GOST 25086-2011
GOST 25086−2011 non-ferrous metals and their alloys. General requirements for methods of analysis (Change No. 1)
GOST 25086−2011
Group B59
INTERSTATE STANDARD
NON-FERROUS METALS AND THEIR ALLOYS
General requirements for methods of analysis
Non-ferrous metals and their alloys. General requirements for methods of analysis
ISS 77.120.01*
___________
* Changed the wording, Rev. N 1.
Date of introduction 2012−10−01
Preface
Goals, basic principles and 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», Open joint-stock company, OAO «uralmekhanobr"
2 SUBMITTED by the Technical Secretariat of the Interstate Council for standardization, Metrology and certification
3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 40 of November 29, 2011)
The adoption voted:
| Short name of the country on MK (ISO 3166) 004−97 |
Country code by MK (ISO 3166) 004−97 |
Abbreviated name of the national authority for standardization |
| Azerbaijan | AZ |
Azstandart |
| Armenia | AM |
Ministry Of Economy 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 |
| Moldova | MD |
Moldova-Standard |
| Russian Federation | EN |
Rosstandart |
| Tajikistan | TJ |
Tajikstandart |
| Turkmenistan | TM |
The MDCSU «Turkmenstandartlary» |
| Uzbekistan | UZ |
Uzstandard |
| Ukraine | UA |
Derzhspozhyvstandart Of Ukraine |
4 by Order of the Federal Agency for technical regulation and Metrology, dated 22 may 2012 N 74 St interstate standard GOST 25086−2011 introduced as a national standard of the Russian Federation from October 1, 2012
5 REPLACE GOST 25086−87
Information about introduction in action (termination) of this standard is published published monthly information index «National standards».
Information about the changes to this standard is published in the annually issued reference index «National standards», and the text changes and amendments — in monthly indexes published information «National standards». In case of revision or cancellation of this standard the appropriate information will be published in a monthly information index «National standards»
The Change N 1, approved and promulgated by the Order of Rosstandart
Change No. 1 made by the manufacturer of the database in the text IUS N 12, 2015
1 Scope
This standard establishes General requirements for methods of analysis of non-ferrous metals and their alloys, as well as safety requirements.
This standard does not apply to carbide materials and metals of high purity.
2 Normative references
This standard uses the regulatory references to the following international standards:
GOST 8.010−2013 State system for ensuring the uniformity of measurements. The techniques of measurements. Main provisions*.
_______________
* On the territory of the Russian Federation GOST R 8.563−2009 «State system for ensuring the uniformity of measurements. Techniques (methods) of measurements».
GOST 8.315−97 State system for ensuring the uniformity of measurements. Standard samples of composition and properties of substances and materials. Key issues*
________________
* On the territory of the Russian Federation in the part of the applications D and e is valid GOST R 8.753−2011 «State system for ensuring the uniformity of measurements. Standard samples of materials (substances). General provisions».
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 12.1.019−79 System of standards of occupational safety. Electrical safety. General requirements and nomenclature of types of protection*
_______________
* On the territory of the Russian Federation GOST R 12.1.019−2009 «the System of occupational safety standards. Electrical safety. General requirements and nomenclature of types of protection».
GOST 12.1.030−81 System of standards of occupational safety. Electrical safety. Protective grounding, neutral earthing
GOST
12.4.009 GOST-83 System of standards of occupational safety. Fire fighting equipment for protection of objects. Principal. The accommodation and service
GOST 12.4.011−89 System safety standards. Means of protection of workers. General requirements and classification
GOST 12.4.021−75 System safety standards. System ventilation. General requirements
GOST 12.4.068−79 System of standards of occupational safety. PPE dermatological. Classification and General requirements
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 4517−87 Reagents. Methods for the preparation of accessory reagents and solutions used in the analysis
GOST 4919.1−77 Reagents and highly purified substances. Methods of preparation of solutions of indicators
GOST 4919.2−77 Reagents and highly purified substances. Methods for the preparation of buffer solutions
GOST ISO 5725−1-2003 Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions*
_______________
* On the territory of the Russian Federation GOST R ISO 5725−1-2002 «Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions».
