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
Website: @unf

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NIST 364

Citations 1

"A Micro-scale Mercury Cathode Electrolysis Procedure For Online Flow Injection Inductively Coupled Plasma Mass Spectrometry Trace Elements Analysis In Steel Samples"
Anal. Chim. Acta 1999 Volume 389, Issue 1-3 Pages 247-255
Aurora G. Coedo, Isabel Padilla, Teresa Dorado and Francisco J. Alguacil

Abstract: An online matrix-analyte separation technique was developed for flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) trace analysis. A µelectrolytic cell was designed to be inserted in the FI manifold. The technique was used to separate Zr, Hf, Y, rare earth elements (REEs), Th and U from a steel-matrix (Fe, Cr, Ni, Co, Mn and Mo). A microwave-assisted HNO3-HCl-HF-H2SO4 digestion procedure, with temperature/pressure regulation, was used for sample dissolution. Obtained solutions were evaporated to SO3 fumes, and 2 mi of this diluted sulfuric solution were introduced in the electrolytic cell through the manifold circuit. After matrix removal, the electrolyte was conducted to load a 300 µl sample loop to be injected into the plasma torch. Direct multielement standard solutions in diluted sulfuric acid (without matrix matching and sample pretreatment) were applied for external calibration. The determination limits, with reference to the solid, were improved by a factor of about 10 compared with that obtained from direct measurements of 0.1% (m/v) sample solutions. The relative standard deviations for all the analytes were better than 3.5% for concentrations above 10 times the limit of quantification. The developed method was applied in the determination of certified elements in Steel Reference Materials: NIST 363 and NIST 364. Recoveries from 0.200 g test portions of high-purity iron spiked at two different concentration levels were found better than 97%.
Zirconium Yttrium Hafnium Metals, rare earth Thorium-232 Uranium Lanthanum Lutetium Cerium Praseodymium Neodymium Samarium Europium Gadolinium Terbium Dysprosium Holmium Erbium Ytterbium Thallium Mass spectrometry Matrix removal Extraction