Microextraction–TQ–ICP–MS for the Direct Analysis of U and Pu from Cotton Swipes

The microextraction sampling technique was integrated with triple quadrupoleinductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–...

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Veröffentlicht in:Analytical chemistry (Washington) 2023-10, Vol.95 (43), p.15867-15874
Hauptverfasser: Bradley, Veronica C., Ticknor, Brian W., Dunlap, Daniel R., Zirakparvar, N. Alex, Metzger, Shalina C., Hexel, Cole R., Manard, Benjamin T.
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container_end_page 15874
container_issue 43
container_start_page 15867
container_title Analytical chemistry (Washington)
container_volume 95
creator Bradley, Veronica C.
Ticknor, Brian W.
Dunlap, Daniel R.
Zirakparvar, N. Alex
Metzger, Shalina C.
Hexel, Cole R.
Manard, Benjamin T.
description The microextraction sampling technique was integrated with triple quadrupoleinductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–MS instrument for isotopic determination. Carbon dioxide (CO2) and helium (He) gases were delivered to a collision reaction cell within the ICP–MS system for ion separation. The CO2 reacts with the U+ forming UO+ which is ultimately separated from the Pu+ ions of interest in the third quadrupole. This study demonstrates direct liquid extraction of U/Pu from a solid surface and subsequent measurement by TQ–ICP–MS in
doi_str_mv 10.1021/acs.analchem.3c01022
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Alex ; Metzger, Shalina C. ; Hexel, Cole R. ; Manard, Benjamin T.</creator><creatorcontrib>Bradley, Veronica C. ; Ticknor, Brian W. ; Dunlap, Daniel R. ; Zirakparvar, N. Alex ; Metzger, Shalina C. ; Hexel, Cole R. ; Manard, Benjamin T. ; Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)</creatorcontrib><description>The microextraction sampling technique was integrated with triple quadrupoleinductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–MS instrument for isotopic determination. Carbon dioxide (CO2) and helium (He) gases were delivered to a collision reaction cell within the ICP–MS system for ion separation. The CO2 reacts with the U+ forming UO+ which is ultimately separated from the Pu+ ions of interest in the third quadrupole. This study demonstrates direct liquid extraction of U/Pu from a solid surface and subsequent measurement by TQ–ICP–MS in &lt;60 s. Flow rates were optimized (0.3 mL min–1 CO2 and 5 mL min–1 He) in the reaction cell of the ICP–MS system to maximize the Pu signal while minimizing U interferences (i.e., 238U+ tail and 238UH+) at m/z 239. Low levels of Pu (∼2 pg) were deposited on a cotton swipe along with U at concentrations ranging from 20 to 200 ng. The 240Pu/239Pu ratio was measured with &lt;7% relative difference from the certified value at all U concentrations. Major and minor U isotope ratios were also measured with &lt;4% relative difference. This highlights that the microextraction–TQ–ICP–MS method can extract a mixed U/Pu sample directly from a cotton swipe and measure both isotopic systems without chemical separation.</description><identifier>ISSN: 0003-2700</identifier><identifier>EISSN: 1520-6882</identifier><identifier>DOI: 10.1021/acs.analchem.3c01022</identifier><language>eng</language><publisher>Washington: American Chemical Society</publisher><subject>Carbon dioxide ; Chemical separation ; Cotton ; extraction ; Flow rates ; Helium ; Inductively coupled plasma mass spectrometry ; INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY ; ions ; Isotope ratios ; isotopes ; Mass spectrometry ; Mass spectroscopy ; organic polymers ; plants ; Plutonium ; Quadrupoles ; Sampling methods ; Solid surfaces ; Uranium</subject><ispartof>Analytical chemistry (Washington), 2023-10, Vol.95 (43), p.15867-15874</ispartof><rights>2023 American Chemical Society</rights><rights>Copyright American Chemical Society Oct 31, 2023</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a380t-6bb87bca52f04ee05c1baed0bff30d49b80e449256dd1f387cb6b81b8106b9d33</citedby><cites>FETCH-LOGICAL-a380t-6bb87bca52f04ee05c1baed0bff30d49b80e449256dd1f387cb6b81b8106b9d33</cites><orcidid>0000-0002-0740-0627 ; 0000-0002-8266-6484 ; 0000000246333009 ; 0000000228679073 ; 0000000207400627 ; 0000000337797730 ; 0000000282666484 ; 0000000181012422</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://pubs.acs.org/doi/pdf/10.1021/acs.analchem.3c01022$$EPDF$$P50$$Gacs$$H</linktopdf><linktohtml>$$Uhttps://pubs.acs.org/doi/10.1021/acs.analchem.3c01022$$EHTML$$P50$$Gacs$$H</linktohtml><link.rule.ids>230,314,776,780,881,2752,27055,27903,27904,56716,56766</link.rule.ids><backlink>$$Uhttps://www.osti.gov/servlets/purl/2205442$$D View this record in Osti.gov$$Hfree_for_read</backlink></links><search><creatorcontrib>Bradley, Veronica C.