GOST 13047.3-2014
GOST 13047.3−2014 Nickel. Cobalt. Methods for determination of cobalt in cobalt
GOST 13047.3−2014
INTERSTATE STANDARD
NICKEL. COBALT
Methods for determination of cobalt in cobalt
Nickel. Cobalt. Methods for determination of cobalt in cobalt
ISS 77.120.40
Date of introduction 2016−01−01
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 interstate technical committees for standardization MTK 501 Nickel and MTC 502 «Cobalt"
2 as AMENDED by the Federal Agency for technical regulation and Metrology (Rosstandart)
3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol of October 20, 2014 N 71-N)
The adoption voted:
| Short name of the country MK (ISO 3166) 004−97 |
Country code MK (ISO 3166) 004−97 |
Abbreviated name of the national authority for standardization |
| Azerbaijan |
AZ | Azstandart |
| Armenia |
AM | The Ministry Of Economic Development Of The Republic Of Armenia |
| Belarus |
BY | Gosstandart Of The Republic Of Belarus |
| Georgia |
GE | Gosstandart |
| Kazakhstan |
KZ | Gosstandart Of The Republic Of Kazakhstan |
| Kyrgyzstan |
KG | Kyrgyzstandard |
| Russia |
EN | Rosstandart |
| Tajikistan |
TJ | Tajikstandart |
| Uzbekistan |
UZ | Uzstandard |
4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St inter-state standard GOST 13047.3−2014 introduced as the national standard of the Russian Federation from 1 January 2016.
5 REPLACE GOST 13047.3−2002
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
1 Scope
This standard specifies electrogravimetry (when the mass fraction of cobalt to 98.8%) and calculated (at a mass fraction of cobalt over the 98.8%) methods for determination of cobalt in cobalt GOST 123.
2 Normative references
This standard uses the regulatory references to the following standards:
GOST 123−2008 Cobalt. Specifications
GOST 199−78 Reagents. Sodium acetate 3-water. Specifications
GOST 3118−77 Reagents. Hydrochloric acid. Specifications
GOST 3760−79 Reagents. The aqueous ammonia. Specifications
GOST 3769−78 Reagents. The ammonium sulfate. Specifications
GOST 4204−77 Reagents. Sulphuric acid. Specifications
GOST 4461−77 Reagents. Nitric acid. Specifications
GOST 5457−75 Acetylene, dissolved and gaseous. Specifications
GOST 5841−74 Reagents. Hydrazine sulfate
GOST 6563−75 technical articles made of noble metals and alloys. Specifications
GOST 8776−2010 Cobalt. Methods of chemical-atomic-emission spectral analysis
GOST 11125−84 nitric Acid of high purity. Specifications
GOST 13047.1−2014 Nickel. Cobalt. General requirements for methods of analysis
GOST 13047.5−2014 Nickel. Cobalt. Methods for determination of Nickel in cobalt
GOST 13047.6−2014 Nickel. Cobalt. Methods for determination of carbon
GOST 13047.7−2014 Nickel. Cobalt. Methods of determining sulphur
GOST 13047.8−2014 Nickel. Cobalt. Method for determination of silicon
GOST 13047.9−2014 Nickel. Cobalt. Method of determination of phosphorus
GOST 13047.10−2014 Nickel. Cobalt. Methods for determination of copper
GOST 13047.11−2014 Nickel. Cobalt. Method of determining zinc
GOST 13047.12−2014 Nickel. Cobalt. Methods for determination of antimony
GOST 13047.13−2014 Nickel. Cobalt. Methods for determination of lead
GOST 13047.14−2014 Nickel. Cobalt. Methods for determination of bismuth
GOST 13047.15−2014 Nickel. Cobalt. Method for determination of tin
GOST 13047.16−2014 Nickel. Cobalt. Methods for determination of cadmium
GOST 13047.17−2014 Nickel. Cobalt. Methods of iron determination
GOST 13047.18−2014 Nickel. Cobalt. Methods for determination of arsenic
GOST 13047.19−2014 Nickel. Cobalt. Method for the determination of aluminium
GOST 13047.20−2014 Nickel. Cobalt. Method for determination of magnesium
GOST 13047.21−2014 Nickel. Cobalt. Methods for determination of manganese
GOST 18300−87 ethyl rectified technical. Specifications
GOST 24147−80 aqueous Ammonia of high purity. Specifications
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 requirements and safety requirements
General requirements for methods of analysis used by the quality of distilled water and laboratory glassware and safety at work — according to GOST 13047.1.
