The concentrations of the impurities in brown coals some of Kazakhstan deposits — «Kulan», «Shoptikol’», «Oi Karogai», «Sarykum» — were determined. Surface inclusions in coals were studied using optical USB microscopes. The composition of inclusions and total composition of coals were analyzed by both X-ray spectrometry with energy dispersion and atomic emission spectrometry using «Grand-Potok» complex with sample introduction by the spill-injection method into an arc discharge and recording spectra with an analyzer MAÉS. Gold was determined on a «Grand-Potok» complex using scintillation method. The coals of «Oi Karogai», «Sarykum», and «Kulan» deposits exhibited inclusions of pyrite in crystalline form. It was shown, that both gold and silver are present only in the coals of the «Shoptikol’» deposit in the form of flat round inclusions. Inclusions formed particles of gold-silver alloy upon melting according to data of scintillation analysis. The average concentrations of gold and silver in the coal samples of the «Shoptikol’» deposit are 0.007 and 0.03 ppm, respectively. It is shown that scintillation determination of precious metals in brown coals of Kazakhstan on a «Grand-Potok» complex with MAÉS analyzer is more rapid compared to the methods of inductively-coupled plasma-mass spectrometry (ICP-MS), atomic emission spectrometry (AES) and atomic absorption spectrometry (AAS) at comparable detection limits.
An additional photodetector array BLPP-369 was installed on a «Grand-Potok» complex for rapid atomic-emission determination of the fluorine concentration in fluorite samples. Introduction of fluorite samples was carried out using the spill-injection method simultaneously with high pure calcium oxide introduction using the second conveyor belt. The use of an additional photodetector array with a spectral range of 528 – 536 nm provides the possibility of expanding the spectrum of CaF molecular lines with the intensity sufficient for determination of fluorine concentrations in fluorite samples. A calibration curve for fluorine determination in a concentration range of 0.12 – 47.63% was plotted using measurement results for 200 fluorite samples. Integration of the additional photodetector array provided increased detection limit for the mass fractions of fluorine up to the maximum possible concentrations in fluorite samples. The observed effect simplifies and speeds up the analysis in the absence of the necessity to dilute the sample, thus reducing the error of measurements. The results show that there is no need to introduce additional buffer mixtures (except CaO) and use reference lines to determine the fluorine concentration, which also simplifies the measurement procedure.
Ìåòîä ñöèíòèëëÿöèîííîé àòîìíî-ýìèññèîííîé ñïåêòðîìåòðèè (ÑÀÝÑ) ïîçâîëÿåò ïðè ïðÿìîì àíàëèçå ïîðîøêîâûõ ïðîá îïðåäåëÿòü ïîìèìî îáùåãî ñîäåðaeàíèÿ ýëåìåíòà ôîðìó åãî íàõîaeäåíèÿ â îáðàçöå è ðàçìåð âêëþ÷åíèé. Ñ èñïîëüçîâàíèåì êîìïëåêñà «Ãðàíä-Ïîòîê» ïðîàíàëèçèðîâàëè ïðîáû êðèñòàëëîâ ïèðèòà ðàçíîãî ðàçìåðà äëÿ îïðåäåëåíèÿ çîëîòà è ôîðìû åãî íàõîaeäåíèÿ. Äëÿ âñåõ èññëåäîâàííûõ ïèðèòîâ íå áûëî îòìå÷åíî çàâèñèìîñòè ñîäåðaeàíèÿ çîëîòà îò ðàçìåðîâ êðèñòàëëà: â îáúåìå êðèñòàëëîâ ïðèñóòñòâóþò ÷àñòèöû ðàçìåðîì ìåíåå åäèíèö ìêì, êðóïíûõ ÷àñòèö Au íåò. Óñòàíîâëåíî, ÷òî çîëîòî è äðóãèå äðàãîöåííûå ìåòàëëû ñîñðåäîòî÷åíû â ïîâåðõíîñòíûõ ñëîÿõ êðèñòàëëîâ ïèðèòà è â äåôåêòàõ êðèñòàëëè÷åñêîé ðåøåòêè â îáúåìå êðèñòàëëà (ïî äàííûì ÑÀÝÑ ïðè ëàçåðíîé àáëÿöèè ïðîáû â äóãîâîé ðàçðÿä).  îáúåìå êðèñòàëëîâ ïèðèòà îáùåå ñîäåðaeàíèå çîëîòà ñîñòàâëÿåò îêîëî 2 ã/ò, ïëàòèíû è ñåðåáðà -ìåíåå 0,02 ã/ò, òîãäà êàê íà ïîâåðõíîñòè ñîäåðaeàíèå Au, Ag, Pt -îò 2 äî 5 ã/ò. Ïðåäåë îáíàðóaeåíèÿ çîëîòà ìåòîäîì ÑÀÝÑ ñîñòàâëÿåò 0,01 ã/ò.
Modernization of «Grand-Potok» atomic emission complex with MAÉS analyzer («VMK-Optoélektronika», Novosibirsk, Russia) first designed for analysis of powder samples is considered in view of the possibility of analysis of solutions and aqueous aerosols avoiding changes in the sample injection. It is shown that upgraded input system equipped with a nebulizer provides determination of platinum and gold in aqueous solutions with detection limits 1 – 5 ppm. Analysis of water aerosols with silver nanoparticles by scintillation method revealed the possibility of detecting separate silver nanoparticles about 200 nm and more. Thus we have demonstrated that modernization of the complex provides the possibility for analysis of solutions and aerosols obtained upon electro-spark and laser ablation of various materials, as well as for microanalysis of the objects.
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