GOST 1293.11-83
GOST 1293.11−83 lead-antimony Alloys. Method for the determination of tellurium (with Amendments No. 1, 2)
GOST 1293.11−83
Group B59
STATE STANDARD OF THE USSR
LEAD-ANTIMONY ALLOYS
Method for the determination of tellurium
Lead-antimony alloys. Method for the determination of tellurium
AXTU 1709*
________________
* Changed the wording, Rev. N 1.
Valid from 01.01.84
to 01.01.89*
_______________________________
* Expiration removed by Protocol No. 7−95
The interstate Council for standardization,
Metrology and certification (I & C N 11, 1995). -
Note the manufacturer’s database.
DEVELOPED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
A. P. Sychev, M. G. Sun, L. I. Maksay, R. D. Kogan
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Member Of The Board Of A. P. Snurnikov
APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards of February 8, 1983 N 705
REPLACE GOST 1293.11−74
MADE: the Change in N 1, approved and put into effect by the Decree of the USSR State Committee for standards from 20.11.87 N 4206 from 01.07.88, Change No. 2 adopted by the Interstate Council for standardization, Metrology and certification (minutes N 13 dated 28.05.98). The state developer of Kazakhstan. By the resolution of Gosstandart of Russia from 11.04.2001 N 173-St introduced on the territory of the Russian Federation from 01.01.2002
Change N 1, 2 made by the manufacturer of the database in the text IUS N 2, 1988, ICS # 7, 2001
This standard sets the photometric method for the determination of the mass fraction of tellurium from 0.003 to 0.08% of lead-antimony alloys.
The method is based on the formation of complex compounds of tellurium with butyrophenom B, the extraction of this compound with benzene and the measurement of its optical density at 530 nm in the spectrophotometer or in a region of wavelengths of 530−540 nm on a photoelectrocolorimeter. Color stability of benzene extract compounds of tellurium strongly depends on the purity of the extractant and utensils.
(Changed edition, Rev. N 1, 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 1293.0−83.
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid GOST 4461−77.
Sulfuric acid GOST 4204−77, diluted 1:1 and the solution 
(
H
SO
)=9 mol/DM
.
Hydrochloric acid by the GOST 3118−77 and diluted 1:1.
Sodium Masakovsky, a solution of 5 g/DM.
Copper sulfate according to GOST 4165−78, a solution of 50 g/DM.
Sodium posterolaterally (hipofosfit sodium) according to GOST 200−76 or potassium posterolaterally, saturated solution in hydrochloric acid (1:1).
Potassium bromide according to GOST 4160−74 or sodium bromide, 1 M solution in sulfuric acid (HSO)=9 mol/DM.
Hydrogen peroxide according to GOST 10929−76.
Tartaric acid according to GOST 5817−77, a solution of 500 g/DM.
Benzene according to GOST 5955−75.
Ascorbic acid, a solution of 20 g/DM.
Acetone according to GOST 2603−79.
Butyl ester of rhodamine B: 0,056 g of reagent was dissolved in 200 cmof sulfuric acid solution (HSO)=9 mol/DM.
(Changed edition, Rev. N 1, 2).
3. PREPARATION FOR ASSAY
3.1. Preparation of standard solutions of tellurium
Solution a: of 0.0500 g of tellurium are dissolved under heating in a mixture of 10 cmof nitric acid and 5−6 drops of hydrochloric acid. Evaporated to a volume of 2−3 cm, pour 10 cmof sulfuric acid solution (1:1) and evaporated to start the selection of sulfuric acid vapor. Wash the side of the Cup with water and again evaporated as above. Then repeat this operation. After cooling, add 15 cmof water, with a solution of sulfuric acid (HSO)=9 mol/DMsolution is transferred into a measuring flask with a capacity of 500 cmand bring the solution to the mark with sulfuric acid solution (HSO)=9 mol/DM.
1 cmof solution A contains 0.1 mg of tellurium.
Solution B: 4 cmmortar And transferred to a volumetric flask with a capacity of 100 cmand dilute to the mark with sulfuric acid solution (HSO)=9 mol/DM.
1 cmof a solution containing 4 micrograms of tellurium.
(Modified re
Doccia, Rev. N 2).
3.2. The preparation of 1 M solution of potassium bromide in sulphuric acid solution (HSO)=9 mol/DM
12 g of potassium bromide dissolved in 40 cmof water, the volume was adjusted to 50 cmof water and 100 cmwith a solution of sulfuric acid (1:1). After cooling, add 0.5−1 g of ascorbic acid (a precipitate of potassium sulfate does not prevent the application of the reagent).
(Changed edition, Rev. N 2
).
3.3. To build a calibration curve in six of the seven separating funnels measure: 0,5; 1,0; 1,5; 2,0; 2,5 and 3.0 cmstandard solution B, corresponding to 2, 4, 6, 8, 10 and 12 ág of tellurium.
The seventh funnel, standard solution B is not administered.
The volume was adjusted to 6.0 cmwith a solution of sulfuric acid (HSO)=9 mol/DM, mix, add 2 cmbutyramide solution B, mix and add 15 cmof benzene. Then add 2 cmof potassium bromide solution, 1 cmof a solution of ascorbic acid and immediately extracted for 1 min in 5−6 minutes after the separation of the liquids poured through a faucet water layer of 1−2 cmof the extract, and then through the top hole cast 10 cmextract in a measuring cylinder with a capacity of 10 cm. Selected extract is transferred to a dry test-tube, measure out the same cylinder 5 cm inacetone and quickly poured it to the extract (to stabilize color), and then stirred. After 10 minutes measure the optical density of the solution at a wavelength of 530 nm on the spectrophotometer or in a region of wavelengths of 530−540 nm on a photoelectrocolorimeter.
