By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST 20997.5-81

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 20997.5−81

INTERSTATE STANDARD

THALLIUM

METHOD OF CHEMICAL-SPECTRAL DETERMINATION OF TIN

The official Islande

BL 6−99

IPK PUBLISHING house of STANDARDS, Moscow

UDC 669.873:546.811.06:006.354 Group B59

INTERSTATE S T, A N D, A R T

THALLIUM

GOST

20997.5−81*

Method of chemical-spectral determination of tin

Thallium.

Method of chemical-spectral determination of tin AXTU 1709

GOST 20997.5−81 C. 2

The acid chloride.

Sodium iodide according to GOST 8422−76 and solutions I and 0.05 M.

Benzene according to GOST 5955−75.

The aqueous ammonia of high purity according to GOST 24147−80.

Oxalic acid according to GOST 22180−76.

Photographic plates «spectrographic» type II.

Developer a metol-hydrochinone.

Fixer is acidic.

Solution India 10%: a portion of India with a mass of 5.0 g is dissolved in 12 cm1 nitric acid, cooled and transferred to volumetric flask with a capacity of 50 cm3.

A solution of tin 0.1%: suspension of fine Olopa a mass of 0.100 g was dissolved in 2 cm3 of nitric acid. After moving the entire tin in metalogeny acid to the beaker was added 20 cm3 of water and 4.0 g of oxalic acid. The solution was transferred to a volumetric flask with a capacity of 100 cm3. The glass is washed several times with water until complete dissolution of oxalic acid. Slipout the washings in the same volumetric flask and bring to mark with water.

Solution a: 10 cm3 of a 0.1% strength solution of tin is transferred to a volumetric flask with a capacity of 100 cm3 and diluted to the mark with water.

1 cm3 of solution contains 0.1 mg of tin.

Solution B: 10 cm3 solution, And transferred to a volumetric flask with a capacity of 100 cm3 and diluted to the mark with water.

1 cm3 of a solution containing 0.01 mg of tin.

Solution In 10 cm3 of a solution transferred to a volumetric flask with a capacity of 100 cm3 and diluted to the mark with water.

1 cm3 of solution contains 0.001 mg of tin.

Standard solutions of S and prepared on the day of use.

Samples of comparison, with a mass fraction of tin MO-4; 2 I0-4; 3 10~2; MO-3; 3 10 3 %\ is prepared simultaneously with the analyzed samples.

Note. Allowed the use of devices with photoelectric registration of spectrum and other spectrographic equipment and facilities other materials and reagents subject to receipt of the accuracy characteristics as specified in this standard.

Section 2. (Changed the wording. Izm. No. 1, 2).

1

ANALYSIS

3.1. A portion of the metal thallium in a mass of 3.0 g was placed in a beaker with a capacity of 100 cm3 and dissolved by heating p 15 cm3 of a solution of sulfuric acid (1:2). Beaker cover watch glass. At the last moment dissolved add one drop of nitric acid. The solution is cooled to a temperature of 50−60 ° C. add 30 cm3 of water and 25 cm3 of 1 M solution of sodium iodide with stirring. The solution continued to stir for another 2.5 and 3.0 min. the precipitate of iodide of thallium in orange yellow color was filtered through a paper filter. The beaker and the filter washed with 10 cm3 of 0.05 M solution of sodium iodide. The filtrate and washings combined in a separating funnel with a capacity of 200 cm3, heated to a temperature of 35−40 *C, add 10 cm3 of perchloric acid, 30 g of sodium iodide and mix thoroughly. Add 10 cm3 of benzene and shaken for 1 min. After separation the aqueous layer is discarded and the upper organic through the throat of the funnel is transferred into a Cup, to which add 2 cm1 benzene after washing the separating funnel.

