GOST 27981.5-2015

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  ГОСТ 27981.5-2015

GOST 27981.5−2015 Copper of high purity. Photometric methods of analysis

GOST 27981.5−2015

INTERSTATE STANDARD

HIGH PURITY COPPER

Photometric methods of analysis

Copper of high purity. Photometric methods of analysis

ISS 77.120.30

Date of introduction 2016−11−01

Preface

Goals, basic principles and main procedure of works on interstate standardization have been established in GOST 1.0−92 «interstate standardization system. Basic provisions» and GOST 1.2−2009 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. Rules of development, adoption, application, renewal and cancellation"

Data on standard

1 DEVELOPED by the Technical Committee for standardization TC 368 «Copper"

2 recorded by the Interstate technical Committee for standardization MTK 503 «Copper"

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (minutes of August 27, 2015 N 79-P)

The adoption voted:

4 by Order of the Federal Agency for technical regulation and Metrology dated 17 February 2016 N 52 St interstate standard GOST 27981.5−2015 promulgated as the national standard of the Russian Federation from November 1, 2016.

5 REPLACE GOST 27981.5−88


Information about the changes to this standard is published in the annual reference index «National standards», and the text changes and amendments — in monthly information index «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in the monthly information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet (www.gost.ru)

1 Scope

This standard establishes photometric methods for determination of components in high purity copper, are given in table 1.


Table 1

2 Normative references

This standard uses the regulatory references to the following international standards:

GOST 61−75 Reagents. The acetic acid. Specifications

GOST 84−76 Reagents. Sodium carbonate 10-water. Specifications

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 859−2014 Copper. Brand

GOST 860−75 Tin. Specifications

GOST 1089−82 Antimony. Specifications

GOST 1770−74 (ISO 1042−83, ISO 4788−80) Glassware volumetric laboratory glass. Cylinders, beakers, flasks, test tubes. General specifications

GOST 1973−77 arsenious Anhydride. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 3652−69 Reagents. Citric acid monohydrate and anhydrous. Specifications

GOST 3760−79 Reagents. The aqueous ammonia. Specifications

GOST 3765−78 Reagents. Ammonium molybdate. Specifications

GOST 3773−72 Reagents. The ammonium chloride. Specifications

GOST 4197−74 Reagents. Sodium atomistically. Specifications

GOST 4198−75 Reagents. Potassium phosphate odnosemjannyj. Specifications

GOST 4204−77 Reagents. Sulphuric acid. Specifications

GOST 4232−74 Reagents. The potassium iodide. Specifications

GOST 4328−77 Reagents. Sodium hydroxide. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 4465−74 Reagents. Nickel (II) sulphate 7-aqueous. Specifications

GOST 5456−79 Reagents. Of hydroxylamine hydrochloride. Specifications

GOST ISO 5725−6-2003 Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice
________________
In the Russian Federation GOST R ISO 5725−6-2002 «Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice».


GOST 5789−78 Reagents. Toluene. Specifications

GOST 5817−77 Reagents. Acid wine. Specifications

GOST 5828−77 Reagents. Dimethylglyoxime. Specifications

GOST 5841−74 Reagents. Hydrazine sulfate

GOST 5845−79 Reagents. Potassium-sodium vinocity 4-water. Specifications

GOST 5848−73 Reagents. Formic acid. Specifications

GOST 5955−75 Reagents. Benzene. Specifications

GOST 6006−78 Reagents. Butanol-1. Specifications

GOST 6008−90 metallic Manganese and nitrated manganese. Specifications

GOST 6259−75 Reagents. Glycerin. Specifications.

GOST 6552−80 Reagents. Orthophosphoric acid. Specifications

GOST 6563−75 technical articles made of noble metals and alloys. Specifications

GOST 6691−77 Reagents. Urea. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9428−73 Reagents. Silicon (IV) oxide. Specifications

GOST 9849−86 iron Powder. Specifications

GOST 10298−79 Selenium technical. Specifications

GOST 10652−73 Reagents. Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid, 2-water (Trilon B). Specifications

GOST 10928−90 Bismuth. Specifications

GOST 10929−76 Reagents. Hydrogen peroxide. Specifications

GOST 11069−2001 primary Aluminium. Brand

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 11773−76 Reagents. Sodium phosphate disodium. Specifications

GOST 12026−76 laboratory filter Paper. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 18300−87 ethyl rectified technical. Specifications
________________
In the Russian Federation GOST R 55878−2013 «ethanol technical rectified hydrolysis. Technical conditions».


