and β are experimentally grown using mixed solvents of water and isopropyl alcohol with nine different mixing compositions at temperatures of 298, 303, and 308 K. The solubility of the commercially available p-ABA is calculated gravimetrically, and the polymorphic crystals are grown using the slow solvent evaporation method for all the mixing ratios at different temperatures. A ternary diagram constructed on the solubility of p-ABA in mixed solvents gives an insight into the nucleation nature of two polymorphs. To understand the nature of nucleation and growth of two forms of p-ABA, an in situ microscopic study is carried out, and the grown crystals are characterized using powder X-ray diffraction analysis and differential scanning calorimetry. This also confirmed that the grown crystals are two solutions grown polymorphs of para aminobenzoic acid, both belonging to monoclinic systems with P21/n space group.
期刊介绍:
The journal Crystal Research and Technology is a pure online Journal (since 2012).
Crystal Research and Technology is an international journal examining all aspects of research within experimental, industrial, and theoretical crystallography. The journal covers the relevant aspects of
-crystal growth techniques and phenomena (including bulk growth, thin films)
-modern crystalline materials (e.g. smart materials, nanocrystals, quasicrystals, liquid crystals)
-industrial crystallisation
-application of crystals in materials science, electronics, data storage, and optics
-experimental, simulation and theoretical studies of the structural properties of crystals
-crystallographic computing