SU1423945A1 - Method of analyzing metallic iron, nickel and cobalt in presence of their sulfides and oxides - Google Patents

Abstract

The invention relates to analytical chemistry and allows simultaneous conversion of iron, nickel, cobalt and copper into the solution in the presence of their sulfides and oxides. The method involves transfer of metals into the solution by treatment with a selective solvent containing (wt.%) 4.5-5.5 ammonium citrate; 2.0-3.0 iodine; 0.9 - 1.5 hydrochloric acid and water - the rest. 3 tab.

Description

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The invention relates to analytical chemistry, namely to phase analysis of products of non-ferrous and ferrous metallurgy containing sulphides and oxides in addition to metals.

The aim of the invention is to simultaneously determine metallic copper and increase the dissolution selectivity.

Example 1. The definition of metals in the standard sample of the magnetic fraction containing, in wt.%: Iron 8.4; Nickel 73.7; cobalt tp2 copper 12, as well as iron sulfides,

copper (I) and nickel.

A sample of the sample (0.1 g) is placed in a conical flask with a capacity of 250 ml, poured 20 ml of a solution containing, wt.%: Ammonium citrate 5; iodine 2.5; hydrochloric acid 1.2. The flask is closed with a stopper, fixed on a shaker, shaken at a rate of 200 oscillations per minute for 1 hour, filtered through a filter paper, washed 3 times with the same solvent, then with room temperature water until there are no iodine traces on the filter.

About 5 ml of nitric acid (density 1.4) are added to the filtrate. The solution is gently heated to remove NIN-iodine. 5 ml of sulfuric acid (1: 1) are added to the clarified solution and heated to sulfur trioxide vapor to precipitate by adding nitric acid to burn the organics. Evaporation was repeated with water until almost dry. 40 ml of a 1% solution of hydrochloric acid are added, - boil - until the precipitate is completely dissolved. Next, iron, nickel i cobalt and copper are determined by atomic absorption spectroscopy.

The results of the analysis are presented in table 1.

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Example 2. Analysis of Feinstein containing, wt.%: Iron 2,2; nickel 13.7; copper 19.2; cobalt 1.27, also nickel, copper and iron sulfides.

A sample of the sample is placed in a conical flask with a capacity of 250 mp, poured 20 ml of a solution containing, wt.% Ammonium citrate 4.5; iodine 2j hydrochloric acid 0.9 - and atalized as described in example 1.

The results of the analysis are presented in table 1.

Example 3 Analysis of metals of the e magnetic fraction containing ,, wt.%: Iron 1,9} nickel 16,2; cobalt 0.50; copper 1.8, as well as sulfides of iron, nickel and copper and iron oxide.

A sample of the sample is placed in a flask, poured 20 ml of a solution containing, wt.%: Ammonium citrate 5.5; iodine 3.0; hydrochloric acid 1.5.

The results of the determination are presented in Table 1.

Table 1

18,073,11,20 12,7

22,011,11,44 19,0

31.8 16,20,56 2,0

Table 2 presents data on the effect of the quantitative composition of the reagent on the results of the analysis of a metal alloy.

table 2

Table 3 presents comparative ™ data on the dissolution of the alloy by known and described methods.

Table 3

Mass fraction of metal,% Fe I Ni Co Cu

Standard sample

8.473.2 1.20 12.7 Defined in a known manner

8.575.4 1.33 Defined by the proposed method

7.4 73.2 1.10 13.4

Note. The sample is a magnetic fraction.

As can be seen from table 3, the results. determination of metals by a known method due to partial dissolution of sulphides.

Claims (1)

Invention Formula Method for determination of metallic iron, nickel and cobalt in the presence of their sulfides, and oxides, including the transfer of metals into solution by treatment with a selective solvent containing iodine, hydrochloric acid and water, so that, in order to increase the dissolution selectivity and simultaneously transfer metallic copper into the solution, the solvent additionally contains ammonium citrate in the following ratio of components, wt.%; Iodine. 2.0-3.0 Salt on acid 0.9-1.5 Ammonium citrate 4.5-5.5 VodyEstalny