GOST 22519.1-77
GOST 22519.1−77 Thallium. Method for determination of iron (with Amendments No. 1, 2, 3)
GOST 22519.1−77
Group B59
STATE STANDARD OF THE USSR
THALLIUM
Method for determination of iron
THALLIUM. Method for the determination of iron
AXTU 1709
Date of introduction 1978−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
A. P. Sychev, M. G. Sun, V. I. Lysenko, I. A. Romanenko, V. A. Kolesnikov
2. APPROVED AND promulgated by the Decree of the State Committee of standards of the USSR Council of Ministers
Change No. 3 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 4 dated 21.10.93)
The adoption voted:
| The name of the state |
The name of the national authority for standardization |
| The Republic Of Armenia |
Armastajad |
| 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 |
| The Republic Of Turkmenistan |
The main state inspection of Turkmenistan |
| The Republic Of Uzbekistan |
Standards |
| Ukraine |
Gosstandart Of Ukraine |
3. INTRODUCED FOR THE FIRST TIME
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph |
| GOST 61−75 |
2 |
| GOST 199−78 |
2 |
| GOST 3760−79 |
2 |
| GOST 4461−77 |
2 |
| GOST 9849−86 |
2 |
| GOST 18337−80 |
Chapeau |
| GOST 22519.0−77 |
1.1 |
5. Limitation of actions taken on the Protocol, the Interstate Council for standardization, Metrology and certification (ICS 2−93)
6. REPRINT (February 1998) with Amendments No. 1, 2, 3, approved in January 1983, March 1987-June 1996 (IUS 5−83, 6−87, 9−96)
This standard establishes photocolorimetric method for determination of iron (at mass fraction of iron from 0.0001 to 0.001%) in thallium brands TL0 and TL1 GOST 18337*.
______________
* On the territory of the Russian Federation GOST 18337−95. — Note the manufacturer’s database.
The method is based on the ability of bivalent iron ions to form Oh-phenantroline complex compound, the color of which photometrically. Thallium definition does not interfere.
The sensitivity of the method was 1 µg in a volume of 25 cm.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis and security requirements — according to GOST 22519.0.
(Changed edition, Rev. N 3).
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter.
Nitric acid according to GOST 4461, diluted 1:1 and 1:3.
Ascorbic acid, a solution of 10 g/DM.
Acetic acid according to GOST 61, solution 2 mol/DM, is prepared as follows: 35 cm
of glacial acetic acid is diluted to a volume of 1 DM
water and stirred.
Sodium acetate according to GOST 199, a solution of 2 mol/DM, is prepared as follows: 272 g sodium acetate and dissolve in 1 volume of DM
water and stirred.
Acetate buffer solution with a pH of 3.7; prepared as follows: 27 cmof a solution acetic acid 2 mol/DM
and 3 cm
of a solution of sodium acetate and 2 mol/DM
dilute with water to volume of 100 cm
and mixed.
Ammonia water according to GOST 3760, diluted 1:3.
Iron powder restored brand MLB-1 according to GOST 9849.
Standard solutions of iron.
Solution A, prepared as follows: 0,100 g of iron powder was dissolved in 5 cmof nitric acid, diluted 1:1, pour 25 cm
of water and heated to boiling. The solution was cooled, transferred to a volumetric flask with a capacity of 1 DM
, poured 10 cm
of nitric acid, dilute to the mark with water and mix.
1 cmof solution A contains 0.1 mg of iron.
Solution B is prepared as follows: 4 cmof solution A is placed in a volumetric flask with a capacity of 100 cm
, is diluted to the mark with water and mix.
1 cmof a solution containing 4 µg of iron.
on-phenanthrolin hydrochloride dnovotny, a solution of 2 g/DM.
(Changed edition, Rev. N 2, 3).
3. ANALYSIS
3.1. The weight of thallium in a mass of 1,000 g is dissolved in 4 cmof nitric acid, diluted 1:3, and gently evaporated to obtain a wet residue, avoiding drying, until it gets dark. Pour 10 cm
of water, boiled and cooled. Add 1 cm
of a solution of ascorbic acid, neutralize the solution with ammonia until the color of Congo paper from blue to purple, add 2.5 cm
of the solution on-phenantroline, 2 cm
acetate buffer solution, the solution was transferred to volumetric flask with a capacity of 25 cm
, is diluted to the mark with water and mix. After 30 min, measure the optical density of the solution on the photoelectrocolorimeter, applying a filter with a transmission area of around 508 nm in a cuvette with the thickness of the light absorbing layer 50 mm Solution of comparison is water.
The amount of iron in kalorimetricheskim the solution set for the calibration schedule.
(Changed edition, Rev. N 2, 3).
3.2. Construction of calibration curve
In six volumetric flasks with a capacity of 25 cmmeasure 0; 0,5; 1,0; 2,0; 3,0 and 4,0 cm
standard iron solution B, which corresponds to 0; 2; 4; 8; 12 and 16 mg of iron, add about 15 cm
of water, 1 cm
of a solution of ascorbic acid and analysis are as indicated in claim 3.1.
(Changed edition, Rev. N 2).
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of iron () in percent is calculated by the formula
where is the mass of iron was found in the calibration schedule, mcg;
the weight of thallium,
4.2. The absolute values of the differences between the results of two parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) with confidence probability of 0.95 should not exceed the values permitted discrepancies listed in the table.
| Mass fraction of iron, % |
The permissible difference for parallel definitions % |
The permissible discrepancy between the results of the analysis % |
| From 0,00010 0,00020 to incl. |
0,00005 |
0,00007 |
| SV. 0,00020 «0,00050 « |
0,00007 |
0,00010 |
| «0,00050» 0,00100 « |
0,00010 |
0,00015 |
(Changed edition, Rev. N 3).
