Certification of total arsenic in blood and urine standard reference materials by radiochemical neutron activation analysis and inductively coupled plasma-mass spectrometry |
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Authors: | Rick L Paul W Clay Davis Lee Yu Karen E Murphy William F Guthrie Dennis D Leber Colleen E Bryan Thomas W Vetter Gulchekhra Shakirova Graylin Mitchell David J Kyle Jeffery M Jarrett Kathleen L Caldwell Robert L Jones Steven Eckdahl Michelle Wermers Melissa Maras C D Palmer M F Verostek C M Geraghty Amy J Steuerwald Patrick J Parsons |
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Institution: | 1. Chemical Sciences Division, National Institute of Standards and Technology, Gaithersburg, MD, 20899, USA 2. Statistical Engineering Division, National Institute of Standards and Technology, Gaithersburg, MD, 20899, USA 3. Inorganic and Radiation Analytical Toxicology Branch, Centers for Disease Control and Prevention, Atlanta, GA, 30341, USA 4. Mayo Clinic, Rochester, MN, 55905, USA 5. Laboratory of Inorganic and Nuclear Chemistry, Wadsworth Center, New York State Department of Health (NYSDOH), Albany, NY, 12201-0509, USA 6. Department of Environmental Health Sciences, School of Public Health, University at Albany, Albany, NY, 12201-0509, USA
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Abstract: | Radiochemical neutron activation analysis (RNAA) was used to measure arsenic at four levels in standard reference material (SRM) 955c Toxic Elements in Caprine Blood and at two levels in SRM 2668 Toxic Elements in Frozen Human Urine for the purpose of providing mass concentration values for certification. Samples were freeze-dried prior to analysis followed by neutron irradiation for 3 h at a fluence rate of 1 × 1014 cm?2 s?1. After sample dissolution in perchloric and nitric acids, arsenic was separated from the matrix either by retention on hydrated manganese dioxide (urine) or by extraction into zinc diethyldithiocarbamate in chloroform (blood). 76As was quantified by gamma-ray spectroscopy. Differences in chemical yield and counting geometry between samples and standards were monitored by measuring the count rate of a 77As tracer added before sample dissolution. RNAA results were combined with inductively coupled plasma-mass spectrometry values from National Institute of Standards and Technology and collaborating laboratories to provide certified values of 10.81 ± 0.54 and 213.1 ± 0.73 μg/L for SRM 2668 Levels I and II, and certified values of 21.66 ± 0.73, 52.7 ± 1.1, and 78.8 ± 4.9 μg/L for SRM 955c Levels II–IV, respectively. Because of discrepancies between values obtained by different methods for SRM 955c Level I, an information value of <5 μg/L was assigned for this material. |
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