Problems and Solutions when Quantifying Nitrogen in Silicate and Oxide Minerals and Glasses Using Electron Probe Microanalysis.
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| Title: | Problems and Solutions when Quantifying Nitrogen in Silicate and Oxide Minerals and Glasses Using Electron Probe Microanalysis. |
|---|---|
| Authors: | Mare, Eleanor R.1 (AUTHOR) eleanor.mare@gmail.com, Chen, Jeff2,3 (AUTHOR), Buisman, Iris4 (AUTHOR), Hayward, Chris5 (AUTHOR), Burnham, Antony D.6 (AUTHOR), Melai, Caterina7 (AUTHOR), Stüeken, Eva E.1 (AUTHOR), Bromiley, Geoffrey5 (AUTHOR), Mikhail, Sami1 (AUTHOR) sm342@st-andrews.ac.uk |
| Source: | Geostandards & Geoanalytical Research. Sep2025, Vol. 49 Issue 3, p569-590. 22p. |
| Subjects: | Nitrogen analysis, Electron probe microanalysis, Scientific method, Silicate minerals, Confidence intervals, Reference sources, Oxide minerals |
| Abstract: | With growing interest in the Earth's deep nitrogen cycle, electron probe microanalysis is increasingly used to quantify nitrogen in minerals and glasses. However, measuring nitrogen by electron microprobe comes with challenges, including beam sensitivity and differences in peak and background shapes between sample and reference materials. This study provides a robust analytical protocol to addresses these issues. We gathered mineral and glass reference materials with known nitrogen mass fractions from previous work, and synthesised additional glasses with nitrogen quantified independently by gas‐source mass spectrometry. Our method uses nitrides as calibration materials because of their beam stability and high nitrogen mass fraction. We assess peak shapes to implement an area‐peak factor correction, and account for curved backgrounds using a four‐point background correction. Importantly, we describe how to estimate uncertainties on both background and area‐peak factor corrections, which is required to assess detection limits but has been largely overlooked in previous studies. Our method yields nitrogen mass fractions within uncertainty for five out of seven reference materials, with two exceptions highlighting the need for further refinement. We provide Python code for applying the corrections and calculating uncertainties, allowing our method to be implemented by any researcher with access to an electron microprobe laboratory. [ABSTRACT FROM AUTHOR] |
| Copyright of Geostandards & Geoanalytical Research is the property of Wiley-Blackwell and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) | |
| Database: | Engineering Source |
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| Header | DbId: egs DbLabel: Engineering Source An: 188363338 AccessLevel: 6 PubType: Academic Journal PubTypeId: academicJournal PreciseRelevancyScore: 0 |
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| Items | – Name: Title Label: Title Group: Ti Data: Problems and Solutions when Quantifying Nitrogen in Silicate and Oxide Minerals and Glasses Using Electron Probe Microanalysis. – Name: Author Label: Authors Group: Au Data: <searchLink fieldCode="AR" term="%22Mare%2C+Eleanor+R%2E%22">Mare, Eleanor R.</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> eleanor.mare@gmail.com</i><br /><searchLink fieldCode="AR" term="%22Chen%2C+Jeff%22">Chen, Jeff</searchLink><relatesTo>2,3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Buisman%2C+Iris%22">Buisman, Iris</searchLink><relatesTo>4</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Hayward%2C+Chris%22">Hayward, Chris</searchLink><relatesTo>5</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Burnham%2C+Antony+D%2E%22">Burnham, Antony D.</searchLink><relatesTo>6</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Melai%2C+Caterina%22">Melai, Caterina</searchLink><relatesTo>7</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Stüeken%2C+Eva+E%2E%22">Stüeken, Eva E.</searchLink><relatesTo>1</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Bromiley%2C+Geoffrey%22">Bromiley, Geoffrey</searchLink><relatesTo>5</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Mikhail%2C+Sami%22">Mikhail, Sami</searchLink><relatesTo>1</relatesTo> (AUTHOR)<i> sm342@st-andrews.ac.uk</i> – Name: TitleSource Label: Source Group: Src Data: <searchLink fieldCode="JN" term="%22Geostandards+%26+Geoanalytical+Research%22">Geostandards & Geoanalytical Research</searchLink>. Sep2025, Vol. 49 Issue 3, p569-590. 