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In this paper, the method of determining arsenic and selenium in the industrial sulphur sample has been studied. Carbon tetrachloride-boromine was used to dissolve the sulphur sample in classical methods, which is complex and harmful, and a little arsenic and selenium will be lost. In this paper, nitric acid and perchloric acid were used to dissolve the sulphur sample, which was simple, and scarcely arsenic and selenium were lost. Under the selected conditions, determination of arsenic and selenium can be determined simultaneously by HG-ICP-AES. The determination limits of arsenic and selenium are 0.6 ng.mL-1 and 0.7 ng.mL-1, respectively, the relatively standard deviations(RSD) (n = 8) are 2.1% for arsenic and 1.9% for selenium, respectively, and the recoveries are 99.6% for arsenic and 101% for selenium, respectively, which was a very satisfying result.
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PMID:[Determination of arsenic and selenium in the industrial sulphur]. 1293 55

The present paper describes the application of a solid phase extraction system in order to separate traces of calcium from glass and ceramics for its spectrophotometric determination. The method is based on the extraction of calcium from sodium hydroxide solution by tri-n-butyl phosphate (TBP) loaded polyurethane foam (PUF), followed by its elution in hydrochloric acid. The spectrophotometric measurement of the absorbance of calcium complex with calconcarboxylic acid (2-hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo)-3-naphthoic acid) takes place at pH 12. The following parameters were studied: effects of sodium hydroxide concentration and temperature on the extraction of calcium, time of equilibration for quantitative calcium extraction, effect of TBP concentration, effect of hydrochloric acid concentration for quantitative elution of calcium from PUF, effect of pH and concentration of calconcarboxylic acid for quantitative formation of the complex with calcium, effect of acetone on the stability of calcium-calconcarboxylic acid complex and influence of diverse ions on calcium sorption by TBP-loaded PUF. The results show that calcium traces can be separated onto TBP-loaded PUF from 0.25 mol L(-1) NaOH at 30 +/- 5 degrees C within 30 min. PUF was loaded with TBP in CCl4 (40% v/v). Elution of calcium was done in 1.0 mol l(-1) HCl. The calcium formed a complex with calconcarboxylic acid at pH 12 and absorbance was measured at 560 nm in acetone-water medium. Molar absorptivity was found to be 1.082 x 10(4) l mol(-1) cm(-1). The method obeys Beer's law from 0.10 to 5.0 microg ml(-1) Ca. The validity of the method was established by its successful application in NIST standard reference materials. The method proposed was applied to determine calcium in glass and ceramic materials. The results of the proposed method are comparable with the results of ICP-AES analysis and they are found to be in good agreement.
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PMID:Selective extraction of calcium on tri-n-butyl phosphate plasticized selective extraction of calcium on tri-n-butyl phosphate plasticized polyurethane foam for its spectrophotometric determination in glass and ceramics. 1637 92

The possibilities for universal calibration based on multi-element aqueous standard solutions and graphite laboratory reference materials (graphite standards) for the electrothermal vaporization inductively coupled plasma optical emission spectrometric (ETV ICP OES) determination of Al, B, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, P, Pb, S, Sr, Ti, V, and Zn in plant materials were investigated. A commercially available state-of-the-art ETV device was coupled with an Echelle ICP spectrometer equipped with a charge-injection-device (CID) camera for spectral detection. The transition area between transport tube and ETV graphite tube and the gas streams for inner gas, bypass gas, and modifier gas were optimized to achieve best transport efficiencies. The influence of four gaseous modifiers (CCl4, CHCl3, CCl2F2, and C3H8) added to the inner gas was studied. Five reference materials (RM P-Alfalfa, Lucerne; NIES CRM No.9 "Sargasso"; CTA-VTL-2 Virginia Tobacco Leaves; NIST SRM 1515 Apple Leaves; IAEA-V-10 Hay Powder) were used for method validation. If certified reference materials are not available, calibration against graphite standards or dried aqueous standard solutions is possible. Three carbonization procedures as sample pretreatment for the plant materials were investigated.
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PMID:Calibration possibilities and modifier use in ETV ICP OES determination of trace and minor elements in plant materials. 1946 19