A. I. Saprykin

Analysis of high-purity germanium dioxide by atomic absorption spectrometry

To ensure analytical support for the growth of bismuth orthogermanate single crystals, we have developed an electrothermal atomic absorption technique for analysis of germanium dioxide with the separation of the host through reactive evaporation in the form of germanium tetrachloride. The technique allows Cd, Co, Cu, Cr, Mn, Ni, and Pb to be determined with detection limits in the range 1 × 10−8 to 1 × 10−8 wt %.

Determination of chlorine in bismuth and bismuth oxide by atomic absorption spectrometry and laser mass spectrometry

To provide analytical tools for the preparation and oxidation of pure bismuth, we have developed techniques for chlorine determination in bismuth and bismuth oxide: indirect, using atomic absorption spectrometry, and direct, using laser mass spectrometry, with detection limits of 1 × 10−3 and 1 × 10−5 wt %, respectively. The techniques were used to assess the purity of bismuth in the refining and oxidation steps.

Determination of gold and palladium in rocks and ores by atomic absorption spectrometry using two-stage probe atomization

The efficiency of two-stage probe atomization for the determination of gold and palladium in geological samples by electrothermal atomic absorption spectrometry is studied. The effects of temperature–time program and the position of the probe in an atomizer on the fractionation of sample components and the magnitude of the analytical signal are studied. It is demonstrated that gold and palladium can be quantitatively determined by atomic absorption spectrometry in rocks and ores, using a two-stage probe atomization with the limits of detection for gold and palladium 0.01 and 0.04 g/t, respectively.

Analysis of Europium, Yttrium and Lanthanum Compounds by Atomic Emission Spectrometry with Inductively Coupled Plasma

The paper presents a multi-element analysis of europium, yttrium and lanthanum compounds by atomic emission spectrometry with inductively coupled plasma (ICP-AES). The plasma power was optimized, the choice of analytical lines of the impurities to be determined and the concentration of matrix element were substantiated. The method allows to determine up to 40 trace elements with the limits of detection (LODs) ranging from 10–6 to 10–3 wt %.

ICP-AES analysis of silicon, germanium, and their oxides

The techniques of atomic emission spectrometry with inductively coupled plasma (ICP-AES) for quantitative determination impurities in silicon, germanium, and their dioxides are developed. Analytical lines for silicon-matrix (29 trace elements) and germanium-matrix (42 trace elements) are selected. Matrix interferences caused by the presence of silicon and germanium in the solutions are studied. The optimal concentrations of matrix are determined. LODs for trace elements are in the range from n × 10–7 to n × 10–5 wt %; RSD < 20%. The accuracy of the results is confirmed by the method of “introduced–found.” The developed techniques are express, simple, and can determine a broad range of trace elements.

A procedure of ICP-AES analysis of silicon using microwave digestion and preconcentration

A combined procedure has been developed for the analysis of high-purity silicon with preliminary vapor-phase digestion and preconcentration in a microwave oven using inductively coupled plasma atomic emission spectrometry (ICP-AES). Liners for high-pressure vessels of microwave oven ensuring the simultaneous distillation of matrices from 3–4 samples without their contact with the acid solution have been designed and manufactured. The procedure ensures the determination of up to 30 elements: Ag, Al, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, Hf, In, K, Li, Mn, Mo, Na, Nb, Ni, P, Rb, Sb, Sn, Sr, Ta, V, W, Zn, and Zr with the limits of detection 10−8 −10−6 wt %.

Determination of impurities in bismuth oxide by laser mass spectrometry

We have developed a technique for the quantitative analysis of bismuth oxide by laser mass spectrometry. The technique makes it possible to determine up to 70 impurities in the range 10−6 to 10−4 wt %. To evaluate relative sensitivity factors and obtain calibration plots, we used reference samples prepared by diluting a standard SOG-21-1 graphite sample with high-purity bismuth oxide powder.

Analysis of high-purity bismuth oxide by atomic absorption spectrometry with reactive distillation of the matrix

A procedure is developed for the analysis of bismuth oxide by electrothermal atomization atomic absorption spectrometry with matrix preseparation by reactive distillation as bismuth trichloride. The procedure allows the determination of Ag, Al, Co, Cu, Mn, Ni, Pb in bismuth oxide with limits of detection of 6 × 10−9 − 6 × 10−8 wt %.

ICP-AES analysis of high purity bismuth oxide

Two ICP-AES techniques for analysis of high-purity bismuth oxide are described. The direct techniques enables determination of 46 impurities in bismuth oxide with limits of detection (LODs) at the level of 10−8–10−5 wt %, and the method with separation matrix allows determination of 22 impurities with LODs at the level of 10−9-10−6 wt %.

Analysis of high-purity cadmium and cadmium dioxide by atomic absorption spectrometry

To ensure high-speed analytical support to the technology of cadmium tungstate single crystal growth, we have developed an electrothermal atomic absorption spectrometry technique for analysis of high-purity cadmium and cadmium oxide for the technologically important impurities Ag, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Sn with detection limits from 2 × 10–7 to 6 × 10–6 wt %.