GOST ISO 5725−6-2003 Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice*
_______________
* On the territory of 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 6563−75 technical articles made of noble metals and alloys. Specifications
GOST 6709−72 distilled Water. Specifications
GOST 9147−80 Glassware and equipment lab porcelain. Specifications
GOST ISO/IEC 17025−2009 General requirements for the competence of testing and calibration laboratories
GOST 19908−90 Crucibles, bowls, beakers, flasks, funnels, test tubes and caps made of transparent quartz 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 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions
GOST 25794.1−83 Reagents. Methods for the preparation of titrated solutions for acid-base titration
GOST 25794.2−83 Reagents. Methods for the preparation of titrated solutions for redox titration
GOST 25794.3−83 Reagents. Methods for the preparation of titrated solutions for titration by precipitation, non-aqueous titration and other methods
GOST 27025−86 Reagents. General instructions for testing
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 29228−91 (ISO 835−2-81) oils. Pipettes are graduated. Part 2. Pipettes graduated without a set timeout
GOST 29229−91 (ISO 835−3-81) oils. Pipettes are graduated. Part 3. Pipettes graduated with a standby time of 15 s
GOST 29251−91 (ISO 385−1-84) oils. Burette. Part 1. General requirements
GOST 29252−91 (ISO 385−2-84) oils. Burette. Part 2. Burette without a set timeout
GOST 29253−91 (ISO 385−3-84) oils. Burette. Part 3. Burette with waiting time 30 s
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 published annually by the information sign «National standards» published as on January 1 of the current year and related information published monthly indexes published in 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.
(Changed edition, Rev. N 1).
3 Terms and definitions
This standard applies the following terms with respective definitions:
3.1 methods of quantitative chemical analysis; method of analysis: the Set of operations and rules, which provide the results of quantitative chemical analysis (hereinafter — the results of the analysis) with the established characteristics of error (uncertainty in accordance with the guidelines [1]).
Notes
1 the Method of analysis is a kind of methodology of measurements.
2 as the measured characteristics take a massive share of one or several components of the sample composition.
3.2 the result of the analysis: the Average value (arithmetic mean value or median) of the results of a single determination.
Note — the test Result represents the average value of the results of single determinations.
3.3 the result of a single determination: the Value of the mass fraction of a component in a sample of substance (material), obtained after a single procedure analysis.
Note — In the document on methods of analysis set how many results of single definitions (a parallel definition) has to be obtained, methods of averaging and reporting as a result of the analysis. In the simplest case (if the method of analysis is not suitable for a parallel definition) the result of a single determination is actually the result of the analysis.
3.4 precision: the Degree of closeness to each other of the results of a single determination (analysis results) obtained in the specific controlled conditions.
3.5 repeatability: Precision under conditions of repeatability.
3.6 repeatability conditions: Conditions under which the result of a single definition of get by one method on identical samples under the same conditions and almost simultaneously (the results of parallel measurements).
3.7 root-mean-square (standard) deviation of repeatability:the Standard deviation (SD) of the results of a single determination obtained by the method in terms of repeatability.
3.8 the limit of repeatability : Acceptable for the accepted probability of 0.95, the absolute discrepancy between the highest and lowest from
the result of a single determination obtained in conditions of repeatability.
3.9 reproducibility: Precision under conditions of repeatability.
3.10 reproducibility conditions: Conditions under which the results of the analysis, receive one and the same method on identical samples but under different conditions (different time, different analysts, different lots of reagents of the same type, different sets of volumetric glassware copies of the measuring instruments of the same type, different lab).
3.11 root-mean-square (standard) deviation of reproducibility:the Standard deviation of the test results obtained under reproducibility.
3.12 reproducibility limit : the Permissible for the adopted level of 0.95, the absolute discrepancy between the two analysis results obtained under conditions of reproducibility.
3.13 — performance analysis techniques (indicators of precision, accuracy, repeatability, intermediate precision, reproducibility): Assigned specifications of error analysis techniques and its (uncertainty) components.
3.14 systematic error of the laboratory (with implementation of methods of analysis): the difference between the mathematical expectation of the results of a single analysis obtained in individual laboratories, and true (or in his absence the accepted reference) value of the designated characteristics.
3.15 accepted reference value: a Value that serves as a consensus for comparison.
Note — the methods of evaluation of quality indicators of the analysis techniques considered in this standard, the reference values can be taken:
a) the certified value of the standard sample;
b) certified value certified mixture;
C) the mathematical expectation of the measured characteristics, i.e. the average value of a given set of analysis results, only in the case when the enumeration of a) and b) is not available.
