GOST 3240.15-76
GOST 3240.15−76 magnesium Alloys. Methods for determination of Nickel (with Change No. 1)
GOST 3240.15−76
Group B59
INTERSTATE STANDARD
MAGNESIUM ALLOYS
Methods for determination of Nickel
Magnesium alloys.
Methods for determination of nickel
ISS 77.120.20
AXTU 1709
Date of introduction 1978−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of aviation industry of the USSR
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. REPLACE GOST 3240−56 in part of sec. VIII
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Item number |
| GOST 8.315−97 |
2.5 |
| GOST 3240.0−76 |
1.1 |
| GOST 3760−79 |
2.2, 3.2 |
| GOST 3773−72 |
2.2 |
| GOST 4212−76 |
3.2 |
| GOST 4461−77 |
3.2 |
| GOST 4465−74 |
2.2, 3.2 |
| GOST 4517−87 |
2.2, 3.2 |
| GOST 5456−79 |
2.2, 3.2 |
| GOST 5828−77 |
2.2 |
| GOST 5962−67 |
2.2, 3.2 |
| GOST 14261−77 |
2.2, 3.2 |
| GOST 25086−87 |
2.5 |
| THAT 6−09−08−2007−89 |
2.2 |
5. Limitation of actions taken by Protocol No. 2−92 of the Interstate Council for standardization, Metrology and certification (ICS 2−93)
6. EDITION with Change No. 1, approved in June 1987 (IUS 11−87)
This standard specifies the extraction-photometric methods for the determination of Nickel (at a mass fraction of Nickel from 0.0005 to 0.4%).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 3240.0.
2. The PHOTOMETRIC METHOD for the DETERMINATION of NICKEL (at a Nickel content of from 0.001 to 0.4%)
2.1. The essence of the method
The method is based on formation of Nickel compounds with dimethylglyoxime, which is extracted with chloroform. Dimethylglyoximate, Nickel photometric at a wavelength of 360 nm at 
(Changed edition, Rev. N 1).
2.2. Apparatus, reagents and solutions
The type СФ4а spectrophotometer or photoelectrocolorimeter type FEK-56, or FEK 60.
Hydrochloric acid according to GOST 14261, diluted 1:1.
Ammonia water according to GOST 3760.
Ammonium chloride according to GOST 3773, 25% solution.
Hydroxylamine hydrochloric acid according to GOST 5456, 10% freshly prepared solution.
Dimethylglyoxime according to GOST 5828, 1% solution in ethanol.
Ethyl alcohol according to GOST 5962*.
________________
* On the territory of the Russian Federation GOST R 51652−2000 (here and below).
Chloroform.
Ammonium vinocity on the other 6−09−08−2007, 20% solution, purified from traces of Nickel.
Nickel sulfate 7-water according to GOST 4465.
Bidistilled water, obtained according to GOST 4517.
Standard solutions of Nickel
Solution A, prepared as follows: 0,4784 g of Nickel sulfate was placed in a volumetric flask with a capacity of 1 DM, dissolved in water, poured 10 cm
of hydrochloric acid diluted 1:1, made up to the mark with water and mix.
1 cmof solution A contains 0.1 mg of Nickel.
Solution B is prepared as follows: 20 cmsolution And placed in a measuring flask with volume capacity of 1000 cm
, poured 5cm
of hydrochloric acid diluted 1:1, made up to the mark with water and mix.
1 cmof a solution contains 0.002 mg of Nickel.
The titer of the solution And set as follows: 50 cmstandard solution And placed in a beaker with a capacity of 300 cm
, adding 100 cm
of water, neutralized with ammonia on litmus paper, heated to a temperature of about 70 °C, added 40 cm
of dimethylglyoxime solution and kept for 2 h at a temperature of 30−50 °C.
Filter the precipitate on a filter «white ribbon», washed with warm water, put a sediment filter in calcined to constant weight and weighed porcelain crucible, dried, incinerated and calcined at a temperature of 950−1000 °C to constant weight.
At the same time conducting follow-up experience with all reagents. The titer of the solution And (), expressed in g/cm
of Nickel, calculated as follows:
where is the mass of the precipitate of oxide of Nickel, g;
— the mass of sediment in the reference experiment, g;
0,7858 — the ratio Nickel oxide to Nickel.
2.1; 2.2. (Changed edition, Rev. N 1).
