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An atomic absorption spectrometry (AAS) method for the determination of total and combined sulphur in rubber and a catalytic method for the determination of free sulphur in rubber are described. The catalytic method is based on the iodine-azide reaction and is followed by an extraction of free sulphur with benzene, toluene or acetone. The catalytic determination, with the aid of gas chromatography,...
Several papers have appeared in the literature describing the determination of antimony, where antimony(V) is extracted into the organic phase and the organic solutions directly analyzed by atomic absorption spectrometry (AAS). This paper describes a procedure where antimony from the organic solution is reductively stripped into an aqueous phase and analyzed for antimony by AAS. The advantage of...
An analytical procedure for dissolving wolframite in order to determine trace elements by atomic absorption is reported. After decomposition of the mineral by alkaline fusion, the cooled flux is dissolved by heating with aqua regia. The finely crystalline precipitate of tungstite, which forms on standing, is filtered and dissolved by heating with aqua regia. Tungstite forms again in the latter solution...
A method for the determination of lead in human hair slurries by electrothermal atomic absorption spectrometry was optimized. Particle size reduction was achieved with a vibrational mill ball equipped with zirconia cups, 20 min being sufficient grinding time to achieve an adequate particle diameter (< 1 μm). The use of different thickening agents, namely glycerol, Triton X-100 and Viscalex HV30,...
Methods for the direct determination of silver and manganese in cocaine and heroin by electrothermal atomic absorption spectrometry using palladium as chemical modifier have been developed. Cocaine samples, 0.5 g, were dissolved in 2 ml of 35.0% (m/v), HNO 3 diluting to 10 ml with ultrapure water. A comparative study of palladium, magnesium nitrate, palladium-magnesium nitrate and nitric...
A rapid and reliable procedure for the determination of gold in geological samples is reported that involves MnO 2 and HCl treatment of the samples followed by ethyl acetate extraction of gold and determination at the ppm and sub-ppm levels by flame atomic absorption spectrometry after evaporating off the organic solvent. The method was tested for the quantitative recovery of gold from the...
Trace metals in water were preconcentrated with silica gel modified with salicylaldoxime and determined by AAS. Optimum conditions for the maximum recovery of metal ions, viz. Cu(II), Ni(II), Co(II), Zn(II) and Fe(III), for both batch and column methods were developed. The efficiency of the adsorbent with respect to different experimental conditions was established.
We have studied the speciation of chromium (VI) in stainless-steel welding dusts. The approach used for the analysis of Cr(VI) and total Cr relies on a flow-injection analyzer (FIA) equipped with two different sequential detectors. The system measures Cr(VI), by colorimetry (with 1,5-diphenyl carbohydrazide) and total chromium content by flame atomic absorption spectroscopy (AAS). The extraction...
The development of reference materials to verify the determination of metals in sludge is described. Effluents from domestic and industrial treatment facilities were dried, size-reduced and homogenized. Multiple aliquots of each material were analyzed in two different government laboratories to determine reference values for the acid-extractable concentrations of more than 15 metals. These acid-extractable...
A poly[styrene-co-(divinylbenzene)] resin (XAD-4) functionalized with 1-hydrazinophthalazine ligand has been prepared and its analytical properties investigated. The pH dependence of sorption of metal ion on the resin has been determined for Cu(II), Ni(II), Co(II), Zn(II), Cd(II), Pb(II), Fe(III) and Cr(III). Trace amounts of these metal ions were quantitatively retained on the resin and recovered...
An endemic peripheral vascular disorder resulting in gangrene of the lower extremities, especially of the feet, is called Blackfoot disease (BFD) . Clinically, the symptoms and signs of Blackfoot disease are similar to those of Buerger's disease. In this study, the objective is to examine the amount of arsenic, mercury, zinc, lead, and selenium in urine samples from BFD patients. After pre-treatment...
An on-line flow injection-hydride generation/atomic absorption spectrometry method was developed for the preconcentration and selective determination of inorganic arsenic [As(III) and As(V)] and its methylated species. The separation of the arsenic species was performed by an automated pH-selective arsines generation technique, using sodium tetrahydroborate(III) as reductant. Each arsine was cryogenically...
Infant formula and powdered milk samples were suspended in a medium containing 20% ethanol, 0.65% nitric acid, 6% hydrogen peroxide and 0.1% ammonium dihydrogenphosphate and directly introduced in the electrothermal atomizer. Liquid milk samples were diluted with this suspension solution. The build-up of carbonaceous residues inside the atomizer was avoided by using a combination of hydrogen peroxide...
Water-insoluble 8-quinolinolato metal chelates were formed and were stably solubilized in the aqueous solution of a water-soluble polymer, poly (N-isopropylacrylamide)(PNIPAAm), at room temperature. When the solution was heated at 50°C, PNIPAAm precipitated and then formed a gum-like aggregate (polymer phase) having a very small volume. Accompanying the polymer precipitation, hydrophobic 8-quinolinolato...
Polymer enhanced ultrafiltration (PEUF) is a newly developed method for the removal of heavy metals from aqueous solutions. This method was applied for the removal of mercury and cadmium with the presence of polyethyleneimine (PEI) as a water soluble polymer. After ultrafiltration experiments for metal–polymer mixtures, two separate streams, namely, retentate and permeate, former of which contains...
An efficient method was developed for the determination of metals in used lubricating oils, by atomic absorption spectrometry. Oil samples were treated with an acid mixture and then emulsified in water (10% w/w) using ethoxy nonylphenol (6% w/w) as surfactant. Emulsion characteristics (oil, surfactant content and acid mixture) were optimized to obtain the best AAS signal. Good agreement was found...
A sequential injection system for the determination of mercury by vapor generation atomic absorption spectrometry (VGAAS) using tetrahydoborate reductant was developed, characterized by prevention of sample and reagent mixing in the holding coil using small air segments and initiation of the vapor generation in a flow-through gas-liquid separator. Extremely small volumes of reductant of 15-30 μl (0...
A rapid and sensitive sorbent extraction hydride generation-flow injection analysis atomic absorption spectrometric (HG-FIAS-AAS) method is described for the determination of As(III) and As(V) based upon online preconcentration on a microcolumn packed with activated alumina. In the present procedure these arsenicals are complexed with quinolin-8-ol-5-sulphonic acid from neutral solutions in the flow...
A simple and fast method for the extraction into xylene of sub μg l -1 concentrations of metals using ammonium diethyldithiophosphate (DDTP) as a complexing reagent and their subsequent determination by flame atomic absorption spectrometry is described. The method was tested in sea water spiked with Au at a concentration of 3.0 μg l -1 . The extraction was carried out until...
The masking action of the dithiophosphoric acid diacylester (DDTP) for the determination of Bi by hydride generation absorption spectrometry (HGAAS) in the presence of high concentrations of copper was studied. Cu/Bi ratios up to 50x10 3 were found to be tolerable in the presence of 2x10 -3 M chelating solutions in 10% HCl, using 1.5% NaBH 4 as reductant. Good agreement...
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