3.16 error analysis result (the result of a single analysis): the Deviation analysis result (the result of a single analysis), obtained by certified methods, from true (or in his absence the accepted reference) value.
3.17 intermediate precision: The precision in the conditions in which the results of the analysis receive the same method on identical samples under variation of one (e.g. time) or more (e.g., artists, and time) factors shaping the spread of the results of the analysis when applying the technique to the specific laboratory.
3.18 calibration characteristics of means of measurements of substances and materials: Functional dependence of analytical signal on the mass fraction of the component that is obtained in the sample of the substance (material), expressed as a formula, graph or table.
3.19 calibration sample: a reference Sample or set of samples used for the calibration of measuring instruments in the analysis of samples of substances.
Note — Variations of the calibration are calibration sample solution or the calibration mixture.
3.20 the aliquot: the volume of a Certain liquid, gaseous or granular homogeneous substance, which is a part of the whole.
3.21 sample of substance (material) (object of analytical control): the separation of the substance (material) objects of analytical control for the purpose of formation samples for the subsequent determination of its composition, structure and/or properties.
3.22 standard sample: Sample of substance (material) established by test results the values of one and more quantities characterizing the composition or property of this substance (material).
3.20−3.22 (Introduced later, Rev. N 1).
4 General provisions
Methods of analysis used in the quality control of non-ferrous metals and their alloys shall meet the requirements of GOST 8.010, GOST, ISO 5725−1, GOST ISO/IEC 17025 and of this standard.
5 requirements for the selection and preparation of samples
The selection and preparation of samples of metals and alloys is carried out according to GOST 24231 and normative documents (ND) for specific products.
6 requirements for the representation of the values of precision in analysis techniques
In the document on the method of analysis should be presented numerical values of the norms of the error of the analysis or value accuracy specifications (or its components) in accordance with GOST 8.010 and/or provides information about the accuracy (correctness and precision) of the standard method of analysis in accordance with the standard ISO 5725−1.
Note — When specifying a minimum set of metrological characteristics of methods of analysis should be the values of error (uncertainty) analysis, limits of repeatability and reproducibility. At the request of the developer, if necessary, you can specify other characteristics.
7 Requirements for measuring instruments, auxiliary equipment, materials and reagents
7.1 the analysis used laboratory scales according to GOST 24104. The class of accuracy of scales must be specified in the method of analysis.
7.2 For analysis use dimensional laboratory glassware not lower than 2nd accuracy class according to GOST 1770, 29169 GOST, GOST 29227, 29228 GOST, GOST 29229, GOST 29251, 29252 GOST, GOST 29253, utensils and equipment according to GOST 25336, crockery and equipment (crucibles, boats, inserts for desiccators, etc.) according to GOST 9147, dishes made of transparent quartz glass (crucibles, flasks, test tubes etc.) according to GOST 19908, and jewelry made of platinum according to GOST 6563, the dishes of glassy carbon brand SU-2000 [2].
7.3 For the measurement of time intervals less than 5 min used an hourglass or a stopwatch, 5 min, timers or clocks of any type.
7.4 Apply the methods of analysis measuring instruments and test equipment must undergo the procedure of recognition of suitability in accordance with the procedure adopted in the territory of a particular state*.
_______________
* On the territory of the Russian Federation the following order: used in the implementation of techniques of the analysis of the measuring instruments should be verified or calibrated; the test equipment must be certified.
7.5 reagents Used should have the qualification «pure for analysis» (h. d. a.). Allowed the use of the reagents lower qualifications provided that their metrological characteristics of the analysis results, normalized in the method of analysis. Mandatory application of reagents a higher qualification stipulated in the framework of analysis.
7.6 For each unit of consumer packaging of chemical reagents and especially pure substance should be attached label indicating the name of the reagent/substance, refer to the relevant normative document for the chemical/substance, qualification, date of manufacture, shelf life of the reagent.
7.7 verification of the fitness for use of laboratory reagents with the expired period of storage should be carried out in accordance with the recommendations of [3] or the procedure provided in the lab.
If necessary:
— the label should be affixed indicating the special storage conditions reagent/substance;
— the label must be protected from external influences.