GOST 19807−91 Titanium and titanium wrought alloys. Brand

GOST 20015−88 Chloroform. Specifications

GOST 20288−74 Reagents. The carbon tetrachloride. Specifications

GOST 20478−75 Reagents. Ammonium neccersarily. Specifications

GOST 20490−75 Reagents. Potassium permanganate. Specifications

GOST 22280−76 Reagents. Sodium citrate 5,5-water. Specifications

GOST 22867−77 Reagents. The ammonium nitrate. Specifications

GOST 24104−2001 laboratory Scales. General technical requirements
________________
In the Russian Federation GOST R 53228−2008 «Scales non-automatic actions. Part 1. Metrological and technical requirements. Test».


GOST 24363−80 Reagents. Potassium hydroxide. Specifications

GOST 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions

GOST 29169−91 (ISO 648−77) oils. Pipette with one mark

GOST 29227−91 (ISO 835−1-81) oils. Pipettes are graduated. Part 1. General requirements

GOST 29251−91 (ISO 385−1-84) oils. Burette. Part 1. General requirements

GOST 31382−2009 Copper. Methods of analysis

Note — When using this standard appropriate to test the effect of reference standards in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet or in the annual information index «National standards» published as on January 1 of the current year, and the editions of the monthly information index «National standards» for the current year. If the reference standard is replaced (changed), when using this standard should be guided by replacing (amended) standard. If the reference standard is cancelled without replacement, then the situation in which the given link applies to the extent that does not affect this link.

3 General provisions

3.1 General requirements for methods of measurements GOST 31382.

4 Photometric method of measuring the mass fraction of bismuth

4.1 characteristics of the indicators of measurement accuracy

Indicators of accuracy of measurements of the mass fraction of bismuth correspond to the characteristics given in table 2 (with R=0,95).

Limit values of repeatability and reproducibility of the measurement at a confidence probability P=0.95 is shown in table 2.


Table 2 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of mass fraction of bismuth at confidence probability P=0,95

4.2 measuring instruments, auxiliary devices, materials, solutions

When performing measurements using the following measuring instruments and auxiliary devices:

— spectrophotometer or photocolorimeter with all accessories necessary for measurements at a wavelength of 450 nm;

slab heating [1]* ensures the heating temperature up to 400 °C, or equivalent;
________________
* POS. [1]-[7], [9]-[14] see Bibliography, here and hereafter. — Note the manufacturer’s database.


glass hour;

— special laboratory scales of accuracy class according to GOST 24104;

— volumetric flasks 2−25−2, 2−100−2, 2−250−2, 2−1000−2 according GOST 1770;

— glasses N-1−100 TCS, N-1−400 TCS according to GOST 25336;

— flasks conical KN-2−250 TCS according to GOST 25336;

— funnels, conical In-36−80 TC GOST 25336;

pipettes not lower than 2nd accuracy class according to GOST and GOST 29169 29227.

When taking measurements, use the following products and solutions:

— distilled water according to GOST 6709;

— nitric acid according to GOST 4461 or nitric acid high purity according to GOST 11125;

— hydrochloric acid according to GOST 3118, diluted 1:1;

— tartaric acid according to GOST 5817, solution mass concentration of 250 g/DM;

— ascorbic acid by [2], a freshly prepared solution of mass concentration of 50 g/DM;

— ammonia water according to GOST 3760 diluted 1:99;

the iron powder according to GOST 9849, solution mass concentration 10 g/DM;

— potassium iodide according to GOST 4232, a freshly prepared solution of the mass concentration of 200 g/DM;

— bismuth GOST 10928;

filters obestochennye in [3] or similar.

Notes

1 allowed the use of other measuring instruments of the approved type, auxiliary devices and materials, technical and metrological characteristics are not inferior to mentioned above.

2 allowed the use of reagents produced by other normative documents, provided that their metrological characteristics of measurement results, given in this standard.

4.3 Method of measurement

The method is based on measuring the optical density at a wavelength of from 420 to 450 nm of the colored iodine complex of bismuth, formed in hydrochloric acid solution in the presence of tartaric acid and reducing agent.

Bismuth is additionally allocated to the iron hydroxide.

4.4 Preparation for measurements

4.4.1 Preparation of solutions for constructing the calibration curve

In preparing the solution And the mass concentration of bismuth 0.1 mg/cma portion of the bismuth mass 0,1000 g placed in a beaker with a capacity of 100 cm, poured from 5 to 10 cmof nitric acid, heated to remove oxides of nitrogen. The solution was cooled and transferred into a measuring flask with volume capacity of 1000 cm, 65 cm pourednitric acid, made up to the mark with water and mix.

