GOST 1367.6-83
l p. vnna B59
INTERSTATE STANDARD
ANTIMONY melody the determination of Nickel
GOST 1367.6−83 Instead of GOST 1367.6−76
Antimony. Methods for the determination of nickel
AXTU 1709
The decision of the State Committee of the USSR No. standards 16 decelle 1983 No. 6013 date of introduction is established 01.01.8 S
The limitation on the duration of shot on the Ss Protocol 4−93 of the Interstate Council for standartini. Metrology and certification (ICS 4−94)
This standard sets the photometric and atomic absorption methods for the determination of Nickel from 0.005 to 0.05% antimony grades Soo and LMS.
(Changed edition, Rev. No. 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis and security requirements — according to GOST 1367.0−83.
2. PHOTOMETRIC METHOD
The method is based on the formation in alkaline environment colored complex compounds of Nickel with dimethylglyoxime in the presence of an oxidant — bromine. To 0.2 g of antimony determination does not prevent, and therefore the separation of Nickel is not performed.
2.1. Up parature, reagents and solutions
Spectrophotometer or photoelectrocolorimeter of any kind for measurements in the visible region of the spectrum.
Beakers, glass, laboratory for GOST 25336−82 with a capacity of 50. 100 cm'.
Volumetric flasks according to GOST 1770−74 with a capacity of 50, 100 cm1 DM and 1\
Pipette with divisions for NTD with a capacity of 1, 2, 5 and 10 cm5.
Sulfuric acid according to GOST 4204−77. diluted 1:1.
Hydrochloric acid by the GOST 3118−77.
Tartaric acid according to GOST 5817−77, a solution with a mass fraction of 25%.
Hydrogen peroxide according to GOST 10929−76, a solution with a mass fraction of 30%.
Ammonia water according to GOST 3760−79. diluted 1:1.
Bromine in GOST 4109−79.
Bromine water: 5 g of bromine are placed in a flask with a glass stopper with a capacity of 200-Zoom3, pour 100 cmj of water and vigorously shake the bottle, occasionally lifting the tube to release the accumulated vapors of bromine.
Ethyl alcohol drinking according to GOST 5963−67*.
Dimethylglyoxime according to GOST 5828−77, alcohol solution with a mass fraction of I %.
Nickel metal according to GOST 492−73.
* On the territory of the Russian Federation GOST R 51723−2001.
Official edition Reprinting is prohibited
Edition with amendments No. J, approved «March 1989 (IUS 6−89).
45
C. 2 GOST 1367.6−83
Standard solutions of Nickel.
Solution a: 0.1 g of metallic Nickel is placed in a beaker with a capacity of 100 cm\ poured 5 cm3 of hydrochloric acid and 2 cm3 of nitric acid. The contents of the Cup is heated and evaporated almost to dryness. Then pour 5 cm3 of hydrochloric acid and again evaporated to dryness. Treatment with hydrochloric acid is repeated twice. After cooling, the dry residue moistened with 5 cm3 of hydrochloric acid, poured approximately 20 cm3 of water heated, cooled, transferred to a volumetric flask with a capacity of I DM3, was adjusted to the mark with water and mix.
1 cm3 of the solution L contains 0.1 mg of Nickel.
Solution B: 10 cm3 of the solution L is transferred to a volumetric flask with a capacity of 100 cm3, made up to the mark with water.
I cm' of a solution contains 0.01 mg of Nickel.
(Amended, NSC. No. I).
2.2. Analysis
2.2.1. A portion of the antimony with a mass of 0.2 g DM Sooo, MSA or a mass of 0.1 g brand SS2 was placed in a beaker with a capacity of 100 cm5 and dissolved by heating and continuous stirring in 5 cm3 of hydrochloric acid with a dropwise addition of hydrogen peroxide. After dissolution of the sample contents of the tubes evaporated to wet salts, pour 5 cm3 of a solution of tartaric acid, And) cm3 oxen and boiled for 1 min.
To the solution add bromine water until the appearance of its yellow colouring, neutralized with ammonia (1:1) to alkaline reaction to litmus and pour 1 cm3 of ammonia in excess. Then add water, approximately 10−20 cm3. 1 cm3 of the solution dimethylglyoxime, 2 cm3 bromine water and transfer the solution into volumetric flask with a capacity of 50 cm\ adding water to the mark. After each addition of the reagent the solution was stirred.
After 10 minutes measure the optical density of the solution at a wavelength of 550 nm in a cuvette with a length of 50 mm. Solution comparison the solution serves as the reference experiment. The mass of Nickel in sample solution set for the calibration schedule.
2.2.2. The construction of the calibration Gras<1>IR
In glasses with a capacity of 50−100 cm3 flow consistently 1,0; 2,0; 3.0; 4.0; 5.0 and 6.0 cm3 of a standard solution b, which corresponds to 0.01; 0.02; 0,03; 0,04; 0.05 and 0.06 mg Nickel. 'Then add in a Cup 5 cm5 solution of tartaric acid, about 10 cm3 of water, pour the bromine water until the yellow coloring, neutralized with ammonia (1:1) to alkaline reaction to litmus, adding it in excess of I cm3, and further receives as indicated in section
On the found values of optical densities and their corresponding weight fractions of Nickel to build a calibration curve.
2.3. Processing of the results
2.3.1. Mass fraction of Nickel (L) in percent is calculated by the formula
t■ 100 t2-1000'
where /I is the mass of Nickel in solution of the sample, was found in the calibration graphics mg;
t2 — the weight of antimony,
2.3.2. The difference between the two results of parallel measurements and the difference of two analysis results with a confidence probability P = 0.95 does not exceed the allowable absolute differences of precision and reproducibility, are given in table. 1.