7.8 For the preparation of solutions and the analysis used distilled water according to GOST 6709, if no other.
7.9 In the expression «diluted 1:1, 1:2, etc.» and the designation (1:1), (1:2) etc. the first digits stand for the volumetric part of the dilute reagent (e.g., concentrated acid), the second volume of the used solvent (e.g., water, butanol, etc.).
7.10 the Concentration of solutions Express:
in units of mass concentration: g/DMg/cm
, mg/DM
µg/cm
;
in units of molar concentration — mol/DM;
— the relative density of the indicating substance, which is density.
Substance content in metals and alloys to Express a mass fraction in percent million(ppm, ppm).
7.11 If the method of analysis not specified the concentration or the degree of dilution of the solution of reagent (acid, alkali, etc.), refers to a concentrated solution of the reagent.
7.12, the Mass concentration of titrant solutions establish not less than three aliquots of a solution or three batches of material with known content of determined component.
The accuracy of establishing the mass concentration is determined by specific conditions of preparation and the purpose of the solution.
(Changed edition, Rev. N 1).
7.13 For the preparation of solutions with known concentrations of metals used metals and their compounds, containing at least 99.9% of the basic substance, if the regulations on the method of analysis not specified; use standard samples (CO) composition of solutions of metal ions.
For the preparation of solutions of known concentration allowed the use of standard samples (CO) composition of ion solution of these elements.
(Changed edition, Rev. N 1).
7.14 Solutions of chemical reagents prepared in accordance with GOST 4212, GOST 4517, 4919.1 GOST, GOST 4919.2, 25794.1 GOST, GOST 25794.2, 25794.3 GOST, GOST 27025.
7.15 preparation of solutions and analysis after each addition of the reagent the solution was stirred.
7.16 the Term «warm» means that the solution should have a temperature of from 40 °C to 75 °C. the Term «hot water (a solution)» means that the water (solution) has a temperature of above 75 °C. the Term «cooling» means cooling to a temperature of from 15 °C to 25 °C.
7.17 Preparation of measuring and test equipment measurement and performance measurement is carried out in accordance with the operating instructions for these devices.
When using (spectrophotometer)photometric methods of analysis the thickness of the light absorbing layer of the cell and the wavelength of the measured component are selected such as to provide measurements in an optimal optical densities for the applied means of measurement.
By using the methods of atomic absorption wavelength, the composition of the gas flame, a reducing or oxidation, its action, flow, type of burner and other conditions are chosen to achieve optimum results in terms of accuracy and sensitivity of the measured component.
When using methods of analysis atomic spectrometry subject to the achievement of the metrological characteristics specified in the documents on methods of analysis allowed:
— to use for the calibration solutions with the introduction of several definable components;
— change the range of the measured component in solutions to calibration subject to calibration function;
— to use when measuring the absorption of other resonance spectral line;
— use automated build system calibration charts, measurements in automated mode with the results of the measurements on paper or electronic media;
— consistently to measure several components in one test portion of the sample after decomposition and the corresponding dilution of the solution so that the mass of measured component in it was in the range of mass concentrations in solutions for calibration.
7.18 If necessary, identification of the main components in the sample, it is recommended to carry out preliminary qualitative analysis.
8 Requirements analysis
8.1 When performing the analysis can be used the following methods: electrogravimetry, photometric, atomic absorption, atomic emission with photoelectric registration of spectrum (spectral), atomic emission with inductively coupled plasma, etc. the Choice of methods due to the presence in the laboratory of measuring instruments test equipment.
8.2 If the performance of analysis provides for the establishment of calibration characteristics of means of measurements of substances and materials, in the corresponding section of methods of analysis lead to ways of establishing and monitoring, as well as the preparation and use of calibration samples, which use standard samples according to GOST 8.315 and certified mixtures in accordance with the recommendations [4].
8.3 at the same time under the same conditions, if necessary, hold the control (blank) experience for the amendment of the results of the analysis, if the control experience is regulated by the methodology. The number of parallel definitions in a control experiment corresponds to the number of parallel measurements specified in the methodology analysis.
8.4 environmental Conditions should ensure the correct execution of the analysis and conform to the requirements specified in the analysis methods or in the operating instructions of the equipment.
9 Requirements for the processing and presentation of analysis results
9.1 the result of the analysis take the average value (arithmetic mean value or median) of the results of parallel measurements. The number of parallel measurements, to be averaged in the calculation of the analysis result, indicate the method of analysis.
