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Synthesis, structures, characterization and deterioration of potassium glycolate hemihydrate.

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Title: Synthesis, structures, characterization and deterioration of potassium glycolate hemihydrate.
Authors: Hu, Mingyang, Yang, Hexiong, Huo, Xiaojia, Lian, Bin
Source: CrystEngComm; 7/28/2025, Vol. 27 Issue 28, p4816-4825, 10p
Subject Terms: X-ray diffraction, CRYSTAL structure, THERMOGRAVIMETRY, STABILITY (Mechanics), GLYCOLATES, CRYSTALLIZATION, HYDRATION, SPECTROMETRY
Abstract: The process of glycolate crystallization is well documented; however, research on the formation of potassium chelate with glycolate and the characteristics of the resulting crystals remains limited. In this study, a potassium glycolate hemihydrate (PGH) crystal, ideally K(C2H3O3)·0.5H2O, was obtained by freeze-drying, evaporation, and liquid phase diffusion. PGH was characterized by single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, DFT calculation, thermogravimetric analysis, and powder X-ray diffraction refinement. A structurally similar compound, potassium glycolate glycolic acid [K(C2H3O3)(C2H4O3), PGGA], was synthesized for comparison. The results revealed that PGH is monoclinic with the space group P21/m and unit cell parameters a = 5.8982(1), b = 7.2515(1), c = 11.0270(1) Å, β = 102.253(1)°, and V = 460.890(11) Å3. The infrared and Raman spectra of PGH and PGGA exhibit notable similarities and are highly consistent with the calculated infrared spectra calculated. Thermogravimetric analysis indicated that PGH dehydrated at approximately 60 °C; however, further experiments showed that PGH gradually transformed into PGGA at 30 °C. This study provides new insights into the bonding behavior of glycolate and the stability of its crystalline forms. [ABSTRACT FROM AUTHOR]
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Abstract:The process of glycolate crystallization is well documented; however, research on the formation of potassium chelate with glycolate and the characteristics of the resulting crystals remains limited. In this study, a potassium glycolate hemihydrate (PGH) crystal, ideally K(C<subscript>2</subscript>H<subscript>3</subscript>O<subscript>3</subscript>)·0.5H<subscript>2</subscript>O, was obtained by freeze-drying, evaporation, and liquid phase diffusion. PGH was characterized by single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, DFT calculation, thermogravimetric analysis, and powder X-ray diffraction refinement. A structurally similar compound, potassium glycolate glycolic acid [K(C<subscript>2</subscript>H<subscript>3</subscript>O<subscript>3</subscript>)(C<subscript>2</subscript>H<subscript>4</subscript>O<subscript>3</subscript>), PGGA], was synthesized for comparison. The results revealed that PGH is monoclinic with the space group P2<subscript>1</subscript>/m and unit cell parameters a = 5.8982(1), b = 7.2515(1), c = 11.0270(1) Å, β = 102.253(1)°, and V = 460.890(11) Å<sup>3</sup>. The infrared and Raman spectra of PGH and PGGA exhibit notable similarities and are highly consistent with the calculated infrared spectra calculated. Thermogravimetric analysis indicated that PGH dehydrated at approximately 60 °C; however, further experiments showed that PGH gradually transformed into PGGA at 30 °C. This study provides new insights into the bonding behavior of glycolate and the stability of its crystalline forms. [ABSTRACT FROM AUTHOR]
ISSN:14668033
DOI:10.1039/d5ce00182j