Journal
ANALYTICAL CHEMISTRY
Volume 73, Issue 11, Pages 2547-2553Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ac001550i
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We have developed a new, simple, and accurate method for the determination of total sulfur at microgram per gram levels in milligram-sized silicate materials with isotope dilution high-resolution inductively coupled plasma mass spectrometry equipped with a now injection system. In this method, sulfur can be quantitatively oxidized by bromine into sulfate with achievement of isotope equilibrium between the sample and spike. Detection limits for S-32(+) and S-34(+) in the ideal solution and silicate samples were 1 and 6 ng mL(-1) and 0.07 and 0.3 mug g(-1) respectively. The total blank was 46 ng, so that a 40-mg silicate sample containing 10 mug g(-1) sulfur can be measured with a blank correction of < 10%. This total blank can be lowered to 8 ng if a low-blank air system is used for evaporations. To evaluate the applicability of this method, we analyzed not only silicate reference materials with sulfur content of 5.25-489 mug g(-1) and sample sizes of 13-40 mg but also the Allende meteorite with a sulfur content of 2%. The reproducibility for various rock types was <9%, even though blank corrections in some samples of low sulfur content were up to 24%, This method is suitable for analyzing geological samples as well environmental samples such as soils, sediments, and water samples.
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