SU1083107A1 - Method of phase analysis of antimony compounds in ores and products processed thereof - Google Patents

Abstract

METHOD FOR PHASE ANALYSIS CONNECTED antimony in ores and products comprising treating the initial sample with selective solvents for dissolving valentinita, stibnite and jamesonite and subsequent quantification of antimony in the selected phases by known methods, characterized in that, in order povsheni reproducibility determining monomineral forms antimony from one sample, a solution of hydrofluoric acid is used as selective solvents. 1: 20-25 for Valentinite and sulphide, 0.10-0.15 Mra sodium hydroxide saturated with sodium fluoride for antimonite and sulphide, and a dilute solution of nitric acid for jamsonite. (L

Description

The invention relates to analytical chemistry, in particular to methods for determining antimony compounds in ore and can be used in phase analysis of antimony ores, including. gems and their products, for geochemical studies and process control. The known method of determining various mineral forms of antimony in pyro-metaplastic products by sequential processing of the initial sample in a solution of hydrochloric acid in a carbon dioxide atmosphere is used to dilute valentine, in a solution of hydrochloric acid containing a 5% solution of hydrogen peroxide; antimony, in a solution of sodium carbonate - to dissolve higher antimony oxides and the subsequent quantitative determination of antimony in the separated phases by the known methods t J. However, the known method is is activated by a low accuracy; when the metal antimony dissolves, the antimonite antimony partially dissolves (up to 30%) 5 and when dissolved, the valentinite dissolves and the antimonite. Furthermore, this method does not allow the use of Jamsonite antimony. The closest in technical essence and the achieved result to the proposed method is the phase analysis of antimony compounds in ores and products from processing, which includes processing the initial sample with selective solvents: tartaric acid solution, sodium hydroxide solution containing glycerin. and a solution of hydrochloric acid containing hydrogen peroxide, for the sequential dissolution of Valentinite, antimonite and jamsonite. From the second sample, the amount of nalentinite and antimonite is determined by dissolving sodium hydroxide containing glycerol C2 in a solution. However, the known method is characterized by a low reproducibility of the analysis of valentine with its low contents (below 0.01%). Unstable dissolution of oxidized antimony compounds will also lead to errors. In addition, it is difficult to determine antimony in the presence of glycerol. The purpose of the invention is to increase the reproducibility of the determination of monomineral forms of antimony. This goal is achieved by the fact that according to the method of phase analysis of antimony compounds in ores and products of their processing, including the treatment of the initial sample with selective solvents for the solution of valenite, antimonite and jozhsonite and the subsequent quantitative determination of antimony in the separated phases by known methods, use selective solution as selective solvents hydrofluoric acid 1; 20-20 for valentine and sulfide, 010-0.15 M solution of sodium hydroxide saturated with sodium fluoride, for antimonite and sulfide and a dilute solution of nitric acid - for jamsonite. Table 1 presents data on the solubility of valentinite in dilute hydrofluoric acid. Table 1

From the data of table 1 it follows that the most

more effective dissolution of valentini-55 studying the effect of caustic concentration

This is observed in the case of treatment of the soda in solution for the effectiveness

a dilute solution of fluoride antimonite and sulfide

hydrogen acid in the range of 1-20: 25 antimony.

89.3

99.2

97.3 99.4

As follows from the data of Table 2, the optimal concentration of caustic soda is its 0.10-0, 15 M solution. Connection Antimony extraction,%, at antimony

99.2

92.7 99.4 99.1 From the data of Table 3 it follows that the most effective antimonite solvent is 0.10-0.15 M sodium hydroxide solution, saturated with sodium fluoride. The most complete release of jamsonite occurs when using a solution of nitric acid with a concentration of 1-2: 1. The use of nitric: acid with a concentration higher than 2: 1 is difficult when working with high concentrations. Example 1.0.1 The ores are placed in a 100 ml beaker, 50 ml of hydrofluoric acid 1:20 are added, stirred for 10 minutes and filtered. The filtrate is used to quantify valentine and antimony sulfide (Y). To do this, 10 ml of 10 M sulfuric acid is added to the filtrate and evaporated to smoke the vapors of sulfuric anhydride. In the sulphate solution, the antimony of valentinite and sulfide is determined.

table 2

.96.1

95.7

99.6 99.0

Table 3 presents the results on the effect of sodium fluoride concentration in the sodium hydroxide solution on the solvent of antimonite and sulfide.