The numerical value of the result of the analysis should be terminated with a figure the same category as the indicator of accuracy specified in the methods of analysis.
9.2 the Discrepancy between the highest and lowest results of parallel measurements with the sample analysis at confidence probability of 0.95 should not exceed the repeatability limit
, the value of which is given in the method of analysis.
If the discrepancy between the highest and lowest results of parallel measurements exceeds the value , the analysis procedure is repeated. The eligibility check is carried out according to the method of analysis. Can be used as methods of verification of admissibility of the results of parallel measurements and establishing the final result in accordance with GOST ISO 5725−6, and the methods given in Appendix A.
Allowed to represent the limit of repeatability for individual mass fraction with the calculation of its values for the intermediate mass fraction by linear interpolation.
It is allowed to insert the limit of repeatability in the form of equations or tables that includes the whole interval of the mass fraction of the designated component to be mounted in the method of analysis and divided into putinterval, in which the appropriate values
can be assumed constant.
Note — If determination is performed in terms of a type of intermediate precision, limit of repeatability should be replaced by the limit of intermediate precision.
9.3 Rounding of the results of the analysis carried out in accordance with the requirements of ST CMEA 543.
9.4 the result of the analysis are in the form of
where is the result of the analysis;
— the value of error.
10 quality Control of analysis results
Quality control of analysis results within the laboratory organized and carried out in accordance with GOST ISO 5725−6, recommendations [5] and according to Appendix B. the Periodicity of the results of the control procedures and their registration lead in the documents of the laboratory, establishing the order and content of works on the organization control methods of stability analysis results in the laboratory.
11 safety Requirements
11.1 Preparation of samples for analysis, conduct the analysis (dissolution in acids, alkalis etc.) and all the operations of chemical analysis related to the release of toxic fumes or gases should be performed in fume cupboards or boxes equipped with local suction device according to GOST
In laboratory premises allowed to store chemicals in a Cabinet, equipped with a ventilation system with corrosion-resistant coating in accordance with the requirements of GOST
11.2 Laboratory areas should be equipped with General dilution ventilation system according to GOST
11.3 When running an analysis in workplace air can be harmful substances, maximum permissible concentration (MPC) in air of working zone should correspond to GOST 12.1.005 and hygienic standards [6].
11.4 Control of content of harmful substances in the air of working zone should be carried out in accordance with the requirements of GOST 12.1.005, GOST 12.1.007 and GOST
11.5 Laboratory facilities which perform work on the chemical analysis of the investigated material must meet fire safety requirements according to GOST 12.1.004 and rules [7]. The means and methods of fire suppression should be applied according to the GOST 12.4.009 depending on the origin and nature of the fire.
11.6 When working with flammable and explosive gases should comply with the requirements of GOST 12.1.004 and GOST
11.7 Electrical instrumentation and laboratory equipment, and the terms of use must comply with the requirements of GOST 12.1.019, GOST 12.1.030, GOST
11.8 Organization of training and testing knowledge of safety requirements of work — according to GOST
11.9 laboratory Personnel must be provided with special clothing, special footwear and other means of individual protection in accordance with GOST 12.4.011, GOST 12.4.068 and rules and regulations adopted on the territory of the CIS.
11.10 laboratory Personnel must be provided with sanitary-household premises in the group production processes 3A in accordance with the building regulations [11].
11.11 When transferring bottles with acids, alkalis and ammonia must be provided reliable protection of the container against damage (crates, etc.).
11.12 When using source materials that have hazardous properties should comply with the safety requirements regulated by normative documents to the appropriate reagents.
11.13 Each source of spectra excitation must have the metal cover or screen for protection against electromagnetic and ultraviolet radiation, electroablation for protection against accidental touching of live parts.
11.14 When performing x-ray analysis it is necessary to observe the rules of radiation safety in accordance with the sanitary-epidemiological rules and norms of radiation security accepted in the territory of the CIS.
11.15 Waste acid and alkali should be collected separately in special containers; after neutralizing, drain into the sewer or in accordance with local conditions in the designated place.
11.16 in the test with the use of solvents or chlorine derivatives of hydrocarbons it is necessary to use personal protective equipment, taking account of the ways of penetration of these substances into the body (e.g., through the skin, respiratory tract).
11.17 Illumination of workplaces must comply with the requirements of sanitary rules and norms on the territory of the CIS.
