Determination of chromium, nickel, copper and zinc in milligram samples of geological materials using isotope dilution high resolution inductively coupled plasma-mass spectrometry

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Abstract

A simple and accurate method for the determination of Cr, Ni, Cu and Zn at μg g-1 levels in milligram-sized bulk silicate materials is reported using isotope dilution high-resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) with a flow injection system. Silicate samples with Cr, Ni, Cu and Zn spikes were digested with HF-HBr and Br2, and subsequently decomposed at 518 K in a Teflon bomb. In this procedure, all sulfides and chromite, major hosts of these elements, were completely decomposed, thus allowing for isotope equilibration between the sample and spike. Magnesium and Al fluorides formed after the digestion of the sample were removed by centrifugation, and the supernatant was directly aspirated into a HR-ICP-MS at a mass resolution of 7500, where interfering oxide ions, ArO +, CaO+, TiO+, CrO+ and VO +, were separated from Cr+, Ni+, Cu+ and Zn+. No matrix effects were observed down to a dilution factor of 50. Detection limits for these elements in silicate samples were <0.04 μg g-1. The effectiveness of the technique was demonstrated by the analysis of 13 to 40 mg test portions of USGS and GSJ silicate reference materials with a major element composition ranging from andesite to peridotite, in addition to 8-23 mg of the Smithsonian reference Allende. Both the reproducibility and the deviation from the reference value for most reference materials of various rock types were <9%, and thus confirm that the method gives accurate analytical results for small sample sizes over a wide range of Cr, Ni, Cu and Zn contents. This method is, therefore, suitable for analysing small and/or precious bulk samples, such as meteorites, mantle peridotites and mineral separates, and for the characterisation of silicate and sulfide minerals for use as calibration samples in secondary ion mass spectrometry or laser ablation ICP-MS.

Original languageEnglish
Pages (from-to)41-51
Number of pages11
JournalGeostandards Newsletter
Volume26
Issue number1
DOIs
Publication statusPublished - 2002

Fingerprint

Silicates
Inductively coupled plasma mass spectrometry
Chromium
Nickel
Isotopes
Dilution
chromium
Zinc
Copper
nickel
dilution
silicate
mass spectrometry
zinc
isotope
copper
plasma
Silicate minerals
Meteorites
Sulfide minerals

Keywords

  • Cr
  • Cu
  • High resolution ICP-MS
  • Isotope dilution
  • Method development
  • Ni
  • Reference materials
  • Zn

ASJC Scopus subject areas

  • Geochemistry and Petrology
  • Geology

Cite this

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title = "Determination of chromium, nickel, copper and zinc in milligram samples of geological materials using isotope dilution high resolution inductively coupled plasma-mass spectrometry",
abstract = "A simple and accurate method for the determination of Cr, Ni, Cu and Zn at μg g-1 levels in milligram-sized bulk silicate materials is reported using isotope dilution high-resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) with a flow injection system. Silicate samples with Cr, Ni, Cu and Zn spikes were digested with HF-HBr and Br2, and subsequently decomposed at 518 K in a Teflon bomb. In this procedure, all sulfides and chromite, major hosts of these elements, were completely decomposed, thus allowing for isotope equilibration between the sample and spike. Magnesium and Al fluorides formed after the digestion of the sample were removed by centrifugation, and the supernatant was directly aspirated into a HR-ICP-MS at a mass resolution of 7500, where interfering oxide ions, ArO +, CaO+, TiO+, CrO+ and VO +, were separated from Cr+, Ni+, Cu+ and Zn+. No matrix effects were observed down to a dilution factor of 50. Detection limits for these elements in silicate samples were <0.04 μg g-1. The effectiveness of the technique was demonstrated by the analysis of 13 to 40 mg test portions of USGS and GSJ silicate reference materials with a major element composition ranging from andesite to peridotite, in addition to 8-23 mg of the Smithsonian reference Allende. Both the reproducibility and the deviation from the reference value for most reference materials of various rock types were <9{\%}, and thus confirm that the method gives accurate analytical results for small sample sizes over a wide range of Cr, Ni, Cu and Zn contents. This method is, therefore, suitable for analysing small and/or precious bulk samples, such as meteorites, mantle peridotites and mineral separates, and for the characterisation of silicate and sulfide minerals for use as calibration samples in secondary ion mass spectrometry or laser ablation ICP-MS.",
keywords = "Cr, Cu, High resolution ICP-MS, Isotope dilution, Method development, Ni, Reference materials, Zn",
author = "Akio Makishima and Katsura Kobayashi and Eizou Nakamura",
year = "2002",
doi = "10.1111/j.1751-908X.2002.tb00622.x",
language = "English",
volume = "26",
pages = "41--51",
journal = "Geostandards and Geoanalytical Research",
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TY - JOUR