4 Electrogravimetry method
4.1 Method of analysis
The method is based on weighing of cobalt, Nickel, copper and zinc emitted by electrolysis on a platinum cathode from the ammonium medium and the determination of the mass of cobalt remaining in the solution after carrying out electrolysis, spectrophotometric or atomic absorption method. The mass fraction of cobalt, Nickel, copper and zinc is determined according to GOST 13047.5, 13047.10 GOST, GOST 13047.11 or GOST 8776 and take into account when processing the results of the analysis.
A spectrophotometric method based on measurement of light absorption at a wavelength of 500 nm of a solution of complex compounds of cobalt with nitroso-R-salt.
Atomic absorption method based on measurement of absorption at a wavelength of 240,7 nm resonance radiation by cobalt atoms, the resulting fiery atomization when spraying the sample solution in flame acetylene-air.
4.2 measuring instruments, auxiliary devices, materials, reagents and solutions
Installation for electrolysis with ammeter, voltmeter and rheostat, providing carrying out the electrolysis while stirring the solution at a current of from 3 to 4 A and a voltage of 2 to 3 V.
Atomic absorption spectrometer for measurements in the flame acetylene-air.
Lamp with hollow cathode for the excitation of spectral lines of cobalt.
Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 490 to 540 nm.
The electrodes are platinum mesh according to GOST 6563.
Acetylene gas according to GOST 5457.
Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1.
Sulfuric acid according to GOST 4204, diluted 1:1 and 1:9.
Ammonia water according to GOST 3760, if necessary, cleaned, or according to GOST 24147, diluted 1:9.
Ammonium sulfate according to GOST 3769.
Hydrochloric acid according to GOST 3118, diluted 1:1.
Hydrazine sulfate according to GOST 5841.
Sodium acetate 3-water according to GOST 199, solution mass concentration of 0.5 g/cm.
Nitroso-R-salt [1]*, solution mass concentration of 0.001 g/cm.
________________
* See Bibliography. — Note the manufacturer’s database.
The technical rectified ethyl alcohol according to GOST 18300.
Universal indicator paper in [2].
Filters obestochennye in [3] or other filter medium density.
Cobalt GOST 123 with a mass fraction of cobalt is not more than 99,25%.
Cobalt solutions of known concentration.
The solution And the mass of cobalt concentration 0.001 g/cmis prepared as follows: a portion of the cobalt ground 1,0000 g were placed in a glass or flask with a capacity of 250 cm
, flow 25 to 30 cm
of nitric acid, diluted 1:1, dissolved by heating, boil for 3−5 min, poured 20 cm
of sulphuric acid diluted 1:1, the solution is evaporated to release vapors of sulfuric acid, cooled, poured from 80 to 100 cm
of distilled water, dissolve salt when heated and cooled. The solution is transferred into a measuring flask with volume capacity of 1000 cm
and adjusted to the mark with distilled water.
Solution B mass concentration of cobalt 0.0001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cm
transfer 10 cm
of solution A, pour 10 cm
of sulphuric acid diluted 1:1, adjusted to the mark with distilled water.
Solution of mass concentration of cobalt 0,00001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cm
transfer 10 cm
of a solution, pour 5 cm
of sulphuric acid, diluted 1:9, adjusted to the mark with distilled water.
4.3 Preparation for analysis
4.3.1 To construct the calibration curve in the determination of the mass of cobalt by spectrophotometric in volumetric flasks with a capacity of 100 cmtransfer 1, 2, 4, 6, 8 and 10 cm
of solution, pour distilled water to a volume of 15 cm
, add one or two drops of sulphuric acid, diluted 1:1, pour 5 cm
of sodium acetate and further carry out the analysis in accordance with
The mass of cobalt in the calibration solutions is 0,00001; 0,00002; 0,00004; of 0.00006; and 0,00010 0,00008 g.
The light absorption values of the calibration solutions and corresponding mass of cobalt to build a calibration curve based on the value of absorption solution, prepared without the introduction of a solution containing cobalt.
4.3.2 For the construction of calibration curve in the mass determination of cobalt by atomic absorption method in a volumetric flask with a capacity of 250 cmcarry 1, 2, 4, 6, 8 and 10 cm
of solution B, adjusted to the mark with distilled water and measure the absorbance in accordance with
The mass of cobalt in the calibration solutions is 0,0001; 0,0002; 0,0004; about 0.0006; and 0,0008 0,0010 g.
4.4 analysis
4.4.1 Sample the sample weight of 1,000 g was placed in a beaker or flask with a capacity of 250 cm, flow 15 to 20 cm
of nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, poured 15 cm
sulphuric acid diluted 1:1, the solution is evaporated to release vapors of sulfuric acid and cooled.
Pour 50 to 60 cmof distilled water, add 3 to 4 g of ammonium sulfate, dissolved salts when heated and cooled. Poured, with stirring, ammonia until the smell and another 80 cm
.
