Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.

This manuscript describes a new protocol for determination of Pa/Th/U in marine sediments. It is based on microwave-assisted digestion and represents an important reduction of working time over conventional hot-plate digestion methods, and the use of HClO(4) is avoided. Although Th and U are complet...

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Main Authors: Negre, C, Thomas, A, Mas, J, Garcia-Orellana, J, Henderson, G, Masqué, P, Zahn, R
Format: Journal article
Language:English
Published: 2009
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author Negre, C
Thomas, A
Mas, J
Garcia-Orellana, J
Henderson, G
Masqué, P
Zahn, R
author_facet Negre, C
Thomas, A
Mas, J
Garcia-Orellana, J
Henderson, G
Masqué, P
Zahn, R
author_sort Negre, C
collection OXFORD
description This manuscript describes a new protocol for determination of Pa/Th/U in marine sediments. It is based on microwave-assisted digestion and represents an important reduction of working time over conventional hot-plate digestion methods, and the use of HClO(4) is avoided. Although Th and U are completely dissolved with a first microwave step, around 40% of (231)Pa remains undissolved, and a short hot-plate step with reverse aqua regia is required to achieve total digestion and spike equilibration. Next, the method involves a separation of these elements and a further purification of the Pa fraction using Dowex AG1-X8 resin. Separation with Bio-Rad and Sigma-Aldrich resins was compared; although both perform similarly for Th and U, Pa yields are higher with Bio-Rad. Finally, samples are measured using a Nu instruments multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS). Overall chemical yields range around 50% for Pa, 60% for Th, and 70% for U.
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spelling oxford-uuid:464924ab-f30a-477f-a364-6058195cc2672022-03-26T15:12:49ZSeparation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.Journal articlehttp://purl.org/coar/resource_type/c_dcae04bcuuid:464924ab-f30a-477f-a364-6058195cc267EnglishSymplectic Elements at Oxford2009Negre, CThomas, AMas, JGarcia-Orellana, JHenderson, GMasqué, PZahn, RThis manuscript describes a new protocol for determination of Pa/Th/U in marine sediments. It is based on microwave-assisted digestion and represents an important reduction of working time over conventional hot-plate digestion methods, and the use of HClO(4) is avoided. Although Th and U are completely dissolved with a first microwave step, around 40% of (231)Pa remains undissolved, and a short hot-plate step with reverse aqua regia is required to achieve total digestion and spike equilibration. Next, the method involves a separation of these elements and a further purification of the Pa fraction using Dowex AG1-X8 resin. Separation with Bio-Rad and Sigma-Aldrich resins was compared; although both perform similarly for Th and U, Pa yields are higher with Bio-Rad. Finally, samples are measured using a Nu instruments multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS). Overall chemical yields range around 50% for Pa, 60% for Th, and 70% for U.
spellingShingle Negre, C
Thomas, A
Mas, J
Garcia-Orellana, J
Henderson, G
Masqué, P
Zahn, R
Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title_full Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title_fullStr Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title_full_unstemmed Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title_short Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.
title_sort separation and measurement of pa th and u isotopes in marine sediments by microwave assisted digestion and multiple collector inductively coupled plasma mass spectrometry
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