</creatorcontrib><creatorcontrib>Ticknor, Brian W.</creatorcontrib><creatorcontrib>Dunlap, Daniel R.</creatorcontrib><creatorcontrib>Zirakparvar, N. Alex</creatorcontrib><creatorcontrib>Metzger, Shalina C.</creatorcontrib><creatorcontrib>Hexel, Cole R.</creatorcontrib><creatorcontrib>Manard, Benjamin T.</creatorcontrib><creatorcontrib>Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)</creatorcontrib><title>Microextraction–TQ–ICP–MS for the Direct Analysis of U and Pu from Cotton Swipes</title><title>Analytical chemistry (Washington)</title><addtitle>Anal. Chem</addtitle><description>The microextraction sampling technique was integrated with triple quadrupoleinductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–MS instrument for isotopic determination. Carbon dioxide (CO2) and helium (He) gases were delivered to a collision reaction cell within the ICP–MS system for ion separation. The CO2 reacts with the U+ forming UO+ which is ultimately separated from the Pu+ ions of interest in the third quadrupole. This study demonstrates direct liquid extraction of U/Pu from a solid surface and subsequent measurement by TQ–ICP–MS in &lt;60 s. Flow rates were optimized (0.3 mL min–1 CO2 and 5 mL min–1 He) in the reaction cell of the ICP–MS system to maximize the Pu signal while minimizing U interferences (i.e., 238U+ tail and 238UH+) at m/z 239. Low levels of Pu (∼2 pg) were deposited on a cotton swipe along with U at concentrations ranging from 20 to 200 ng. The 240Pu/239Pu ratio was measured with &lt;7% relative difference from the certified value at all U concentrations. Major and minor U isotope ratios were also measured with &lt;4% relative difference. 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Alex</au><au>Metzger, Shalina C.</au><au>Hexel, Cole R.</au><au>Manard, Benjamin T.</au><aucorp>Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)</aucorp><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Microextraction–TQ–ICP–MS for the Direct Analysis of U and Pu from Cotton Swipes</atitle><jtitle>Analytical chemistry (Washington)</jtitle><addtitle>Anal. Chem</addtitle><date>2023-10-31</date><risdate>2023</risdate><volume>95</volume><issue>43</issue><spage>15867</spage><epage>15874</epage><pages>15867-15874</pages><issn>0003-2700</issn><eissn>1520-6882</eissn><abstract>The microextraction sampling technique was integrated with triple quadrupoleinductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–MS instrument for isotopic determination. Carbon dioxide (CO2) and helium (He) gases were delivered to a collision reaction cell within the ICP–MS system for ion separation. The CO2 reacts with the U+ forming UO+ which is ultimately separated from the Pu+ ions of interest in the third quadrupole. This study demonstrates direct liquid extraction of U/Pu from a solid surface and subsequent measurement by TQ–ICP–MS in &lt;60 s. Flow rates were optimized (0.3 mL min–1 CO2 and 5 mL min–1 He) in the reaction cell of the ICP–MS system to maximize the Pu signal while minimizing U interferences (i.e., 238U+ tail and 238UH+) at m/z 239. Low levels of Pu (∼2 pg) were deposited on a cotton swipe along with U at concentrations ranging from 20 to 200 ng. The 240Pu/239Pu ratio was measured with &lt;7% relative difference from the certified value at all U concentrations. Major and minor U isotope ratios were also measured with &lt;4% relative difference. 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ispartof Analytical chemistry (Washington), 2023-10, Vol.95 (43), p.15867-15874
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source ACS Publications
subjects Carbon dioxide
Chemical separation
Cotton
extraction
Flow rates
Helium
Inductively coupled plasma mass spectrometry
INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ions
Isotope ratios
isotopes
Mass spectrometry
Mass spectroscopy
organic polymers
plants
Plutonium
Quadrupoles
Sampling methods
Solid surfaces
Uranium
title Microextraction–TQ–ICP–MS for the Direct Analysis of U and Pu from Cotton Swipes
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