GOST 13047.11-2014

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  ГОСТ 13047.11-81

GOST 13047.11−2014 Nickel. Cobalt. Method of determining zinc

GOST 13047.11−2014

INTERSTATE STANDARD

NICKEL. COBALT

Method of determining zinc

Nickel. Cobalt. Method for determination of zinc

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:

4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St inter-state standard GOST 13047.11−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.11−2002


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 establishes the atomic absorption method for the determination of zinc (at a mass fraction of zinc from from 0.0002% to 0,010%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 3640−94 Zinc. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 13047.1−2014 Nickel. Cobalt. General requirements for 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 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 Atomic absorption method

4.1 Method of analysis

The method is based on measuring absorption at a wavelength of 213,9 nm resonance radiation by atoms of zinc, the resulting fiery atomization when spraying the sample solution in flame acetylene — air.

4.2 measuring instruments, auxiliary devices, materials, reagents and solutions

Atomic absorption spectrometer for measurements in the flame acetylene — air.

Lamp with hollow cathode for the excitation of spectral lines of zinc.

Acetylene gas according to GOST 5457.

Filters obestochennye [1]* or other thick filters.
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* See Bibliography. — Note the manufacturer’s database.


Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1, 1:9 and 1:19.

Nickel powder according to GOST 9722 or standard sample of Nickel, for example [2], pre-installed (certified) mass fraction of zinc is not more than 0,0002%.

Cobalt GOST 123 or standard sample of cobalt, for example, [3], pre-installed (certified) mass fraction of zinc is not more than 0,0002%.

Zinc GOST 3640.

Solutions of known zinc concentration.

The solution And the mass of zinc concentration 0.0001 g/cmis prepared as follows: a portion of the zinc mass 0,1000 g were placed in a glass or flask with a capacity of 250 cm, flow 15 to 20 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, transferred into a measuring flask with volume capacity of 1000 cm, adjusted to the mark with distilled water.

Solution B mass of zinc concentration 0,00001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution A and bring to the mark with nitric acid, diluted 1:19.

4.3 Preparation for analysis

4.3.1 To construct a calibration chart 1 in determining the mass fraction of zinc of not more than 0,0020% suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 3,000 g were placed in a glass or flask with a capacity of 250 cm. The number of batches must match the number of points of calibration curve, including Supervisory experience.

To a suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt go from 40 to 50 cmof nitric acid, diluted 1:1 and dissolved by heating. When using the Nickel powder in the solution was filtered through a filter (red or white ribbon), washed two or three times with nitric acid, diluted 1:9. The filters are washed two or three times with hot distilled water. The solutions were evaporated to a volume of 15 to 20 cm, flow from 40 to 50 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm.

In the flask transfer 0,5; 1,0; 2,0; 4,0; 5,0 and 6,0 cmof solution B. the flask with the solution in the reference experiment, the solution containing zinc, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.

The mass of zinc in the calibration solutions is 0,000005; 0,000010; 0,000020; 0,000040; 0,000050 and 0,000060 G.

4.3.2 For the construction of calibration curve 2 in determining the mass fraction of zinc more than 0,0020% in volumetric flasks with a capacity of 100 cmstand for 20 cmof the solution in the reference experiment, prepared in accordance with 4.3.1, poured 0,5; 1,0; 2,0; 4,0; 5,0 and 6,0 cmof solution B. In one of the flasks with a solution of the reference experiment a solution containing zinc, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 4.4.

The mass of zinc in the calibration solutions specified in 4.3.1.

4.4 analysis

A portion of the sample with a mass of 3,000 g were placed in a glass or flask with a capacity of 250 cm, flow from 40 to 50 cmof nitric acid, diluted 1:1, is dissolved when heated, is evaporated to a volume of 15 to 20 cm, cooled, transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with distilled water.

When the mass fraction of zinc more than 0,0020% in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution a volume of 20 cm, adjusted to the mark with nitric acid, diluted 1:19.

The absorbance of the sample solution and the calibration solutions at a wavelength of 213,9 nm, slit width is not more than 1.0 nm is measured at least two times, sequentially spraying in the flame acetylene — air, spray rinsed the system with distilled water, check the zero point and the stability of the calibration curve. To check the zero point solution is used, the appropriate control experience, prepared in accordance with 4.3.

The values of absorption of the calibration solutions and corresponding mass of zinc build a calibration curve.

The value of absorbance of sample solution find the mass of zinc according to the calibration schedule.

4.5 Processing the analysis results

Mass fraction of zinc in the sample X, %, is calculated by the formula

, (1)

where is the mass of zinc in the sample solution, g;

K — dilution factor of sample solution;

M — weight of sample, g.

4.6 accuracy Control analysis

Control of accuracy of analysis results is carried out according to GOST 13047.1.

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are shown in table 1.


Table 1 — Requirements of control precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis at a confidence probability P=0,95

Percentage

Bibliography

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* Operates in the Russian Federation.
THAT is not given. For additional information, please refer to the link. — Note the manufacturer’s database.