GOST 19863.16-91
GOST 19863.16−91 Alloy titanium-Nickel. Method for the determination of Nickel
GOST 19863.16−91
Group B59
STATE STANDARD OF THE USSR
ALLOY TITANIUM-NICKEL
Method for the determination of Nickel
Titanium-nickel alloy.
Method for the determination of nickel
AXTU 1709
Date of introduction 1992−07−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of aviation industry of the USSR
DEVELOPERS
V. G. Davydov, doctor of engineering. Sciences; V. A. Moshkin, PhD. tech. Sciences; G. I. Friedman, PhD. tech. Sciences; L. A. Tenyakova, A., Korolyov
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 5.05.91 N 626
3. INTRODUCED FOR THE FIRST TIME
4. The frequency of inspection — 5 years
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Section number, paragraph |
| GOST 849−70 |
3 |
| GOST 3118−77 |
3 |
| GOST 3652−69 |
3 |
| GOST 3760−79 |
3 |
| GOST 4204−77 |
3 |
| GOST 4236−77 |
3 |
| GOST 4461−77 |
3 |
| GOST 5456−79 |
3 |
| GOST 10652−73 |
3 |
| GOST 18300−87 |
3 |
| GOST 25086−87 |
1.1 |
| THAT 6−09−1678−86 |
3 |
This standard specifies the method of chelatometric determination of Nickel for the mass concentration of from 40.0 to 60.0% of.
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086 with the Supplement.
1.1.1. For the results analysis be the arithmetic mean of results of two parallel measurements.
2. THE ESSENCE OF THE METHOD
The method is based on dissolving the sample in sulfuric acid, the precipitation of Nickel dimethylglyoxime of ammonia solution containing citric acid, dissolving the precipitate of dimethylglyoximate of Nickel in hydrochloric acid, the binding of Nickel Trilon B and titrate the excess Trilon B nitrate lead indicator of acid chrome dark blue.
3. APPARATUS, REAGENTS AND SOLUTIONS
Drying oven with thermostat.
Thermometer liquid-in-glass or mercury up to 100 °C with interval 1 °C.
Ashless filters on the other 6−09−1678.
Hydrochloric acid according to GOST 3118 density of 1.19 g/cm, a solution of 1:1.
Hydroxylamine hydrochloride according to GOST 5456, solution 100 g/DM.
Nitric acid according to GOST 4461 density of 1,35−1,40 g/cmand a solution of 1:1.
Citric acid according to GOST 3652, a solution of 500 g/DM.
The technical rectified ethyl alcohol according to GOST 18300.
Dimethylglyoxime, a solution of 5 g/l5 g dimethylglyoxime dissolved in 1000 cm
of ethanol.
Ammonia water according to GOST 3760.
Indicator of acid chrome dark blue: 0.1 g of the reagent was placed in a conical flask with a capacity of 100 cm, 50 cm pour the
water and dissolve in low heat. After complete dissolution the solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
The indicator Congo red: 0.1 g of the reagent dissolved in 100 cmof water at low heat.
Indicator paper Congo: medium-density filters («white ribbon») is impregnated with a solution of the Congo, dried in a drying Cabinet at a temperature of (110±5) °C, sliced and stored in boxe. The paper is suitable for use within one month.
Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652, solution with molar concentration of 0.025 mol/DM: 9,31 g Trilon B dissolved in 200 cm
of water, filtered through a medium density filter (white ribbon) in a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
Lead nitrate according to GOST 4236, solution with molar concentration of 0.025 mol/DM: of 8.28 g of lead nitrate dissolved in 30 cm
of a solution of nitric acid and evaporated to dryness. To the dry residue poured 100 cm
of water and heated to dissolve the salts, cooled to room temperature and filtered through a medium density filter (white ribbon) in a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
Nickel GOST 849* stamps N22.
_______________
* On the territory of the Russian Federation GOST 849−97. — Note the manufacturer’s database.