22p. – Name: Subject Label: Subjects Group: Su Data: <searchLink fieldCode="DE" term="%22Nitrogen+analysis%22">Nitrogen analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Electron+probe+microanalysis%22">Electron probe microanalysis</searchLink><br /><searchLink fieldCode="DE" term="%22Scientific+method%22">Scientific method</searchLink><br /><searchLink fieldCode="DE" term="%22Silicate+minerals%22">Silicate minerals</searchLink><br /><searchLink fieldCode="DE" term="%22Confidence+intervals%22">Confidence intervals</searchLink><br /><searchLink fieldCode="DE" term="%22Reference+sources%22">Reference sources</searchLink><br /><searchLink fieldCode="DE" term="%22Oxide+minerals%22">Oxide minerals</searchLink> – Name: Abstract Label: Abstract Group: Ab Data: With growing interest in the Earth's deep nitrogen cycle, electron probe microanalysis is increasingly used to quantify nitrogen in minerals and glasses. However, measuring nitrogen by electron microprobe comes with challenges, including beam sensitivity and differences in peak and background shapes between sample and reference materials. This study provides a robust analytical protocol to addresses these issues. We gathered mineral and glass reference materials with known nitrogen mass fractions from previous work, and synthesised additional glasses with nitrogen quantified independently by gas‐source mass spectrometry. Our method uses nitrides as calibration materials because of their beam stability and high nitrogen mass fraction. We assess peak shapes to implement an area‐peak factor correction, and account for curved backgrounds using a four‐point background correction. Importantly, we describe how to estimate uncertainties on both background and area‐peak factor corrections, which is required to assess detection limits but has been largely overlooked in previous studies. Our method yields nitrogen mass fractions within uncertainty for five out of seven reference materials, with two exceptions highlighting the need for further refinement. We provide Python code for applying the corrections and calculating uncertainties, allowing our method to be implemented by any researcher with access to an electron microprobe laboratory. [ABSTRACT FROM AUTHOR] – Name: AbstractSuppliedCopyright Label: Group: Ab Data: <i>Copyright of Geostandards & Geoanalytical Research is the property of Wiley-Blackwell and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.) |
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| RecordInfo | BibRecord: BibEntity: Identifiers: – Type: doi Value: 10.1111/ggr.12605 Languages: – Code: eng Text: English PhysicalDescription: Pagination: PageCount: 22 StartPage: 569 Subjects: – SubjectFull: Nitrogen analysis Type: general – SubjectFull: Electron probe microanalysis Type: general – SubjectFull: Scientific method Type: general – SubjectFull: Silicate minerals Type: general – SubjectFull: Confidence intervals Type: general – SubjectFull: Reference sources Type: general – SubjectFull: Oxide minerals Type: general Titles: – TitleFull: Problems and Solutions when Quantifying Nitrogen in Silicate and Oxide Minerals and Glasses Using Electron Probe Microanalysis. Type: main BibRelationships: HasContributorRelationships: – PersonEntity: Name: NameFull: Mare, Eleanor R. – PersonEntity: Name: NameFull: Chen, Jeff – PersonEntity: Name: NameFull: Buisman, Iris – PersonEntity: Name: NameFull: Hayward, Chris – PersonEntity: Name: NameFull: Burnham, Antony D. – PersonEntity: Name: NameFull: Melai, Caterina – PersonEntity: Name: NameFull: Stüeken, Eva E. – PersonEntity: Name: NameFull: Bromiley, Geoffrey – PersonEntity: Name: NameFull: Mikhail, Sami IsPartOfRelationships: – BibEntity: Dates: – D: 01 M: 09 Text: Sep2025 Type: published Y: 2025 Identifiers: – Type: issn-print Value: 16394488 Numbering: – Type: volume Value: 49 – Type: issue Value: 3 Titles: – TitleFull: Geostandards & Geoanalytical Research Type: main |
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