GOST 16274.3-77
GOST 16274.3−77 Bismuth. Method for the determination of copper content (with Amendments No. 1, 2, 3)
GOST 16274.3−77
Group B59
STATE STANDARD OF THE USSR
BISMUTH
Method for the determination of copper content
Bismuth.
Method for determination of copper content
AXTU 1709
Date of introduction 1978−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
PS Poklonsky, F. M. Manji, G. V. Khabarova
2. APPROVED AND promulgated by the DECREE of the State Committee of standards of Ministerial Council of the USSR from
3. The frequency of inspection 5 years
4. REPLACE GOST 16274.3−70
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
The partition number |
GOST 859−78 |
Sec. 2 |
GOST 1770−74 |
Sec. 2 |
GOST 3652−69 |
Sec. 2 |
GOST 3760−79 |
Sec. 2 |
GOST 4461−77 |
Sec. 2 |
GOST 7851−74 |
Sec. 2 |
GOST 13647−78 |
Sec. 2 |
GOST 16274.0−77 |
Sec. 1 |
6. Resolution of the state standard from
7. REPRINT (July 1997) with Amendments No. 1, 2, 3, approved in January 1983, June 1987, July 1992 (IUS 5−83, 11−87, 10−92)
This standard applies to metallic bismuth brands Vi1 and Vi2 and sets the colorimetric method for the determination of copper content (when the copper content from 0.005 to 0.02%).
The method is based on colorimetrically pyridinediamine complex of copper extracted in the chloroform layer. Bismuth in the solution is bound in the complex with citric acid.
1. GENERAL REQUIREMENTS
General requirements for method of analysis according to GOST 16274.0
2. REAGENTS AND SOLUTIONS
The colorimetric glass cylinders.
Volumetric flasks with a capacity of 1000, 100 cmaccording to GOST 1770.
Pipettes with a capacity of 10 and 20 cmfor NTD.
Heat-resistant conical flask with a capacity of 50 cmaccording to GOST 7851.
Nitric acid according to GOST 4461, diluted 1:1.
Citric acid according to GOST 3652, 80% solution.
Ammonia water according to GOST 3760.
Pyridine according to GOST 13647.
Ammonium radamisty according to GOST 27067, 30% solution.
Copper of brand of M00 according to GOST 859*.
_______________
* On the territory of the Russian Federation GOST 859−2001. — Note the manufacturer’s database.
Standard solutions of copper.
Solution 1; prepared as follows: 1 g of copper is dissolved in 10 cmof nitric acid, diluted 1:1, boiled, transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water.
1 cmof solution of 1 contains 1 mg of copper.
Solution 2; prepared as follows: 10 cmof the solution 1 is transferred to a volumetric flask with a capacity of 100 cmand top up with water to the mark.
1 cm2 of solution contains 0.1 mg of copper.
Solution 3; prepared as follows: 20 cmsolution of 2 placed in a volumetric flask with a capacity of 100 cmand top up with water to the mark.
The solution for three days.
1 cmof the solution contains 0.02 mg of copper.
(Changed edition, Rev. N 1).
3. ANALYSIS
A portion of the bismuth of 1 g was placed in a flask with a capacity of 50 cm, add 5 cmdiluted 1:1 nitric acid and dissolve in low heat until the disappearance of nitrogen oxides. After dissolution, add 5 cmof 80% strength citric acid solution and neutralize the solution with ammonia on the indicator paper «the Congo» until the transition of color from blue to red, priliva it quickly and vigorously. After this solution was cooled, poured 1 cmof pyridine, 4 cmof a solution of ammonium thiocyanate and mix, then pour 4 cmof chloroform, mix again for 2−3 minutes and transfer the solution into the cylinder to colorimetrically.
In another cylinder are transferred solutions from the flask to which was added all reagents and solutions, in addition to bismuth, and add from a burette a standard solution of 3 to equalize colors of the layers of chloroform in both cylinders.
4. PROCESSING OF THE RESULTS
4.1. The content of copper () in percent is calculated by the formula
,
where the amount of copper in the model 3 solution consumed for titration, mg;
— hitch, g;
1000 — conversion factor for grams to milligrams.
4.2. The maximum discrepancy between the results of three parallel measurements () and the results of two tests () at a confidence probability of 0.95, should not exceed the values given in the table.
Mass fraction of copper, % |
The discrepancy between the results of three parallel definitions % |
The discrepancy between the results of two tests, % |
0,005 |
0,002 | 0,003 |
0,010 |
0,004 | 0,005 |
0,020 |
0,006 | 0,008 |
Permitted discrepancies for the intermediate mass fraction calculated using linear interpolation or according to the formulas:
for the range of mass fraction from 0.005 to 0.01%;
for a mass fraction in excess of 0.01%,
where is the arithmetic mean of results of three parallel measurements;
— the arithmetic mean of the results of the two tests.
(Changed edition, Rev. N 3).