4.3 Article

Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II

Journal

BULLETIN OF THE KOREAN CHEMICAL SOCIETY
Volume 34, Issue 2, Pages 531-538

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.5012/bkcs.2013.34.2.531

Keywords

Purity assay; Oraganic substance; GC-FID; K-F coulometry; TGA

Funding

  1. Korea Research Institute of Standards and Science under the project 'Establishment of standard system in food and environmental measurements' [12011026]

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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 mu g 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.

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