Solution and the precipitate is kept in a warm place for 25−30 min., filtered through a filter (red or white ribbon), collecting the filtrate in a beaker with a capacity of 250 cm, the filter and the precipitate washed two or three times with ammonia diluted 1:9, the filtrate is used in accordance with
The filter cake is dissolved in a volume of 10 to 15 cmhot hydrochloric acid, diluted 1:1, the filter is washed three or four times with hot water, collecting the filtrate in a beaker, in which was conducted the deposition. The solution is poured 10 cm
of sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid, cooled, poured 20 to 30 cm
of distilled water and dissolved salts when heated. The solution was transferred to a volumetric flask with a capacity of 250 cm
and used in accordance with
4.4.2 To the filtrate add 2.0 g of hydrazine, topped up with distilled water to a volume of 200 cmand the electrolysis is carried out for 1−1. 5 h while stirring the solution using a pre-weighed platinum electrodes at a current of from 3 to 4 A and a voltage of 2 to 3 V. After the bleaching solution the side of the Cup and protruding parts of the electrodes are washed with distilled water, poured from 15 to 20 cm
of distilled water and continue electrolysis for 10−15 min.
The electrodes taken out from the solution, washed with distilled water and turn off the current. The electrodes are washed with ethanol, dried at a temperature of from 95 °C to 105 °C for 15−20 minutes, cool and weigh.
4.4.3 After the electrolysis, the solution is evaporated to a volume of 40 to 50 cmand poured sulphuric acid, diluted 1:1, to pH 1−2 by universal indicator paper. The solution attached to the solution in a volumetric flask with a capacity of 250 cm
, adjusted to the mark with distilled water and determine the mass of cobalt by spectrophotometry in accordance with 4.4.4 or atomic absorption method in accordance with
4.4.4 When using the spectrophotometric method in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution for 4.4.3, poured ammonia until the appearance of the precipitate of iron hydroxide and dissolve it in two or three drops of sulphuric acid, diluted 1:1.
The solution is poured 5 cmsodium acetate, boil for 2−3 min, poured 10 cm
of the solution, nitroso-R-salt, boil for 2−3 min, poured 10 cm
of nitric acid, diluted 1:1, boiled for 1 min. the Solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and adjusted to the mark with distilled water.
After 5−7 min. measure the light absorption of the solution on the spectrophotometer at a wavelength of 500 nm or photoelectrocolorimeter at a wavelength range from 490 to 540 nm. A solution of comparison, using the calibration solution, prepared without the introduction of a solution containing cobalt.
The value of the light absorption of the sample solution find the mass of cobalt in the calibration graphics, built in 4.3.1, taking into account the dilution factor of the solution.
4.4.5 When using the atomic absorption method, the absorption of sample solution in 4.4.3 and calibration solutions for 4.3.2 at a wavelength of 240,7 nm, slit width is not more than 1.0 nm is measured at least two times, sequentially spraying them in the flame acetylene-air, spray rinsed the system with distilled water, check the zero point and the stability of the calibration curve.
According to the obtained values of absorbance of the calibration solutions and corresponding masses of cobalt build the calibration graph.
The value of absorbance of sample solution find the mass of cobalt in the calibration schedule.
In one analysis performed two or three parallel definitions.
4.5 Processing the analysis results
Mass fraction of cobalt , X, %, is calculated by the formula
where Mis the mass of the cathode after electrolysis, g;
M — mass of the cathode before electrolysis, g;
M — mass of the anode before the electrolysis, g;
M — mass of anode after electrolysis, g;
Mis the mass of cobalt in the sample solution, g;
M — weight of sample, g;
X — mass fraction of Nickel in the sample, %;
X — mass fraction of copper in the sample, %;
X — mass fraction of zinc in sample, %.
4.6 accuracy Control analysis
Control of accuracy of analysis results is carried out according to GOST 13047.1.
The expanded uncertainty of the results of the analysis of U is 0.3%.
Regulations control precision — the repeatability limits r the results of two or three parallel definitions are, respectively, 0.2% and 0.3%; the limit of reproducibility R for the two analysis results is 0.4% at a confidence probability P=0,95.
5 Calculation method
Fraction of total mass of cobalt (in mass fraction of cobalt in excess of 98.8 per cent) define the calculation method. To do this, find the sum of the mass fraction of impurities, normalized to GOST 123 and a mass fraction of silicon and aluminum, determined according to GOST 13047.5 — 13047.21 GOST or GOST 8776 taken, without rounding, and subtracted from 100%.
The result is rounded up to the number of significant digits specified in the tables of chemical composition according to GOST 123.
