GOST 12645.13-87
GOST 12645.13−87 indium. Chemical-spectral method for the determination of gallium (Change No. 1)
GOST 12645.13−87
Group B59
STATE STANDARD OF THE USSR
INDIUM
Chemical-spectral method for the determination of gallium
Indium. Chemicospectral method for determination of gallium
AXTU 1709
Date of introduction 1989−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
G. I. Ivanov, A. B. Mineev, L. K. Larin, N. G. Pelevin
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
The change in N 1 taken by the Interstate Council for standardization, Metrology and certification
The adoption voted:
| The name of the state |
The name of the national standardization body |
| The Republic Of Azerbaijan |
Azgosstandart |
| The Republic Of Armenia |
Armastajad |
| The Republic Of Belarus |
Gosstandart Of Belarus |
| The Republic Of Kazakhstan |
Gosstandart Of The Republic Of Kazakhstan |
| The Republic Of Moldova |
Moldovastandart |
| Russian Federation |
Gosstandart Of Russia |
| Turkmenistan | The main state inspection of Turkmenistan |
| The Republic Of Uzbekistan |
Standards |
| Ukraine |
Gosstandart Of Ukraine |
3. INTRODUCED FOR THE FIRST TIME
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Section number, paragraph, sub-paragraph |
| GOST 1770−74 |
Sec. 2 |
| GOST 6709−72 |
« |
| GOST 10297−94 |
« |
| GOST 11125−84 |
« |
| GOST 12645.0−83 |
1.1; 1.1.1 |
| GOST 12797−77 |
Sec. 2 |
| GOST 14261−77 |
« |
| GOST 14919−83 |
« |
| GOST 19908−90 |
« |
| GOST 22300−76 |
1.1.1, sec. 2 |
| GOST 22306−77 |
1.1 |
5. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)
6. REPRINT (January 1998) with amendment No. 1, approved in June 1996 (IUS 9−96)
This standard specifies the chemical-spectral method for the determination of gallium in India for the mass concentration from 5·10to 5·10
%.
The method is based on extraction of gallium in the allocation of butyl ether of acetic acid from hydrochloric acid medium, Stripping it into aqueous phase, the deposition of nitrate India and spectrographic analysis of the resulting concentrate.
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis and security requirements — according to GOST and GOST 12645.0 22306 with the Supplement.
1.1.1. In the determination of gallium in India along with indium and reagents specified in GOST 12645.0, used butyl ether acetic acid which may have a harmful effect on the human body. When it is necessary to use the security requirements set forth in GOST 22300.
2. APPARATUS, REAGENTS AND MATERIALS
The diffraction type spectrograph DFS-8 spectrograph, or STE-1 being the illumination system of the slit.
Arc generator AC types DG-2, PS-39 and IVS-28.
Generator DC arc providing a voltage of at least 200 V and a current not less than 18 A.
Microphotometer designed to measure pucherani spectral lines.
Spectromancer of PS-18.
Analytical scale, allows to weigh with an accuracy of 0.0002 g. more
The infrared lamp of any type with capacity up to 500 W with a laboratory autotransformer type CTL-250−2.
Hot plate heating according to GOST 14919.
Muffle furnace, allowing you to adjust the temperature to 700 °C.
Grinding machine graphite electrodes of the type CP-35, or any other type.
Boxes of organic glass.
Glassware measuring glass according GOST 1770.
Quartz ware according to GOST 19908.
Electrodes of graphite rods brand C-2 or C-3 of 6 mm in diameter with a crater size 4x4 mm Contractrate — sharpened to a truncated cone area with a diameter of 1.5−2.0 mm.
Photographic plates spectrographic types SFC-02, the SFC-03, NT-2SV.
Indium brand Ин00 according to GOST 10297 and a solution of nitrate India, India containing 100 mg/cm.
Hydrochloric acid of high purity according to GOST 14261 and the solution (HCl)= 6 mol/DM
.
Nitric acid of high purity according to GOST 11125.
Butyl ether acetic acid according to GOST 22300.
Distilled water according to GOST 6709, distilled in a quartz apparatus.
Gallium GOST 12797.
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.
Sec. 2. (Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
3.1. A solution of gallium: 0.05 g metallic gallium is dissolved in 5 cmof a mixture of nitric and hydrochloric acids is 1:3. Transferred to a volumetric flask with a capacity of 100 cm
, adjusted to the mark with water, mix.
1 cmof solution A contains 0.5 mg of gallium.
10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm
, adjusted to the mark with water, mix.
