Inhomogeneity of sediment samples in analysis of hexabromocyclododecane

The repeatability test of the analytical method for hexabromocyclododecane (HBCD) was conducted with sediment sample. The maximum HBCD concentration exceeded the minimum by a factor of 90 even though the identical sediment samples were used. Therefore, we examined which step of the analytical method was the factor causing variability. We examined the blank test, and confirmation test of the extraction and purified procedure. From these results, we confirmed that there was nothing wrong with the accuracy of our analytical method. These results indicate that the variability of HBCD concentration in the repeatability test was attributed not to the analytical method, but to the inhomogeneity of the sediment sample. Aluminum, silicon, and organic carbon in sediments were measured to compare the variability of these concentrations with that of HBCD concentration. These concentrations were similar values within identical samples which showed variability in HBCD concentration. HBCD concentration in several samples did not correlate with organic carbon content. These results suggests that sediment samples were homogeneous by itself, and HBCD was heterogeneously distributed in spite of homogeneity of organic carbon in sediment. The sediment sample with variability in HBCD concentration showed different HBCD diastereomer compositions in identical sediment. It implies that the sample contained HBCD derived from different histories or point sources. Even though we increased sample amounts to analyze the homogeneity of the sample, HBCD concentration varied within identical samples if the sample had a hot spot. Past monitoring data may contain overestimation or underestimation of HBCD concentration in sediment.