GOST 23859.11-90

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  ГОСТ 23859.11-90

GOST 23859.11−90 in Bronze heat resistant. Determination of chromium, Nickel, cobalt, iron, zinc, magnesium and titanium by method of atomic absorption spectrometry

GOST 23859.11−90

Group B59

INTERSTATE STANDARD

BRONZE HIGH-TEMPERATURE

Determination of chromium, Nickel, cobalt, iron, zinc, magnesium and titanium by method of atomic absorption spectrometry

Heat-resistant bronze. Determination of chromium, nickel, cobalt, iron, zinc, magnesium
and titanium by method of atomic-absorption spectrometry

AXTU 1709

Date of introduction 1991−07−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 30.03.90 N 726

3. REPLACE GOST 23859.11−79

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)

6. REISSUE


This standard establishes the method of atomic absorption spectrometry for determination of chromium, Nickel, cobalt, iron, zinc, magnesium and titanium in the heat-resistant bronze.

The method is designed to determine the major components and impurities in the high-temperature bronzes in the following ranges of mass fraction, %:

chrome from 0.1 to 1.3;

Nickel from 0.005 to 0.9 and 2.0 to 3.0;

cobalt, from 0.1 to 2.0;

iron from 0.005 to 0.08;

zinc — 0.0008 to 0.03;

magnesium — from 0.0005 to 0.06;

Titan — from 0.02 to 0.09, and from 0.5 to 2.0.

The method is based on measuring the absorption of light by atoms of elements formed during the introduction of the analyzed solution in the flame acetylene-air or acetylene — nitrous oxide.

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 25086 with the addition of a GOST 23859.1 in sect.1.

2. EQUIPMENT, REAGENTS, SOLUTIONS

The atomic absorption spectrometer.

Lamp with a hollow cathode, or other sources of resonance radiation.

Nitric acid according to GOST 4461 and diluted 1:1.

Hydrochloric acid according to GOST 3118.

Sulfuric acid according to GOST 4204, diluted 1:1, 1:4 and 1:10.

Hydrofluoric acid according to GOST 10484.

Acetylene according to GOST 5457.

Nitrous oxide according to GOST 9293.

Copper according to the GOST 859.

Standard copper solution: 10 g of copper was dissolved with heating in 80 cmof nitric acid (1:1). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof the solution contains 0.1 g of copper.

Chrome sulfate according to GOST 4472.

Standard solutions of chromium

Solution a: 0,481 g of chromium sulfate was dissolved with heating in 20 cmof sulphuric acid (1:4). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof the solution contains 0.001 g of chromium.

Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof a solution contains 0.0001 g of chromium.

Nickel GOST 849.

Standard solutions of Nickel

Solution a: 1 g of Nickel is dissolved by heating in 20 cmof nitric acid (1:1). The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand top up with water to the mark.

1 cmof the solution contains 0.001 g of Nickel.

Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water.

1 cmof a solution contains 0.0001 g of Nickel.

Cobalt GOST 123.

Standard solutions of cobalt

Solution a: 1 g of cobalt is dissolved by heating in 20 cmof nitric acid (1:1). The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand topped to the mark with water.

1 cmof the solution contains 0.001 g of cobalt.

Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof a solution contains 0.0001 g of cobalt.

Iron carbonyl or the State standard sample 666−81 type 1.

Standard iron solution

Solution a: 1 g of iron was dissolved with heating in 20 cmof nitric acid (1:1). The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand top up with water to the mark.

1 cmof the solution contains 0.001 g of iron.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof a solution contains 0.0001 g of iron.

Zinc GOST 3640.

Standard solutions of zinc

Solution a: 0.1 g of zinc is dissolved by heating in 10 cmof nitric acid (1:1). The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand top up with water to the mark.

1 cmof the solution contains 0.0001 g of zinc.

Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof solution B contains 0,00001 g of zinc.

Magnesium GOST 804.

Standard solutions of magnesium

Solution a: 0.1 g of magnesium are dissolved in 10 cmof nitric acid (1:1). The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand top up with water to the mark.

1 cmof the solution contains 0.0001 g of magnesium.

Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cmand top up with water to the mark.

1 cmof solution B has the 0.00001 g of magnesium.

The titanium metal.

Standard solutions of titanium

Solution a: 1 g of the titanium is dissolved by heating in 50 cmof sulphuric acid (1:4). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cmand top up with sulphuric acid (1:10) to the mark.

1 cmof solution A contains 0.01 g of titanium.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cmand top up with sulphuric acid (1:10) to the mark.

1 cmof the solution contains 0.001 g of titanium.

3. ANALYSIS

3.1. Used sample alloys is given in table.1.

Table 1

3.2. A portion of the alloy (see table.1) is placed in a platinum Cup and dissolve by heating in 10−30 cmof nitric acid (1:1) and 1−3 cmhydrofluoric acid. The Cup is cooled, poured 10 cmof sulphuric acid (1:1) and removed prior to the allocation of thick white smoke of sulfuric acid. Cup cooled and the residue is dissolved in 50 cmof water when heated. The solution was cooled, transferred to a volumetric flask (see table 1) and top up with water to the mark. At the same time conducting follow-up experience with all applicable acids.

3.3. Preparation of the calibration solutions

In the preparation of the calibration solutions injected solution element, which is determined in the sample.

In a volumetric flask with a capacity of up to 100 cmis placed aliquote volumes of standard solutions of the elements listed in table.2 add 10 cmsulphuric acid (1:1). If the weight is 0.5; 2 or 3 g, then all flasks add 5, 20, or 30 cmof a standard solution of copper and topped to the mark with water.

Table 2

3.4. Measure the atomic absorption of the elements in solutions of the analyzed alloys and in the calibration solutions, recording the analytical signals. Chromium, Nickel, cobalt, iron, zinc, and magnesium is determined in the flame acetylene-air, titanium — flame acetylene — nitrous oxide, use the analytical lines given in table.3. According to the obtained values build the calibration graphs.

Table 3

4. PROCESSING OF THE RESULTS

4.1. Mass fraction of element (a) in percent is calculated by the formula

,

where is the concentration of element in the analyzed solution alloy, was found in the calibration schedule, g/cm;

is the concentration of element in solution in the reference experiment, was found in the calibration schedule, g/cm;

 — the volume of the analyzed solution, cm;

 — weight alloy, g

.

4.2. Discrepancies in the results of three parallel definitions should not exceed the values permitted by the divergence (the rate of convergence), calculated by the formula:

(for the interval of 0.0005−0,005%);

(for the interval 0,005−0,05%);

(for the interval 0,05−0,5%);

(for the interval of 0.5−3%),

where  — mass fraction of element in alloy, %.

4.3. Discrepancies in the results analysis, obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values calculated by the formulae:

(for the interval of 0.0005−0,005%);

(for the interval 0,005−0,05%);

* (for the interval from 0.05 to 0.5%).

________________
* Formula conforms to the original. — Note the CODE.

(for the interval of 0.5−3%),

where  — mass fraction of element in alloy, %.

4.4. Control of accuracy of analysis results is carried out according to State standard samples of heat-resistant (CR) bronze or supplements method, or comparison of results obtained by other methods in accordance with GOST 25086.