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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High purity

Classification: Metal -> zinc -> high purity

Citations 3

"Determination Of Cadmium And Bismuth In High-purity Zinc Metal By Inductively Coupled Plasma Mass Spectrometry With Online Matrix Separation"
Fresenius J. Anal. Chem. 1995 Volume 353, Issue 2 Pages 162-166
Yasumasa Sayama, Yutaka Hayashibe and Masamitsu Fukuda

Abstract: High-purity Zn metal was dissolved in 7 M HNO3 and evaporated to near dryness. The residue was dissolved in 0.5 M HNO3 and injected into a carrier stream 1 ml/min) of 0.1 M KI. The resulting solution passed through an anion-exchange mini-column (10 cm x 1 mm i.d.) which adsorbed Cd and Bi as the iodide complex. After 3.3 min, the column was washed with 0.1 M HNO3 for 20 min at 0.4 ml/min, the ICP-MS instrument was cleaned with 0.4 M HNO3 (0.4 ml/min), Cd and Bi were eluted from the column with 2 M HNO3 and the eluate was introduced directly into the ICP-MS instrument. The ICP-MS instrumental parameters are tabulated. Calibration graphs were obtained for up to 10 ng/ml of Bi and Cd with detection limits of 0.075 and 0.81 ng/g, respectively, for single injections and 0.014 and 0.16 ng/g. respectively, for multiple injections. Recoveries were 109% Cd and 92% Bi at 10 ng levels.
Bismuth Cadmium Mass spectrometry Sample preparation Resin Preconcentration Complexation

"Determination Of Nickel, Cobalt, Copper, Thorium And Uranium In High-purity Zinc Metal By ICP-MS With Online Matrix Separation"
Anal. Sci. 1995 Volume 11, Issue 1 Pages 13-16

Abstract: Zn metal (5 g) was dissolved in 9 M HCl and evaporated almost to dryness. The residue was dissolved in 50 mL 2 M HCl and a 170 µL portion was injected into a stream of 2 M HCl at 0.4 ml/min. The carrier stream flows through a BIORAD AG1-X8 anion-exchange column (3 cm x 2 mm i.d.) where the matrix Zn was absorbed and the analytes passed directly into the ICP-MS. After 700 s of sample injection the zinc matrix was flushed from the column with 2 M HNO3 at a flow rate of 3 ml/min. The column was regenerated by washing with 2 M HCl at 0.4 ml/min for 300 s. The calibration graphs were linear up to 10 ng/ml for each analyte. The detection limits were 0.12, 0.48, 1.2, 3.1 and 4 ng/g, respectively, for Th, U, Co, Ni and Cu. RSD (n = 3) were 5% at 10 ng/ml. The method was applied to the analysis of high-purity zinc metals and three NIST standard reference zinc standards. Recoveries were 95-116%.
Cobalt Copper Nickel Thorium-232 Uranium Ion exchange Mass spectrometry Column Matrix removal Reference material Resin Biorad

"Sensitive And Precise Analytical Methods For The Determination Of Impurities In Hydrometallurgical Zinc Refining By Utilizing The Flow Injection Technique"
Bunseki Kagaku 1996 Volume 45, Issue 1 Pages 1-18
Hayashibe, Y.;Sayama, Y.;Oguma, K.

Abstract: A flow sheet for a hydrometallurgical zinc-refining process stream is presented, and the typical compositions of the initial and purified electrolyte are tabulated. A block diagram of a computer-controlled FIA system is given, and manifolds are illustrated for the determination of (i) Cu at 810 nm, (ii) Cu at 525 nm with 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolinesulfonate, (iii) Co at 480 nm with nitroso-R salt, (iv) Co at 617 nm with 3-[3-amino-4-(5-bromo-2-pyridylazo)-N-propylanilino]propanesulfonate, and (v) Cd at 480 nm with cadion and also for a flow injection ICP-MS system. Investigations are reported of (i) the use of a non-dispersed high-volume sample zone to overcome the effects of high salt concentrations, (ii) corrections for system variation and (iii) a computer-controlled variable-volume injector to extend the dynamic range of the system. Finally, the introduction into FIA of online anion exchange to permit the determination of trace metals in high-purity zinc by ICP-MS is discussed.
Cadmium Cobalt Copper Ion exchange Spectrophotometry Mass spectrometry Computer Linear dynamic range