In the preparation of a solution of mass concentration of bismuth 0.01 mg/cma 25 cm aliquotof solution A is placed in a volumetric flask with a capacity of 250 cm, pour 5 cmof nitric acid, made up to the mark with water and mix.

The solution is ready for use within 5 hours.

4.4.2 preparation of the solution of iron mass concentration 10 g/DM

A sample of iron weighing 1.0 g was placed in a beaker with a capacity of 100 cm, flow 10 to 15 cmof hydrochloric acid and dissolved by heating. After cooling, the solution is transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

4.4.3 Construction of calibration curve

In six conical flasks with a capacity of 250 cm, each is placed 0,0; 1,0; 2,0; 3,0; 4,0 and 5,0 cmof solution B, which corresponds to 0,0; 0,01; 0,02; 0,03; 0,04 and 0,05 mg of bismuth, pour 5 cmof nitric acid, 20 cmof hydrochloric acid. The solutions were heated and evaporated to a volume of 3 to 5 cm. Pour 5 cmof a solution of iron, from 100 to 120 cmof water, heated to a temperature from 60 °C to 70 °C and poured ammonia to transition copper ammonium complex and then another 5 cm. Heating was continued for 5−7 min and leave the solution to the coagulation of sludge in a warm place plate.

The precipitate of hydroxides is filtered on a loose filter and washed 3 to 5 times a hot ammonia diluted 1:99. The precipitate from the filter washed into the flask in which the precipitation was carried out, and poured 15 to 20 cma hot hydrochloric acid diluted 1:1. The resulting solution was diluted with water to a volume of 80 to 100 cmand re-precipitated hydroxides with ammonia. The precipitate was filtered on the same filter and washed 3 to 4 times of hot ammonia diluted 1:99. Funnel with a filter placed over the flask in which the precipitation was carried out, to the residue was poured 10 to 15 cmhot hydrochloric acid, diluted 1:1, the filter is washed 2−3 times with hot water. The filter is discarded. The filtrate is evaporated to a volume of 10 cm, after cooling it is placed in a volumetric flask with a capacity of 25 cm, pour 4 cmof solution of tartaric acid, 5 cmof a solution of potassium iodide, 1.0 to 1.5 cmof a solution of ascorbic acid and top up with water to the mark.

After 10−15 minutes, measure the optical density of solutions on the spectrophotometer or photocolorimeter at a wavelength of from 420 to 450 nm in a cuvette with an optimum thickness of the layer. Solution comparison is water.

According to the obtained values of optical densities and corresponding concentrations of bismuth build the calibration graph.

4.5 performance measurement

The weight of copper weight of 2,0000 g placed in a beaker with a capacity of 400 cm, flow 25 to 30 cmof nitric acid, cover with watch glass and allowed to stand without heating until the cessation of the violent reaction of the allocation of nitrogen oxides.

Remove the glass, wash water over the glass, poured from 20 to 25 cmhydrochloric acid and evaporated solution when heated to a volume of 3 to 5 cm.

Then pour into a glass from 80 to 100 cmwater and 5 cmof a solution of iron. Heat and then continue the measurement as specified in 4.4.3.

The measurements are carried out in accordance with the manual spectrophotometer or photocolorimeter, the mass of bismuth set calibration schedule.

4.6 Processing of measurement results

4.6.1 Mass fraction of bismuth X, %, is calculated by the formula

, (1)

where mis the mass of bismuth, was found in the calibration schedule, mcg;

mis the mass of bismuth, obtained as a result of the idle experience, mcg;

m — weight of copper,

4.6.2 the measurement result taking the arithmetic mean of two parallel definitions, provided that the absolute difference between them in terms of repeatability does not exceed the value (at confidence probability P=0,95) repeatability limit rgiven in table 2.

If the difference between the highest and lowest results of parallel measurements exceeds the limit value of the frequency of occurrence, perform the procedure described in GOST ISO 5725−6 (paragraph 5.2.2.1).

4.6.3 Differences between measurements obtained in two laboratories, should not exceed the values of the limit of reproducibility shown in table 2. In this case, the final result may be decided to their arithmetic mean value. At default of this condition can be used the procedure set out in GOST ISO 5725−6 (paragraph 5.3.3).

5 Photometric method of measuring the mass fraction of manganese

5.1 characteristics of the indicators of measurement accuracy

Indicators of accuracy of measurements of mass fraction of manganese corresponding to the characteristics given in table 3 (with R=0,95).

