GOST 23859.6-79
GOST 23859.6−79 heat-resistant Bronze. Method for the determination of Nickel (with Amendments No. 1, 2)
GOST 23859.6−79
Group B59
INTERSTATE STANDARD
BRONZE HIGH-TEMPERATURE
Method for the determination of Nickel
Bronze fire-resistance. Method for the determination of nickel
AXTU 1709
Date of introduction 1981−01−01
Resolution of the USSR State Committee for standards, dated 16 October 1979, N 3937 time of the introduction set with 01.01.81
Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)
EDITION with Amendments No. 1, 2 approved in June 1985, March 1990 (IUS 9−85, 7−90).
This standard sets the photometric method for the determination of Nickel (at a mass fraction of Nickel from 0.005 to 0.9%) and titrimetric method for the determination of Nickel (at a mass fraction of Nickel from 0.4 to 0.9%) in high-temperature copper alloys.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086−87 with the addition of a GOST 23859.1−79, sec. 1.
(Changed edition, Rev. N 2).
The photometric method for the determination of Nickel
The method is based on formation of Nickel coloured compounds with dimethylglyoxime in an alkaline medium in the presence of an oxidant and measuring the optical density of colored solution.
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid GOST 4461−77 diluted 1:1.
Sulfuric acid GOST 4204−77, diluted 1:1.
Tartaric acid according to GOST 5817−77, a solution of 200 g/DM.
Hydrofluoric acid according to GOST 10484−78.
Potassium hydroxide GOST 9285−78, 200 solution and 50 g/DM.
Ammonium neccersarily according to GOST 20478−75, a solution of 30 g/DM, freshly prepared.
Deacetyltaxol (dimethylglyoxime) according to GOST 5828−77 a solution of 10 g/DMsolution of potassium hydroxide 50 g/DM
.
Nickel brand H0.
Standard solutions of Nickel.
Solution A. 1 g of metallic Nickel dissolved in 20 cmof nitric acid and nitrogen oxides is removed by boiling. The solution was transferred to volumetric flask with a capacity of 1 DM
, made up to the mark with water and mix. 1 cm
of the solution contains 0.001 g of Nickel.
Solution B. 10 cmof the solution is placed in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix. 1 cm
of a solution contains 0.0001 g of Nickel.
Sec. 2. (Changed edition, Rev. N 1, 2).
3. ANALYSIS
3.1. For bronzes containing chromium
The sample of bronze with a weight of 1 g was placed in a platinum Cup, add 10 cmof nitric acid, 2 cm
hydrofluoric acid and dissolved by heating. Then add 5 cm
of sulphuric acid and the solution is evaporated prior to the allocation of white smoke of sulfuric acid. The residue is cooled, rinse the walls of the Cup with water and again evaporated prior to the allocation of white smoke of sulfuric acid. After cooling, the residue is dissolved in water when heated. The solution was cooled, transferred to a beaker with a capacity of 300 cm
, is diluted with water to a volume of 150 cm
and produce copper by electrolysis according to GOST 23859.1−79.
The electrolyte is evaporated to a volume of 60−70 cm, transferred into a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
Aliquot part of the solution (see table) is placed in a volumetric flask with a capacity of 100 cm, add with constant stirring 10 cm
of a solution of tartaric acid, 20 cm
of a solution of potassium hydroxide (200 g/DM
) 10 cm
solution dimethylglyoxime 10 cm
of a solution of ammonium naternicola, made up to the mark with water and mix.
| Mass fraction of Nickel, % |
The volume aliquote part selected for analysis, see |
The weight of the portion corresponding to aliquote part of the solution, g |
| From 0.005 to 0.2 incl. |
20 | 0,2 |
| SV. Of 0.2 «to 0.9 « |
5 |
0,05 |
The optical density was measured after 15 min in the spectrophotometer at 445 nm or photoelectrocolorimeter with a blue filter in a cuvette with a thickness of absorbing layer 1 cm relative to the same solution, but without adding dimethylglyoxime.
(Changed edition, Rev. N 1, 2).
3.2. For bronzes not containing chromium
The sample of bronze with a weight of 1 g was placed in a beaker with a capacity of 300 cm, cover with a watch glass, add 15 cm
of nitric acid and carefully dissolved by heating. Once dissolved, rinse the glass and walls of glass with water and remove the oxides of nitrogen by boiling. The solution was then diluted with water to a volume of 150 cm
, up to 4 cm
of sulphuric acid and produce copper by electrolysis according to GOST 23859.1−79.
The electrolyte is evaporated to a volume of 60−70 cmand then do as described in claim 3.1.
