GOST 11930.6-79

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  ГОСТ 11930.6-79

GOST 11930.6−79 Materials surfacing. Methods for determination of Nickel (with Amendments No. 1, 2)

GOST 11930.6−79

Group B09

INTERSTATE STANDARD

MATERIALS SURFACING

Methods for determination of Nickel

Hard-facing materials. Methods of nickel determination

ISS 25.160.20
AXTU 1709

Date of introduction 1980−07−01

The decision of the State Committee USSR on standards on March 21, 1979 N 982 date of introduction is established 01.07.80

Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)

REPLACE GOST 11930−66 in part of sec. 5

EDITION (August 2011) with Amendments No. 1, 2 approved in December 1984, December 1989 (IUS 3−85, 3−90)


This standard establishes photocolorimetric methods for determination of Nickel rods for welding and powder alloys for surfacing.

(Changed edition, Rev. N 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 11930.0−79.

2. PHOTOCOLORIMETRIC METHOD for the DETERMINATION of NICKEL (at a mass fraction of Nickel from 1 to 5%)

2.1. The essence of the method

The method is intended for analysis of bars and powders for welding of alloys based on iron.

The method is based on formation of colored complex compounds of Nickel with dimethylglyoxime in an alkaline medium in the presence of an oxidant. The intensity of the colored solutions are measured on a photoelectrocolorimeter.

2.2. Apparatus, reagents and solutions

Photoelectrocolorimetry brands FEK-56, FEK-56M or any other type.

Sodium hydroxide according to GOST 4328−77, a solution with a mass fraction of 20%.

Congo red.

Potassium-sodium vinocity 4-water according to GOST 5845−79, a solution with a mass fraction of 20%.

Nitric acid GOST 4461−77 diluted 1:1.

Dimethylglyoxime according to GOST 5828−77, a solution with a mass fraction of 1%, is prepared by dissolving the reagent in the sample solution with a mass fraction of 5% alkali.

Ammonium neccersarily according to GOST 20478−75, a freshly prepared solution with a mass fraction of 10%.

Nickel GOST 849−70* with a Nickel content of not less than 99.95%.

_______________

* From 1 July 2009 standards 849−2008.


A standard solution of Nickel A; is prepared as follows: 0.1 g of Nickel dissolved in 20 cmof nitric acid, diluted 1:1. The resulting solution was transferred into a measuring flask with volume capacity of 1000 cm, is diluted to the mark with water and mix.

1 cmof the prepared solution contains 0.0001 g of Nickel.

2.3. Analysis

2.3.1. Nickel is determined in the filtrate after separation of the silicon GOST 11930.3−79. Of volumetric flasks with a capacity of 200 cmselect 5−25 cmof the analyzed solution into another volumetric flask with a capacity of 100 cm. In a flask pour 10 cmof a solution with a mass fraction of 20% Rochelle salt, is neutralized on a piece of paper, Congo solution with a mass fraction of 20% alkali and injected 5 cmof alkali in excess. Add 5 cmof solution with a mass fraction of 10% ammonium persulfate and 10 cmof a 1% strength solution dimethylglyoxime. After perelivania each of the reagent contents of the flask was stirred, topped up to the mark with water and mix again. Measure the optical density of colored solutions after 10 min by the photoelectrocolorimeter (540 nm) in a cuvette with a thickness of the absorbing layer 10 mm.

Background for the measurement is the solution, not containing dimethylglyoxime. The Nickel content in grams found by the calibration schedule.

2.1, 2.2. (Changed edition, Rev. N 2).

2.3.2. Construction of calibration curve

In a volumetric flask with a capacity of 100 cmis placed from 1 to 8 cmof a standard solution of Nickel with an interval of 1 cm. Enter a 10 cmsolution of Rochelle salt and further analysis are as indicated in claim 2.3.1.

2.4. Processing of the results

2.4.1. Mass fraction of Nickel () in percent is calculated by the formula

,

where is the mass of Nickel was found in the calibration schedule g;

 — aliquota part of the analyzed solution, cm;

 — the weight of the portion,

2.4.2. The difference between the largest and smallest results of the three parallel measurements, and the two results of the analysis at a confidence level of 0.95 does not exceed the permissible differences given in table.1.

