Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels
Rationale Existing methods for the measurement of the 15N/14N isotopic composition of ammonium and nitrate are either only suitable for labelled samples or require considerable sample preparation efforts (or both). Our goal was to modify an existing analytical approach to allow for natural abundance...
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| Veröffentlicht in: | Rapid communications in mass spectrometry 2021-05, Vol.35 (10), p.e9077-n/a |
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| creator | Dyckmans, Jens Eschenbach, Wolfram Langel, Reinhard Szwec, Lars Well, Reinhard |
| description | Rationale
Existing methods for the measurement of the 15N/14N isotopic composition of ammonium and nitrate are either only suitable for labelled samples or require considerable sample preparation efforts (or both). Our goal was to modify an existing analytical approach to allow for natural abundance precision levels.
Methods
Published reaction protocols were used to convert ammonium into N2 by NaOBr and nitrate into N2O by TiCl3. A membrane inlet system was developed and coupled to an isotope ratio mass spectrometer to allow precise determination of the analytes.
Results
Concentrations of ≥35 μmol/L N for both ammonium or nitrate could be analysed for δ15N values with precisions of better than 0.9 mUr. While ammonium analyses exhibited a small concentration dependency and an offset of 2.7 mUr at high ammonium concentrations irrespective of the standard isotopic composition, nitrate analysis showed no offset but a blank contribution visible at very low concentrations.
Conclusions
The presented method is capable of fast measurement of δ15N values in ammonium and nitrate from aqueous samples with reasonable accuracy at natural abundance levels. It will thus facilitate the application of isotopic methods to studies of nitrogen cycling in ecosystems. |
| doi_str_mv | 10.1002/rcm.9077 |
| format | Article |
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Existing methods for the measurement of the 15N/14N isotopic composition of ammonium and nitrate are either only suitable for labelled samples or require considerable sample preparation efforts (or both). Our goal was to modify an existing analytical approach to allow for natural abundance precision levels.
Methods
Published reaction protocols were used to convert ammonium into N2 by NaOBr and nitrate into N2O by TiCl3. A membrane inlet system was developed and coupled to an isotope ratio mass spectrometer to allow precise determination of the analytes.
Results
Concentrations of ≥35 μmol/L N for both ammonium or nitrate could be analysed for δ15N values with precisions of better than 0.9 mUr. While ammonium analyses exhibited a small concentration dependency and an offset of 2.7 mUr at high ammonium concentrations irrespective of the standard isotopic composition, nitrate analysis showed no offset but a blank contribution visible at very low concentrations.
Conclusions
The presented method is capable of fast measurement of δ15N values in ammonium and nitrate from aqueous samples with reasonable accuracy at natural abundance levels. It will thus facilitate the application of isotopic methods to studies of nitrogen cycling in ecosystems.</description><identifier>ISSN: 0951-4198</identifier><identifier>EISSN: 1097-0231</identifier><identifier>DOI: 10.1002/rcm.9077</identifier><identifier>PMID: 33660370</identifier><language>eng</language><publisher>England: Wiley Subscription Services, Inc</publisher><subject>Abundance ; Composition ; Isotope ratios ; Isotopes ; Low concentrations ; Mass spectrometry ; Membranes ; Nitrates ; Nitrogen isotopes</subject><ispartof>Rapid communications in mass spectrometry, 2021-05, Vol.35 (10), p.e9077-n/a</ispartof><rights>2021 The Authors. published by John Wiley & Sons Ltd.</rights><rights>2021 The Authors. Rapid Communications in Mass Spectrometry published by John Wiley & Sons Ltd.