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Abstract:We have applied the sequential extraction procedure developed by the Community Bureau of Reference (BCR) to eight Japanese geochemical reference materials. By using this method, we attempt to extract exchangeable and carbonate phases in step 1, extract iron hydroxide and manganese oxide in step 2, and extract metal sulfide and organic material in step 3. We use X-ray diffractometry (XRD) to measure untreated samples and the residue of samples after each step of the extraction process to determine whether the target material is satisfactorily decomposed during the procedure. For JSd-1 and JSd-3, XRD patterns do not change significantly by using the BCR procedure. Actually, most of the elements in these materials are scarcely extracted by BCR scheme. The peaks of calcite in JSd-4, JMs-1 and JMs-2 disappear in the XRD patterns after the first extraction procedure. The result suggests that the target phase of step 1 process is fully decomposed. JLk-1 and JMs-2 show high concentrations of the Fe and Mn extracted in step 2. However, it is difficult to clearly confirm the full decomposition of iron hydroxide and manganese oxide in step 2 because these materials do not show distinct peaks in the XRD patterns. Pyrite in JMs-1 disappears in step 3 of the extraction, which suggests that sulfide is satisfactorily decomposed in this process. X-ray reflection intensities of some peaks for quartz and plagioclase in JSO-1 increase significantly after step 3 of the extraction. It is assumed that organic material thickly covered the mineral surfaces and reduced the X-ray reflection from the minerals prior to the third procedure. Although this evidence is indirect, we conclude that organic material is successfully decomposed and removed from the mineral surface during the third extraction procedure. On the basis of these results, it is confirmed that the BCR protocol can properly extract target materials from the geochemical reference materials.

The contents of total carbon, hydrogen, nitrogen and sulfur in twenty‐seven geological reference materials, issued by five producer organisations (USGS, CCRMP, ANRT, NIST and GSJ) were determined using an automated simultaneous elemental analyser following combustion. In order to complete gasification of C and N in some geological materials, the combustion temperature needed to be greater than 1150 °C. The calibrator prepared from known amounts of reagent material was not adopted for more than 1.2% m/m of H. Unrealistically high values in certain materials supposed to contain less than 1000 μg g−1 S may be due mainly to memory effects. The limit of detection was 50 μg g−1 for C and N, 500 μg g−1 for H and 1000 μg g−1 for S. Although the blank value of C and N was always stable and less than one third of the detection limit, it had a slightly higher value for N and S. By repeating long‐term analysis, high reproducibility for each of the four elements was verified. The method has been applied satisfactorily to a variety of geological reference materials, and recommended values for C, H and N for most of the reference materials studied have been tabulated.