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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Spectrophotometry

Citations 39

"Speciation Of Antimony(III) And Antimony(V) Using Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry Combined With The Rate Of Pre-reduction Of Antimony"
Anal. Chim. Acta 1999 Volume 386, Issue 3 Pages 297-304

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Yong-Lai Feng, Hisatake Narasaki, Hong-Yuan Chen and Li-Ching Tian

Abstract: Antimony(III) and antimony(V) were speciated by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-AES) based on the pre-reduction kinetics of antimony(V) to antimony(III) with L-cysteine. A linear relationship between the reduced amount of antimony(V) with 3 mg mL-1 of L-cysteine and the reaction time was achieved within 10 min. The reduced amount of antimony(V) were determined after 2 and 8 min, respectively, by using HG-ICP-AES in this method. Mutual interferences of antimony(III) and antimony(V) were investigated. Interferences from transition metals were removed by a Chelex 100 resin column. The method was successfully applied to speciate antimony(III) and antimony(V) in spiked water samples. The detection limits of the method for antimony(III) and antimony(V) were 1.2 and 4.5 ng mL-1 respectively.
Arsenic(3+) Arsenic(5+) Environmental Speciation Volatile generation Chelex

"Determination Of Antimony Species With Fluoride As Modifier And Flow Injection Hydride Generation Inductively-coupled Plasma Emission Spectrometry"
Anal. Chim. Acta 2000 Volume 417, Issue 2 Pages 201-209

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Nina Ulrich

Abstract: A new method for the determination of species of antimony(III) [Sb(III)], antimony(v) [Sb(V)] and trimethylstiboxide [TMeSbO] with fluoride as modifier is introduced. A flow injection (FI) system for hydride generation was used in combination with an inductively-coupled plasma atomic emission spectrometer as detector. The pre-reduction was accomplished with potassium iodide dissolved in hydrochloric acid and the reduction with sodium borohydride. The influence of fluoride on the reduction and pre-reduction step was investigated by adding different amounts of sodium fluoride to the solvent stream. At a concentration of 100 mg/l fluoride and 1.2% potassium iodide, the hydride formation of Sb(V) and Sb(III) was suppressed below the detection limit, while TMeSbO showed no signal depression. The use of 100 mg/l fluoride without potassium iodide led to complete signal suppression for Sb(V) with apparently no influence on the signal intensity of Sb(III) and TMeSbO. The concentration of TMeSbO was measured directly, the concentrations of Sb(III) and Sb(V) were calculated on the basis of the three analyzing steps, giving detection limits and relative standard deviations of 1.1 (2.6%), 1.2 (5.3%) and 1.4 µg/l (8.1%), respectively. The method was applied to orange juice samples.
Antimony(3+) Antimony(5+) Trimethylstibine oxide Juice Leachates Speciation Interferences Method comparison

"A Flow Injection/hydride Generation System For The Determination Of Arsenic By Inductively-coupled Plasma Atomic Emission Spectrometry"
Anal. Chim. Acta 1984 Volume 161, Issue 1 Pages 275-283

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R. R. Liversage and J. C. Van Loon, J. C. De Andrade

Abstract: After optimizing the concentration. of HCl and NaI in the test solution, the concentration. of NaBH4, sample and reductant volume and flow rate, Ar carrier-gas flow rate and r.f. power, As (10 to 1000 ppb) was determined in NBS orchard leaves, coal fly ash and river sediment and NRCC MESS-1 and BCSS-1 standard reference materials with good accuracy and precision by using an ARL 34000 Quantometer. The coefficient of variation (n = 10) at the 100-ppb level of As was 7.2%, and the detection limit was 1.4 ng for a 0.17 mL sample volume The calibration graph was rectilinear for 0.01 to 1 ppm of As. Cobalt, Ni, Ag, Au, Bi, Te and Sn interfered. About 200 injections h-1 were possible.
Arsenic NIST 1571 NIST 1633 NIST 1645 NRCC BCSS-1 NRCC MESS-1 River Interferences Reference material