Solution comparison is the solution not containing a standard solution of tellurium.
According to the obtained values of optical density of the solutions and the corresponding content of tellurium to build the calibration graph.
(Changed edition, Rev. N 1, 2).
4. ANALYSIS
A portion of the alloy weight 0,5000 g is placed in a conical flask with a capacity of 100 cm, dissolved in a mixture of 15 cmof nitric acid (1:1) and 1 cmof a solution of tartaric acid. Add 5 cmof sulfuric acid solution (1:1), 30 cmof water and heated to boiling. The solution was cooled, allow to stand for about 1 h and filtered off the precipitate through an ash-free filter «blue ribbon» in a conical flask with a capacity of 250 cm. Washed precipitate of sulphate of lead 4−5 times in cold water. The solutions were evaporated to the appearance of sulphuric acid fumes, then cooled, poured 8−10 drops of hydrogen peroxide and again heated the solution. If the color of the solution disappeared add more hydrogen peroxide and repeat the heating. After the disappearance of coloration, and the solution is cooled, washed the walls of the flask with water and again heated until the appearance of sulphuric acid fumes. Cooled, poured 100 cmof hydrochloric acid (1:1), 1 cmof solution of copper sulphate, 0.5 cmof the solution Myslakowice of sodium, a little filtrowanie mass and heated to 70−80 °C. the hot solution add 10 cmof hot hypophosphite solution of potassium or sodium and leave until the next day.
The precipitate is filtered off and letting it dry, immediately washed 5−6 times with hot water.
Carry a funnel with a filter flask in which the precipitation was carried out, and dissolve precipitate on the filter with a hot mixture of acids (5 cmof hydrochloric acid, add 5−7 drops of nitrogen) and washed 3−4 times with a little water (to dissolve one filter is about 5 cmof the mixture of acids).
The flask is cooled, transfer the filtrate into a measuring flask with a capacity of 50 cm, made up to the mark with water and mix. Aliquot part of the solution is 2−5 cm(it should contain 2−10 ág of tellurium) is placed in a Cup with a capacity of 50 cm, add 1.4 cmof sulfuric acid solution (1:1) and heated until the appearance of sulphuric acid fumes.
To a solution of the reference experiment, which is carried out simultaneously with the main analysis, impose 2.8 cmof sulfuric acid solution (1:1) and throughout the course of the analysis of the injected double the amount of reagents (for further filling two cuvettes).
The glass is cooled, wash the side of the Cup with water, pour 1 cmof hydrochloric acid and again evaporate the solution until the appearance of sulphuric acid fumes. This operation is repeated. This completely removes the nitric acid. Vaporization surgery chernososhnyh solutions should only lead to the first appearance of sulphuric acid fumes.
The amount of residual solution in the cups after evaporation should be 0.5−0.6 cm. If necessary, add sulfuric acid dropwise until the volume of 0.5−0.6 cm. The solution is cooled and added 1.5 cmof water. Transfer the solution into the separatory funnel with a capacity of 50 cm, washing the Cup with 4 cmof sulfuric acid solution (HSO)=9 mol/DM. Poured into separating funnel of 2 cmof solution butylamine B, mix, add 15 cmof benzene and then do as stated in claim 3.3.
As a solution comparison using the solution in the reference experiment.
Mass of tellurium find for the calibration schedule.
(Changed edition, Rev. N 2).
5. PROCESSING OF THE RESULTS
5.1. Mass fraction of tellurium (
) in percent is calculated by the formula
,
where 
is the mass of tellurium in the sample solution, found by calibration schedule, mcg;
— volume of initial solution alloy, cm;
— weight alloy, g;
— volume aliquote part of the solution, cm.
5.2. The discrepancy between the results of parallel measurements 
(the difference between the largest and smallest results of parallel measurements) and the discrepancy between the results of the analysis 
(the difference between the larger and the smaller of the results of the analysis) at a confidence level 
=0.95 does not exceed the allowable absolute values of the differences given in the table.
| |
|
|
|
| Mass fraction of tellurium, % |
The limit of error of the results of the analysis  , % |
The discrepancy between the results of parallel measurements , % |
The discrepancy between the results of the analysis , % |
From to 0,0030 0,0050 incl.
|
About 0.0006 |
0,0008 |
0,0008 |
SV. 0,0050 «0,010 «
|
0,0009 |
0,0012 |
0,0012 |
«0,010» 0,020 «
|
0,002 |
0,002 |
0,002 |
«0,020» 0,050 «
|
0,002 |
0,003 |
0,003 |
«0,050» 0,080 «
|
0,004 |
0,005 |
0,005 |
The control accuracy of the analysis is carried out using standard samples or by other methods stipulated by GOST 1293.0−83.
The error analysis results (at a confidence probability =0,95) does not exceed the limit values given in the table, under the following conditions: the discrepancy between the results of parallel measurements does not exceed the permissible, the results of accuracy control positive.
(Changed edition, Rev. N 2).
