RESUMEN

Using the proposed high-pressure pressed powder pellet technique, a coal sample was pressed into an ideal pellet without binders, which provides a solution to the poor self-binding quality of coal for the determination by X-ray fluorescence spectroscopy (XRF). The pellet produced by this method was more compact and smoother, which was particularly meaningful for spectrometer, where the sample is placed over the tube window. Additionally, the high-pressure sample preparation technique effectively eliminated the effect of falling powder and contamination in the Measuring chamber of the spectrometer. Wavelength Dispersive X-ray Fluorescence Spectroscopy (WDXRF) was applied successfully to the determination of carbon, nitrogen and ash content in coal samples. This could provide an alternative method for the rapid analysis of carbon, nitrogen and ash content in the coal rather than the combustion method or the high-frequency infrared absorption with a slow ashing method. Furthermore, WDXRF could provide simultaneous determination of other major, minor and trace elements by X-ray fluorescence spectroscopy. The XRF results indicated that the sensitivity, precision, and limit of detection for most components were improved when the coal sample was pressed at 1600kN compared with preparation at 400kN.

RESUMEN

To reduce the limit of detection (LOD) and allow the accurate determination of Ge, a dry ashing method was performed to enrich the Ge in plant samples. A method for the determination.of trace Ge in plant samples by HG-AFS was established. Study of the effect of temperature on the ashing of plant samples showed that no volatile loss of Ge occurred even at 900 °C. Additional experiments indicated that a 4 h burning process at 600 °C would be sufficient to fully ash the plant samples. Various digestion methods (involving nitric acid, hydrofluoric acid, and sulfuric acid digestion methods) for ashed samples were investigated. High-temperature ashing with large sample weights was used, which could reduce the reagent doses and the method's LOD effectively and simultaneously, the precision of the method was improved. The method's LOD was 0.27 ng · g(-1), and the relative standard deviation was 3.99%-6.81%. Verified with national biological reference materials (grade I), the proposed method was accurate and reliable.

Asunto(s)

RESUMEN

Using the independently designed high pressure sample preparation mold and high pressure sample preparation technology (patent number: 201310125772. 5), studies on the high pressure pressed various geological samples such as rocks, soils and stream sediments were first described in the present paper. It is the first experiment conducted in this field with significant achievements obtained. Without any binder, various types of geological powder samples can be pelleted well using 1600KN high pressure method. Such pellet has the characteristics of dense, flat, smooth and shiny surface, no cracks, no delamination, and no powder dropping. The study provides a new and contamination-free approach to sample preparation of X-ray fluorescence spectrum analysis. The comparison study conducted between the same samples pelleted under the low pressure (400 kN) and high pressure (1 600 kN) showed that using the high pressure the element peak to background ratios, and sensitivities are significantly improved, the detection limits are lowed, and the accuracies, the precisions and sample preparation repeatability are greatly improved. The Si FWHM became wider for the high pressure (1 600 kN) pellet than the same sample pelleted under the lower pressure (400 kN). The further SEM observation revealed that variation of Si spectrum shape may be caused by that the silica crystal lattices are destroyed and the particle size becomes smaller by using the high pressure pelleting techniques. So the particle size and mineral effects are also effectively reduced and the precisions and accuracies of the analytical method are improved.

RESUMEN

A simple, rapid and useful method for the determination of water-soluble antimony(III) and antimony(V) in soil was established using hydride generation atomic fluorescence spectrometry. The method was based on the different chemical reaction efficiency between Sb(III) and Sb(V) with KBH4 in the media of HCl. The amounts of Sb(III) and Sb(V) can be obtained through measuring antimony fluorescence intensities before and after reduction with reductant. The effects of HCl and KBH4 on the sensitivities of Sb(III) and Sb(V) were investigated, and the interferences from coexistent elements were studied. The reduction efficiencies of both reductants were compared. The detection limits of the method were 1.11 ng x g(-1) for Sb(III) and 1.57 ng x g(-1) for Sb(V). The accuracy of the method was verified by recovery experiments on spiked real soil samples.