Determination of molybdenum, antimony and tungsten at sub μg g -1 levels in geological materials by ID-FI-ICP-MS

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Abstract

We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94% for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81%. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g-1 level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was <9%. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates.

Original languageEnglish
Pages (from-to)137-148
Number of pages12
JournalGeostandards Newsletter
Volume23
Issue number2
DOIs
Publication statusPublished - 1999

Fingerprint

Antimony
Tungsten
Molybdenum
antimony
tungsten
molybdenum
peridotite
andesite
Silicates
Geological surveys
basalt
Isotopes
geological survey
Dilution
dilution
silicate
isotope
Meteorites
Recovery
Inductively coupled plasma mass spectrometry

Keywords

  • Flow injection
  • ICP-MS
  • Isotope dilution
  • Method development
  • Mo
  • Reference materials
  • Sb
  • W

ASJC Scopus subject areas

  • Geochemistry and Petrology
  • Geology

Cite this

@article{533e35dcb604433cb53fd535a1665517,
title = "Determination of molybdenum, antimony and tungsten at sub μg g -1 levels in geological materials by ID-FI-ICP-MS",
abstract = "We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94{\%} for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81{\%}. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g-1 level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was <9{\%}. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates.",
keywords = "Flow injection, ICP-MS, Isotope dilution, Method development, Mo, Reference materials, Sb, W",
author = "Akio Makishima and Eizou Nakamura",
year = "1999",
doi = "10.1111/j.1751-908X.1999.tb00569.x",
language = "English",
volume = "23",
pages = "137--148",
journal = "Geostandards and Geoanalytical Research",
issn = "0150-5505",
publisher = "Wiley-Blackwell",
number = "2",

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TY - JOUR

T1 - Determination of molybdenum, antimony and tungsten at sub μg g -1 levels in geological materials by ID-FI-ICP-MS

AU - Makishima, Akio

AU - Nakamura, Eizou

PY - 1999

Y1 - 1999

N2 - We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94% for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81%. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g-1 level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was <9%. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates.

AB - We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94% for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81%. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g-1 level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was <9%. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates.

KW - Flow injection

KW - ICP-MS

KW - Isotope dilution

KW - Method development

KW - Mo

KW - Reference materials

KW - Sb

KW - W

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U2 - 10.1111/j.1751-908X.1999.tb00569.x

DO - 10.1111/j.1751-908X.1999.tb00569.x

M3 - Article

VL - 23

SP - 137

EP - 148

JO - Geostandards and Geoanalytical Research

JF - Geostandards and Geoanalytical Research

SN - 0150-5505

IS - 2

ER -