Limit values of repeatability and reproducibility of the measurement at a confidence probability P=0.95 is shown in table 3.


Table 3 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of mass fraction of manganese at confidence probability P=0,95

5.2 measurement Means, auxiliary devices, materials, solutions

When performing measurements using the following measuring instruments and auxiliary devices:

— spectrophotometer or photocolorimeter with all accessories necessary for measurements at a wavelength of from 520 to 540 nm;

slab heating [1], providing temperature up to 400 °C, or equivalent;

— bath water;

— special laboratory scales of accuracy class according to GOST 24104;

— glasses N-1−100 TCS, N-1−250 TCS according to GOST 25336;

— flasks conical KN-1−250−14/23 TCS GOST 25336;

— volumetric flasks 2−50−2, 2−100−2, 2−1000−2 according GOST 1770;

pipettes not lower than 2nd accuracy class according to GOST and GOST 29169 29227.

When taking measurements, use the following products and solutions:

— distilled water according to GOST 6709;

— nitric acid according to GOST 4461 or nitric acid high purity according to GOST 11125 and diluted 1:1, 1:3;

— potassium ignominy in [4], the solution of the mass concentration of 50 g/DM;

manganese metal according to GOST 6008.

Notes

1 allowed the use of other measuring instruments of the approved type, auxiliary devices and materials, technical and metrological characteristics are not inferior to mentioned above.

2 allowed the use of reagents produced by other normative documents, provided that their metrological characteristics of measurement results, given in this standard.

5.3 Method of measurement

The method is based on measuring the optical density of the colored complex compounds pneumococcal of manganese at a wavelength of from 520 to 540 nm.

5.4 Preparation for measurements

5.4.1 Preparation of solutions for constructing the calibration curve

In preparing the solution And the mass concentration of manganese 0.1 mg/cma portion of the manganese with a mass of 0.1 g was placed in a beaker with a capacity of 100 cm, flow 10 to 15 cmof nitric acid, diluted 1:1, heated to remove oxides of nitrogen. The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmand top up with water to the mark.

In the preparation of a solution of mass concentration of manganese 0.01 mg/cma 10 cm aliquotof solution A is placed in a volumetric flask with a capacity of 100 cm, pour 1 cmof nitric acid, diluted 1:1 and top up with water to the mark.

In preparing the solution In mass concentrations 0.005 mg/cmaliquot of 50 cmof a solution is placed in a volumetric flask with a capacity of 100 cm, pour 0.5 cmof nitric acid, diluted 1:1 and top up with water to the mark.

5.4.2 preparation of the solution jednolitego potassium mass concentration of 50 g/DM

A portion jednolitego potassium weight of 50 g was dissolved in nitric acid solution diluted 1:3 and topped up with the same solution to 100 cm.

5.4.3 Construction of calibration curve

In glasses with a capacity of 250 cm, each is placed 0,0; 1,0; 2,0 and 5,0 cmsolution and 1,0; 2,0; 3,0; 4,0 and 5,0 cmstandard solution B, which corresponds to 0,0; 0,005; 0,010; 0,025; 0,100; 0,200; 0,300; 0,400; 0,500 mg of manganese. All glasses poured water to a volume of 20 cm, and then boiled for 5 min.

In the boiling solution poured 5 cmof a solution of potassium jednolitego and continue boiling for another 5 min. Then the beaker placed on a boiling water bath and kept for 20 min.

After cooling, transfer the solution into a volumetric flask with a capacity of 50 cm, made up to the mark with water (stock solution) and mix.

Absorbance measured on the spectrophotometer at a wavelength of 530 nm or photocolorimeter with a filter having the wavelength corresponding to maximum light transmission from 520 to 540 nm in a cuvette with a layer thickness of 20 or 30 mm.

Solution comparison is part of the basic sample solution, in which manganese (VII) is reduced to manganese (II) by adding 1 to 2 drops of solution sodium attestatio.

According to the obtained values of optical density of solutions and their corresponding concentrations of manganese build a calibration curve in rectangular coordinates.

5.5 performance measurement

The weight of copper weight of 2,0000 g (with mass fraction of manganese from 0.0002% to 0.001%) or 1,0000 g (with mass fraction of manganese from 0.001% to 0.005%) is placed in a conical flask with a capacity of 250 cm, flow 20 to 25 cmof nitric acid and boil until the cessation of the violent reaction of allocation of oxides of nitrogen and dissolving the sample. The solution was evaporated to half and then continue as specified in 5.4.3.

