New results are reported from an ongoing international research effort to accurately determine the Avogadro constant by counting the atoms in an isotopically enriched silicon crystal. The surfaces of two 28 Si-enriched spheres were decontaminated and reworked in order to produce an outer surface without metal contamination and improved sphericity. New measurements were then made on these two reconditioned spheres using improved methods and apparatuses. When combined with other recently refined parameter measurements, the Avogadro constant derived from these new results has a value of N A = 6.022 140 76(12) × 10 23 mol -1 . The X-ray crystal density method has thus achieved the target relative standard uncertainty of 2.0 × 10 -8 necessary for the realization of the definition of the new kilogram.
The molar mass of a 28Si-enriched crystal was measured at the National Metrology Institute of Japan to determine the Avogadro constant by the x-ray crystal density method as part of the International Avogadro Coordination project. The molar mass was determined by isotope ratio measurements using a multicollector inductively coupled plasma mass spectrometer combined with an isotope dilution technique. The 28Si-enriched crystal was dissolved in tetramethylammonium hydroxide and three different blended solutions were used to correct for mass bias in the measurement. The molar mass of the 28Si-enriched crystal was determined to be 27.976 970 09 g mol−1 with a standard uncertainty of 0.000 000 14 g mol−1. This corresponds to a relative standard uncertainty of 5.2 × 10−9. This result is consistent with measurements reported by the Physikalisch-Technische Bundesanstalt, Germany.
Highly efficient single-cell elemental analysis of microbial cells was achieved using a developed ICP-MS system with approximately 100% cell introduction efficiency and high time resolution.
A monitoring test for arsenic species in white rice flour was developed and applied to flours made from 20 samples of polished rice collected from locations all over Japan. The arsenic species in white rice flour made from five samples each of four types of rice were analyzed by HPLC-ICP-MS after a heat-assisted aqueous extraction. The total arsenic and major and minor element concentrations in the white rice flours were measured by ICP-MS and ICP-OES after microwave-assisted digestion. 91 ± 1% of the arsenic in the flours was extractable. Concentrations of arsenite [As(III)], arsenate [As(V)], and dimethylarsinic acid (DMAA) were closely positively correlated with the total arsenic concentrations. The total arsenic concentration in flours made from rice collected around Japan was 0.15 ± 0.07 mg kg(-1) (highest, 0.32 mg kg(-1)), which is very low. It was thus confirmed that the white rice flour samples collected in this experiment were not suffered from noticeable As contamination.
A method for the direct determination of dissolved silica in seawater by ion exclusion chromatography in combination with inductively coupled plasma mass spectrometry is described. This method was developed as a second, independent method to complement the usual colorimetric procedure in the determination of a certified concentration of dissolved silica in a planned seawater reference material. Ion exclusion affords a separation of the dissolved silica not only from the major seawater cations but also from potentially interfering anions. The detection limit, conservatively estimated at 2.3 ng g -1 as Si (0.08 µM), is superior to that achievable by direct analysis by inductively coupled plasma atomic emission spectrometry.
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