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7 protocols using 18o2 pfhxs

1

Quantifying Perfluoroalkyl Substances in Solutions

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Calibration solutions were created by combining 2 solutions produced by the NIST reference materials 8446 Perfluorinated Carboxylic Acids and Perfluorooctane Sulfonamide in Methanol and 8447 Perfluorinated Sulfonic Acids in Methanol. Together, the solution contained 15 PFAAs as follows: PFBA, perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), perfluorododecanoic acid (PFDoA), perfluorotridecanoic acid (PFTriA), perfluorotetradecanoic acid (PFTA), PFBS, perfluorohexanesulfonic acid (PFHxS), PFOS, and perfluorooctanesulfonamide (PFOSA).
Internal standards were purchased from Cambridge Isotope Laboratories, RTI International, and Wellington Laboratories to create an internal standard mixture comprised of 11 isotopically labeled PFAAs, as follows: 13C4-PFBA, 13C2-PFHxA, 13C8-PFOA, 13C9-PFNA, 13C9-PFDA, 13C2-PFUnA, 13C2-PFDoA, 18O2-PFBS, 18O2-PFHxS, 13C4-PFOS, and 18O2-PFOSA.
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2

Quantitative Analysis of Perfluoroalkyl Substances

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Twelve PFASs (standards purchased from
Sigma-Aldrich) were analyzed, i.e., C3–C5 and C7–C9 perfluoroalkyl carboxylates
(PFCAs), C4, C6, and C8 perfluoroalkyl
sulfonates (PFSAs), perfluorooctane sulfonamide (FOSA), and 6:2 and
8:2 fluorotelomer sulfonates (6:2 and 8:2 FTSA). For quantification
as well as for quality assurance and control (QA/QC), eight mass-labeled
internal standards (ISs) (i.e., 13C4-PFBA, 13C2-PFHxA, 13C4-PFOA, 13C5-PFNA, 13C2-PFDA, 18O2-PFHxS, 13C4-PFOS, 13C8-FOSA, purities > 99%, Wellington Laboratories,
Guelph, ON) were also included. For details on the included PFASs
and their internal standards, see Table S1 in the Supporting Information.
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3

Comprehensive PFAS Analysis Protocol

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A total of
14 PFAS were investigated
in this work, including 1 perfluoroalkyl sulfonamide (FASA), 9 perfluoroalkyl
carboxylic acids (PFCAs), and 4 perfluoroalkyl sulfonic acids (PFSAs)
(Table S3). Authentic standards of perfluooctane
sulfonamide (FOSA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic
acid (PFHpA), PFOA, perfluorononanoic acid (PFNA), perfluorodecanoic
acid (PFDA), perfluoroundecanoic acid (PFUnDA), perfluorododecanoic
acid (PFDoDA), perfluorotridecanoic acid (PFTriDA), perfluorotetradecanoic
acid (PFTeDA)), PFBS, perfluorohexanesulfonic acid (PFHxS), PFOS,
and perfluorodecanesulfonic acid (PFDS) as well as the internal standards 13C2–PFHxA, 13C4–PFHpA, 13C4–PFOA, 13C5–PFNA, 13C2–PFDA, 13C2–PFUnDA, 13C2–PFDoDA, 18O2–PFHxS, 13C4–PFOS, and 13C8–FOSA were purchased from Wellington Laboratories (Guelph,
ON, Canada).
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4

Quantitative Analysis of Perfluorinated Compounds

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Calibration solutions were created by combining two solutions produced by the NIST Reference Materials (RMs) 8446 Perfluorinated Carboxylic Acids and Perfluorooctane Sulfonamide in Methanol and RM 8447 Perfluorinated Sulfonic Acids in Methanol. Together, the solution contained 15 PFAAs as follows: perfluorobutyric acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, PFNA, perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), perfluorododecanoic acid (PFDoA), perfluorotridecanoic acid (PFTriA), perfluorotet-radecanoic acid (PFTA), perfluorobutanesulfonic acid (PFBS), perfluorohexanesulfonic acid (PFHxS), PFOS, and perfluorooc-tanesulfonamide (PFOSA).
Internal standards (ISs) were purchased from Cambridge Isotope Laboratories (Andover, MA), RTI International (Research Triangle Park, NC), and Wellington Laboratories (Guelph, Ontario) to create an IS mixture comprised of eleven isotopically labeled PFAAs, and they were as follows: 13C4-PFBA, 13C2-PFHxA, 13C8-PFOA, 13C9-PFNA, 13C9-PFDA, 13C2-PFUnA, 13C2-PFDoA, 18O2-PFBS, 18O2-PFHxS, 13C4-PFOS, and 18O2-PFOSA.
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5

