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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Classification: Reference Material -> NRCC -> CASS-2 -> Coastal seawater

Citations 5

"Determination Of Trace Elements In Seawater By Flow Injection Anodic Stripping Voltammetry Preceded By Immobilized Quinolin-8-ol Silica Gel Preconcentration"
Anal. Chim. Acta 1992 Volume 258, Issue 2 Pages 245-252
Bor-Jian Daih and Hsuan-Jung Huang*

Abstract: The sample (5 or 10 ml), adjusted to pH 1.6 to 7 for Cu, 3 to 4 for Bi or In, or 6 to 7 for Pb, Cd or Zn, was passed through a column (5 cm x 3 mm) of the cited gel, and the metals were eluted with 1.0 M HCl - 0.1 M HNO3 at 0.22 or 0.33 mL min-1. After being mixed with 0.5 M Na acetate the solution was analyzed in a flow-through cell at a vitreous-carbon working electrode. The coefficient of variation (n = 10) for 1.0 µg L-1 of the test ions were from 2.5 to 6.9%. The results on CASS-2 reference seawater gave reasonably good agreement with the certified values for Cd and Cu, but the Pb concentration was larger and the Zn concentration smaller than the certified value. Procedures based on the application of immobilized quinolin-8-ol silica gel and stripping voltammetry were developed for the determination of Cu, Pb, Cd, Bi, In and Zn in seawater. As two concentration steps are involved, better sensitivity and lower detection limits could be achieved with the application of smaller sample volumes. The feasibility and reliability of the procedures were confirmed by the anal. of a near-shore seawater sample and CASS-2 reference seawater.
Copper Lead Cadmium Bismuth Indium Zinc Voltammetry Immobilized reagent 8-Hydroxyquinoline Reference material Silica gel Preconcentration

"Determination Of Traces Of Copper, Cadmium, And Lead In Biological And Environmental Samples By Flow Injection Isotope Dilution Inductively Coupled Plasma Mass Spectrometry"
Anal. Chim. Acta 1993 Volume 284, Issue 1 Pages 181-188
Pei-Ling Lu, Kuang-Shie Huang and Shiuh-Jen Jiang*

Abstract: Flow injection isotope dilution ICP-MS was used in the determination of Cu, Cd, and Pb in SLRS-2 river water and CASS-2 seawater reference materials (National Research Council of Canada) and in freeze-dried urine (NIST SRM 2670) with use of 65Cu, 111Cd and 204Pb as reference isotopes. Isotope ratios for each injection (200 µL) were calculated from the areas of the flow injection peaks and precision was generally 1%. Detection limits were 45, 25 and 58 ng/l for Cu, Cd and Pb, respectively. Both Na and Mg interfered in the determination of Cu and their prior removal was necessary for the analysis of highly saline samples such as seawater. A Tracecon sample pre-treatment system (cf., Ibid., 1993, 282, 437) was used for the separation of Mg and Na and for the pre-concentration of traces of Cu, Cd and Pb in the natural water reference materials. Results obtained for all reference materials agreed well with certificate values.
Copper-65 Cadmium-111 Lead-204 Spectrophotometry Mass spectrometry Reference material Isotope ratio Interferences Preconcentration

"Application Of Multielement Time-resolved Analysis To A Rapid Online Matrix Separation System For Inductively-coupled Plasma-mass Spectrometry"
J. Anal. At. Spectrom. 1995 Volume 10, Issue 11 Pages 929-933
Simon M. Nelms, Gillian M. Greenway and Robert C. Hutton