1 cmof the solution contains 0.05 mg of gallium.
3.2. Samples of comparison: the basis for the preparation of samples of comparison is the indium oxide obtained by dissolving India brand Ин000 in nitric acid, drying, and calcining nitrate of indium to the oxide in a muffle furnace at a temperature of ~500 °C for 40−50 min. the resulting basis is ground thoroughly in a mortar.
The basic sample containing 1·10% of gallium in a quartz Cup with a capacity of 50 cm
is placed 12,091 g of indium oxide and added dropwise 2 cm
of a solution of gallium B. the Solution is dried and calcined for 20−30 minutes at a temperature of ~500 °C in a muffle furnace. Then dilution of the primary and each newly prepared samples the basis for preparing a series of samples of comparison workers in accordance with the table.
g
| Sample number comparison | Mass fraction of gallium in the reference sample, % |
The number of diluted sample | The number of bases needed for the dilution |
| 1 |
1·10 |
- | - |
| 2 |
3,3·10 |
2,000 (sample No. 1) | 4,000 |
| 3 |
1·10 |
1,000 (sample No. 2) | 9,000 |
| 4 |
5·10 |
3,000 (sample No. 3) | 3,000 |
(Changed edition, Rev. N 1).
3.3. The basis and calibration samples stored in buksh or tightly sealed jars for 1 year.
4. ANALYSIS
4.1. The weight India weight of 1,000 g was placed in a quartz Cup with a capacity of 30−50 cmand dissolved in 5−7 cm
of hydrochloric acid when heated. Cup of shut watch glass. After complete dissolution of the sample solution is evaporated to dry salts under a heat lamp. The dry salt is dissolved in 5 cm
of hydrochloric acid solution
(HCl)=6 mol/DM
and transferred to a separatory funnel with a capacity of 100 cm
. The Cup is washed with 5 cm.
of the same hydrochloric acid solution; the wash solution is drained into the same separating funnel. Add 10 cm
of butyl acetate and vigorously shaken for 1 min. After phase separation, the lower layer discarded, the extract washed twice with 2−3 cm
of hydrochloric acid.
Stripping gallium from the organic layer is performed twice 10 cmof water for 1 min.
The aqueous layer after the first and second Stripping decanted into a quartz Cup in which was added 1 cmof a solution of indium and 2−3 cm
of nitric acid. The solution is dried under a lamp, on the hot plate and the precipitate is then calcined in a muffle furnace at a temperature of ~500 °C for 25−30 min to obtain indium oxide. The calcined precipitate is weighed, wear quartz wand in the Cup.
The enrichment coefficient () is calculated by the formula
where - mass of India taken for analysis, g;
- the mass of concentrate obtained after beneficiation,
At the same time through the analysis of spend control experience to account for the purity of the reagents, glassware and experience, conducting the same operations and using the same amount of reagents, which is required to obtain a concentrate of the impurities of the sample. Ratio of enrichment is calculated by the same formula as that for the sample analyzed.
To obtain the result of analysis from each sample is taken at the two sample and receive two concentrate.
(Changed edition, Rev. N 1).
4.2. Sample samples of comparison and concentrates of samples and control experience with a mass of 50 mg was placed in carbon electrodes with the size of the crater in a 4x4 mm (for each sample and concentrate to prepare 2 electrodes), and burn in the arc of DC power 15 A for 3 min (to burnout). The spectra are photographed on the type of spectrograph DFS-8, or STE-1 (first order). The width of the slit of a spectrograph 0,02 mm.
5. PROCESSING OF THE RESULTS
5.1. In the spectrogram, using microphotometry measure the blackening of a line of gallium 287,4 nm and the surrounding background. The calibration graphs are built in coordinates 
is the mass fraction of gallium in the samples comparison, %.
Mass fraction of gallium in the sample is calculated by the formula
where and
— mass fraction of gallium in the concentrate samples and in the reference experiment, respectively, was found in the calibration schedule, %;
and
the enrichment factors for the sample and reference experiment, respectively.
5.2. For the results analysis be the arithmetic mean of results of two parallel measurements obtained on the same photographic plate (each simultaneous determination of the two spectrograms).
The difference between the smaller and larger of the two results of parallel measurements with a confidence probability of 0.95 does not exceed the value of permissible differences
, is calculated according to the formula
is 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 of 0.95 does not exceed the value of permissible differences
, is calculated according to the formula
is the average of the two matched analyses.
(Changed edition, Rev. N 1).
