Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation

Boggess, Andrew; Crump, Stephen; Gregory, Clint; Young, John; Kessinger, Glen

doi:10.1016/j.forc.2017.12.001

Title: Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation

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Abstract

Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automation and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstratedmore »« less

Authors:

Boggess, Andrew ^[1]; Crump, Stephen ^[1]; Gregory, Clint ^[1]; Young, John ^[1]; Kessinger, Glen ^[2]

Savannah River National Lab., Aiken, SC (United States)
Savannah River Nuclear Solutions, Aiken, SC (United States)

Publication Date:: Wed Dec 06 00:00:00 EST 2017

Research Org.:: Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1419842

Report Number(s):: SRNL-L4100-2017-00009
Journal ID: ISSN 2468-1709; PII: S2468170917300887

Grant/Contract Number:: AC09-08SR22470

Resource Type:: Accepted Manuscript

Journal Name:: Forensic Chemistry

Additional Journal Information:: Journal Volume: 7; Journal Issue: C; Journal ID: ISSN 2468-1709

Publisher:: Elsevier

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Nitroaromatic explosives; Radiological forensics; GC/MS; Radiological safety; Proficiency testing

Citation Formats


                    Boggess, Andrew, Crump, Stephen, Gregory, Clint, Young, John, and Kessinger, Glen. Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation.  United States: N. p., 2017. 
Web.  doi:10.1016/j.forc.2017.12.001.

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                    Boggess, Andrew, Crump, Stephen, Gregory, Clint, Young, John, & Kessinger, Glen. Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation.  United States.  https://doi.org/10.1016/j.forc.2017.12.001

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                    Boggess, Andrew, Crump, Stephen, Gregory, Clint, Young, John, and Kessinger, Glen. Wed .  
"Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation".  United States.  https://doi.org/10.1016/j.forc.2017.12.001.  https://www.osti.gov/servlets/purl/1419842.

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@article{osti_1419842,

  title        = {Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation},

  author       = {Boggess, Andrew and Crump, Stephen and Gregory, Clint and Young, John and Kessinger, Glen},

  abstractNote = {Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automation and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstrated that 99% recovery of target analytes was achieved. To the knowledge of the authors, this represents the first safe, accurate, and reproducible quantitative method for nitroaromatic explosives in soil for specific use on radiologically contaminated samples within the constraints of a nuclear analytical lab.},

  doi          = {10.1016/j.forc.2017.12.001},

  journal      = {Forensic Chemistry},

  number       = C,

  volume       = 7,

  place        = {United States},

  year         = {Wed Dec 06 00:00:00 EST 2017},

  month        = {Wed Dec 06 00:00:00 EST 2017}

}

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