T1 - Determination of chromium, nickel, copper and zinc in milligram samples of geological materials using isotope dilution high resolution inductively coupled plasma-mass spectrometry

AU - Makishima, Akio

AU - Kobayashi, Katsura

AU - Nakamura, Eizou

PY - 2002

Y1 - 2002

N2 - A simple and accurate method for the determination of Cr, Ni, Cu and Zn at μg g-1 levels in milligram-sized bulk silicate materials is reported using isotope dilution high-resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) with a flow injection system. Silicate samples with Cr, Ni, Cu and Zn spikes were digested with HF-HBr and Br2, and subsequently decomposed at 518 K in a Teflon bomb. In this procedure, all sulfides and chromite, major hosts of these elements, were completely decomposed, thus allowing for isotope equilibration between the sample and spike. Magnesium and Al fluorides formed after the digestion of the sample were removed by centrifugation, and the supernatant was directly aspirated into a HR-ICP-MS at a mass resolution of 7500, where interfering oxide ions, ArO +, CaO+, TiO+, CrO+ and VO +, were separated from Cr+, Ni+, Cu+ and Zn+. No matrix effects were observed down to a dilution factor of 50. Detection limits for these elements in silicate samples were <0.04 μg g-1. The effectiveness of the technique was demonstrated by the analysis of 13 to 40 mg test portions of USGS and GSJ silicate reference materials with a major element composition ranging from andesite to peridotite, in addition to 8-23 mg of the Smithsonian reference Allende. Both the reproducibility and the deviation from the reference value for most reference materials of various rock types were <9%, and thus confirm that the method gives accurate analytical results for small sample sizes over a wide range of Cr, Ni, Cu and Zn contents. This method is, therefore, suitable for analysing small and/or precious bulk samples, such as meteorites, mantle peridotites and mineral separates, and for the characterisation of silicate and sulfide minerals for use as calibration samples in secondary ion mass spectrometry or laser ablation ICP-MS.

AB - A simple and accurate method for the determination of Cr, Ni, Cu and Zn at μg g-1 levels in milligram-sized bulk silicate materials is reported using isotope dilution high-resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) with a flow injection system. Silicate samples with Cr, Ni, Cu and Zn spikes were digested with HF-HBr and Br2, and subsequently decomposed at 518 K in a Teflon bomb. In this procedure, all sulfides and chromite, major hosts of these elements, were completely decomposed, thus allowing for isotope equilibration between the sample and spike. Magnesium and Al fluorides formed after the digestion of the sample were removed by centrifugation, and the supernatant was directly aspirated into a HR-ICP-MS at a mass resolution of 7500, where interfering oxide ions, ArO +, CaO+, TiO+, CrO+ and VO +, were separated from Cr+, Ni+, Cu+ and Zn+. No matrix effects were observed down to a dilution factor of 50. Detection limits for these elements in silicate samples were <0.04 μg g-1. The effectiveness of the technique was demonstrated by the analysis of 13 to 40 mg test portions of USGS and GSJ silicate reference materials with a major element composition ranging from andesite to peridotite, in addition to 8-23 mg of the Smithsonian reference Allende. Both the reproducibility and the deviation from the reference value for most reference materials of various rock types were <9%, and thus confirm that the method gives accurate analytical results for small sample sizes over a wide range of Cr, Ni, Cu and Zn contents. This method is, therefore, suitable for analysing small and/or precious bulk samples, such as meteorites, mantle peridotites and mineral separates, and for the characterisation of silicate and sulfide minerals for use as calibration samples in secondary ion mass spectrometry or laser ablation ICP-MS.

KW - Cr

KW - Cu

KW - High resolution ICP-MS

KW - Isotope dilution

KW - Method development

KW - Ni

KW - Reference materials

KW - Zn

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