GOST 1293.1-83

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  ГОСТ 1293.1-83

GOST 1293.1−83 lead-antimony Alloys. Methods for determination of antimony (adjusted with Amendments No. 1, 2)

GOST 1293.1−83*
______________________
* The designation of the standard.
Changed the wording, Rev. N 2.

Group B59

STATE STANDARD OF THE USSR

LEAD-ANTIMONY ALLOYS

Methods for determination of antimony

Lead-antimony alloys. Methods for the determination of antimony*

AXTU 1709*
________________
* The name of the standard. Changed the wording, Rev. N 2.

** Changed revision, Rev. N 1.

Valid from 01.07.83
prior to 01.07.88*
_______________________________
* 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 706

REPLACE GOST 1293.1−74


AMENDED, published in the IUS N 11, 1985

An amendment made by the manufacturer of the database

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 4205 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 specifies two methods for determination of antimony in lead-antimony alloys: titrimetric method when the mass fraction of antimony from 0.05 to 20% and the atomic absorption method for the mass fraction of antimony from 0.05 to 10%.

(Changed edition, Rev. N 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 1293.0−83.

(Changed edition, Rev. N 2).

1A. TITRIMETRIC METHOD FOR THE DETERMINATION OF ANTIMONY

1a.1. The essence of the method

The method is based on dissolution of lead-antimony alloy in sulphuric acid, to remove arsenic by boiling with hydrochloric acid and titration of the antimony branovacki potassium potentiometric or visual in the presence of the indicator methyl orange.

Section 1A. (Added, Rev. N 2).

2. APPARATUS, REAGENTS AND SOLUTIONS

pH meter-millivolt types of pH-341 pH-121 and other types.

Electromagnetic stirrer types MM-3, MM-01 and other types.

The platinum measuring electrode.

The auxiliary electrode — saturated calomel, silver chloride or mercuriality any brand. Measuring and auxiliary electrodes connected to a pH meter according to the instructions supplied with the device.

Sulfuric acid according to GOST 4204−77.

Hydrochloric acid by the GOST 3118−77.

Potassium branovitsky according to GOST 4457−74, solutions: (CRSC)= 0,1; 0,05 and 0,01 mol/DM.

Copper sulfate 5-water according to GOST 4165−78.

Methyl orange (pair-диметиламиноазобензолсульфокислый sodium) solution 0.1 g/100 cm.

Antimony GOST 1089−82 not below grade su 00.

(Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. Preparation of solutions of potassium polnovatogo (CRSC)=0,1; 0,05 and 0,01 mol/DM.

2,7835; 1,3917 and 0,2783 g of salt, respectively, is placed in a measuring flask with volume capacity of 1000 cm, dissolved in water, diluted to the mark with water and mix.

(Changed edition, Rev. N 1, 2).

3.2. The installation mass concentration of solutions of potassium polnovatogo

A portion of the antimony mass 0,1000; of 0.0500 or 0,0100 g (for installing the mass concentration of solutions polnovatogo potassium (CRSC)=0,1, 0,05 and 0,01 mol/DM, respectively) was placed in a conical flask with a capacity of 250 cm, add 20 cmof sulphuric acid and heated until dissolved. Cooled, diluted with water and transferred into a flask with a capacity of 500 cm, flow 20 cmof hydrochloric acid, dilute with water to 200 cmand boil for 10−15 min Cool to 60 °C, add 2−3 drops methyl orange and titrate with a solution of potassium polnovatogo (CRSC)=0,1; 0,05 and 0,01 mol/luntil the disappearance of the red color.

The mass concentration of a solution of potassium bromoperoxidase () for antimony in grams per cubic centimeter is calculated by the formula

,

where  — the weight of antimony, g;

 — the volume of solution of potassium Bromeliaceae, spent on titration, sm.

(Added, Rev. N 2).

4. ANALYSIS

4.1. The weight of the portion of the alloy is selected depending on the expected mass fraction of antimony in accordance with the table.1.

Table 1

The sample of alloy is placed in a conical flask with a capacity of 500 cm, add 30 cmof sulfuric acid, cover the flask with a glass bulb and heated to dissolve sample. For recovery of antimony and arsenic into the flask after cooling down a part of ashless filter 9 cm in diameter and heated to a decolorizing solution. To a solution of the reference experiment add along with ashless filter 1−2 crystal of copper sulphate. The flask is cooled down, wash the walls of the flask with water and again heated to a decolorizing solution. Then continue to heat for another 20−30 minutes.

The solution was cooled, poured 100 cmof water 100 cmof hydrochloric acid and boil moderately for the removal of arsenic and sulfur oxide (IV) until the solution volume is reduced to 100 cm. Then add 20 cmof hydrochloric acid.

If the test sample contains less than 0.01% arsenic and more than 0.1% antimony, arsenic removal by boiling is not required. In this case, the amount of hydrochloric acid is reduced to 20cmand boil for 5−6 min to remove sulphur oxide (IV).