Abstract: A rapid online matrix separation system for ICP-MS, using multi-element time-resolved analysis, was developed for the determination of several trace elements in complex matrix samples, A flow injection manifold was constructed consisting of a mini-column of 8-hydroxyquinoline covalently immobilized on to controlled pore glass, Analytes retained on the column were eluted using 0.1 mi of 2.0 mol L-1 nitric acid, Sample volumes of 0.5 mi were analyzed, yielding a pre-concentration factor of 5 in addition to matrix separation, The system was optimized with respect to the variables of buffer concentration, buffer pH and eluent acid volume and concentration, Calibrations from both pure water and synthetic seawater compared well and showed good linearity, with correlation coefficients of 0.988-0.999 for a range of analytes, The method showed good within-run reproducibility with precisions (s(r)) at the 1 ng mL-1 level of typically <3%, In general, recoveries between 89 and 104% were obtained, with the exception of Ni, which showed a recovery of 78% under the compromise conditions used. The method was validated by the analysis of estuarine (SLEW-1) and coastal (CASS-2) certified reference materials, Good agreement with the certified values was obtained for both of these materials. (17 references)
Metals, trace Mass spectrometry Sample preparation 8-Hydroxyquinoline Controlled pore glass Optimization Preconcentration Reference material Solid phase extraction

"Online Solid-phase Chelation For The Determination Of Eight Metals In Environmental Waters By Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1996 Volume 11, Issue 3 Pages 187-191
Daniel B. Taylor, H. M. Kingston, Donald J. Nogay, Dagmar Koller and Robert Hutton

Abstract: Seawater was mixed with 4 M ammonium acetate buffer, the pH was adjusted to 5.5 and diluted with water. The prepared seawater or natural water was loaded into a flow injection system at 2.4 ml/min and the sample merged with a buffer solution (2 ml/min) of 4 M ammonium acetate of pH 5.8 which had passed through a clean up Al-clad PEEK column (7.5 cm x 4.6 mm i.d.) packed with Muromac A-1 (50-100 mesh). The resulting solution was loaded on to a PEEK column (5 cm x 4 mm i.d.) and the column was washed with water. Weakly retained matrix components were eluted with buffer and the buffer was washed off the column with water. The metal analyzes were eluted with 1 M HNO3 and the eluate passed to the ICP-MS instrument via a V groove nebulizer. Eight metals (14 isotopes) were determined with detection limits of 0.5-60 ng/l for a 10 mL sample to 0.11-12 ng/l for a 50 mL sample (results tabulated). The results for the analysis of water reference materials are tabulated and discussed.
Metals Mass spectrometry Sample preparation Reference material Chelation Solid phase extraction Muromac

"Determination Of Seven Trace Elements In Environmental Water Samples By Inductively Coupled Plasma Mass Spectrometry With Online Preconcentration"
Bunseki Kagaku 1993 Volume 42, Issue 7 Pages 423-428
Akatsuka, K.;McLaren, J.W.;Berman, S.S.

Abstract: An online pre-concentration method was studied to allow the simultaneous determination of Mn, Co, Ni, Cu, Zn, Cd and Pb in 5 mL environmental water samples by inductively coupled plasma mass spectrometry. A semiautomated system with a microprocessor-controlled high performance quaternary gradient pump and valves was used to lead and transport the mobile phase. The system includes a column containing silica-immobilized 8-hydroxyquinoline. The pH of the samples was adjusted to 8 to improve the retention of several elements, in particular manganese. Quantitative elution from the column took 3.5 min with a 1.5 M HCl/0.6 M HNO3 mixture at a flow rate of 2.0 mL min-1. Mn and Co were determined by a standard additions technique, and stable isotope dilution was applied for Ni, Cu, Zn, Cd and Pb. The good precision and accuracy of this method are demonstrated by analyzing standard samples of riverine water (SLRS-2), estuarine water (SLEW-1) and coastal seawater (CASS-2). The detection limits of the method range from 7 ng L-1 for Cd to 130 ng L-1 for Zn. [References: 18]
Manganese Cobalt Nickel Copper Zinc Cadmium Lead Mass spectrometry Preconcentration Computer Column Immobilized reagent Silica 8-Hydroxyquinoline Reference material Standard additions calibration