3.3. Construction of calibration curve
In a volumetric flask with a capacity of 100 cmpour consistently 0; 1,0; 2,0; 3,0; 4,0 and 5,0 cm
standard solution B of Nickel, dilute with water to volume of 20 cm
, add 10 cm
of a solution of tartaric acid and then act as described in claim 3.1.
3.2, 3.3. (Changed edition, Rev. N 1).
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part of the solution,
4.2. Discrepancies in the results of three parallel definitions should not exceed the values permitted by the divergence (
the rate of convergence), calculated according to the formula
where — mass fraction of Nickel in the alloy, %.
(Changed edition, Rev. N 2).
4.3. Discrepancies in the results analysis, obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values calculated according to the formula
where — mass fraction of Nickel in the alloy, %.
4.4. Control of accuracy of analysis results is carried out according to State standard samples of heat-resistant (CR) bronze or supplements method, or comparison of the results obtained by atomic absorption method in accordance with GOST 25086−87.
4.3, 4.4. (Added, Rev. N 2).
Titrimetric method for the determination of Nickel
The method is based on precipitation of Nickel in ammoniacal solution dimethylglyoxime in the form of slightly soluble chelation in the presence of citric or tartaric acid and determining the Nickel chelatometric titration with eriochrome black T or murexide as indicators.
5. REAGENTS AND SOLUTIONS
Nitric acid GOST 4461−77 and diluted 1:1.
Hydrochloric acid by the GOST 3118−77 and diluted 1:1.
Sulfuric acid GOST 4204−77, diluted 1:1.
The mixture of acids to dissolve: to mix one part of concentrated nitric acid and three parts concentrated hydrochloric acid.
Tartaric acid according to GOST 5817−77, a solution of 100 g/DM.
Citric acid according to GOST 3652−69, a solution of 100 g/DM.
Ammonia water according to GOST 3760−79.
Rectified ethyl alcohol GOST 18300−87.
Dimethylglyoxime according to GOST 5828−77, alcoholic solution of 10 g/DM.
Ammonium chloride according to GOST 3773−72.
Ammonium sulfate according to GOST 3769−78.
Hydrogen peroxide according to GOST 10929−76.
Salt is the disodium Ethylenediamine — N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652−73; 0,02 mol/DMsolution: 7.44 g Trilon B dissolved in 500 cm
of water, the solution is placed in a volumetric flask 1 DM
and topped to the mark with water.
Sodium hydroxide according to GOST 4328−77, a solution of 200 g/DM.
Methyl red indicator, ethanolic solution of 1 g/DM.
Eriochrome black T, saturated aqueous solution.
Buffer solution with pH 10: 570 cmof ammonia solution is added 70 g of ammonium chloride and dilute to 1 cm
of water.*
________________
* The text matches the original. — Note the CODE.
Magnesium sulfate according to GOST 4523−77, 0.02 mol/DMof a solution of 4.93 g of magnesium sulfate dissolved in 500 cm
of water, the solution is placed in a volumetric flask with a capacity of 1 DM
and topped to the mark with water.
Murexide, mixture with sodium chloride 1:100.
Nickel stamps BUT* according to GOST 849−97.
________________
* The text matches the original. — Note the CODE.
A standard solution of Nickel: 1 g of Nickel is dissolved in a beaker with a capacity of 250 cmto 20 cm
of hydrochloric acid (1:1) and 10 cm
of hydrogen peroxide, added in small portions. After reconstitution, the solution boiled for 1 min to decompose excess hydrogen peroxide, cooled, transferred to a volumetric flask with a capacity of 1 DM
, made up to the mark with water and mix.
1 cmof the solution contains 0.001 g of Nickel.
5.1. The installation of the mass concentration of the solution Trilon B Nickel
In a glass or flask with a capacity of 500 cmis placed 10 cm
to the standard solution of Nickel, dilute with water to volume 160−70* cm
, and further receives, as specified in clause 6.1 or 6.2.
__________________
* The text matches the original. — Note the CODE.
5.2. The mass concentration of the solution Trilon B (), expressed in grams of Nickel per 1 cm
of the solution for titration according to claim 6.1, is calculated by the formula
where is the mass of Nickel in aliquotes part taken for the titration, g;
— volume of solution Trilon B, mass concentration of which is determined, cm
;
— the volume of solution of magnesium sulfate, used for titration of Trilon B, cm
;
— a correction factor to the mass concentration of the solution Trilon B.
