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GOST 12645.8-82

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 12645.8−82 indium. Chemical-spectral method of determination of tin (with Amendments No. 1, 2)


GOST 12645.8−82

Group B59


STATE STANDARD OF THE USSR

INDIUM

Chemical-spectral method of determination of tin

Indium. Method of chemical and spectral analysis for the determination of tin


AXTU 1709

Date of introduction 1983−07−01

INFORMATION DATA

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

DEVELOPERS

A. P. Sychev, L. K. Larin, N. With. References:

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 7.04.82 G. N 1459

Change No. 2 adopted by the Interstate Council for standardization, Metrology and certification 15.03.94 (report of the Technical Secretariat N 1)

The adoption voted:

   
The name of the state
The name of the national standardization body
The Republic Of Azerbaijan
Azgosstandart
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. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
Section number, paragraph, sub-paragraph
GOST 860−75
Sec. 3
GOST 4204−77
«
GOST 5955−75
«
GOST 6709−72
«
GOST 8422−76
«
GOST 10297−94
«
GOST 11125−84
«
GOST 12645.0−83
1.1; 1.2
GOST 19908−90
Sec. 3
GOST 22180−76
«
GOST 22306−77
1.1
GOST 24147−80
Sec. 3

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

5. REPRINT (January 1998) with Amendments No. 1, 2 approved in December 1987-June 1996 (IUS 3−88, 9−96)


This standard specifies the chemical-spectral method of determination of tin in India with a mass fraction of tin from 1·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)to 5·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)%.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

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

1.2. Safety requirements — according to GOST 12645.0.

1.1, 1.2. (Changed edition, Rev. N 1).

1.3. (Deleted, Rev. N 1).

Sec. 2. (Deleted, Rev. N 1).

3. APPARATUS, REAGENTS AND MATERIALS


The diffraction type spectrograph DFS-8 with a grating of 600 lines/mm, first order, being the illumination system of the slit.

The generator of the arc AC of PS-39, DG-2 or IVS-28.

A constant current source providing a voltage of at least 200 V and a current not less than 20 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

Libra torsion bar type W, allowing you to weigh with an accuracy of not more than 0.001 g.

Boxes of organic glass.

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

Grinding machine carbon electrodes of the type CP-35, or any other type.

Tile electric heating.

Ware and quartz glass (glasses, flasks, separating funnels, etc.) according to GOST 19908.

Mortar made of organic glass with a pestle.

Muffle furnace that allows the temperature to 500 °C.

Electrodes, carbon, high purity, 6 mm in diameter with the size of the crater in a 4x4. Contractrate coal, one end of which is sharpened to a truncated cone with ground diameter of 1.5−2.0 mm.

Indium metal brand Ин000 or Ин000у according to GOST 10297.

Tin GOST 860.

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

Sulfuric acid according to GOST 4204, diluted 1:3.

Nitric acid brand OS.H. 19−4 GOST 11125.

The acid chloride.

Sodium iodide according to GOST 8422.

Benzene according to GOST 5955.

Ammonia water according to GOST 24147.

Oxalic acid according to GOST 22180.

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

India a solution of 100 g/DMГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2): India hitch weight 2,500 g dissolved in 12.5 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of nitric acid under heating, cooled and transferred to volumetric flask with a capacity of 25 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2).

A solution of tin 1 g/DMГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2): a portion of finely ground tin weight 0,100 g dissolved in 2 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of nitric acid. After dissolution of tin in the beaker was added 20 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)water and 4,000 g of oxalic acid. The solution was transferred to a volumetric flask with a capacity of 100 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2). The glass is washed several times with water for complete dissolution of oxalic acid. The washings decanted into the same volumetric flask and bring to mark with water.

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. 3. (Changed edition, Rev. N 1, 2).

4. PREPARATION FOR ASSAY

4.1. References

The basis for the preparation of samples of comparison is the oxide of indium: indium metal stamps Ин000 or Ин000у dissolved by heating in nitric acid, the solution was evaporated to dryness and the dry residue is calcined first on a hotplate and then in a muffle furnace at a temperature of 400−500 °C before the termination of allocation of vapors of oxides of nitrogen (30−40 min). You should pay particular attention to the completeness of removal of nitrogen oxides, as their presence in the basis increases the background in the spectrum, which distorts the results of the analysis. The content of tin in the basis determined by the method of additives and then introduced an amendment to samples comparison.

4.2. The main sample with a mass fraction of tin of 0.03% (calculated as metal indium) is prepared nakapyvaniem 3 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of a solution of tin in the basis (12,1 g of indium oxide). The sample is dried on the hot plate and in a muffle furnace at 300 °C, triturated in a mortar and, if necessary, analyze the chemical or atomic absorption methods, is ground in a mortar.

