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

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 <TEX>${\mu}g$</TEX> 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 (<TEX>$99.17{\pm}0.14$</TEX>)%. 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.