GOST 1293.13-83
GOST 1293.13−83 lead-antimony Alloys. Methods for determination of Nickel (with Amendments No. 1, 2)
GOST 1293.13−83*
Group B59
STATE STANDARD OF THE USSR
LEAD-ANTIMONY ALLOYS
Methods for determination of Nickel
Lead-antimony alloys. Methods for the determination of nickel
AXTU 1709**
_______________
* The designation of the standard. Changed the wording, Rev. N 2.
** Changed revision, Rev. N 1.
Valid from 01.01.84
to 01.01.89*
_______________________________
* Expiration removed by Protocol No. 7−95
The interstate Council for standardization,
Metrology and certification (I & C N 11, 1995). -
Note the manufacturer’s database.
DEVELOPED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
A. P. Sychev, M. G. Sun, L. I. Maksay, R. D. Kogan
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Member Of The Board Of A. P. Snurnikov
APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards of February 8, 1983 N 703
MADE: the Change in N 1, approved and put into effect by the Decree of the USSR State Committee for standards from
Change N 1, 2 made by the manufacturer of the database in the text IUS N 2, 1988, ICS # 7, 2001
This standard establishes the atomic absorption and photometric methods for determination of mass fraction of Nickel from 0.0005 to 0.005% of lead-antimony alloys.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
General requirements for methods of analysis GOST 1293.0−83.
2. ATOMIC ABSORPTION METHOD
2.1. The essence of the method
The method is based on dissolving the sample in a mixture of nitric and tartaric acids, the spraying solutions in the air-acetylene flame and measuring the absorption lines of Nickel 232,0 nm.
2.2. Equipment and reagents
Atomic absorption spectrophotometer of any brand.
Air, compressed under a pressure of 2·10-6·10
PA (2−6 ATM), depending on equipment.
Acetylene in cylinders GOST 5457−75.
Tartaric acid according to GOST 5817−77, a solution of 400 g/DM.
Nitric acid GOST 4461−77, distilled in a quartz apparatus, or nitric acid according to GOST 11125−84 and diluted 1:1 and 1:3.
Lead nitrate according to GOST 4236−77, a solution of 200 g/DM.
Nickel GOST 849−70*.
________________
* On the territory of the Russian Federation GOST 849−97, here and hereafter. — Note the manufacturer’s database.
(Changed edition, Rev. N 1, 2).
2.3. Preparation for assay
2.3.1. Preparation of standard solutions of Nickel
Solution a: 0,1000 g of Nickel dissolved in 10 cmof nitric acid (1:1) when heated, transferred to a volumetric flask with a capacity of 1000 cm
, adjusted to the mark with water and mix.
1 cmof the solution contains 100 micrograms of Nickel.
Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm
, adjusted to the mark with water and mix.
1 cmof solution contains 10 mcg of Nickel.
(Changed edition, Rev. N 2).
2.3.2. To build a calibration curve in five out of six volumetric flasks with a capacity of 100 cmmake 2,5; 4; 6; 8 and 10 cm
standard solution B, which corresponds to 0,25; 0,4; 0,6; 0,8 and 1 µg/cm
of Nickel. All flasks is poured 10 cm
of a solution of tartaric acid, 25 cm
of nitric acid (1:3) and 40 cm
of a solution of nitrate of lead, adjusted to the mark with water and mix.
2.4. Analysis
A portion of the alloy weight of 5,0000 g is placed in a conical flask with a capacity of 250 cm, 10 cm poured
the solution of tartaric acid, 35 cm
of a solution of nitric acid (1:3) and dissolved by heating. After cooling, the solution was transferred to volumetric flask with a capacity of 100 cm
, adjusted to the mark with water and mix.
Analyzed and standard solutions sprayed in air-acetylene flame and measure the magnitude of the absorption line of Nickel 232,0 nm on an atomic absorption spectrophotometer.
Measurement conditions selected in accordance with the applicable device. Use two ways to measure the magnitude of the absorption depending on the instrument model.
For spectrophotometers with work mode «concentration», «concentration» and get the result on the scoreboard, µg/cm, or in the mode «absorption» method «limiting solutions», or by the calibration schedule.
On the other spectrophotometers operate in the mode «absorption» recording on a recording potentiometer or by deposition on a dial or digital device.
The method of «limiting solutions» is to obtain the counts for the analyzed solution and the two standard solutions, one of which gives a higher and the other lower count compared to the count for the analyzed solution.
(Changed edition, Rev. N 2).
2.5. Processing of the results
2.5.1. If the measurement is performed at the recording potentiometer, a ruler measure the height of the peaks in millimeters and build a calibration curve in the coordinates: — the concentration of the element in solution, mg/cm
;
is the peak height, mm.
When measurement of the absorption line of the element by analog and digital instrument calibration curve constructed in the coordinates: — the concentration of the element in the solution, µg/cm
;
— the readings of a dial or digital device.
Mass fraction of Nickel () in percent is calculated by the formula
where is the concentration of Nickel in sample solution, µg/cm
;
— Nickel concentration in solution in the reference experiment, µ g/cm
;
the volume of the solution of the alloy, cm
;
— weight alloy, g
.
