GOST 9853.18-96

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  ГОСТ 9853.18-96

GOST 9853.18−96 Titan spongy. Method of determination of manganese

GOST 9853.18−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Method of determination of manganese

Sponge titanium. Method for determination of manganese

ISS 77.120
AXTU 1709

Date of introduction 2000−07−01

Preface

1 DEVELOPED by the Interstate technical Committee for standardization MTK 105, Ukrainian research and design Institute of titanium

SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 9 dated April 12, 1996)

The adoption voted:

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated 19 October 1999 No. 353-St inter-state standard GOST 9853.18−96 introduced directly as state standard of the Russian Federation from July 1, 2000.

4 INTRODUCED FOR THE FIRST TIME

1 Scope

This standard sets the photometric method for the determination of manganese in spongy titanium (with mass fraction of manganese from 0.0005% to 0.1%) according to GOST 17746.

The method is based on dissolving the sample in sulfuric acid, the oxidation of manganese to manganese-acid potassium Iodate (sodium) and subsequent measurement of optical density of the solution.

2 Normative references

The present standard features references to the following standards:

GOST 8.315−97 State system for ensuring the uniformity of measurements. The standard samples. The main provisions, the order of development, certification, approval, registration and application

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 6008−90 metallic Manganese and nitrated manganese. Specifications

GOST 10929−76 Hydrogen peroxide. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 17746−96 spongy Titanium. Specifications

GOST 23780−96 spongy Titanium. Methods of sampling and sample preparation

GOST 25086−87 non-ferrous metals and their alloys. General requirements for methods of analysis

3 General requirements

3.1 General requirements for the method of analysis according to GOST 25086.

3.2 Selection and preparation of samples is carried out according to GOST 23780.

3.3 Mass fraction of manganese is determined in two batches.

3.4 the construction of calibration curve, each calibration point is based on the average of the results of the two measurements.

4 measuring instruments and auxiliary devices

Spectrophotometer type SF-46 or photoelectric concentration colorimeter or similar device.

Sulfuric acid according to GOST 4204, concentrated, and diluted 1:1 and 2:5.

Nitric acid according to GOST 4461, diluted 1:3 and 1:4.

Hydrochloric acid (hydrochloric) according to GOST 14261.

Hydrogen peroxide according to GOST 10929, diluted 1:1, and the solution of the mass concentration of 100 g/DM.

Potassium permanganate (potassium permanganate), standard-titer according to the current normative document.

Sodium Iodate (sodium jednotky) metallisticheskoy according to the current normative document, solution mass concentration of 50 g/lprepared: 25 grams of sodium Iodate are dissolved in 400 cmof hot nitric acid (1:4), cooled and diluted to 500 cmsolution of nitric acid.

Manganese metal according to GOST 6008.

Standard samples according to GOST 8.315.

Standard solutions of manganese.

Solution a: potassium permanganate solution of molar concentration of 0.02 mol/DM, made with standard-titre (fixanal), transferred into a measuring flask with volume capacity of 1000 cm, flow 10 cmof sulphuric acid diluted 1:1, and dropwise added a solution of hydrogen peroxide (1:1), with continuous stirring to the bleaching solution, made up to the mark with water and mix.

1 cmof solution A contains 0.0011 g of manganese.

Solution a': 1,1 g of metallic manganese is dissolved by heating in 20 cmof hydrochloric acid, carefully added dropwise 1−2 cmof nitric acid and boil to remove oxides of nitrogen. The solution is transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmof solution A containing 0.0011 g of manganese.

Solution B: 2 cmof solution A is placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

1 cmof solution B contains 0,000022 g of manganese.

5 procedures for measuring

5.1 a sample mass of 0.1−1.0 g are placed in two glasses with a capacity of 100 cm, 45 cm pouredsulphuric acid, diluted 2:5, cover with a watch glass or glass funnel and dissolved by heating.

Upon completion of the dissolution of the sample in the solution was dropwise added a solution of hydrogen peroxide to the disappearance of a purple color, then the solution is evaporated until fumes of sulphuric anhydride. The solution was cooled, poured 15 cmwater 7 cmof nitric acid, diluted 1:3 in one of the glasses is administered 15 cmof a solution of Iodate of sodium (or about 0.5 g of dry crystal) and boiled for 10 min. the Solution was cooled, transferred to a volumetric flask with a capacity of 50 cm, made up to the mark with water and mix. After 15 min measure the optical density of the solution at a wavelength of 530 nm and the thickness of the absorbing layer is 50 mm.

Solution comparison is the sample solution without the addition of sodium Iodate (potassium).

5.2 For constructing the calibration curve in seven of the eight glasses with a capacity of 100 cmplaced 0,2; 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 cmstandard solution B, which corresponds to 0,0000044; 0,000011; 0,000022; 0,000044; 0,000066; 0,000088; 0,00011 g of manganese.

A seventh solution of the flask is a solution of the control experience and is solution comparisons.

All glasses poured 12 cmof sulfuric acid solution, diluted 2:5 add 15 cmof water, 7 cmof nitric acid (1:3) and heated to boiling. Then do as specified in 5.1.

6 Processing of measurement results

Mass fraction of manganese , %, is calculated by the formula

, (1)

where is the mass of manganese in the sample solution found by the calibration schedule g;

 — the weight of the portion,

7 the Permissible error of measurement

7.1 the Difference between the two measurements and analysis results (at a confidence probability of 0.95) shall not exceed the permissible values given in table 1.

Table 1

Percentage

7.2 accuracy Control of the results of the analysis carried out according to standard sample in accordance with GOST 25086.

Control the accuracy of the results of the analysis carried out by the method of additives in accordance with GOST 25086.

Additives is a standard solution And'.

8 qualifications

To perform analysis allowed the analyst qualification not less than 4th level.