Table 3

83,8

81.8 94.3 95.1 Concentration of sodium fluoride antimony (V) by the bromatometric method and the extraction-photometric method using ethyl rdamin C. The content of Valentinite is 0, 22%. The insoluble residue after dissolution of the sample is used to determine antimonite and antimony sulfide (U). Dp of this residue is transferred to a conical flask with a capacity of 100-150 mp, 50 ml of 0.1 M sodium hydroxide solution, saturated with sodium fluoride, are poured in and stirred on a mechanical stirrer for two hours. The undissolved residue is filtered off. 10 ml of YuM sulfuric acid is poured into the filtrate and evaporated to sulfuric anhydride vapor. Antimonite antimony and antimony sulfide (V) are determined in a sulphate solution by bromatometric and extraction-photometric methods using ethyl rodamine C. The antimonite content is 1.07%.

The insoluble residue after treatment with a composite solution (0.1 M sodium hydroxide, saturated with sodium fluoride) is transferred to a 250 MP beaker, 50 ml of Is 1 nitric acid is poured in and stirred for one hour. The insoluble residue is filtered off and 10 ml of YuM sulfuric acid is added to the filtrate, evaporated to smoke the sulfuric anhydride vapor. In sulphate solution, jamsonite antimony is determined by extraction-photometric method using ethyl rhodamine C, Jamsonite is absent.

The undissolved residue after treatment with 1: 1 nitric acid, together with the filters, is dried at room temperature and slowly heated in a muffle furnace at 500-550 ° C. The calcined residue is determined by the amount of higher antimony oxides using an ethyl photo-amine C. The content of pentoxide is em 0.10%. Example 2. 0.1 g Jamsonito 25

The ore is poured into a beaker, 50 ml of hydrofluoric acid 1:23 is poured in, stirred and filtered. In the filtrate, valentine and sulfide are determined as indicated in Example 1. The content of valentine is 0.11%. The insoluble residue is treated with 50 ml of 0.13 M sodium hydroxide solution, saturated with sodium fluoride, and stirred for two hours. The antimonite and antimony sulfide antimony are detected in the filtrate and the antimony is determined. The content of antimonite composition61, 001,071,24 ches ore t 50,160,170,82 Sulphide 90,720,701,03 Jemsonito ore 42, 082,101,70 va ore 43,603,722,06

It is 2.10%. The insoluble residue is transferred to a beaker, 50 ml of 1.5-1 nitric acid are added and stirred for one hour. The filtrate is filtered and the Jamsonite antimony is determined in the filtrate. Jamsonite content is 6.80%. The residue is dried and ash. In the calcined residue, the antimony of the higher oxides is determined. Pentoxide is absent.

Example 3. About 5 g of cubic ore is placed in a glass, 50 ml of hydrofluoric acid 1:25 are poured in, stirred and filtered. In the filtrate, the valentinite is determined as described in Example 1. The content of valentinite is 0.19%. The undissolved residue is treated with 50 ml of a 0.15 M sodium hydroxide solution, HacbmjeHHoro is sodium fluoride, and stirred for 2 hours. The antimonite and antimony sulfide are determined in the filtrate and determined. The antimonite content is 0.70%.

and zotic acid 2; 1 and stirred for 1 h. After filtration in the filtrate, the antimony of jamsonite is determined as in example 1. No jamsonite was detected. The residue is dried, ash, and the antimony of the higher oxides is determined in it, as in Example 1. The content of pentoxide is 0.10%.

Table 4 shows the results of the phase analysis of antimony in the ores by the proposed method in comparison with the known. The residue is transferred to a beaker, tide 2,080,240,241,121,66 1,030,070,060,770,96 2,360,160,190,911,10 3,300,100,110,820,97 3,150,360,401,461,73

As can be seen from Table 4, the proposed method is more), THEREFORE, the way of characterization allows to increase the reproduction of a smaller scatter of the range of determination of various mono-recurrences of single measurable forms of antimony (accuracy margin YO: -NI.

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Claims (1)

METHOD FOR PHASE ANALYSIS OF ANTIMONY COMPOUNDS IN ORES AND PRODUCTS OF THEIR PROCESSING, including processing the initial sample with selective solvents for dissolving valentinite, antimonite and jamsonite and subsequent quantitative determination of antimony in the separated phases by known methods, characterized in that, in order to increase the reproducibility of determination one weighed sample, a solution of hydrofluoric acid is used as selective solvents .1: 20-25 for valentinite and sulfide, 0.10-0.15 M solution sodium idroksida saturated sodium fluoride for antimonite and sulfide, and the diluted nitric acid solution - for jamesonite. SU „„ 1083107