GOST 12645.1-77

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  ГОСТ 12645.1-77

GOST 12645.1−77 indium. Spectral method for the determination of gallium, iron, copper, Nickel, tin, lead, thallium and zinc (with Amendments No. 1, 2, 3)

GOST 12645.1−77

Group B59

STATE STANDARD OF THE USSR

INDIUM

Spectral method for the determination of gallium, iron, copper, Nickel,
tin, lead, thallium and zinc

Indium. Spectral method for determination of gallium, iron, copper,
nickel, tin, lead, thallium and zinc

AXTU 1709

Date of introduction 1978−07−01

INFORMATION DATA

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

DEVELOPERS

A. P. Sychev, L. K. Larina (supervisor), M. G. Saun (supervisor), V. N. Makarceva, N. With. References: E. V. Lisitsyn, N. Romanenko, V. A. Kolesnikov

2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from 08.07.77 N 1715

Change No. 3 adopted by the Interstate Council for standardization, Metrology and certification 15.03.94 (report of the Technical Secretariat N 1)

The adoption voted:

3. REPLACE GOST 12645.67 in part of sec. 1

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)

6. REVISED (March 1998) with Amendments No. 1, 2, 3, approved in February 1983, December 1987-June 1996 (IUS 5−83, 3−88, 9−96)


This standard establishes a spectral method for the determination of gallium, iron, copper, Nickel, tin, lead, thallium and zinc in India to mass fractions in percent:

gallium from 0.0001 to 0.005;

— iron from 0.0001 to 0.01;

— copper from 0.0001 to 0.002;

— Nickel from 0,00007 to 0.005;

— tin from 0.0001 to 0.01;

— lead from 0.0002 to 0.01;

of thallium from 0.0001 to 0.005;

— zinc from 0.003 to 0.01.

Determination of impurities in India is carried out by the method of «three standards» with the evaporation of impurities from a crater of the carbon electrode in the arc DC.

Before analysis the sample is transferred into the oxide by dissolving in nitric acid and calcining in a muffle furnace at 400−500 °C for 30−40 min until complete removal of nitrogen oxides. When determining the content of thallium in a sample of the oxide is not transferred.

(Changed edition, Rev. N 1, 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis and security requirements — according to GOST and GOST 22306 12645.0.

(Changed edition, Rev. N 2).

2. APPARATUS, REAGENTS AND MATERIALS

The diffraction type spectrograph DFS-8 with a being system of the slit illumination and a three-stage attenuator (first order).

A constant current source providing the voltage to 200 V and currents up to 20 A, type PN-145, 2ВН-20 etc.

Arc generator types of PS-39, DG-2 or IVS-28 with an external resistor for operation at power current 15 A.

Microphotometer designed to measure pucherani spectral lines.

Muffle furnace with temperature up to 600 °C.

Libra torsion bar type W with a weighing error of no more than 0.001 g.

Analytical scale with a weighing error of no more than 0,0002 g.

Quartz apparatus for the distillation of reagents.

Box of organic glass.

The infrared lamp of any type with laboratory auto-transformer type CTL-250−2.

The hotplate.

Indium brand Ин000 according to GOST 10297.

Mortar made of organic glass.

Quartz tableware (glasses, cups, etc.) according to GOST 19908.

Distilled water according to GOST 6709, distilled or purified on a column of ionization.

Nitric acid according to GOST 4461 or double-distilled nitric acid of high purity according to GOST 11125.

The technical rectified ethyl alcohol according to GOST 18300.

Electrodes of graphite rods-2 high purity with a diameter of 6 mm and crater depth of 6 mm and a hole diameter of 4 mm.

Photographic plates «spectrographic» types SFC-02, the SFC-03, NT-2 SV.

Samples comparison. The basis for the preparation of samples of comparison is indium oxide. Prepare the Foundation in the following way. Indium metal brand Ин000 dissolved in nitric acid. The resulting solution was evaporated to dryness and the dry residue is calcined first on a hotplate and then in a muffle furnace at 400−500 °C to stop the allocation of vapors of oxides of nitrogen (30−40 min). You must completely remove the oxides of nitrogen, as their presence in the basis increases the background in the spectra, which distorts the results of the analysis.

The basic pattern is prepared nakapyvaniem the basis of solutions of impurity elements (table.1), prepared according with Appendix 1 GOST 12645.4.

The sample is dried on a hotplate, and then calcined in a muffle furnace at a temperature of 300 °C for 30 min, grind in a mortar. By diluting the primary and the newly prepared samples the basis for preparing a series of samples of comparison workers in accordance with the table.2. Prepared samples and a basis stored in buksh or jars with lids.

Note. Allowed the use of devices with photovoltaic spectra and other spectral instruments, other reagents and materials, providing the accuracy that rivals regulated in this standard.

(Changed edition, Rev. N 1, 2, 3).

Table 1

Table 2

3. ANALYSIS

3.1. A sample of metallic indium was transferred to the oxide, as described in sec. 2.

3.2. The source of spectra excitation is DC-arc 15 A power between vertical carbon electrodes. Samples comparison 60 mg placed in the deepening of a carbon electrode (anode) with a diameter and a depth of 4 mm. (in determining the content of zinc in India brand Ин2 use carbon electrodes with the size of the crater 4x6 mm).

Carbon rod used as contradicted, sharpened to a truncated cone with a diameter of 2 mm. the pad Electrode pre-calcined in the arc of DC power 15 A for 10 s.

Determination of thallium is carried out under the same conditions, but trial India do not translate into oxide, and in the form of small pieces of 50 mg is placed in a recess of the coal electrode and seal the kick ball made of organic glass. References — in the form of indium oxide.

Arc spectra photographed with a diffraction spectrograph with being an illumination system of the slit and the three-step attenuator. The width of the slit of a spectrograph 0.015 mm, the distance between electrodes of 2.5 to 3.0 mm shall be maintained constant throughout the exposure (3−4 minutes). When determining the zinc exposure time 30 s. the Cassette spectrograph charge two photographic plates of type I for determination of copper and zinc and type II to define other elements.

Spectra of the samples photographed for six samples comparison — three times on the same photographic plate.

(Changed edition, Rev. N 1, 2, 3).

4. PROCESSING OF THE RESULTS

4.1. In the spectrogram, using microphotometry measure the blackening of analytical lines of the determined elements and the surrounding background. The calibration graphs are built in coordinates , where ; is the mass fraction of the element in the samples comparison.

For the calibration chart find the contents of the determined elements in the sample.

For the results analysis be the arithmetic mean of results of two parallel measurements obtained on the same photographic plate (each of the three spectrograms).

Photometric the following analytical lines (wavelengths in nanometers):

— gallium — Ga I, 287, 424;

iron Fe I 248,327;

— Nickel Ni I 300,249;

— tin — Sn I 283,999;

— lead — Pb I 283,307;

— copper — si I 327,394;

— thallium — Tl I 276,787;

— zinc — Zn I 334,502.

The difference between the smaller and larger of the two results of parallel measurements with a confidence level should not exceed the value of permissible differences , calculated by the formula:

 — mass fraction of impurities from the 7·10to 5·10%;

 — mass fraction of impurities of more than 5·10%,

where  — the average of the two mapped results of parallel measurements.

The difference between the smaller and larger of the two results of the analysis of the same samples with a confidence level should not exceed the value of permissible differences calculated by the formulae:

for a mass fraction of 7·10to 5·10%;

 — mass fraction of impurities of more than 5·10%,

where  — the average of the two matched analyses.

(Changed edition, Rev. N 1, 2, 3).