5.3. Setting the correction factor to the mass concentration of the solution Trilon B ()
In a glass or flask with a capacity of 500 cmfrom burette measure out 10 cm
of the solution Trilon B, add 100−120 cm
of water, 2−3 drops methyl red, 1 drop of sodium hydroxide solution, 4 cm
buffer solution, 4−5 drops eriochrome black
, water to 200 cm
and titrated with a solution of sulphate of magnesium to transition blue-green color to pink-purple.
Correction factor () is calculated by the formula
where — volume of solution Trilon B taken in the titration, cm
;
— the volume of solution of magnesium sulfate, spent on titration, sm
.
5.4. The mass concentration of the solution Trilon B (), expressed in grams of Nickel per 1 cm
, for titration according to claim 6.2 is calculated by the formula
where is the mass of Nickel in aliquotes part taken for the titration, g;
— volume of solution Trilon B, spent on titration, sm
.
Note. Allowed to set, the mass concentration Trilon B on Nickel and on State standard samples of heat-resistant (CR) bronzes.
Sec. 5. (Changed edition, Rev. N 2).
6. ANALYSIS
The weight of bronze weighing 2 g were placed in a glass with a capacity of 300 cm, added 40 cm
of a mixture of acids and dissolved by heating. Upon dissolution of the sample add 30 cm
of sulphuric acid (1:1) and the solution is evaporated prior to the allocation of white smoke of sulfuric acid. The residue is cooled, carefully add 5 cm
of nitric acid (1:1), dilute with water to 150 cm
and the electrolysis is carried out according to GOST 23859.1−79. At the end of the electrolysis, the electrodes are washed with a small amount of water over the electrolyte. Heat the glass with a solution (~ 30 °C), add 5 cm
of solution wine (citric) acid and neutralized with ammonia to slightly alkaline environment (pH 10) universal indicator paper and 2−3 drops excess. Then add 5−6 cm
solution dimethylglyoxime, is kept on the warm bath for 10 minutes, add to best minimize 1 g of ammonium sulfate. The solution with precipitate was cooled, the precipitate is filtered off on a medium density filter, washed 8 times with hot water with addition of 5 cm
of ammonia per 1 DM
of water and finally 2 times with hot water, stirring the sediment with a jet of water from the washed
Ki.
6.1. Titration with indicator eriochrome black T
The precipitate from the filter washed with water in a glass, which conducted the deposition, dissolved in 10 cmof hot hydrochloric acid (1:1), the filter was washed 2−3 times with hot water and the filter discarded. Solution and the precipitate was heated until complete dissolution. Cool the solution to room temperature, add water to 160−170 cm
, 15 cm
of Trilon B solution, 2−3 drops of methyl red and neutralize with sodium hydroxide solution, adding the last of the burette at the end of neutralization dropwise until the pink color transition to yellow. Add 4 cm
of buffer solution, 5 drops of solution eriochrome black
, dilute with water to 200 cm
and titrated with a solution of magnesium sulfate until the colour blue-green to pink-purple.
6.2. Titration with indicator murexide
The precipitate is dissolved on the filter with 20−25 cmof hot nitric acid (1:1) in glass, which conducted the deposition. The filter was washed 5−6 times with hot water and discarded. The solution was boiled for 8−10 min until dissolution of dimethylglyoximate of Nickel, cooled, diluted with water to 160−170 cm
, add ammonia solution till the odor (slightly alkaline medium), 0.01 g of murexide and titrated with a solution of Trilon B to switch the yellow color of the solution in red-violet.
Sec. 6. (Changed edition, Rev. N 2).
7. PROCESSING OF THE RESULTS
7.1. Long mass of Nickel () in percentage during the titration according to claim 6.1 is calculated by the formula
where — volume of solution Trilon B taken in the titration, cm
;
— the volume of solution of magnesium sulfate consumed in the titration, cm
;
— correction factor of the solution Trilon B Nickel, g/cm
;
— mass concentration of the solution Trilon B Nickel, g/cm
;
— the weight of the portion of the alloy,
G.
7.2. Mass fraction of Nickel () in percentage during the titration according to claim 6.2 is calculated by the formula
where — volume of solution Trilon B, used for titration, cm
;
— mass concentration of the solution Trilon B Nickel, g/cm
;
— the weight of the portion of alloy,
7.3. Discrepancies in the results of three parallel definitions should not exceed the values permitted by the divergence (
the rate of convergence) of 0.04%.
7.4. Discrepancies in the results analysis, obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed 0.06 percent.
7.5. Control of accuracy of analysis results is carried out according to State standard samples of heat-resistant (CR) bronze or comparison of the results obtained photometric or atomic absorption methods in accordance with GOST 25086−87.
Sec. 7. (Added, Rev. N 2).
