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Title: SOLID PHASE MICROEXTRACTION SAMPLING OF HIGH EXPLOSIVE RESIDUES IN THE PRESENCE OF RADIONUCLIDES AND RADIONUCLIDE SURROGATE METALS

Abstract

The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) evidence while maintaining evidentiary value. One experimental method for the isolation of HE residue involves using solid phase microextraction or SPME fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ({sup 239/240}Pu, {sup 238}U, {sup 237}Np, {sup 85}Sr, {sup 133}Ba, {sup 137}Cs, {sup 60}Co and {sup 226}Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Zr, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection.

Authors:
; ; ;
Publication Date:
Research Org.:
SRS
Sponsoring Org.:
USDOE
OSTI Identifier:
902854
Report Number(s):
WSRC-STI-2007-00190
Journal ID: ISSN 0236-5731; JRNCDM; TRN: US200719%%38
DOE Contract Number:
DE-AC09-96SR18500
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Radioanalytical and Nuclear Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CHEMICAL EXPLOSIVES; EXTRACTION; RADIOISOTOPES; RESIDUES; SAMPLING; METALS; AFFINITY; FIBERS; SORPTIVE PROPERTIES; SAMPLE PREPARATION

Citation Formats

Duff, M, S Crump, S, Robert02 Ray, R, and Donna Beals, D. SOLID PHASE MICROEXTRACTION SAMPLING OF HIGH EXPLOSIVE RESIDUES IN THE PRESENCE OF RADIONUCLIDES AND RADIONUCLIDE SURROGATE METALS. United States: N. p., 2007. Web. doi:10.1007/s10967-007-7116-0.
Duff, M, S Crump, S, Robert02 Ray, R, & Donna Beals, D. SOLID PHASE MICROEXTRACTION SAMPLING OF HIGH EXPLOSIVE RESIDUES IN THE PRESENCE OF RADIONUCLIDES AND RADIONUCLIDE SURROGATE METALS. United States. doi:10.1007/s10967-007-7116-0.
Duff, M, S Crump, S, Robert02 Ray, R, and Donna Beals, D. Fri . "SOLID PHASE MICROEXTRACTION SAMPLING OF HIGH EXPLOSIVE RESIDUES IN THE PRESENCE OF RADIONUCLIDES AND RADIONUCLIDE SURROGATE METALS". United States. doi:10.1007/s10967-007-7116-0. https://www.osti.gov/servlets/purl/902854.
@article{osti_902854,
title = {SOLID PHASE MICROEXTRACTION SAMPLING OF HIGH EXPLOSIVE RESIDUES IN THE PRESENCE OF RADIONUCLIDES AND RADIONUCLIDE SURROGATE METALS},
author = {Duff, M and S Crump, S and Robert02 Ray, R and Donna Beals, D},
abstractNote = {The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) evidence while maintaining evidentiary value. One experimental method for the isolation of HE residue involves using solid phase microextraction or SPME fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ({sup 239/240}Pu, {sup 238}U, {sup 237}Np, {sup 85}Sr, {sup 133}Ba, {sup 137}Cs, {sup 60}Co and {sup 226}Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Zr, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection.},
doi = {10.1007/s10967-007-7116-0},
journal = {Journal of Radioanalytical and Nuclear Chemistry},
number = ,
volume = ,
place = {United States},
year = {Fri Apr 13 00:00:00 EDT 2007},
month = {Fri Apr 13 00:00:00 EDT 2007}
}
  • The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating highly radioactive fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of FD residue from radionuclide metals involves using solid phase microextraction (SPME) fibers to remove the residues of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most (radioactive) metals. The focus of this research was to develop an examination protocol that was applicable to safe work inmore » facilities where high radiation doses are shielded from the workers (as in radioactive shielded cells or ''hot cells''). We also examined the affinity of stable radionuclide surrogate metals (Co, Ir, Re, Ni, Ba, Cs, Nb, Zr and Nd) for sorption by the SPME fibers. This was done under exposure conditions that favor the uptake of FD residues under conditions that will provide little contact between the SPME and the FD material (such as charred carpet or wood that contains commonly-used accelerants). Our results from mass spectrometric analyses indicate that SPME fibers show promise for use in the room temperature head space uptake of organic FD residue (namely, diesel fuel oil, kerosene, gasoline and paint thinner) with subsequent analysis by gas chromatography (GC) with mass spectrometric (MS) detection. No inorganic forms of ignitable fluids were included in this study.« less
  • Solid-matrix fluorescence (SMF) and solid-matrix phosphorescence (SMP) have been used in conjunction with solid-phase microextraction to characterize mixtures of polycyclic aromatic hydrocarbons (PAHs) isolated from water. Whatman 1PS paper was used to extract the PAH from water, and then the isolated PAHs were directly identified on the paper by obtaining SMF and SMP spectra. The SMF and SMP properties of 10 PAH were obtained, and the PAHs in a two-component mixture, a three-component mixture, and a four-component mixture were easily identified by a combination of SMF and SMP. No external heavy atom was needed to acquire the SMP data. Benzo[{italmore » e}]pyrene gave a limit of detection of 6.2 pg/mL with SMP, and with SMF benzo[{ital a}]pyrene gave a limit of detection of 19 pg/mL. {copyright} {ital 1999} {ital Society for Applied Spectroscopy}« less
  • A solid-phase microextraction (SPME)–GC–MS method for three esters and the corresponding alcohols was tested for responses in accuracy, within-run precision (repeatability), and between-run precision (reproducibility) due to individual operators, individual analysis days, and differing analyte concentrations. At 5 ppm (v/v) [ppmv], three of the six analytes showed significant (p < 0.05) operator effects, while five of six analytes gave a significant effect due to the days of analysis. At 20 ppmv, five of the six analytes gave significant operator and daily effects. At 100 ppmv, all the analytes showed significant daily effects but no operator effects were observed. The repeatabilitymore » was concentration dependent, with all six analytes combining for an average RSD of 12.1 ± 6.1% at 1 ppmv, becoming most precise at 50 ppmv at 1.01 ± 0.45%, then increasing at 100 ppmv to 4.12 ± 1.88%. The contributors to error trended as: concentration > daily effects > operator.« less
  • A number of critical field applications require monitoring air samples for trace levels of chemical warfare agents. Solid-phase microextraction (SPME) is a convenient format to conduct these analyses. Measurements could be significantly improved if a SPME phase selective for nerve agents were substituted for nonselective polymers typically used (e.g., polydimethylsiloxane). This paper evaluates a novel stationary phase, previously developed for methylphosphonate sensor applications, for use with SPME sampling. The phenol-based polymer, BSP3, was found to offer far higher selectivity toward sarin (GB) than polydimethylsiloxane due to a pronounced affinity toward the target analyte and a lower affinity toward hydrocarbons.
  • A number of critical field applications require monitoring air samples for trace levels of chemical warfare agents. Solid-phase microextraction (SPME) is a convenient format to conduct these analyses. Measurements could be significantly improved if a SPME phase selective for nerve agents were substituted for nonselective polymers typically used (e.g.,polydimethylsiloxane). This paper evaluates a novel stationary phase, previously developed for methylphosphonate sensor applications, for use with SPME sampling. The phenol-based polymer, BSP3, was found to offer far higher selectivity toward sarin (GB) than polydimethylsiloxane due to a pronounced affinity toward the target analyte and a lower affinity toward hydrocarbons.