Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II

  • Kim, Seung-Hyun (Division of Metrology for Quality Life Korea Research Institute of Standards and Science) ;
  • Lee, Joonhee (Division of Metrology for Quality Life Korea Research Institute of Standards and Science) ;
  • Ahn, Seonghee (Division of Metrology for Quality Life Korea Research Institute of Standards and Science) ;
  • Song, Young-Sin (Division of Metrology for Quality Life Korea Research Institute of Standards and Science) ;
  • Kim, Dong-Kyum (Division of Metrology for Quality Life Korea Research Institute of Standards and Science) ;
  • Kim, Byungjoo (Division of Metrology for Quality Life Korea Research Institute of Standards and Science)
  • Received : 2012.09.12
  • Accepted : 2012.11.19
  • Published : 2013.02.20
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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. Non-volatile 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 ($99.17{\pm}0.14$)%. 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.

Keywords

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