Method of determination of content of palladium and platinum in ores

FIELD: methods of determination of content of palladium and platinum in ores containing considerable amount of iron, copper, zinc and other metals.

SUBSTANCE: proposed method includes decomposition of ore by hydrofluoric and nitric acids followed by further decomposition by aqua regia, boiling-off to moist salts, dissolving of them in hydrochloric acid and extraction. Determination of content of palladium is carried out in organic phase thus obtained and that of platinum is carried out in hydrochloric acid phase. Extractants used for such determination are s-alkylisothiouronium halides and alcohols of C5-C8 fractions, as well as kerosene, benzene, toluene and xylols used as diluents. Used as s-alkylisothiouronium halides are chlorides, bromides and iodides from C7 to C14 and their fractions.

EFFECT: extended range of reagents and inert diluents.

2 cl, 2 ex

 

The invention relates to the determination of palladium and platinum ores containing large amounts of iron, copper, zinc and other metals by atomic absorption spectrometry with electrothermal atomization.

There is a method of determining the content of palladium and platinum ores, including their translation into solution, for example, by decomposition in Aqua Regia, evaporation and dissolution in hydrochloric acid and further determination by atomic absorption spectrometry with electrothermal atomization (Ginzburg SR and other Guidance on chemical analysis of platinum metals and gold. M., Nauka, 1965, p.205, 272-273).

The closest analogue to the present invention is a method of determination of palladium and platinum ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and the content of platinum in hydrochloric acid phase. As extractant used undecalactone chloride in a mixture of toluene and isoamyl alcohol in the ratio of 80% and 20%, and the concentration of the extractant 0,5-2,5% (RF patent No. 2226224, With 22 In 4/03, 2004).

Lack of oksanapopova is the limited range of extractants and inert diluents (mixture of toluene and ISO-amyl alcohol).

An object of the invention is the expansion of the range of extractants and inert diluents.

The technical result is achieved in that in the method of determining the content of palladium and platinum ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction with an extractant in an inert diluent, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and platinum in hydrochloric acid phase, as extractants used s-alkalization halides from C7to C14(chlorides, bromides, iodides), and as an inert diluent - alcohols fraction5-C8and kerosene, benzene, toluene, xylenes.

The method is as follows. The sample at 1-2 grams pour a mixture of 10 ml HF and 1 ml of nitric acid, the solution evaporated at 160-200°to wet salts, the remainder of the double-pour 15 ml of Aqua Regia and both times evaporated to moist salts at the same temperature. Then the residue is dissolved in 4 M hydrochloric acid, transferred to a flask and bring to the mark with hydrochloric acid. Then spend the extraction of palladium from hydrochloric acid solution. The volume of solenoidoperated palladium is mixed with an equal volume of extractant solution in an inert diluent. Stirred or shaken, after which the mixture is allowed to stand for 0.5 to 2 hours, after which the organic phase define palladium, and from hydrochloric phase - platinum by atomic absorption spectrometry with electrothermal atomization "quantum-Z.". As extractants used s-alkalization halides from C7to C14or their fractions. As inert diluents used alcohols fraction C5-C8(amyl, hexyl, p), as well as kerosene, benzene, toluene, xylenes or mixtures thereof.

When using s-alkalization halides from hydrocarbon radical, a smaller 7 decreases their solubility in the inert diluent and they are poorly extracted precious metals from hydrochloric acid solution. S-alkalization halides from hydrocarbon radical, a large 14, reduced solubility in hydrochloric acid solution, and this also leads to deterioration of the extraction of noble metals from solutions.

The invention is illustrated by examples.

Example 1. Carry out analysis of samples No. 4330-2 (depth 284,8-287,3 m, composition: carbon slate with striated silicification, the content of graphite 7-20%). A sample of 1.2 grams treated with acid, then with 5 ml of hydrochloric acid solution is extracted with palladium 2% solution of s-captilization chloride in 5 ml Attila is on alcohol. The concentration of palladium on the peak of 50.2 ág/l, the integral of 50.2 ág/L. Data without extraction: peak 27,1 µg/l, the integral 28.5 ug/l

Example 2. Carry out analysis of samples No. 33035 (depth 270,6-271,8 m, composition: carbonaceous shale with pyrite content to 20%, the content of graphite 7-20%). 1.8 g of the sample is treated with acid, then with 5 ml of hydrochloric acid solution is extracted with platinum a 2.5% solution of s-tetradecylammonium chloride. From hydrochloric acid solution determine platinum. The value of concentration: peak of 11.6 µg/l, the integral of 12.2 ág/L. Data analysis without extraction: at the peak of 29.4 ág/l is integral to 26.2 ág/L.

1. The method of determining the content of platinum and palladium in ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction with an extractant in an inert diluent, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and platinum in hydrochloric acid phase, characterized in that as extractants for the extraction using s-alkalization halides from hydrocarbon radical from C7to C14or their fractions, as well as inert solvents - alcohols fraction C5-C8and kerosene, benzene, toluene, xylenes./p>

2. The method according to claim 1, characterized in that as s-alkalization halides using chlorides, bromides, iodides.



 

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