Table 1
| Masson fraction of Nickel, % | Absolute tolerance? my discrepancy. % | |
| convergence | NOSE L ROI 1ВОЛІІ bridges | |
| Og 0.0<)50-0.010 in key. | 0.0015 | 0.002 |
| SV. 0.010. 0.020 * | 0,002 | 0.003 |
| . 0.020. 0.050 « | 0.004 | 0.005 |
(Changed edition, Rev. Ss 1).
2.3.3. The method is applied when differences in the assessment of the quality of the antimony.
46
GOST 1367.6−83 C. 3
3. AGANO ABSORPTION METHOD
The method is based on measuring atomic absorption of Nickel in the introduction of the sample solution and solutions compare to the flames of propane-butane-air or acetylene -air.
3.1. Apparatus, reagents and solutions
Spectrophotometer atomic absorption Perkin-Elmer 503 or equivalent atomic absorption spectrophotometer.
Gas propane-butane according to GOST 2044I-90.
Beakers, glass, laboratory for GOST 25336−82 with a capacity of 50. 100 cm'.
Volumetric flasks according to GOST 1770−74 with a capacity of 25, 50 cm3, 1 DM3.
Pipette with divisions for NTD with a capacity of 1, 2, 5 and 10 cm3.
Sulfuric acid according to GOST 4204−77, diluted 1:1.
Hydrochloric acid by the GOST 3118−77.
For nitric acid GOST 4461−77.
Tartaric acid according to GOST 5817−77, a solution with a mass fraction of 25%.
Hydrogen peroxide according to GOST 10929−76, a solution with a mass fraction of 30%.
Nickel metal according to GOST 492−73.
Standard Nickel solution: 0.1 g of metallic Nickel is placed in a beaker with a capacity of UW cm3, pour 5 cm3 of hydrochloric acid. 2 cm3 of nitric acid. The contents of the Cup is heated and evaporated almost to dryness. Then pour 5 cm3 of hydrochloric acid and again evaporated to dryness. Treatment with hydrochloric acid is repeated twice. After cooling, the dry residue moistened with 5 cm3 of hydrochloric acid, poured approximately 20 cm' of water, heated, cooled, transferred to a volumetric flask with a capacity of 1 DM3, was adjusted to the mark with water and mix.
1 cm3 of solution contains 0.1 mg of Nickel.
(Changed edition, Rev. No. 1).
3.2. Analysis
3.2.1. A portion of the antimony in weight 0.5 g brands, Soooo, MSA or a mass of 0.1 g brand SS2 is placed in a beaker with a capacity of 50−100 cm3, pour 5 cm3 of hydrochloric acid dropwise while stirring, add the hydrogen peroxide. After dissolution of the sample poured 5 cm3 of tartaric acid, 5−10 cm-' of water and heated to boiling. The solution was boiled, cooled, poured into a volumetric flask with a capacity of 25 cm5, made up to the mark with water and mix.
The resulting solution of antimony sprayed into the flame and measure the absorbance at the wavelength of 232.1 nm.
At the same time carried out two test experience with all the applied reagents. The average value of absorption solution in the reference experiment is subtracted from the magnitude of absorption of a solution of the sample. The mass of Nickel in solution of the sample determined by the calibration schedule.
3.2.2. The construction of the calibration gra^shka
In a glass with a capacity of 50−100 cm3 hurt to 0.5 g of antimony brand Su0000, poured in 5 cm3 of hydrochloric acid and dissolved antimony when heated with the dropwise addition of hydrogen peroxide. After the dissolution of antimony is added 0,2; 0,4: 0.6 and 0.8 cm3 of a standard solution, which corresponds to 0,02; 0,04; 0.06; 0.08 mg of Nickel. Then pour in each Cup and 5 cm3 of tartaric acid, 5−10 cm3 of water. The solutions are boiled, cooled, transferred to a volumetric flask with a capacity of 25 cm3, bring to the mark with water and mix.
The concentration of Nickel in solution, respectively equal to 0.8; 1,6; 2,4: 3,2 mg/DM3.
The solutions comparison is sprayed into the flame in order of increasing Nickel content. Measurement of analytical signal, And for each solution and sample solution is carried out three times
and calculate the corresponding said arithmetic means, = (L + A: + A}) for each
solution. According to the average values of «L for comparison of solutions to build the calibration graph. The abscissa shows the lay concentration of Nickel in mg/DM3 and y-axis — absorption.
47
C. 4 GOST 1367.6−83
3.3. Processing of the results
3.3.1. Mass fraction Nickel (X) in percent is calculated by the formula
Y_ — 100 t I OOO 1000 •
where C is the concentration of Nickel in the sample solution found by the calibration graph and the average value A obtained for sample solution, mg/DM5;
Y — volume of sample solution, cm'; t — the weight of antimony,
3.3.2. The difference between the two results of parallel measurements and the difference of two analysis results with a confidence probability P = 0.95 does not exceed the allowable absolute differences of precision and reproducibility, are given in table. 2.
The 6L and ia 2
| Masson l<>.1 I Nickel. % | The absolute maximum discrepancy. % | |
| convergence | Worm (VISIBILITY | |
| Or 0.005 to 0.010 ncloc. | 0.002 | 0.003 |
| SV. 0.010. 0,020 * | 0.003 | 0.004 |
| * 0.020 ► 0.050 * | 0,005 | 0.006 |
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