The method of determining the content of palladium and platinum ores

 

The invention relates to methods for determination of palladium and platinum ores containing large amounts of iron, copper, zinc and other metals. The technical result of the invention is to improve the accuracy of analysis of the content of palladium and platinum ores. For this purpose, the method including the decomposition of the Royal vodka, evaporation, dissolution in hydrochloric acid to obtain hydrochloric acid solution and determination of metal content by atomic absorption spectrometry with electrothermal atomization, before the decomposition of the Royal vodka conduct the decomposition of the ore hydrofluoric and nitric acids. The solution is evaporated to moist salts, the resulting solution was subjected to extraction using as extractant 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%, followed by agitation, settling the mixture for half an hour. The determination of the content of palladium is carried out in the organic phase, and the content of platinum in hydrochloric acid solution. 2 Il.

The invention relates to the determination of palladium and platinum ores containing large amounts of iron, copper, zinc, and d is the procedure of determining the content of palladium, platinum, rhodium by atomic absorption spectrometry after preconcentration on the sorbent (Stanisenko E. B., Kubrakov Century. And. and others - Journal of analytical chemistry, 1995, T. 50, S. 1243-1246).

The closest analogue to the present invention 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 and S. I. and other Guidance on chemical analysis of platinum metals and gold. - M.: Nauka, 1965, S. 205, 272-273).

The disadvantage of these methods is the low accuracy of the analysis, due to the high ionic strength of the solution, the influence of background, the mutual influence of the platinum metals on the individual determination of each of them.

The technical result of the invention is to improve the accuracy and sensitivity of the analysis through selection and concentration.

The technical result is achieved by the fact that according to the method of determining the content of palladium and platinum ores, including the decomposition of the Royal vodka, evaporation, dissolution in hydrochloric acid with polycrystallites atomization, before the decomposition of the Royal vodka conduct the decomposition of the ore hydrofluoric and nitric acids and evaporation to wet salts, the resulting solution was subjected to extraction using as extractant 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%, followed by agitation, 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.

The method is as follows. The sample in the amount of 1-2 g pour a mixture of 10 ml of hydrofluoric acid and 1 ml of nitric acid, the solution evaporated at a temperature of 160-200To moist 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 hold the extraction of palladium from hydrochloric acid solution, the volume of solution is mixed with an equal volume of extractant solution. As extractant used undecalactone chloride in a mixture of toluene and ISO-amyl alcohol (toluene 80%, isoamyl is that in the organic phase define palladium, in hydrochloric acid platinum by atomic absorption spectrometry with electrothermal atomization.

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 (1 g pour a mixture of 10 ml of hydrofluoric acid and 1 ml of nitric acid, the solution evaporated at a temperature of 160-200To moist 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. Spend the extraction of palladium from hydrochloric acid solution, the volume of solution is mixed with an equal volume of extractant solution. As extractant used undecalactone chloride in a mixture of toluene and ISO-amyl alcohol (toluene 80%, isoamylase alcohol 20%), the concentration of the extractant 0,5-2,5%. The solution is shaken out, after which the mixture is allowed to stand for half an hour, then into the organic phase define palladium, platinum in hydrochloric acid by the method of atomic absorption spectrometry with electrothermal atomizzatori time and atomization in the determination of palladium without extraction, a in Fig.1B - after extraction.

Data without extraction: peak 27,28 g/l, the integral on 20, 23 g/L. Peak And the curve appears before the atomization of certain elements. The accuracy of the analysis is reduced due to the influence of the background.

Data after extraction (Fig.1B): the concentration peak of 51 g/l, the integral of 51 g/l Is pronounced peak at the point of atomization of the designated elements of the sample.

Example 2. Analyze samples No. 33035 (depth 270,6-271,8 m, composition: carbonaceous shale with pyrite content to 20%, the content of graphite 7-20%). A sample of 2 g pour a mixture of 10 ml of hydrofluoric acid and 1 ml of nitric acid, the solution evaporated at a temperature of 160-200To moist 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. Spend the extraction of palladium from hydrochloric acid solution, the volume of solution is mixed with an equal volume of extractant solution. As extractant used undecalactone chloride in a mixture of toluene and ISO-amyl alcohol (toluene 80%, isoamylase alcohol 20%), the concentration extraradical palladium, in hydrochloric acid - platinum by atomic absorption spectrometry with electrothermal atomization.

The essence of the example illustrated in Fig.2A, which shows the dependence of the absorption intensity on temperature and time of atomization when determining the content of platinum without extraction, and Fig.2B is the same after extraction.

Data analysis without extraction: value: concentration: peak 29,83 g/l, the integral 26,14 g/L. Peak And give atomserver impurities in the sample, which leads to a dramatic overestimation of the defined values.

Data analysis after extraction: value: concentration: peak 11,54 g/l is integral to 12.0 g/l Peak And the background level.

Claims

The method of determining the content of palladium and platinum ores, including the decomposition of the Royal vodka, evaporation, dissolution in hydrochloric acid to obtain hydrochloric acid solution and determination of metal content by atomic absorption spectrometry with electrothermal atomization, characterized in that before the decomposition of the Royal vodka conduct the decomposition of the ore hydrofluoric and nitric acids and evaporation to wet salts, the resulting solution was subjected to extraction using cachesentry extractant 0,5-2,5%, followed by agitation, by 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.

 

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