</rights><rights>2021. This article is published under http://creativecommons.org/licenses/by-nc-nd/4.0/ (the “License”). Notwithstanding the ProQuest Terms and Conditions, you may use this content in accordance with the terms of the License.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c3497-e7933084a08bc011b72b11ec0dd00baa3db5b7dc051df0c47d58eb3bd43cbf803</citedby><cites>FETCH-LOGICAL-c3497-e7933084a08bc011b72b11ec0dd00baa3db5b7dc051df0c47d58eb3bd43cbf803</cites><orcidid>0000-0003-4746-4972 ; 0000-0003-3359-4389</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Frcm.9077$$EPDF$$P50$$Gwiley$$Hfree_for_read</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Frcm.9077$$EHTML$$P50$$Gwiley$$Hfree_for_read</linktohtml><link.rule.ids>314,776,780,1411,27901,27902,45550,45551</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/33660370$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Dyckmans, Jens</creatorcontrib><creatorcontrib>Eschenbach, Wolfram</creatorcontrib><creatorcontrib>Langel, Reinhard</creatorcontrib><creatorcontrib>Szwec, Lars</creatorcontrib><creatorcontrib>Well, Reinhard</creatorcontrib><title>Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels</title><title>Rapid communications in mass spectrometry</title><addtitle>Rapid Commun Mass Spectrom</addtitle><description>Rationale
Existing methods for the measurement of the 15N/14N isotopic composition of ammonium and nitrate are either only suitable for labelled samples or require considerable sample preparation efforts (or both). Our goal was to modify an existing analytical approach to allow for natural abundance precision levels.
Methods
Published reaction protocols were used to convert ammonium into N2 by NaOBr and nitrate into N2O by TiCl3. A membrane inlet system was developed and coupled to an isotope ratio mass spectrometer to allow precise determination of the analytes.
Results
Concentrations of ≥35 μmol/L N for both ammonium or nitrate could be analysed for δ15N values with precisions of better than 0.9 mUr. While ammonium analyses exhibited a small concentration dependency and an offset of 2.7 mUr at high ammonium concentrations irrespective of the standard isotopic composition, nitrate analysis showed no offset but a blank contribution visible at very low concentrations.
Conclusions
The presented method is capable of fast measurement of δ15N values in ammonium and nitrate from aqueous samples with reasonable accuracy at natural abundance levels. It will thus facilitate the application of isotopic methods to studies of nitrogen cycling in ecosystems.</description><subject>Abundance</subject><subject>Composition</subject><subject>Isotope ratios</subject><subject>Isotopes</subject><subject>Low concentrations</subject><subject>Mass spectrometry</subject><subject>Membranes</subject><subject>Nitrates</subject><subject>Nitrogen isotopes</subject><issn>0951-4198</issn><issn>1097-0231</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2021</creationdate><recordtype>article</recordtype><sourceid>24P</sourceid><recordid>eNp1kU1v1DAQhi0EoktB4hcgS1zKIWUcJ5vkiFZ8VOqCVOAcje0JcuWPxU6K8iv4y3hpKRISJx_m8TN652XsuYBzAVC_TtqfD9B1D9hGwNBVUEvxkG1gaEXViKE_YU9yvgYQoq3hMTuRcrsF2cGG_fxo5xS_UeA2xzkeiGNAt2abeZw4fl8oLpmj9zHYxZeh4aH8wJm4WrknrxIG4jY4mu8VZWwj95gzzwfSZYGnOa38bH9xtf_8iuPMA85LQsdRLcFg0MQd3ZDLT9mjCV2mZ3fvKfv67u2X3Yfq8tP7i92by0rLpgSkbpAS-gahV7rEUl2thCANxgAoRGlUqzqjoRVmAt10pu1JSWUaqdXUgzxlZ7feQ4olZJ5Hb7Mm50qaknisy5bjaWVT0Jf_oNdxSeVKhWph2NZCgvgr1CnmnGgaD8l6TOsoYDyaxlLSeCypoC_uhIvyZO7BP60UoLoFflhH639F49Vu_1v4C4E3nUQ</recordid><startdate>20210530</startdate><enddate>20210530</enddate><creator>Dyckmans, Jens</creator><creator>Eschenbach, Wolfram</creator><creator>Langel, Reinhard</creator><creator>Szwec, Lars</creator><creator>Well, Reinhard</creator><general>Wiley Subscription