"Determination Of Arsenic In Glycerol By Flow Injection Hydride Generation And Inductively Coupled Plasma Atomic-emission Spectrometry"
Anal. Chim. Acta 1986 Volume 184, Issue 1 Pages 205-212

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Ngee-Heng Tioh, Yecheskel Israel and Ramon M. Barnes

Abstract: A flow injection system is used to mix glycerol solution, containing 0.12 to 3.0 µg g-1 of As, with 1.1% NaBH4 solution (in 0.2 or 0.5 M NaOH) - 6 M HCl (10:49). The generated AsH3 is removed in a vapor - liquid flow cell and determined directly by ICP-AES at 193.7 nm, with Ar as carrier gas (0.39 l min-1). The calibration graph was rectilinear in the range 0.12 to 3.0 µg mL-1 of As with a coefficient of variation of 1.4%.
Arsenic Organic compound

"Study Of The Influence Of Ordered Media On The Determination Of Lead By Hydride-generation Inductively Coupled Plasma Atomic-emission Spectrometry"
Anal. Chim. Acta 1993 Volume 283, Issue 1 Pages 175-182

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M. C. Valdés-Hevia y Temprano, B. Aizpún Fernández, M. R. Fernández de la Campa and A. Sanz-Medel*

Abstract: Several micelle- and vesicle-forming substances were examined for use in the continuous-flow generation of plumbane. The best results were obtained with hexadecyltrimethylammonium bromide (I) micelles and didodecyldimethylammonium bromide (II) vesicles. For the analyzes, the test solution (containing 0.1 mM I or 1 mM II), 2% HNO3 and aqueous 6% ammonium thiosulfate were merged in a four-channel union cross and the resulting solution was merged with 10% NaBH4 solution in aqueous 0.1% NaOH before passing to the grid nebulizer of an ICP spectrometer with a 40 MHz source unit. Best results were obtained with the I-containing system; the detection limit was 9 ng/ml and the RSD (n = 50) was 1.4% at 50 ng/ml. Interference studies for a range of elements and anions showed that Se, As, Hg and Sn were less troublesome in the presence of I. The method was applied to the determination of Pb in commercial apple, orange and pineapple juices without pre-treatment.
Lead Fruit Micelle Interferences

"Determination Of Germanium By Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry Combined With Flow Injection"
J. Anal. At. Spectrom. 1988 Volume 3, Issue 4 Pages 579-582

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Fumio Nakata, Hiroshi Sunahara, Hiroyoshi Fujimoto, Manabu Yamamoto and Takahiro Kumamaru

Abstract: The sample (20 to 40 mg) of single-crystal gallium arsenide was dissolved in HNO3 and the solution was diluted with water to 25 mL. A 1 mL aliquot was analyzed by a system (illustrated) consisting of a PTFE flow injection manifold by which the sample is mixed with sodium phosphate buffer (pH 6.5), NaBH4 solution and Ar (carrier gas), and a gas - liquid separator, constructed from micro-porous PTFE (cf. Yamamoto et al., Anal. Chem., 1987, 59, 2446), that delivers the generated hydrides directly into the sample introduction tube of the ICP torch (central orifice 0.6 mm i.d.) for determination of Ge at 265.18 nm. The calibration graph was rectilinear for 1 ng mL-1 to 10 µg mL-1 of Ge; the detection limit was 0.4 ng mL-1. By using the method of standard additions, recovery of 4 ng mL-1 of Ge from non-doped, Zn-doped and Si-doped gallium arsenide was satisfactory, but no indigenous Ge was detected. The method was also applied in the analysis of poly(ethylene terephthalate) (sample prep. described); recoveries were 90 to 120%, and 2.5 to 3.1 ng mL-1 of Ge was detected, which is better than the detection limit (5 ng mL-1) of the official method. The sample throughput was ~150 h-1.
Germanium Inorganic compound Polymer Gas diffusion Method comparison Standard additions calibration Teflon membrane

"Lead Hydride Generation For Isotope Analysis By Inductively Coupled Plasma Mass Spectrometry"
J. Anal. At. Spectrom. 1988 Volume 3, Issue 6 Pages 821-827

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