2.3. Analysis
2.3.1. A sample of alloy weighing 1 g is placed in a beaker with a capacity of 250 cm, moistened with water and carefully poured in small portions of 20 cm
of hydrochloric acid diluted 1:1. After a violent reaction of the side of the Cup then rinsed with water and the contents of the Cup was heated until complete dissolution of the alloy. Then the side of the Cup washed with water and transferred the solution into a volumetric flask with a capacity of 100 cm
or 250 cm
, and then diluted to the mark with water and taken in a glass aliquot part of the solution in accordance with the table.1.
Table 1
| Mass fraction of Nickel, % |
Volume volumetric flasks, cm |
Aliquota part of the solution, see |
| From 0.001 to 0.008 |
100 |
50 |
| SV. 0,008 «0,040 |
100 |
10 |
| «0,040» 0,16 |
250 |
5 |
| «Of 0.16» to 0.40 |
250 |
2 |
Add 1−3 cmof hydrochloric acid hydroxylamine solution, 10 cm
of a solution of ammonium chloride and 5 cm
mortar Vinokurova ammonium, dilute the solution with water to 100 cm
and poured drop by drop ammonia solution, first diluted 2:3, and then diluted 1:5, to obtain a slightly alkaline reaction on litmus paper. The solution was transferred to a separatory funnel with a capacity of 200−300 cm
, add 3 cm
of a solution dimethylglyoxime, 6 cm
of chloroform and shaken for 1−2 min.
The solution is kept for delamination for 1−2 minutes, and then poured the chloroform extract in a dry test-tube with a glass stopper. Re-extraction was carried out for 1 min with 5 cmof chloroform.
The extract is decanted into the same vial. The combined extracts filtered through a dry filter and measure the optical density of the solution at 
Solution comparison is the chloroform extract control experience. To prepare the solution control the experience of taking hydrochloric acid in the quantity taken for analysis, the evaporated volume and is then carried out through all stages of the analysis.
Mass fraction of Nickel is determined by the calibration count
the IR.
2.3.2. Construction of calibration curve
Seven of cups with a capacity of 100 cmselect 0; 2,5; 5,0; 7,5; 10,0 and so on to 20 cm
with an interval of 2.5 cm
of a solution, top up with water up to 70 cm
and poured 5 cm
Vinokurova of ammonia, 2−3 drops of ammonia solution and perform the extraction with chloroform. Measure the optical density of the solution, as mentioned in paragraph
On the found values of optical density calibration curve building.
2.4. Processing of the results
2.4.1. Mass fraction of Nickel () in percent is calculated by the formula
where — volume of the initial solution, cm
;
— volume aliquote part of the solution, cm
;
— the weight of a Nickel, was found in the calibration schedule g;
— the weight of the portion of alloy,
(Changed edition, Rev. N 1).
2.4.2. Allowable absolute differences of the results of the parallel definitions should not exceed the values given in the table.
Table 2
| Mass fraction of Nickel, % |
The absolute allowable difference, % |
| From 0.001 to 0.003 |
0,0003 |
| SV. Of 0.003 «to 0.01 |
0,0005 |
| «Is 0.01» to 0.03 |
0,003 |
| «0,03» 0,10 |
0,005 |
| «To 0.10» to 0.20 |
0,01 |
| «Of 0.20» to 0.40 |
0,02 |
2.5. Control of measurement accuracy
Control the accuracy of measuring the mass fraction of Nickel is carried out using the State standard sample GSO 3363.
In addition, use the national standard samples of magnesium alloys, newly released, and industry standard samples of the enterprise of magnesium alloys, issued in accordance with GOST 8.315. Accuracy control measurement is carried out in accordance with GOST 25086.
Allowed to control the accuracy of measuring the mass fraction of Nickel by the method of additions.
(Added, Rev. N 1).
3. The PHOTOMETRIC METHOD for the DETERMINATION of NICKEL (at a mass fraction of Nickel from 0.0005 to 0.25%)
3.1. The essence of the method
The method is based on the education -furildioxime with Nickel ions in water hardly soluble complex compounds, which is well extracted with chloroform. The extraction is carried out at pH 9. The interfering effect of copper can be eliminated by adding sodium thiosulfate. The effect of manganese can be eliminated by introduction into the solution of hydroxylamine. Effects of magnesium, zirconium, iron, rare earth elements, cadmium and zinc to the introduction of tartrate of ammonium. The optical density measurement was carried out at
3.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Hydrochloric acid according to GOST 14261, diluted 1:1.
Nitric acid according to GOST 4461.
Hydroxylamine hydrochloric acid according to GOST 5456, 10% solution.