By diluting the primary and the newly prepared samples based get series of working samples comparison, the mass fraction of tin in which is given in the table.

g

       
Sample number
Mass fraction of tin, %
The number of diluted sample
The number of bases needed for the dilution
1

5·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)

2,000 basic sample
10,000
2

1·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)

3,000 sample N 1
12,000
3

3,3·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)

3,500 sample N 2
7,000
4

1·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)

1,000 sample N 1
9,000

4.1, 4.2. (Changed edition, Rev. N 1, 2).

5. ANALYSIS

5.1. Sample metallic indium with a mass of 1,000 g was placed in a beaker with a capacity of 100 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)and dissolved under the watch glass when heated in 20 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of sulfuric acid solution (1:3). Upon evaporation of the solution should be dropwise adding water, avoiding salt precipitation. The solution was cooled to 30−40 °C, is added for oxidation of divalent tin to tetravalent 10 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of perchloric acid, mix and add 20 g of sodium iodide. After complete dissolution of sodium iodide and the solution transferred to a separatory funnel and shaken for 1 min with 10 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of benzene. After separation, wash the throat of the funnel 1−2 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of benzene, to separate the inorganic phase and the organic through the throat of the funnel is poured into a quartz crucible with a capacity of 50 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2). The funnel is washed with benzene, draining it into the same crucible. There also add 1 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of a solution of India and placed under a heat lamp for distilling off the benzene at 50−60 °C for 30−40 min in a box made of organic glass.

Then tin hydroxide Coosada with India is added to the solution of nitrate India ammonia dropwise until a strong odor (20 drops), washing the walls of the crucible and thoroughly stirring the resulting slurry quartz wand. The resulting hydroxide dried under a lamp and then calcined in a muffle furnace at 350 to 400 °C. After calcination, the indium oxide crushed quartz with the pestle to a fine grist, and transmitted to a spectrographic analysis. Enrichment of lead from the two batches. At the same time conducting a test experience to verify the purity of reagents used. To do this in a glass with a capacity of 100 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)is placed 0.1 g of metallic indium with a mass fraction of tin is less than 1·10ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)%. Dissolve it under the watch glass when heated in 20 cmГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of sulfuric acid solution (1:3) and then do the same as in the enrichment test.

(Changed edition, Rev. N

1).

5.2. Samples of comparison and the resulting concentrate for 45 mg is placed in the recess a carbon electrode (anode) with a diameter and a depth of 4 mm and burn in the arc of DC power 15 A for 3 min (to burnout). The spectra photographed using a diffraction spectrograph DFS-8 in the first order on photos types SFC-02, the SFC-03, NT-2SV. The width of the slit of a spectrograph 0.020 mm, distance between electrodes of 2.5 to 3.0 mm shall be maintained constant throughout the exposure.

On a photographic plate samples comparison photographed three times, each resulting concentrate twice.

(Changed edition, Rev. N 2).

6. PROCESSING OF THE RESULTS

6.1. In the spectrogram, using microphotometry measure the blackening of a line the tin with a wavelength 283,99 nm and the surrounding background.

The calibration graphs are built in coordinates ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2), where ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)(ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — blackening line of tin and background; ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — blackening of the background to the right of the line); ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — mass fraction of tin in the samples comparison, %. Darkening of the tin lines and the background should be in the region of normal pochernenija.

According to the calibration schedule find the mass fraction of tin in concentrate of the sample and control experience.

Mass fraction of tin in India (ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)) in percent is calculated by the formula

ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2),


where ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — mass fraction of tin in concentrate samples was found in the calibration schedule, %;

ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — mass fraction of tin in a control experiment, was found in the calibration schedule, %;

ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)the weight India taken for analysis, mg.

100 — weight of the obtained concentrate, mg.

The reproducibility of the analysis of the same samples characterized by the relative standard deviation is 0.13. Repeatability of results of parallel measurements is characterized by the relative standard deviation is 0.11.

For the results analysis be the arithmetic mean of results of four parallel measurements obtained on the same photographic plate.

(Changed edition, Rev. N 1, 2).

6.2. The difference between the highest and lowest of the four results of parallel measurements with a confidence probability ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of 0.95 does not exceed the value of permissible differences ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)calculated by the formula ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)where ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — the average of four matched results of parallel measurements.

The difference between the smaller and larger of the two results of analysis with confidence probability ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)of 0.95 does not exceed the value of permissible differences ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)calculated by the formula ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2)where ГОСТ 12645.8-82 Индий. Химико-спектральный метод определения олова (с Изменениями N 1, 2) — the average of the two matched analyses.

(Changed edition, Rev. N 1