Services, Inc</general><scope>24P</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>JQ2</scope><scope>L7M</scope><scope>7X8</scope><orcidid>https://orcid.org/0000-0003-4746-4972</orcidid><orcidid>https://orcid.org/0000-0003-3359-4389</orcidid></search><sort><creationdate>20210530</creationdate><title>Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels</title><author>Dyckmans, Jens ; Eschenbach, Wolfram ; Langel, Reinhard ; Szwec, Lars ; Well, Reinhard</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c3497-e7933084a08bc011b72b11ec0dd00baa3db5b7dc051df0c47d58eb3bd43cbf803</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2021</creationdate><topic>Abundance</topic><topic>Composition</topic><topic>Isotope ratios</topic><topic>Isotopes</topic><topic>Low concentrations</topic><topic>Mass spectrometry</topic><topic>Membranes</topic><topic>Nitrates</topic><topic>Nitrogen isotopes</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Dyckmans, Jens</creatorcontrib><creatorcontrib>Eschenbach, Wolfram</creatorcontrib><creatorcontrib>Langel, Reinhard</creatorcontrib><creatorcontrib>Szwec, Lars</creatorcontrib><creatorcontrib>Well, Reinhard</creatorcontrib><collection>Wiley Online Library Open Access</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>ProQuest Computer Science Collection</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>MEDLINE - Academic</collection><jtitle>Rapid communications in mass spectrometry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Dyckmans, Jens</au><au>Eschenbach, Wolfram</au><au>Langel, Reinhard</au><au>Szwec, Lars</au><au>Well, Reinhard</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels</atitle><jtitle>Rapid communications in mass spectrometry</jtitle><addtitle>Rapid Commun Mass Spectrom</addtitle><date>2021-05-30</date><risdate>2021</risdate><volume>35</volume><issue>10</issue><spage>e9077</spage><epage>n/a</epage><pages>e9077-n/a</pages><issn>0951-4198</issn><eissn>1097-0231</eissn><abstract>Rationale
Existing methods for the measurement of the 15N/14N isotopic composition of ammonium and nitrate are either only suitable for labelled samples or require considerable sample preparation efforts (or both). Our goal was to modify an existing analytical approach to allow for natural abundance precision levels.
Methods
Published reaction protocols were used to convert ammonium into N2 by NaOBr and nitrate into N2O by TiCl3. A membrane inlet system was developed and coupled to an isotope ratio mass spectrometer to allow precise determination of the analytes.
Results
Concentrations of ≥35 μmol/L N for both ammonium or nitrate could be analysed for δ15N values with precisions of better than 0.9 mUr. While ammonium analyses exhibited a small concentration dependency and an offset of 2.7 mUr at high ammonium concentrations irrespective of the standard isotopic composition, nitrate analysis showed no offset but a blank contribution visible at very low concentrations.
Conclusions
The presented method is capable of fast measurement of δ15N values in ammonium and nitrate from aqueous samples with reasonable accuracy at natural abundance levels. It will thus facilitate the application of isotopic methods to studies of nitrogen cycling in ecosystems.</abstract><cop>England</cop><pub>Wiley Subscription Services, Inc</pub><pmid>33660370</pmid><doi>10.1002/rcm.9077</doi><tpages>5</tpages><orcidid>https://orcid.org/0000-0003-4746-4972</orcidid><orcidid>https://orcid.org/0000-0003-3359-4389</orcidid><oa>free_for_read</oa></addata></record> |
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| issn | 0951-4198 1097-0231 |
| language | eng |
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| source | Wiley Online Library Journals Frontfile Complete |
| subjects | Abundance Composition Isotope ratios Isotopes Low concentrations Mass spectrometry Membranes Nitrates Nitrogen isotopes |
| title | Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels |
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