GOST 13047.1-2014

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  ГОСТ 13047.1-2014

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

GOST 13047.1−2014

Group B59

INTERSTATE STANDARD

NICKEL. COBALT

General requirements for methods of analysis

Nickel. Cobalt. General requirements for methods of analysis

ISS 77.120.40
AXTU 1732

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 13047.1−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.1−2002


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 applies to primary Nickel GOST 849, Nickel powder according to GOST 9722, cobalt GOST 123 and cobalt powder to GOST 9721 and establishes General requirements for methods of chemical analysis and safety requirements when carrying out chemical analysis of primary Nickel, Nickel powder, cobalt, and cobalt powder.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 12.0.004−90 System of standards of occupational safety. Organization of training safety. General provisions

GOST 12.1.004−91 System safety standards. Fire safety. General requirements

GOST 12.1.005−88 standards System of labor safety. General hygiene requirements for working zone air

GOST 12.1.007−76 System of standards of occupational safety. Harmful substances. Classification and General safety requirements

GOST 12.1.010−76 System of standards of occupational safety. No danger of explosion. General requirements

GOST 12.1.016−79 System of standards of occupational safety. The air of the working area. Requirements for measurement techniques of concentrations of harmful substances

GOST 12.1.030−81 System of standards of occupational safety. Electrical safety. Protective grounding, neutral earthing

GOST 12.2.007.0−75 System safety standards. Products electrical. General safety requirements

GOST 12.3.002−75 System safety standards. The process of production. General safety requirements

GOST 12.3.019−80 standards System of labor safety. Test and measurement electrical. General safety requirements

12.4.009 GOST-83 System of standards of occupational safety. Fire fighting equipment for protection of objects. Principal. The accommodation and service

GOST 12.4.021−75 System safety standards. System ventilation. General requirements

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

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

GOST 4212−76 Reagents. Methods of preparation of solutions for colorimetric and nephelometric analysis

GOST 6012−2011 Nickel. Methods of chemical-atomic-emission spectral analysis

GOST 6709−72 distilled Water. Specifications

GOST 8776−2010 Cobalt. Methods of chemical-atomic-emission spectral analysis

GOST 9721−79 cobalt Powder. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 13047.4−2014 Nickel. Cobalt. Methods for determination of cobalt in Nickel

GOST 13047.5−2014 Nickel. Cobalt. Methods for determination of Nickel in cobalt

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 13047.12−2014 Nickel. Cobalt. Methods for determination of antimony

GOST 13047.14−2014 Nickel. Cobalt. Methods for determination of bismuth

GOST 13047.17−2014 Nickel. Cobalt. Methods of iron determination

GOST 13047.18−2014 Nickel. Cobalt. Methods for determination of arsenic

GOST 13047.21−2014 Nickel. Cobalt. Methods for determination of manganese

GOST 13047.22−2014 Nickel. Cobalt. Methods for determination of thallium in Nickel

GOST 13047.25−2014 Nickel. Cobalt. Methods for determination of selenium in Nickel

GOST 23148−98 Powders used in powder metallurgy. Sampling

GOST 23932−90 Glassware and laboratory equipment made of glass. General specifications

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


GOST 24231−80 non-ferrous metals and alloys. General requirements to selection and preparation of samples for chemical analysis

GOST 25086−2011 non-ferrous metals and their alloys. General requirements for methods of analysis ST SEV 543−77 Number. Record rules and rounding

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

3.1 General requirements for methods of analysis GOST 25086 with additions.

3.2 Selection and preparation of samples primary Nickel is carried out according to GOST and GOST 24231 849, cobalt — 24231 GOST and GOST 123, Nickel and cobalt powder to GOST 23148, GOST 9721 9722 and GOST.

3.3 apply When weighing laboratory scales special and high accuracy classes of any type according to GOST 24104. The permissible error of weighing is set to the standard methods of analysis by specifying the category in the numeric value of the mass of sample.

3.4 calcination and fusion of samples and reagents used laboratory muffle furnace, providing temperatures up to 1200 °C. During the drying of samples and reagents used laboratory drying oven providing temperatures up to 250 °C. For dissolution and evaporation of solutions used the electric oven with closed coil that provides heating to a temperature of 350 °C.