The measurements are carried out in accordance with the manual spectrophotometer or photocolorimeter, a lot of manganese in milligrams set by the calibration schedule.

5.6 the Processing of the measurement results

5.6.1 Mass fraction of manganese X, %, is calculated by the formula

, (2)

where mis the mass of manganese was found in the calibration graphics mg;

mis the mass of manganese resulting idle experience, mg;

m — weight of copper,

5.6.2 For the measurement result taking the arithmetic mean of two parallel definitions, provided that the absolute difference between them in terms of repeatability does not exceed the value (at confidence probability P=0,95) repeatability limit rgiven in table 3.

If the difference between the highest and lowest results of parallel measurements exceeds the limit value of the frequency of occurrence, perform the procedure described in GOST ISO 5725−6 (paragraph 5.2.2.1).

5.6.3 Differences between measurements obtained in two laboratories, should not exceed the limit values repeatability, are shown in table 3. In this case, the final result may be decided to their arithmetic mean value. At default of this condition can be used the procedure set out in GOST ISO 5725−6 (paragraph 5.3.3).

6 Photometric method of measuring the mass fraction of cobalt

6.1 characteristics of the indicators of measurement accuracy

Indicators of accuracy of measurements of the mass fraction of cobalt correspond to the characteristics given in table 4 (with R=0,95).

Limit values of repeatability and reproducibility of the measurement at a confidence probability P=0.95 is given in table 4.


Table 4 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of the mass fraction of cobalt at confidence probability P=0,95

6.2 measurement Means, auxiliary devices, materials, solutions

When performing measurements using the following measuring instruments and auxiliary devices:

— spectrophotometer or photocolorimeter with all accessories necessary for measurements at a wavelength of 410 nm;

slab heating [1], providing temperature up to 400 °C, or equivalent;

glass hour;

— special laboratory scales of accuracy class according to GOST 24104;

— flasks conical KN-2−250−18 TCS GOST 25336;

— volumetric flasks 2−100−2, 2−500−2 according GOST 1770;

— glasses N-1−50 TCS, N-1−100 TCS according to GOST 25336;

— separating funnel VD-1−250 (100) TC GOST 25336;

pipettes not lower than 2nd accuracy class according to GOST and GOST 29169 29227.

When taking measurements, use the following products and solutions:

— distilled water according to GOST 6709;

— nitric acid according to GOST 4461 (boiled to remove oxides of nitrogen), diluted 1:1;

— hydrochloric acid according to GOST 3118 and the solution molar concentration of 4 mol/DM;

— citric acid according to GOST 3652, solution mass concentration of 250 g/DM;

— potassium hydroxide according to GOST 24363, solution mass concentration of 50 g/DM;

— acetic acid according to GOST 61;

— aluminium GOST 11069;

— toluene according to GOST 5789;

1 nitroso-2-naphthol [5], the solution of the mass concentration of 0.5 g/DM;

— hydrogen peroxide according to GOST 10929 (stable product);

— cobalt GOST 123;

— copper according to GOST 859, not containing cobalt.

Notes

1 allowed the use of other measuring instruments of the approved type, auxiliary devices and materials, technical and metrological characteristics are not inferior to mentioned above.

2 allowed the use of reagents produced by other normative documents, provided that their metrological characteristics of measurement results, given in this standard.

6.3 Method of measurement

The method is based on measuring the optical density at a wavelength of 410 nm painted cobalt compounds 1 nitroso-2-naphthol after extraction with toluene, and his prior separation of metallic copper on aluminium.

6.4 Preparation for measurements

6.4.1 Preparation of solutions for constructing the calibration curve

In preparing the solution And the mass of cobalt concentration 1.0 mg/cmthe weight of cobalt metal mass 0,1000 g placed in a beaker with a capacity of 100 cm, flow 20 cmof a mixture of nitric and hydrochloric acids (in the ratio 1:3), is heated to remove oxides of nitrogen. The solution was evaporated to wet salts. Pour 10 cmof hydrochloric acid and evaporated to dryness. Treatment with hydrochloric acid is repeated 2 times.

To the dry residue poured from 30 to 50 cmof hot water, cooled, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

In the preparation of a solution of mass concentration of cobalt 0.01 mg/cma 5 cm aliquotof solution A is placed in a volumetric flask with a capacity of 500 cm, made up to the mark with water and mix.

When cooking solution To the mass concentration of cobalt 0.001 mg/cma 10 cm aliquotof a solution is placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix. The solution used freshly.