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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 34, Number 2
BKCSDE 34(2)
February 20, 2013 

 
Title
Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II
Author
Seung-Hyun Kim, Joonhee Lee, Seonghee Ahn, Young-Sin Song, Dong-Kyum Kim, Byungjoo Kim*
Keywords
Purity assay, Oraganic substance, GC-FID, K-F coulometry, TGA
Abstract
A mass balance method established in this laboratory was applied to determine the purity of an endosulfan-II pure substance. Gas chromatography-flame ionization detector (GC-FID) was used to measure organic impurities. Total of 10 structurally related organic impurities were detected by GC-FID in the material. Water content was determined to be 0.187% by Karl-Fischer (K-F) coulometry with an oven-drying method. Nonvolatile residual impurities was not detected by Thermal gravimetric analysis (TGA) within the detection limit of 0.04% (0.7 μg in absolute amount). Residual solvents within the substance were determined to be 0.007% in the Endosulfan-II pure substance by running GC-FID after dissolving it with two solvents. The purity of the endosulfan-II was finally assigned to be (99.17 ± 0.14)%. Details of the mass balance method including interpretation and evaluating uncertainties of results from each individual methods and the finally assayed purity were also described.
Page
531 - 538
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