GOST 21877.11-76

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  ГОСТ 21877.11-76

GOST 21877.11−76 Babbit tin and lead. Methods for determination of Nickel (with Amendments No. 1, 2)

GOST 21877.11−76

Group B59

STATE STANDARD OF THE USSR

BABBIT TIN AND LEAD

Methods for determination of Nickel

Tin and lead babbits. Methods for the determination of nickel*

AXTU 1709**
________________
* The name of the standard. Changed the wording, Rev. N 1, 2.
** Added, Rev. N 2.

Valid from 01.01.78
to 01.01.83*
_______________________________
* Expiration removed
according to the Protocol of the Intergovernmental Council
for standardization, Metrology and certification
(IUS N 2, 1993). — Note
manufacturer database.

DEVELOPED by the Central research Institute for tin industry (Tsniiolovo)

Director V. A. Arsenico

Supervisor S. V. Meshkov

Executor G. V. Ivanova

INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

Zam. Minister N.N. Chepelenko

The draft all-Union scientific research Institute of standardization (VNIIS)

Director A. V. Gichev

APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from may 24, 1976 N 1264

REPLACE GOST 1380.6−70

MADE: the Change in N 1, approved and put into effect by the Decree of the USSR State Committee for standards from 14.02.83 N 805 with 01.07.83, Change No. 2, approved and put into effect by the Decree of the USSR State Committee for standards from 25.06.87 N 2464 with 01.03.88

Change N 1, 2 made by the manufacturer of the database in the text N 6 ICS 1983 ICS N 10 1987

This standard applies to tin and lead babbits and sets photocolorimetric and atomic absorption methods for the determination of Nickel (at a Nickel content of from 0.1 to 0.5%).

The method is based on dissolving the sample in a mixture of hydrochloric and bromatological acids with bromine. Tin and antimony is distilled off in the form of bromides, lead is removed in the form of chloride. Measure the optical density of the coloured compounds of Nickel with dimethylglyoxime in an alkaline medium at a wavelength of 520−550 nm. Copper is associated in a complex with Trilon B.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 21877.0−76.

2. APPARATUS, REAGENTS AND SOLUTIONS

Photoelectrocolorimeter or spectrophotometer with all accessories.

Hydrochloric acid by the GOST 3118−77 and diluted 1:1.

Bromatologia acid according to GOST 2062−77.

Bromine according to GOST 4109−79.

Mix to dissolve; prepared as follows: mix 45 cmbromatological acid, 45 cmof hydrochloric acid and 10 cmof bromine.

Hydrogen peroxide according to GOST 10929−76, a solution of 300 g/DM.

Potassium hydroxide according to GOST 24363−80, a solution of 50 g/DM.

Potassium-sodium vinocity according to GOST 5845−79, a solution of 50 g/DM.

Ammonium neccersarily according to GOST 20478−75, a solution of 50 g/DM.

Dimethylglyoxime according to GOST 5828−77, a solution of 10 g/DMin the solution is 50 g/DMof potassium hydroxide.

Salt is the disodium Ethylenediamine — N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652−73, solution 20 g/l; prepared as follows: 20.0 g Trilon B dissolved in water, the solution was transferred to volumetric flask with a capacity of 1 liter, adjusted to the mark with water and mix.

Nickel, standard solution; is prepared as follows: 0.1 g of metallic Nickel GOST 492−73 dissolved in 40−50 cmof hydrochloric acid diluted 1:1, 10−20 cmof hydrogen peroxide. After dissolution the contents of the beaker evaporated to dryness, add 20 cmof hydrochloric acid diluted 1:1 and again evaporated to dryness. The dry residue is dissolved in 100 cmof hydrochloric acid diluted 1:1, transferred into a volumetric flask with a capacity of 1 liter, adjusted to the mark with water and mix.

1 cmof the solution contains 0.1 mg of Nickel.

The copper solution; prepared as follows: 1.0 g of electrolytic copper is dissolved in 50 cmof nitric acid with a weak heating, the solution was cooled, transferred into a measuring flask with volume capacity of 1000 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.001 g of copper.

(Changed edition, Rev. N 1, 2).

2A. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF NICKEL CONTENT

2A.1. The essence of the method

The method is based on dissolution in a mixture of hydrochloric and bromatological acids with bromine. Tin and antimony is distilled off in the form of bromides, lead is removed in the form of chloride.

Measure the optical density of the coloured compounds of Nickel with dimethylglyoxime in an alkaline medium at a wavelength of 520−550 nm. Copper is associated in a complex with Trilon B.

Section 2A. (Added, Rev. N 1).

3. ANALYSIS

3.1. Photocolorimetric method for the determination of Nickel without separation of copper and lead by electrolysis

In a glass with a capacity of 250 cmis placed 0.5 g of sample and dissolve in 15 cmof the mixture for dissolution.

After dissolution of the samples the contents of the glass is evaporated to dryness, add 5 cmof the mixture to dissolve and evaporated again to dryness. This operation is repeated twice.

