GOST 13047.15-2014

• gost-1304715-81.pdf (757.28 KiB)
  ГОСТ 13047.15-81

GOST 13047.15−2014 Nickel. Cobalt. Method for determination of tin

GOST 13047.15−2014

INTERSTATE STANDARD

NICKEL. COBALT

Method for determination of tin

Nickel. Cobalt. Method for determination of tin

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 13047.15−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.15−2002


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 tin (with tin mass fraction of from 0.0001% to 0,0020%) 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 860−75 Tin. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 13047.1−2014 Nickel. Cobalt. General requirements for methods of analysis

GOST 14261−77 hydrochloric Acid 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 Atomic absorption method

4.1 Method of analysis

The analysis method is based on measurement of absorption at a wavelength of 235,5 nm resonance radiation by atoms of tin, the resulting electrothermal atomization of the sample solution.

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

Atomic absorption spectrometer for measurements with electrothermal atomization, the correction non-selective absorption and the automated flow of the solution into the atomizer.

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

Argon gas according to GOST 10157.

Filters obestochennye [1]* other filters or medium density.
________________
* 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.

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation, or according to GOST 14261, diluted 1:1.

Nickel powder according to GOST 9722 or standard sample of Nickel pre-installed (certified) mass fraction of tin is not more than 0.0001%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of tin is not more than 0.0001%.

Tin GOST 860.

The tin solutions of known concentration.

The solution And the mass concentration of tin 0.0001 g/cmis prepared as follows: a portion of tin mass 0,1000 g placed in a beaker with a capacity of 100 cm, flow 20 to 30 cmof hydrochloric acid, dissolve while heating on a boiling water bath, cooled, transferred into a measuring flask with volume capacity of 1000 cm, flow 50 cmhydrochloric acid and adjusted to the mark with distilled water.

Solution B is the mass concentration of tin 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.

Solution of the mass concentration of tin 0,000001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution B 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 tin is not more than 0,0010% suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 1,000 g was placed in a beaker or flask with a capacity of 250 cm. The number of batches must match the number of points of calibration curve, including Supervisory experience.

The suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in 15−20 cmof nitric acid, diluted 1:1. When using the Nickel powder in the slurries 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 10 to 15 cm, flow from 40 to 50 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm.

Flasks transfer 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof solution B. the flask with the solution in the reference experiment, the solution containing tin, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.

The mass of tin in the calibration solutions is 0,000001; 0,000002; 0,000004; 0,000006; 0,000008; 0,000010 G.

4.3.2 For the construction of calibration curve 2 in determining the mass fraction of tin greater than 0.001% in a volumetric flask with a capacity of 100 cmstand for 20 cmof the solution in the reference experiment, prepared in accordance with 4.3.1, poured 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof solution V. one of the flasks with a solution of the reference experiment a solution containing tin, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 4.4.

The mass of tin in the calibration solutions is given in 4.3.1.

4.4 analysis

A portion of the sample with a mass of 1,000 g was placed in a beaker or flask with a capacity of 250 cm, flow 15 to 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 5 to 7 cm, transferred to a volumetric flask with a capacity of 100 cm, cooled and adjusted to the mark with distilled water.

When the mass fraction of tin over 0,0010% in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution a volume of 20 cmand was adjusted to the mark with nitric acid, diluted 1:19.

The absorbance of the sample solution and the calibration solutions at a wavelength of 235,5 nm, slit width of not more than 0.7 nm with a correction non-selective absorption in the current of argon is measured at least two times, sequentially spraying them in an atomizer. Depending on the type of spectrometer to select the optimal amount of solution injected into the atomizer, from 0.005 to 0.050 cmor optimal time, aerosol spray from 5 to 50 C. Washed the spray 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.

Selection of optimal temperature regimes for the atomizer is carried out individually for the used spectrometer for the calibration solutions. Recommended operating conditions of the atomizer are given in table 1.


Table 1 — operating conditions of the atomizer

The values of absorption of the calibration solutions and their corresponding masses tin build a calibration curve.

The value of absorbance of sample solution find the mass of the tin on the appropriate calibration schedule.

4.5 Processing the analysis results

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

, (1)

where  — weight of tin in the sample solution, g;

K — dilution factor of sample solution;

M — weight of sample, g.

4.6 Control of accuracy of analysis results

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 2.


Table 2 — 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

_______________

* Valid on the territory of the Russian Federation.
THAT is not given. For additional information, please refer to the link. — Note the manufacturer’s database.