Slurry Sampling Atomic Absorption Spectrometry Research Articles

Comparison of action of mixed permanent chemical modifiers for cadmium and lead determination in sediments and soils by slurry sampling graphite furnace atomic absorption spectrometry

Slurry sampling atomic absorption spectrometry with electrothermal atomization was used to the determination of cadmium (Cd) and lead (Pb) in soils and sediments using permanent modifiers. Comparison of action of mixed permanent modifiers niobium (Nb)/iridium (Ir) and tungsten (W)/iridium (Ir) were studied in detail. The effect of amount of Ir, W and Nb on analytical signals of Cd and Pb was examined. The optimal amounts of modifiers for Cd and Pb determination were stated. Niobium carbide formation on graphite surface was studied for different pyrolysis temperatures. Finally for Cd determination in sediments and soils 200 μg of Nb mixed with 5 μg of Ir was used as permanent modifiers and 15 μg of Nb mixed with 200 μg of Ir for Pb determination. Suspensions were prepared in 5% HNO 3. The analytical procedure was optimized carefully basing on data from pyrolysis and atomization curves studies. Ammonium dihydrogen phosphate was used additionally as matrix modifier during Cd determination in samples in order to prevent interferences coming from matrix components. The analysis of CRMs confirmed the reliability of the proposed approach. The precision and accuracy of Cd and Pb determination by the described method for soils and sediments were acceptable.

Determination of tin in marine sediments by slurry sampling atomic absorption spectrometry with electrothermal atomization using a permanent modifier

Slurry sampling atomic absorption spectrometry with electrothermal atomization was used for the determination of tin in marine sediments. A mixture of 4 μg of iridium and 40 μg of tungsten and 12 μg of niobium alone were used as permanent modifiers. Suspensions were prepared in 7% nitric acid. The influence of amounts of tungsten on iridium removal from graphite tubes modified by iridium and the mechanism of atomization of tin in slurries were studied in detail. The effect of the amount of added iridium, tungsten and niobium on the analytical signal, and of the soil matrix on the background signal is described. In order to prevent interferences by sulfur compounds, barium chloride was added as a matrix modifier. Calibration was performed directly using aqueous standards. The analysis of certified reference materials confirmed the reliability of the approach. The precision and accuracy of the determination of tin in sediments by this method is acceptable.

Determination of trace mercury in geological samples by direct slurry sampling cold vapor generation atomic absorption spectrometry

A new method based on ultrasonic slurry sampling atomic absorption spectrometry (AAS) was established for the determination of trace mercury in geological samples by use of recently developed mercury cold vapor generation using formic acid under ultraviolet (UV) irradiation. The generated mercury cold vapor was rapidly separated from the matrix and swept into a T-tube for the measurement of atomic absorbance. Under the optimal experimental conditions, up to 1000-fold of Cu(II), Co(II), Ni(II), Cr(VI), Mn(II), Fe(III), and Zn(II) caused no significant interference with the determination of 50 µg L−1 Hg. The limit of detection at sub-ppb level was obtained for mercury. The method was applied to the determination of mercury in geological samples with satisfactory results.

Current Status of Direct Solid Sampling for Electrothermal Atomic Absorption Spectrometry—A Critical Review of the Development between 1995 and 2005

The literature about direct solid sampling (SS) and slurry sampling atomic absorption spectrometry (AAS) over the past decade has been surveyed critically. It became apparent that a very significant change had occurred, particularly in the relation between the two major techniques used for that purpose. In the 1990s, slurry sampling was typically considered the technique of choice, combining the significant advantages of the solid and the liquid sampling methods, at least in part because of the availability of a commercial accessory for automatic slurry sampling. The situation is completely inverted now, as the above accessory has been discontinued and rugged and reliable accessories for direct SS became available. Direct SS electrothermal (ET) AAS has been shown to provide the best limits of detection because of the absence of any dilution and a minimal risk of contamination. Calibration against aqueous standards appears to be feasible after careful program optimization. The absence of any significant sample handling makes SS ET AAS ideally suited for fast screening analyses. The introduction of high‐resolution continuum source AAS appears to open additional attractive features for SS ET AAS because of the significantly simplified optimization of furnace programs and the visibility of the spectral environment, which makes it easy to avoid spectral interferences. New calibration strategies make a “dilution” of samples unnecessary, which used to be one of the major limitations of SS ET AAS. Finally, direct SS analysis is an important contribution to clean chemistry, as practically no reagents are used.