3.5 the Term «warm» means that the solution should have a temperature of from 40 °C to 75 °C. the Term «cool» means that the solution should have a temperature of from 15 °C to 25 °C.

3.6 measurement time less than 5 min used hourglasses and stopwatches, 5 min, timers and clocks of any type.

3.7 When carrying out analysis of samples performed by two parallel definitions for test portions taken from one sample, and the differences in the evaluation of the chemical composition of products between the supplier and the consumer — three parallel determinations.

3.8 For the preparation of solutions of reagents using distilled water according to GOST 6709 with further purification through filters with ion-exchange resin.

3.9 storage Conditions and use of the solutions of the identified elements of known concentration — according to GOST 4212 if the standards governing methods of analysis that are not otherwise required.

3.10 For the preparation of solutions of elements of known concentration is allowed to use the state standard samples of composition of the solution of ions of these elements.

3.11 Requirements governing quality of used glass ware, described in GOST 23932.

3.12 Requirements governing quality of used glass laboratory volumetric glassware, set in GOST 1770.

3.13 in determining the mass fraction of impurity elements along with the analysis under the same conditions conduct control experience for contamination of reagents.

Supervisory experience considered satisfactorily carried out if the result does not exceed half of the analytic signal is the first point of the calibration curve specified in the standard methods of analysis. Otherwise, the analysis used reagents of high purity or purified further.

When using atomic-absorption methods of analysis of a control experiment is conducted with the introduction of the same sample of Nickel or cobalt, which are used in the preparation of the calibration solutions and the mass of which is equal to the weight of the sample.

Other modalities of the control of the experience and take it into account when calculating the result of the analysis are given in the standards governing methods of analysis.

3.14 For Nickel and cobalt used in the preparation of the calibration solutions in atomic-absorption methods of analysis, make a preliminary assessment of the content of impurity elements. For this purpose, 8776 GOST, GOST 6012, spectrophotometric methods described in GOST 13047.4, 13047.5 GOST, GOST 13047.8, 13047.10 GOST, GOST 13047.12, 13047.14 GOST, GOST 13047.17, 13047.18 GOST, GOST 13047.21, 13047.22 GOST, GOST 13047.25, and the method of addition of solution of known concentration of the element. The mass of the additive element should correspond to the mass of that element in the first calibration solution specified in the relevant standard method atomic absorption analysis.

When using the addition method samples of Nickel and cobalt acknowledge useable, if the value of the measured values of absorption for the sample without additive does not exceed half the value of the measured values of absorption for the sample with the additive. Otherwise, the samples of Nickel and cobalt is replaced with new.

3.15 When using spectrophotometric methods of analysis the thickness of the absorbing layer of the cell are selected such as to provide measurements in the optimal range of values of optical density for the applied means of measurement.

3.16 the use of atomic absorption methods of analysis under condition of achievement of the metrological characteristics specified in the standards regulating the methods of analysis are permitted:

— use the calibration solutions with the introduction of several of the identified elements;

— change the range of content of the determined elements in calibration solutions subject to the linearity of the calibration curve;

— to use when measuring the absorption of other resonance spectral line;

— use automated build system calibration charts, measurements in automatic mode with the results of the analysis result to the printer of the automated spectrometer;

— consistently determine several elements of one sample of the sample after decomposition and appropriate dilution of the sample solution so that the mass of the element it was in the range of calibration curve.

3.17 checking the admissibility of the results of two or three definitions, obtained in conditions of repeatability, is carried out by comparing the differences of the maximum and minimum results of parallel measurements with the repeatability limit r. The result of the analysis is calculated as the arithmetic mean of the results of parallel measurements, if the condition

, (1)

where r=2,77 — limit frequency for the two parallel measurements and r=3,31 — limit frequency for three parallel definitions for confidence level 95%;

 — standard deviation (SD) of the results of parallel measurements.

If the condition (1) analysis is repeated to obtain one or two results of parallel measurements.

If you are performing four definitions range () of the results of the four definitions of equal or less value of the critical range CR(4) for a confidence level of 95%, the final result should be recorded, the arithmetic mean of the results of the four definitions.

The value of the critical range CR(4) for the four parallel measurements is calculated by the formula

, (2)

where  — standard deviation results of parallel measurements obtained in conditions of repeatability.