Quantifying Perfluorinated Compounds in Samples

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The target PFASs comprised: six perfluoroalkyl carboxylates (PFCAs), namely perfluorobutanoate (PFBA), perfluorohexanoate (PFHxA), perfluorooctanoate (PFOA), perfluorononanoate (PFNA), perfluorodecanoate (PFDA), and perfluoroundecanoate (PFUnDA); two perfluoroalkyl sulfonates (PFSAs), namely perfluorohexane sulfonates (PFHxS) and perfluorooctane sulfonates (PFOS); and one perfluorooctanesulfonamide (FOSA) (purity >99%, Wellington Laboratories, Guelph, ON). A total of nine isotopically labeled internal standards (IS) were used: 13C4-PFBA, 13C2-PFHxA, 13C4-PFOA, 13C5-PFNA, 13C2-PFDA, 13C2-PFUnDA, 18O2-PFHxS, 13C4-PFOS, and 13C8-FOSA (purity >99%, Wellington Laboratories, Guelph, ON).
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6

Quantitative Analysis of PFAAs in Environmental Samples

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The used abbreviations of PFAAs are according to Buck et al. (2011) . The target analytes included 4 PFSAs (PFBS, PFHxS, PFOS and PFDS) and 8 PFCAs (PFBA, PFHxA, PFOA, PFNA, PFDA, PFDoA, PFTrA and PFTeA).
The isotopically mass-labelled internal standards (ISTDs) comprised [1,2-13 C2]PFHxA, 13 C8-PFOA, 13 C9-PFNA, [1,2,3,4,5,6-13 C6]PFDA, [1,2,3,4,5,6,7-13 C7]PFUdA, [1,2,3,4,5,6,7-13 C7]PFDoA, 18 O2-PFHxS and 13 C8-PFOS and were purchased by Wellington Laboratories (Guelph, Canada). HPLC-grade Acetonitrile (ACN) and water (Acros Organics, New Jersey, USA) were used.
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7

Quantification of Perfluorinated Compounds

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Perfluorooctane sulfonamide (PFOSA); a mixture of PFBA, perfluoro-n-pentanoic acid (PFPeA), perfluoro-n-hexanoic acid (PFHxA), perfluoro-n-heptanoic acid (PFHpA), PFOA, perfluoro-n-nonanoic acid (PFNA), perfluoro-n-decanoic acid (PFDA), perfluoro-n-undecanoic acid (PFUnDA), perfluoro-n-dodecanoic acid (PFDoDA), perfluoro-n-tetradecanoic acid (PFTrDA), perfluoro-n-tetradecanoic acid (PFTeDA), perfluoro-n-hexadecanoic acid (PFHxDA), perfluoro-n-octadecanoic acid (PFOcDA), potassium perfluoro-1-butanesulfonate (PFBS), PFHxS, PFOS, and sodium perfluoro-1-decanesulfonate (PFDS); and mixture of 13C4-PFOS, 13C2-PFDA, 13C5-PFNA, 13C4-PFOA, 13C4-PFBA, 13C2PFHxA, 13C2PFUnDA, 13C2PFDoDA, and 18O2PFHxS were purchased from Wellington Laboratories Inc. (Guelph, Ontario, Canada). Purities of the individual chemicals and mass-labeled chemicals are >98%. Oasis weak anion exchange solid-phase extraction cartridges (WAX; 6cc, 150 mg) were purchased from Waters Corp. (Milford, MA, USA). Methanol (LC-MS grade) was purchased from Merck Ltd. (Darmstadt, Germany), and ammonium solution (25%) was purchased from Sigma-Aldrich GmbH (Seelze, Germany). Milli-Q water was used during the experiment.
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