The solution is quantitatively transferred into a beaker with capacity of 500 cm, 100 cm pourhot water, heated to 70−80 °C, add 2−3 drops of methyl orange solution, immerse electrodes into the solution and, with stirring, potentiometric titrated with a solution of antimony potassium polnovatogo appropriate concentration to the jump capacity or visually until the disappearance of the pink color of the indicator methyl orange. For a more distinct transition of color at the end of the titration add one more drop of the indicator solution, and lead the titration slowly with vigorous stirring of the solution.

(Changed edition, Rev. N 1, 2).

5. PROCESSING OF THE RESULTS

5 1. Mass fraction of antimony () in percent is calculated by the formula

,

where  — volume of the solution polnovatogo potassium, used for titration of the test solution, cm;

the volume of the solution polnovatogo potassium consumed for titration of the solution in the reference experiment, cm;

 — mass concentration of a solution of potassium Bromeliaceae, expressed in grams of antimony per 1 cmtitrant;

 — the weight of the portion of alloy,

(Changed edition, Rev. N 2)

.

5.2. The discrepancy between the results of parallel determination (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 permissible values of absolute differences are given in table.2.

Table 2

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 table.2, if the following conditions are true: the discrepancy between the results of parallel measurements does not exceed the permissible, the results of accuracy control positive.

(Changed edition, Rev. N 2).

5.3. The method used in the disagreement in assessing the quality of the alloy.

(Added, Rev. N 2).

6. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF ANTIMONY

6.1.The essence of the method

The method is based on dissolving the sample in a mixture of nitric and tartaric acids, the spraying solutions in the air-acetylene flame and measuring the absorption lines of antimony 217,6 nm.

6.2. Apparatus, reagents and solutions

Atomic absorption spectrophotometer of any brand.

Air, compressed under a pressure of 2·10-6·10* PA (2−6 ATM.) depending on the equipment.
_______________
* Consistent with the original. — Note the manufacturer’s database.

Acetylene in cylinders GOST 5457−75.

Tartaric acid according to GOST 5817−77, a solution of 400 g/DM.

Nitric acid GOST 4461−77 diluted 1:2.

Antimony GOST 1089−82 not below grade Su00.

6.3. Preparation for assay

6.3.1. Preparation of standard solutions of antimony

Solution a: 0,1000 g of crushed in an agate mortar of antimony is dissolved in 15 cmof nitric acid with addition of 15 g of tartaric acid when heated. After cooling, the solution is transferred to a volumetric flask with a capacity of 100 cm, is diluted to the mark with water and mix.

1 cmof the solution contains 1 mg of antimony.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cmadd 6 cmof nitric acid was adjusted to the mark with water and mix.

1 cmof the solution contains 100 micrograms of antimony.

Solution: 10 cmof a solution transferred to a volumetric flask with a capacity of 100 cmadd 6 cmof nitric acid was adjusted to the mark with water and mix.

1 cmof solution contains 10 mcg su

Remy.

6.3.2. Construction of calibration curve

In eight of the nine volumetric flasks with a capacity of 100 cmeach placed 10 to 30 cmof solution, 5; 8; 10; 20 cmof a solution; 4; 6 cmof solution A, which corresponds to 1; 3; 5; 8; 10; 20; 40 and 60 g/cmof antimony.

To all flasks add 5 cmof nitric and tartaric acids, adjusted to the mark with water and mix.

6.4. Analysis

6.4.1. The weight of the portion of the alloy is selected depending on the expected mass fraction of antimony in accordance with the table.3.

Table 3

The sample of alloy is placed in a conical flask with a capacity of 250 cm, 5 cm pourthe tartaric acid solution and 15 cmof nitric acid solution 1:2 (further dilution of solution in a volumetric flask with a capacity of 100 cm) or 10 cmof a solution of tartaric acid and 30 cmof a solution of nitric acid 1:2 (further dilution of solution in a volumetric flask with a capacity of 200 cm) and dissolved by heating. The solution was cooled, transferred to a volumetric flask in accordance with table.3, adjusted to the mark with water and mix.

Analyzed and standard solutions sprayed in air-acetylene flame and measure the value of the absorption line of antimony 217,6 nm.

Measurement conditions selected in accordance with the applicable device.

For spectrophotometers with work mode «concentration», «concentration» and get on the scoreboard in µg/cmor in the «absorption» method «limiting solutions», or by the calibration schedule.

On the other spectrophotometers operate in the mode «absorption» method «limiting solutions» or via the calibration curve

.

6.5. Processing of the results

6.5.1. Mass fraction of antimony () in percent is calculated by the formula

,

where is the concentration of antimony in the sample solution, µg/cm;

 — the concentration of antimony in solution in the reference experiment, µ g/cm;

the volume of the solution of the alloy, cm;

 — weight alloy, g

.

6.5.2. Allowable absolute differences of the results of parallel determination (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 values of permissible differences given in table.4.

Table 4

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 table.4, when the following conditions are true: the discrepancy between the results of parallel measurements does not exceed the permissible, the results of accuracy control positive.

Section 6. (Added, Rev. N 2).