In a Cup make I cm3 of solution India. The benzene is evaporated at a temperature of 40 *C (30−40 min) and the concentrate of tin Coosada with the hydroxide India, what to India labatut nitrate solution dropwise with stirring a glass Pato? ka 20 drops of ammonia to a strong smell. The resulting hydroxide dried under a lamp, on a hotplate, and then pumped in a muffle furnace at a temperature of 350 to 400 *C for 30 min. After prokashani obtained oxide India crushed quartz with the pestle to a fine grist, and transmitted to a spectrographic analysis.

Enrichment of lead from the four batches. At the same time to check the purity of reagents used spend control experience.

2

In parallel with the analyzed sample. mi to spectrographically prepare samples comparison. For this five glasses with a capacity of 100 cm3 hurt weighing 0.2−0.5 g sample of thallium containing tin of 1 at least 10~s %. In glasses nakatyvaet respectively 0.1: 0,2; 0.3; 1.0 and 3.0 cm3 solution Q. what per 100 mg India meets MO-4; 2)-4; 310"4; 1 10_3 3 and 10~3%

C. 3 GOST 20997.5−81

tin in concentrate. In each glass add 1 cm3 solution of sulphuric acid (1:2) and under the watch glass, the contents of the beaker are transferred into the solution. At the last moment dissolved add one drop of nitric acid and further analysis are as under sample preparation.

3.2. The obtained concentrates of samples comparison reference experiment and samples of 45 mg will prevent the craters of graphite electrodes (anodes) with a diameter and a depth of 4 mm and burn in the arc of a DC power of 15 L for 3 min (to burnout). The spectra photographed with a diffraction spectrograph of the DFS-8 on photos of type II: width of the slit of a spectrograph 0.020 mm, distance between electrodes of 2.5 to 3.0 mm should be maintained throughout the exposure. Each photographic plate is photographed koncertov spectra of samples comparison at two times, and the spectra of the concentrates of the samples and control experiments for four times.

Section 3. (Changed edition, Rev. No. 1, 2).

4. PROCESSING OF THE RESULTS

4.1. On the spectrogram with the aid of microphotometer measure the blackening of the lines of the tin with a wavelength 283.99 them and the surrounding background. Grigorovichi build graphics in the coordinates D — IgC, where AS = 5, d, f — 5 °F, C — mass fraction of tin in the samples of the comparison in percent.

For the calibration chart to find the mass fraction of tin in concentrate samples (and the reference experiment (S).

Mass fraction of tin in the sample (L) in percent is determined by the formula

S — P. 100

X=-1-,

t

where 100 is the mass of the obtained concentrate, mg;

t — the weight of the portion of the sample of thallium, taken for analysis, mg.

For constructing a calibration curve allowed to use semilog paper.

The relative standard deviation of repeatability of the results of parallel measurements does not exceed 0.15.

4.2. Discrepancies in the results of four parallel samples (d). as well as the discrepancies of the results of the two analyses (D) shall not exceed the values given in the table (R= 0,95).

M associe proportion of tin. The divergence of the four results of the parallel definitions «v The discrepancy between the results of two tests. %
3−10 11 1.5 10 „ 2−10“ 6
<И0-S 3−10"6 410"6
M0-* 5 10-6 6 10-s
2 10* 5 7 u-6 9 10-6
410"4 2−10-5 210» 5
8−10"4 3−10"* 4−10 3
Ы0"4 4 10-5 510-5

Permitted discrepancies for the intermediate mass fraction calculated using linear interpolation.

Relacor M. I. Maksimova Technical relacor I. S. Grishakova Concealer R. L. Mitova desktop publishing L. L. Circular

Them. eggs. No. 1)2354 from 14.07.2000. Put in a set of 31.01.2001. Signed on print from 22.02.2001.e.l. PECs. L. 0.47.

Uch.-them. I. 0.43. Circulation 124 ski. With 387. Zach. 197.

IPK And j: iaie.'ii.ci standards. 107076. My. Well… 14.

Recruited and Publisher on a PC Branch of IPK Publishing house of standards — TMI. «Moscow printer», 103062. Moscow. Lyalin per. 6.

PCR Of MT 080102