Determination of zirconium, niobium, hafnium and tantalum at ng g -1 levels in geological materials by direct nebulisation of sample HF solution into FI-ICP-MS

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Abstract

We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble Mg and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were, 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder.

Original languageEnglish
Pages (from-to)7-20
Number of pages14
JournalGeostandards Newsletter
Volume23
Issue number1
DOIs
Publication statusPublished - 1999

Fingerprint

Hafnium
Niobium
Tantalum
hafnium
tantalum
niobium
Silicates
peridotite
Isotopes
Dilution
andesite
Meteorites
Inductively coupled plasma mass spectrometry
dilution
silicate
basalt
Mass spectrometers
isotope
Fluorides
Powders

Keywords

  • Flow injection
  • Geological reference materials
  • Hf
  • ICP-MS
  • Nb
  • Peridotite
  • Ta
  • Zr

ASJC Scopus subject areas

  • Geochemistry and Petrology
  • Geology

Cite this

@article{dc7a85af2d754629ab0aa6a2bd80999a,
title = "Determination of zirconium, niobium, hafnium and tantalum at ng g -1 levels in geological materials by direct nebulisation of sample HF solution into FI-ICP-MS",
abstract = "We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble Mg and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were, 96{\%} for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85{\%}). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder.",
keywords = "Flow injection, Geological reference materials, Hf, ICP-MS, Nb, Peridotite, Ta, Zr",
author = "Akio Makishima and Eizou Nakamura and Toshio Nakano",
year = "1999",
doi = "10.1111/j.1751-908X.1999.tb00555.x",
language = "English",
volume = "23",
pages = "7--20",
journal = "Geostandards and Geoanalytical Research",
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TY - JOUR

T1 - Determination of zirconium, niobium, hafnium and tantalum at ng g -1 levels in geological materials by direct nebulisation of sample HF solution into FI-ICP-MS

AU - Makishima, Akio

AU - Nakamura, Eizou

AU - Nakano, Toshio

PY - 1999

Y1 - 1999

N2 - We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble Mg and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were, 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder.

AB - We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble Mg and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were, 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder.

KW - Flow injection

KW - Geological reference materials

KW - Hf

KW - ICP-MS

KW - Nb

KW - Peridotite

KW - Ta

KW - Zr

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U2 - 10.1111/j.1751-908X.1999.tb00555.x

DO - 10.1111/j.1751-908X.1999.tb00555.x

M3 - Article

VL - 23

SP - 7

EP - 20

JO - Geostandards and Geoanalytical Research

JF - Geostandards and Geoanalytical Research

SN - 0150-5505

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