To the dry residue add 5 cmof hydrochloric acid density of 1.19 g/cm, 2−3 drops of hydrogen peroxide, and again evaporated to dryness. Treatment with hydrochloric acid is repeated. Add 2 cmof hydrochloric acid density of 1.19 g/cm, 50 cmwater, heated to dissolve the salts, cool, transfer the solution into volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

The resulting solution was filtered through a dry filter medium density, discarding first portion of filtrate.

Select aliquote part in accordance with the table.1.

Table 1

Aliquot part of the solution is placed in a volumetric flask with a capacity of 50 cm, add water to volume of 10 cm, 2 cmof a solution of potassium-sodium Vinokurova 10 cmof a solution of potassium hydroxide, 2 cmof mortar naternicola aluminum and 5 cmmortar dimethylglyoxime. After addition of each reagent the contents of the flask stirred. The resulting solution was left for 7−10 min. At the end of the time add 5 cmof the solution Trilon B, stirred, adjusted to the mark with water and after 5 minutes measure the optical density of the solution at 520−550 nm using cuvettes with a length of 1 cm with a Solution of comparison is water. To a solution of the reference experiment add the copper solution in the same amount as in the solution used to build the calibration curve.

(Changed edition, Rev. N 1, 2)

.

3.1.1. Photocolorimetric method for the determination of Nickel after separation of copper and lead by electrolysis (after the determination of cadmium chelatometric method).

The decomposition of babbit are in accordance with GOST 21877.9−76.

For the determination of Nickel in a glass with a capacity of 100 cmis taken 5 cmof the solution, add 5 cmRochelle salt (potassium-sodium vinocity, 4-water), 5 cmof a solution of potassium hydroxide, 5 cmsolution dimethylglyoxime. After each addition of reagent solution mix thoroughly. Leave the solution for 10 min, add 5 cmof the solution Trilon B concentration 0.05 mol/l, stirred, adjusted to the mark with water in a volumetric flask with a capacity of 50 cm. After 5 min measure the optical density of the solution in a cuvette with a layer thickness of 10 mm at a wavelength of 520−550 nm. Solution comparison is water.

(Added, Rev. N 1).

3.2. Construction of calibration curve

Eight volumetric flasks with a capacity of 50 cmeach make 0; 0,2; 0,4; 0,6; 0,8; 1,0; 1,2; 1,4 cmstandard solution of Nickel, added 1.5 cmof the copper solution in the analysis of babbit brand B88, 1.0 or 0.5 cm — in the analysis of babbit grade bn (depending on the size aliquote part of the solution) and continue the analysis as described in section 3.1.

(Changed edition, Rev. N 1).

4. PROCESSING OF THE RESULTS

4.1. The Nickel content () 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 of the original solution, cm;

 — the weight of the portion of the sample,

(Changed edition, Rev. N 1).

4.2. Allowable absolute differences the results of the analysis shall not exceed the values specified in table.2.

Table 2

(Changed edition, Rev. N 2).

5. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF NICKEL CONTENT

5.1. The essence of the method

The method is based on selective absorption of light from a standard source of Nickel atoms. The solution is sprayed in an acetylene-air flame atomic absorption spectrometer and measure the absorbance at the wavelength of 232,0 nm.

5.2. Apparatus, reagents and solutions

Equipment and reagents are the same as in the determination of copper (GOST 21877.3−76) and in addition:

Nickel metal according to GOST 492−73.

Standard solution of Nickel is prepared as follows: 0,1000 g of metallic Nickel is dissolved in 30 cmof nitric acid, diluted 1:1, and boil to remove oxides of nitrogen. The solution was cooled, transferred to a volumetric flask with a capacity of 1 DM, adjusted to the mark with water and mix.

1 cmof the solution contains 0.1 mg of Nickel.

5.3. Analysis

5.3.1. A portion of the Babbitt weight specified in the table.3, is placed in a beaker made of PTFE and poured in small portions to 10 cmof the mixture for dissolution. Next, carry out analysis as specified in GOST 21877.3−76.

Table 3

The obtained solution is sprayed in air-acetylene flame atomic absorption spectrometer and photometric at a wavelength of 232,0 nm under the conditions specified in GOST 21877.3−76.

The Nickel concentration set at the calibration schedule, fotometriya simultaneously with the analyzed solutions a series of solutions with known Nickel content.

5.3.2. To build graduirovochnyh graphics in volumetric flasks with a capacity of 50 cm, measure off microburette 0; 1,0; 2,0; 3,0; 4,0; 5,0 cmstandard solution of Nickel, is poured 10 cmof the mixture for dissolution, adjusted to the mark with water and mix.

Photometric solutions as well as analizziamo solutions.

According to the obtained average values of absorption and the known content of the Nickel to build the calibration graph.

5.4. Processing of the results

5.4.1. The Nickel content () in percent is calculated by the formula

,

where is the concentration of Nickel in fotometriya solution, µg/ml;

 — volume fotometricheskogo solution, cm;

 — the weight of the portion of the babbit, g;

 — conversion factor from micrograms to grams.

5.4.2. Allowable absolute discrepancies in the results of parallel measurements at a confidence probability of 0.95 should not exceed the values given in table.4.

Table 4

Section 5. (Added, Rev. N 1).