Clumped isotope analysis of carbonates: comparison of two different acid digestion techniques

Publikationstyp:
Zeitschriftenaufsatz
Metadaten:
Autoren
Autoren-URL
https://www.webofscience.com/api/gateway?GWVersion=2&SrcApp=fis-test-1&SrcAuth=WosAPI&KeyUT=WOS:000331440700003&DestLinkType=FullRecord&DestApp=WOS_CPL
DOI
10.1002/rcm.6609
eISSN
1097-0231
Externe Identifier
  • Clarivate Analytics Document Solution ID: AA9VI
  • PubMed Identifier: 23765611
ISSN
0951-4198
Ausgabe der Veröffentlichung
14
Zeitschrift
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
Paginierung
1631 - 1642
Datum der Veröffentlichung
2013
Status
Published
Titel
Clumped isotope analysis of carbonates: comparison of two different acid digestion techniques
Sub types
  • Article
Ausgabe der Zeitschrift
27

Datenquelle: Web of Science (Lite)

Andere Metadatenquellen:
Abstract
<jats:sec><jats:title>RATIONALE</jats:title><jats:p>The kinetic nature of the phosphoric acid digestion reaction enables clumped isotope analysis of carbonates using gas source isotope ratio mass spectrometry (IRMS). In most laboratories acid digestions are performed at 25°C in sealed vessels or at 90°C in a common acid bath. Here we show that different Δ<jats:sub>47</jats:sub> results are obtained depending on the digestion technique employed.</jats:p></jats:sec><jats:sec><jats:title>METHODS</jats:title><jats:p>Several replicates of a biogenic aragonite and NBS 19 were reacted with 104% H<jats:sub>3</jats:sub>PO<jats:sub>4</jats:sub> in sealed vessels at 25°C and at 90°C using a common acid bath. The sample size varied between 4 mg and 14 mg. Purification methods that are standard for clumped isotope analyses were applied to the evolved CO<jats:sub>2</jats:sub> before measuring the abundances of masses 44 to 49 relative to a reference gas by IRMS.</jats:p></jats:sec><jats:sec><jats:title>RESULTS</jats:title><jats:p>A systematic trend to lower and more consistent Δ<jats:sub>47</jats:sub> values is observed for reactions at 25°C if the sample size is increased. We suggest that secondary re‐equilibration of evolved CO<jats:sub>2</jats:sub> or reaction intermediates with free water molecules preferentially occurs for relatively small samples (4–7 mg), finally yielding elevated Δ<jats:sub>47</jats:sub> values compared with &gt;7 mg aliquots. In contrast, no such sample size effect on Δ<jats:sub>47</jats:sub> values is observed for carbonates that are digested at 90°C using the common acid bath.</jats:p></jats:sec><jats:sec><jats:title>CONCLUSIONS</jats:title><jats:p>The determination of Δ<jats:sub>47</jats:sub> values of carbonate samples smaller than 7 mg becomes more precise and accurate if digestions are performed at 90°C. Based on our results we propose that the difference in phosphoric acid fractionation factor between 25°C and 90°C is 0.07‰ for both calcite and aragonite. Copyright © 2013 John Wiley &amp; Sons, Ltd.</jats:p></jats:sec>
Autoren
DOI
10.1002/rcm.6609
eISSN
1097-0231
ISSN
0951-4198
Ausgabe der Veröffentlichung
14
Zeitschrift
Rapid Communications in Mass Spectrometry
Sprache
en
Online publication date
2013
Paginierung
1631 - 1642
Datum der Veröffentlichung
2013
Status
Published
Herausgeber
Wiley
Herausgeber URL
http://dx.doi.org/10.1002/rcm.6609
Datum der Datenerfassung
2023
Titel
Clumped isotope analysis of carbonates: comparison of two different acid digestion techniques
Ausgabe der Zeitschrift
27