Table 1

(Changed edition, Rev. N 2).

3. PHOTOCOLORIMETRIC METHOD for the DETERMINATION of NICKEL (at a mass fraction of Nickel from 0.5 to 2%) IN the PRESENCE of COBALT

3.1. The essence of the method

The method is intended for analysis of bars for welding cobalt-based.

The method is based on formation of colored complex compounds of Nickel with dimethylglyoxime in the presence of an oxidant in an alkaline medium after the separation of chromium and cobalt.

3.2. Reagents and solutions

Potassium-sodium vinocity according to GOST 5845−79, a solution with a mass fraction of 20%.

Sodium hydroxide according to GOST 4328−77, a solution with a mass fraction of 20 and 5%.

Ammonium neccersarily according to GOST 20478−75, a freshly prepared solution with a mass fraction of 10%.

Dimethylglyoxime according to GOST 5828−77, a solution with a mass fraction 1%; prepared by dissolving in a solution with a mass fraction of 5% sodium hydroxide.

The acid chloride.

Sodium chloride according to GOST 4233−77.

Ammonium chloride according to GOST 3773−72.

Ammonium phosphate according to GOST 10651−75.

Ammonia water according to GOST 3760−79, a solution with a mass fraction of 25%.

Standard solution B of Nickel with a content of 1 cm0,00001 g of Nickel, prepared by dilution of a standard solution of Nickel A, see p.2.2.

3.3. Analysis

3.3.1. Nickel is determined in the filtrate after separation of the silicon GOST 11930.3−79. Of volumetric flasks with a capacity of 200 cm25 cm selecttest solution in a glass with a capacity of 100−200 cm, flow 10 cmof perchloric acid and heated to release heavy fumes of perchloric acid. To the boiling solution cautiously add 0.1−0.2 g sodium chloride and continue heating. The operation is repeated until the complete disappearance of the color of chrome. The solution is diluted with water to about 10−20 cmand poured into the glass with a solution containing 50 cmof distilled water, 2 g of ammonium chloride, 2 g of ammonium phosphate and 10−15 cmof an aqueous solution of ammonia.

The contents of the beaker are heated to boiling and boil for 1−2 min. the Solution was cooled, poured into a volumetric flask with a capacity of 100 cm, diluted with distilled water to the mark and mix.

Part of the solution was filtered into a dry beaker and taken 5−25 cmof solution, depending on the Nickel content in a volumetric flask with a capacity of 100 cm. Pour 5 cmof ammonia solution, 10 cmof solution with a mass fraction of 20% Rochelle salt, 10 cmsolution with a mass fraction of 10% ammonium naternicola 10 cmof a solution with a mass fraction of 1% dimethylglyoxime. After addition of each reagent the contents of the flask stirred. Measure the optical density of the colour solution after 10 minutes on a photoelectrocolorimeter with a green optical filter (490 nm) in a cuvette with a thickness of the absorbing layer is 50 mm.

As a solution comparison solution is used in the reference experiment on the content of Nickel in chemicals. The value of optical density of the colored test solution find the mass of Nickel in the calibration schedule.

3.3.2. Construction of calibration curve

In a volumetric flask with a capacity of 100 cmplaced 1, 2, 3,…, 10 cmstandard solution B of Nickel, on the Congo neutralized with aqueous ammonia and impose an excess of 5 cm; flow 10 cmof a solution with a mass fraction of 20% Rochelle salt and further analysis are as indicated in claim 3.3.1.

3.4. Processing of the results

3.4.1. Mass fraction of Nickel () in percent is calculated by the formula

,

where is the mass of Nickel was found in the calibration schedule g;

 — aliquota part of the analyzed solution, cm;

 — the weight of the portion,

3.4.2. The difference between the largest and smallest results of the three parallel measurements, and the two results of the analysis at a confidence level of 0.95, should not exceed the values of permissible differences given in table.2.

Table 2

(Changed edition, Rev. N 2).