Determination of total sulfur at microgram per gram levels in geological materials by oxidation of sulfur into sulfate with in situ generation of bromine using isotope dilution high-resolution ICPMS

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Abstract

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 flow 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 32S+ and 34S+ in the ideal solution and silicate samples were 1 and 6 ng mL-1 and 0.07 and 0.3 μg g-1, respectively. The total blank was 46 ng, so that a 40-mg silicate sample containing 10 μg 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 μg 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

Original languageEnglish
Pages (from-to)2547-2553
Number of pages7
JournalAnalytical Chemistry
Volume73
Issue number11
DOIs
Publication statusPublished - Jun 1 2001

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Bromine
Silicates
Sulfur
Isotopes
Dilution
Sulfates
Oxidation
Meteorites
Inductively coupled plasma mass spectrometry
Evaporation
Rocks
Air

ASJC Scopus subject areas

  • Analytical Chemistry

Cite this

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title = "Determination of total sulfur at microgram per gram levels in geological materials by oxidation of sulfur into sulfate with in situ generation of bromine using isotope dilution high-resolution ICPMS",
abstract = "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 flow 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 32S+ and 34S+ in the ideal solution and silicate samples were 1 and 6 ng mL-1 and 0.07 and 0.3 μg g-1, respectively. The total blank was 46 ng, so that a 40-mg silicate sample containing 10 μg 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 μg 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",
author = "Akio Makishima and Eizou Nakamura",
year = "2001",
month = "6",
day = "1",
doi = "10.1021/ac001550i",
language = "English",
volume = "73",
pages = "2547--2553",
journal = "Analytical Chemistry",
issn = "0003-2700",
publisher = "American Chemical Society",
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T1 - Determination of total sulfur at microgram per gram levels in geological materials by oxidation of sulfur into sulfate with in situ generation of bromine using isotope dilution high-resolution ICPMS

AU - Makishima, Akio

AU - Nakamura, Eizou

PY - 2001/6/1

Y1 - 2001/6/1

N2 - 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 flow 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 32S+ and 34S+ in the ideal solution and silicate samples were 1 and 6 ng mL-1 and 0.07 and 0.3 μg g-1, respectively. The total blank was 46 ng, so that a 40-mg silicate sample containing 10 μg 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 μg 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

AB - 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 flow 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 32S+ and 34S+ in the ideal solution and silicate samples were 1 and 6 ng mL-1 and 0.07 and 0.3 μg g-1, respectively. The total blank was 46 ng, so that a 40-mg silicate sample containing 10 μg 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 μg 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

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U2 - 10.1021/ac001550i

DO - 10.1021/ac001550i

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