Datenquelle: Crossref

Abstract
<h4>Rationale</h4>The kinetic nature of the phosphoric acid digestion reaction enables clumped isotope analysis of carbonates using gas source isotope ratio mass spectrometry (IRMS). In most laboratories acid digestions are performed at 25°C in sealed vessels or at 90°C in a common acid bath. Here we show that different Δ47 results are obtained depending on the digestion technique employed.<h4>Methods</h4>Several replicates of a biogenic aragonite and NBS 19 were reacted with 104% H3 PO4 in sealed vessels at 25°C and at 90°C using a common acid bath. The sample size varied between 4 mg and 14 mg. Purification methods that are standard for clumped isotope analyses were applied to the evolved CO2 before measuring the abundances of masses 44 to 49 relative to a reference gas by IRMS.<h4>Results</h4>A systematic trend to lower and more consistent Δ47 values is observed for reactions at 25°C if the sample size is increased. We suggest that secondary re-equilibration of evolved CO2 or reaction intermediates with free water molecules preferentially occurs for relatively small samples (4-7 mg), finally yielding elevated Δ47 values compared with >7 mg aliquots. In contrast, no such sample size effect on Δ47 values is observed for carbonates that are digested at 90°C using the common acid bath.<h4>Conclusions</h4>The determination of Δ47 values of carbonate samples smaller than 7 mg becomes more precise and accurate if digestions are performed at 90°C. Based on our results we propose that the difference in phosphoric acid fractionation factor between 25°C and 90°C is 0.07‰ for both calcite and aragonite.
Addresses
  • Institute of Geosciences, Goethe-University, Frankfurt am Main, Germany. u.wacker@em.uni-frankfurt.de
Autoren
DOI
10.1002/rcm.6609
eISSN
1097-0231
Externe Identifier
  • PubMed Identifier: 23765611
Open access
false
ISSN
0951-4198
Ausgabe der Veröffentlichung
14
Zeitschrift
Rapid communications in mass spectrometry : RCM
Sprache
eng
Medium
Print
Paginierung
1631 - 1642
Datum der Veröffentlichung
2013
Status
Published
Datum der Datenerfassung
2013
Titel
Clumped isotope analysis of carbonates: comparison of two different acid digestion techniques.
Sub types
  • Journal Article
Ausgabe der Zeitschrift
27

Datenquelle: Europe PubMed Central

Abstract
RATIONALE: The kinetic nature of the phosphoric acid digestion reaction enables clumped isotope analysis of carbonates using gas source isotope ratio mass spectrometry (IRMS). In most laboratories acid digestions are performed at 25°C in sealed vessels or at 90°C in a common acid bath. Here we show that different Δ47 results are obtained depending on the digestion technique employed. METHODS: Several replicates of a biogenic aragonite and NBS 19 were reacted with 104% H3 PO4 in sealed vessels at 25°C and at 90°C using a common acid bath. The sample size varied between 4 mg and 14 mg. Purification methods that are standard for clumped isotope analyses were applied to the evolved CO2 before measuring the abundances of masses 44 to 49 relative to a reference gas by IRMS. RESULTS: A systematic trend to lower and more consistent Δ47 values is observed for reactions at 25°C if the sample size is increased. We suggest that secondary re-equilibration of evolved CO2 or reaction intermediates with free water molecules preferentially occurs for relatively small samples (4-7 mg), finally yielding elevated Δ47 values compared with >7 mg aliquots. In contrast, no such sample size effect on Δ47 values is observed for carbonates that are digested at 90°C using the common acid bath. CONCLUSIONS: The determination of Δ47 values of carbonate samples smaller than 7 mg becomes more precise and accurate if digestions are performed at 90°C. Based on our results we propose that the difference in phosphoric acid fractionation factor between 25°C and 90°C is 0.07‰ for both calcite and aragonite.
Date of acceptance
2013
Autoren
Autoren-URL
https://www.ncbi.nlm.nih.gov/pubmed/23765611
DOI
10.1002/rcm.6609
eISSN
1097-0231
Ausgabe der Veröffentlichung
14
Zeitschrift
Rapid Commun Mass Spectrom
Sprache
eng
Country
England
Paginierung
1631 - 1642
Datum der Veröffentlichung
2013
Status
Published
Datum, an dem der Datensatz öffentlich gemacht wurde
2013
Titel
Clumped isotope analysis of carbonates: comparison of two different acid digestion techniques.
Sub types
  • Journal Article
Ausgabe der Zeitschrift
27

Datenquelle: PubMed

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