A standard solution of Nickel
1 g of Nickel is placed in a conical flask with a capacity of 250 cm, 40 cm pour the
nitric acid solution and dissolved by heating. After complete dissolution of Nickel poured 20 cm
of sulfuric acid solution 1:1 and evaporated until the appearance of white fumes of sulfuric acid. After cooling to room temperature the solution was carefully poured 100 cm
of water and boil for 2 min. the Solution was cooled to room temperature, poured into a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
1 cmof the solution contains 0.001 g of Nickel.
To establish the mass concentration of Trilon B by Nickel () in three conical flasks with a capacity of 250 cm
is placed aliquot part of a standard solution of Nickel at 10 cm
, 30 cm, pour the
hydrochloric acid solution, 70 cm
of water, 20 cm
of a solution of Trilon B. the Solution is neutralized with ammonia until the color of Congo paper from blue to red, and 15−20 drops of ammonia added in excess, pour 1 cm
of the indicator acid chrome dark blue and titrate with a solution of nitrate of lead to sharp changes in the solution colour from blue to crimson.
Mass concentration of Trilon B Nickel (), g/cm
, is calculated by the formula
where mass concentration of a standard solution of Nickel, g/cm
;
— the volume of a standard solution of Nickel, used for titration, cm
;
— volume of solution Trilon B, used for titration, cm
;
— the volume of solution of nitrate of lead consumed for titration, cm
;
— the relation between the solutions of Trilon B and nitrate of lead.
Set the ratio between the solutions of Trilon B and nitrate of lead in a conical flask with a capacity of 250 cm
is placed 10 cm
solution of Trilon B, go 30 cm
of the hydrochloric acid solution, 70 cm
of water. The solution is neutralized with ammonia until the color of Congo paper from blue to red, add 15−20 drops of ammonia in excess, pour 1 cm
of the indicator solution acid chrome dark blue and titrate with a solution of nitrate of lead to the transition of the blue color of the solution in raspberry.
4. ANALYSIS
4.1. A portion of sample weighing 0.25 g was placed in a conical flask with a capacity of 250 cm, 40 cm poured
sulfuric acid solution is 1:2 and heated to complete dissolution. Add nitric acid dropwise until the disappearance of the violet color of the solution and three drops in excess, is evaporated until the appearance of white fumes of sulfuric acid and heating was continued for 2 minutes After cooling to room temperature the solution is poured 50 cm
of water and boil for 1−2 min.
The solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix.
4.2. Aliquot part of the solution was 50 cm,transferred to a conical flask with a capacity of 500 cm
, flow 15 cm
of the citric acid solution and neutralized with ammonia to a faint smell, add 100 cm
of solution dimethylglyoxime, ammonia to smell and incubated for 20 min at a temperature of 50−60 °C.
4.3. The precipitate was filtered off through a filter medium density («white ribbon»), washed 10−12 times with hot water, dissolve on the filter in 30 cmof a hydrochloric acid solution, and the filter washed with hot water (until the red color of Congo paper, is placed on the edge of the filter), collecting the washings in the same flask.
4.4. If the copper alloy is present, the deposition operation is repeated, adding ammonia to smell, 80 cmdimethylglyoxime solution, incubated for 20 min at a temperature of 50 — 60 °C and continue according to claim 4.3.
4.5. Poured into a solution of Trilon B in the table and incubated for 20 min at room temperature.
| Mass fraction of Nickel, % |
The volume of solution Trilon B, cm |
| From 40.0 to 50.0 incl. |
20 |
| SV. 50,0 «60,0" |
25 |
The solution is poured ammonia until the blue color of the transfer paper, Congo red, 15−20 drops in excess, is added 1 cmof the indicator acid chrome dark blue and titrate with a solution of nitrate of lead to a sharp change in the blue color of the solution in raspberry.
5. PROCESSING OF THE RESULTS
5.1. Mass fraction of Nickel () in percent is calculated by the formula
where — volume of solution Trilon B, used for titration, cm
;
— the volume of solution of nitrate of lead consumed for titration, cm
;
— established mass concentration of the solution Trilon B Nickel, g/cm
;
— the relation between the solutions of Trilon B and nitrate of lead;
— weight of sample in aliquote part of the solution
G.
5.2. The absolute maximum discrepancy should not exceed: results of parallel measurements is 0.3%; the results of the analysis of 0.4%.