In exceptional cases, if the range of the results of the four definitions more critical range CR(4), we proceed as follows: to investigate the cause of exceedance of critical range and repeat the analysis on samples obtained by repeated sampling. If in this case the range of the results of the four definitions more critical range CR(4), it is allowed to record the median of the results of the four definitions:

(3)

as indicative values mass fraction of the element in the sample. This value lead without indication of measurement uncertainty.

The result of the analysis in the documents that use it are in the form of: X or X±U with k=2, where k is the coverage factor according to the recommendations [1]. In case of submission of result analysis in the form X provide a link to the document outlining the U — value expanded uncertainty (limit of the total error).

The regulations control the precision — limits of repeatability for two and three results of parallel measurements, the limit of reproducibility of the two analysis results and increased control precision — the expanded uncertainty of the results of the analysis are given in each standard for all defined elements in Nickel and cobalt. For intermediate values of the mass fraction of elements the values of the metrological characteristics find using linear interpolation.

3.18 the Numerical value of the result of the analysis should be terminated with a figure the same category as the value of expanded uncertainty U, as specified in the standard methods of analysis.

In the preparation of quality document production on the basis of the results of the analysis allowed to represent the value of the mass fraction of an element with the same number of significant figures as in the tables of chemical composition to GOST 849, GOST 9722, GOST 123 and GOST 9721.

3.19 Rules for rounding of numbers shall conform to the requirements of ST CMEA 543.

3.20 Intralaboratory quality control results of analysis carried out by the following procedure:

a) monitoring the error on the standard samples of composition of Nickel -, cobalt -, Nickel -, and cobalt powders;

b) monitoring the error using the sample dilution and addition method;

C) control the stability of the results of the analysis with the use of checklists for systematic errors of the average values, differences in the conditions of repeatability;

g) monitoring the stability of calibration curve.

Specific procedures, periodicity of their performance, as well as guidance on the marking (masking) of samples for monitoring are regulated in the documents of the laboratory.

Along with the above procedures, the laboratory can confirm the accuracy of the analysis results by participating in interlaboratory comparative tests.

4 safety Requirements

Analysis of Nickel and cobalt should be carried out in accordance with the regulatory documents regulating the requirements for safe operation in laboratories of analytical control.

4.1 carry out All work on the appliances and electrical systems that meet the requirements of GOST 12.2.007.0 and rules of electrical devices [2].

4.2 When the equipment and installations required to comply with the requirements of GOST 12.3.019 and rules [3], [4].

4.3 All equipment and installations should be equipped with devices for grounding in accordance with the requirements of GOST 12.2.007.0 and GOST 12.1.030. Grounding must conform to the rules [2].

4.4 Facilities the laboratory must have a General ventilation according to GOST 12.4.021, meet the fire safety requirements according to GOST 12.1.004 and [5], to have a means of extinguishing according to GOST 12.4.009.

4.5 When working with flammable and explosive gases should comply with the requirements of GOST 12.1.010, GOST 12.1.004 and [6].

4.6 in conducting chemical analysis of Nickel, cobalt, and Nickel and cobalt powders using the reagents and materials which have a harmful effect on the human body: acids, alkalis and organic solvents. Their content in the air of working zone shall conform to the requirements of GOST 12.1.005.

4.7 Storage and use of chemicals and materials with hazardous and harmful properties, must meet the requirements regulated in the regulations on these chemicals and materials.

4.8 Monitoring of content of harmful substances in the air of working zone should be carried out in accordance with the requirements of GOST 12.1.007, GOST 12.1.005 and GOST 12.1.016.

4.9 Disposal, deactivation and destruction of hazardous wastes from chemical analysis of Nickel, cobalt, and Nickel and cobalt powders should be carried out in accordance with the sanitary regulations [7].

4.10 the Organization of training of the working personnel to the requirements of labour safety — according to GOST 12.0.004.

4.11 Requirements for professional selection and testing of knowledge of employees — according to GOST 12.3.002.

4.12 laboratory Personnel must be provided with household premises in the group production processes IlIa according to [8].

4.13 laboratory Personnel must be provided with special clothing, special footwear and other means of individual protection [9].