Ammonium vinocity on the other 6−09−08−2007, 20% solution.
Chernovetskiy sodium (sodium thiosulfate), 50% solution.
Ethyl alcohol according to GOST 5962.
Ammonia water according to GOST 3760, diluted 1:1 and 2% solution.
Nickel sulfate 7-water according to GOST 4465.-furildioxime, 1% alcoholic solution.
Chloroform, H. h
Standard solutions of Nickel concentration of 1 mg/cm(solution A) and 0.001 mg/cm
(solution B); prepared and stored according to GOST 4212.
Bidistilled water, obtained according to GOST 4517.
Universal indicator paper to determine the pH of 7,0−14,0.
3.1; 3.2. (Changed edition, Rev. N 1).
3.3. Analysis
3.3.1. A sample of alloy weighing 0.5 g is dissolved in 20 cmof hydrochloric acid in the beakers with a capacity of 300 cm
, 1−3 cm oxidize
nitric acid and boil to remove oxides of nitrogen. The solution was evaporated to wet salts, the residue is dissolved in 20−30 cm
of water when heated in a glass ready to fotomaterialy from the entire sample when the mass fraction of Nickel, up to 0.003%. When the mass fraction of Nickel in excess of 0.003% of the contents of the beaker transferred to a volumetric flask with a capacity of 100 cm
, is diluted to the mark with water, mixed and taken in a glass aliquot part of the solution in accordance with the table.3.
Table 3
| Mass fraction of Nickel, % |
Volume volumetric flasks, cm |
Aliquota part, cm |
| From 0.005 to 0.003 |
- |
Of the entire sample |
| SV. 0,003 «0,03 |
100 |
10 |
| «0,03» 0,08 |
100 |
4 |
| «Of 0.08» to 0.15 |
100 |
2 |
| «0,15» 0,25 |
100 |
1 |
If, after the dissolution of the sample is present in the insoluble zirconium, the latter filtered off.
To the solution in the beaker add 5 cmof hydrochloric acid hydroxylamine, 30 cm
Vinokurova ammonium 5 cm
of sodium thiosulfate, 4 cm
solution
-furildioxime and set the pH of the solution by universal indicator paper with ammonia to pH=9.
The solution is poured into a separating funnel with a capacity of 200 cm, the volume was adjusted with water to 100 cm
in 15 min and extracted with 5 cm
of chloroform for 5 min. Extraction was repeated two more times for 5 min, priliva the same amount of chloroform, draining every portion of the chloroform extract in a volumetric flask with a capacity of 25 cm
(pre-washed and dried), made up to the mark with chloroform and mixed well. If the extracts in the volumetric flasks turbid, filter them through a dry filter, the average density in the cell for photometry.
Measure the optical density of the solution on photocolorimeter or spectrophotometer at 
Mass fraction of Nickel is determined by the calibration count
the IR.
3.3.2. Construction of calibration curve
In glasses with a capacity of 250 cmis added a standard solution of Nickel B 0; 1; 3; 5; 7; 9; 11; 13; 15; 17; 19 and 20 cm
, which corresponds to 0; 0,001; 0,003; 0,005; 0,007; 0,009; 0,011; 0,013; 0,015; 0,017; 0,019 and 0.020 mg of Nickel. In all the cups add 5 cm
of hydrochloric acid hydroxylamine, 5 cm
Vinokurova ammonium 5 cm
of sodium thiosulfate, at 4 cm
-furildioxime and dilute with water to 50 cm
. Set pH 9 and further analysis are as indicated in claim 3.3.
1.
3.3.1;
3.4. Processing of the results
3.4.1. Mass fraction of Nickel () in percent is calculated by the formula
where the quantity of Nickel was found in the calibration schedule g;
— volume of initial solution, cm
;
— volume aliquote part, cm
;
— the weight of the portion of alloy,
3.4.2. Allowable absolute differences of the results of the parallel definitions should not exceed the values given in table.4.
Table 4
| Mass fraction of Nickel, % |
The absolute allowable difference, % |
| From 0.0005 to 0.001 |
0,0002 |
| SV. Of 0.001 «to 0.003 to |
0,0004 |
| «0,003» 0,009 |
0,0008 |
| «0,009» 0,02 |
0,0015 |
| «To 0.02» to 0.06 |
0,005 |
| «Of 0.06» to 0.15 |
0,01 |
| «0,15» 0,25 |
0,03 |
3.5. Control of measurement accuracy
Accuracy control measurement is carried out according to claim 2.5.
(Added, Rev. N 1).
