University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Mass spectrometry

Citations 3

"Development Of Isotope Dilution Cold Vapor Inductively Coupled Plasma Mass Spectrometry And Its Application To The Certification Of Mercury In NIST Standard Reference Materials"
Anal. Chem. 2001 Volume 73, Issue 10 Pages 2190-2199

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S. J. Christopher, S. E. Long, M. S. Rearick, and J. D. Fassett

Abstract: An isotope dilution cold vapor inductively coupled plasma mass spectrometry (ID-CV-ICPMS) method featuring gaseous introduction of mercury via tin chloride reduction has been developed and applied to the quantification and certification of mercury in various NIST standard reference materials: SRM 966 Toxic Metals in Bovine Blood (30 ng mL-1); SRM 1641d Mercury in Water (1.6 µg mL-1); and SRM 1946 Lake Superior Fish Tissue (436 ng g-1). Complementary mercury data were generated for SRMs and NIST quality control standards using cold vapor atomic absorption spectroscopy (CVAAS). Certification results for the determination of mercury in SRM 1641d using two independent methods (ID-CV-ICPMS and CVAAS) showed a degree of agreement of 0.3% between the methods. Gaseous introduction of mercury into the ICPMS resulted in a single isotope sensitivity of 2 x 10(6) counts s-1 ng-1 g for Hg-201 and significantly reduced the memory and washout effects traditionally encountered in solution nebulization ICPMS. Figures of merit for isotope ratio accuracy and precision were evaluated at dwell times of 10, 20, 40, 80, and 160 ms using SRM 3133 Mercury Spectrometric Solution. The optimum dwell time of 80 ms yielded a measured Hg-201/Hg-202 isotope ratio within 0.13% of the theoretical natural value and a measurement precision of 0.34%, on the basis of three replicate injections of SRM 3133.
Mercury NIST 3133 NIST 1641d NIST 966 NIST 1946 Amalgamation Volatile generation Reference material Method comparison

"The Use Of Reference Materials In The Fossil Fuels Quality Control"
Microchim. Acta 1996 Volume 123, Issue 1-4 Pages 217-230

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Maurizio Bettinelli, Sandro Spezia, Umberto Baroni and Gabriele Bizzarri

Abstract: Quality control procedures used for the determination of trace elements in fuel oil and coal are described. Two standard reference materials (NIST 1632a and 1632b) were used to evaluate the accuracy in the determination of As, Hg and Se in coal by flow injection (FI) hydride-generation (HG) AAS and FI HG ICP-MS after microwave solubilization (Anal. Chim. Acta, 1989, 225, 159). RSD over 2 years were 10% for As, 8.11% for Se and 15% for Hg. The use of real fuel oil samples to compare results obtained for the determination of Ni and V by NAA, ICP-MS, ETAAS and ICP-AES in 54 laboratories is discussed. Similarly, the use of real samples to detect significant bias in the determination of As, Hg and Se in coal using various techniques (NAA, FI HG AAS, FI HG ICP-MS, ETAAS) is discussed.
Trace elements Arsenic Mercury Selenium Nickel Vanadium NIST 1632 Oil Reference material Method comparison

"Determination Of Mercury In SRM Crude Oils And Refined Products By Isotope Dilution Cold Vapor ICP-MS Using Closed-system Combustion"
Anal. Bioanal. Chem. 2003 Volume 376, Issue 5 Pages 753-758

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W. Robert Kelly, Stephen E. Long and Jacqueline L. Mann

Abstract: Mercury was determined by isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICP-MS) in four different liquid petroleum SRMs. Samples of approximately 0.3 g were spiked with stable (201)Hg and wet ashed in a closed system (Carius tube) using 6 g of high-purity nitric acid. Three different types of commercial oils were measured: two Texas crude oils, SRM 2721 (41.7±5.7 pg g-1) and SRM 2722 (129±13 pg g-1), a low-sulfur diesel fuel, SRM 2724b (34±26 pg g-1), and a low-sulfur residual fuel oil, SRM 1619b (3.5±0.74 ng g-1) (mean value and 95% CI). The Hg values for the crude oils and the diesel fuel are the lowest values ever reported for these matrices. The method detection limit, which is ultimately limited by method blank uncertainty, is approximately 10 pg g-1 for a 0.3 g sample. Accurate Hg measurements in petroleum products are needed to assess the contribution to the global Hg cycle and may be needed in the near future to comply with reporting regulations for toxic elements.
Mercury NIST 2721 NIST 2722 NIST 1619b NIST 2724b Reference material