2.5.2. The discrepancy between the results of parallel measurements (the difference between the largest and smallest results of parallel measurements) and the discrepancy between the results of the analysis
(the difference between the larger and the smaller of the results of the analysis) at a confidence level
=0.95 does not exceed the allowable absolute values of the differences given in the table.
| Mass fraction of Nickel, % | The limit of error of the results of the analysis |
The discrepancy between the results of parallel |
The discrepancy |
| To from 0,0005 0,0010 incl. | 0,0002 |
0,0002 | 0,0002 |
| SV. 0,0010 «0,0020 « | 0,0002 |
0,0003 | 0,0003 |
| «0,0020» 0,0050 « | 0,0004 |
0,0005 | 0,0005 |
The control accuracy of the analysis is carried out using standard samples or by other methods stipulated by GOST 1293.0−83.
The error analysis results (at a confidence probability =0,95) does not exceed the limit values
given in the table, under the following conditions: the discrepancy between the results of parallel measurements does not exceed the permissible, the results of accuracy control positive.
(Changed edition, Rev. N 2).
3. PHOTOMETRIC METHOD
3.1. The essence of the method
The method is based on dissolving the samples in nitric acid in the presence Vinokurova of sodium, extraction of the complex compound of Nickel with dimethylglyoxime chloroform from the ammonia solution. After Stripping with hydrochloric acid and oxidation with bromine to measure the optical density of the complex compound of Nickel with dimethylglyoxime at a wavelength of 445 nm in the spectrophotometer or in a region of wavelengths 440−455 nm in the photoelectrocolorimeter.
(Changed edition, Rev. N 1).
3.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Nitric acid GOST 4461−77 and diluted 1:1 and 1:2.
Hydrochloric acid by the GOST 3118−77, 0.5 M solution.
Sodium vinocity, a solution of 200 g/DM.
Ammonia water according to GOST 3760−79 diluted 1:1 and 1:50.
Dimethylglyoxime according to GOST 5828−77, a solution of 1 g/DMin ammonia solution 1:1.
Chloroform.
Bromine according to GOST 4109−79.
Bromine water, saturated.
Nickel GOST 849−70.
(Changed edition, Rev. N 2).
3.3. Preparation for assay
3.3.1. Preparation of standard solutions of Nickel.
Solution a: 0,1000 g of Nickel dissolved in 10 cmof nitric acid (1:1) in a beaker with a capacity of 250 cm
and boil to remove oxides of nitrogen. After cooling, the solution is transferred into a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
1 cmof solution A contains 0.1 mg of Nickel.
Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
1 cmof a solution contains 0.01 mg of Nickel.
(Changed edition, Rev. N 2)
.
3.3.2. To build a calibration curve in five out of six volumetric flasks with a capacity of 50 cmpour 1, 2, 3, 4 and 5 cm
standard solution B, which corresponds to 0,01; 0,02; 0,03; 0,04 and 0,05 mg of Nickel. In the sixth flask standard solution of Nickel is not introduced. To all flasks add 0.5−1 cm
of a solution of sodium Vinokurova and 1 cm of
bromine water. After 10 minutes, pour 5 cm
of ammonia solution (1:1) 5 cm
solution dimethylglyoxime, adjusted to the mark with water and mix. After 10 minutes measure the optical density of the solution at a wavelength of 445 nm in the spectrophotometer or in a region of wavelengths 440−455 nm in the photoelectrocolorimeter. Solution comparison is water.
According to the obtained values of optical density of the solutions (minus the optical density of the solution, which has not imposed a standard solution of Nickel) and their respective contents of Nickel to build a calibration curve.
(Changed edition, Rev. N 1).
3.4. Analysis
A portion of the alloy weight of 2,0000 g when the mass fraction of Nickel from 0.0005 to 0.001% or 1,0000 g when the mass fraction of Nickel from 0.001 to 0.005% is placed in a conical flask with a capacity of 250 cmand dissolved, respectively, in 30 or 15 cm
of nitric acid (1:2). Boil to remove oxides of nitrogen. Add 15 cm
of a solution of sodium Vinokurova and cooled. Transfer the solution into a separating funnel with a capacity of 100 cm
. Ammonia solution (1:1) was adjusted pH to 8−9 on the indicator paper, add 2cm
of a solution dimethylglyoxime, mix and leave for 5 min Then the solution was extracted twice, using each time 5 cm
of chloroform and shaking for 1 min.
The combined extracts are washed once with 5 cmof ammonia solution (1:50). Then the chloroform extract extravert two times by applying 5 cm
of hydrochloric acid solution and shaking each time for 1 min the combined water reextract transferred quantitatively into a measuring flask with a capacity of 50 cm
, add 0.5−1 cm
of solution Vinokurova sodium, 1 cm of
bromine water and then do as stated in claim
Solution comparison is the solution of the reference experiment.
The mass of a Nickel find in the calibration schedule.
(Changed edition, Rev. N 2).
3.5. Processing of the results
3.5.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in sample solution, found by calibration schedule, mcg;
— the weight of the portion of alloy,
3.5.2. The discrepancy between the results of parallel measurements (the difference between the largest and smallest results of parallel measurements) and the discrepancy between the results of the analysis
(the difference between the larger and the smaller of the results of the analysis) at a confidence level
=0.95 does not exceed the allowable absolute values of the differences given in the table.
The control accuracy of the analysis is carried out using standard samples or by other methods stipulated by GOST 1293.0−83.
The error analysis results (at a confidence probability =0,95) does not exceed the limit values
given in the table, under the following conditions: the discrepancy between the results of parallel measurements does not exceed the permissible, the results of accuracy control positive.
(Changed edition, Rev. N 2).