Annex a (recommended). Methods of testing the acceptability of results obtained in conditions of repeatability and reproducibility
Appendix A
(recommended)
A. 1 verification of the admissibility of the results of parallel measurements obtained in conditions of repeatability, is carried out upon receipt of each result of the analysis of work samples.
A. 2 procedure for checking the acceptability of the results involves comparing the absolute differences between the largest 
made in accordance with the method of analysis, with a limit of repeatability
.
If the condition
for the result of the analysis taking the arithmetic mean of the results of a single analysis
(
1, …,
).
If the method of analysis indicator of the frequency of occurrence specified as standard deviation (SD), the repeatability limit is calculated by the formula
where 
of individual analysis results, obtained in conditions of repeatability and confidence
. Coefficient values
for the acceptance probability of
0.95 is given in table A. 1;
— Standard deviation of repeatability given in the method of analysis.
Table A. 1 — Values of coefficient 
of 0.95
|
|
| 2 |
2,8 |
| 3 |
3,3 |
| 4 |
3,6 |
| 5 |
3,9 |
| 6 |
4,0 |
| 7 |
4,2 |
| 8 |
4,3 |
| 9 |
4,4 |
| 10 |
4,5 |
)
If the condition (A. 1) is not satisfied, perform the procedure described in A. 3.
(Changed edition, Rev. N 1).
A. 3 Receive parallel definitions,
1 if the analysis is expensive.
The result of the analysis taking the arithmetic mean 
where 
The critical range 
where 
. Coefficient values
0.95 is given in table A. 1;
— Standard deviation of repeatability established in the method of analysis.
A. 4 If the condition (A. 3) is not fulfilled, you must find out the reasons of unsatisfactory results of analysis and take action to correct for the final result of the analysis can be accepted by the median 
A. 5 the discrepancy between the analysis results obtained in two laboratories, should not exceed the limit of reproducibility. If this condition is acceptable both results of analysis and as the final can be used by their overall average.
If you exceed the limit of reproducibility can be used methods for assessing the acceptability of the results of the analysis according to GOST ISO 5725−6.
A. 6 the test of the two analysis results obtained by one method of analysis with different values of precision (if the interval representation), the limits of repeatability , intermediate precision
are calculated according to formulas
where and
indicators of the frequency of occurrence for the values of determined component in a sample;
where 
where and
indicators of reproducibility.
Appendix B (recommended). The quality control analysis results in the laboratory
Appendix B
(recommended)
B. 1 accuracy Control of the results of the analysis within the laboratory to carry out analysis with the established indices of accuracy (correctness and precision) and approved for use in the prescribed manner in accordance with the recommendations of [5], [12] and GOST ISO 5725−6.
B. 2 During the implementation of analysis methods in the laboratory provide operational control procedures for the analysis and control of stability analysis results.
Algorithm of operative control of the analysis procedures should be given in the document on the method of analysis.
Control procedures of stability analysis results reglamentary in the quality manual of the laboratory.
B. 3 as a means of control can be used:
— samples for control (s): standard samples (SS) according to GOST 8.315 or certified mixture (AC) according to the recommendations [4];
— working samples with known additive detectable component;
— working samples of a stable composition;
— work samples, diluted in a specific ratio;
— other methods of analysis with the established indices of accuracy (control techniques).
B. 4 Control procedures analysis of samples for control (QA) consists in the comparison result of the control determining the certified properties of the specimen to control with the certified value according to the recommendations [5]. At the same time OK must be adequate to the analyzed samples (possible differences in the compositions of the analyzed samples should not contribute to the results of the analysis of statistically significant error). The error of the certified value of CR should be not more than one-third of the accuracy specifications of the analysis.
If during the inspection, samples are used to control that have not been used in establishing the accuracy rate of the results of the analysis, in case of exceeding the error of the OK one third of the error of the analysis techniques, allowed the ratio control is calculated by the formula
where — error certified value is OK;
— the indicator of the accuracy of analysis results corresponding to the certified value approx.
B. 5 Operational control procedures of the analysis using the addition method, the reference methods of analysis or method of a sample dilution implemented in accordance with the algorithms given in the recommendations [5].
Allowed to use other methods of operational control procedures of analysis.
B. 6 To test the stability of analysis results within the lab using the control procedure according to GOST ISO 5725−6 and recommendations [5].
B. 7 Choice of method of control depends on the objects analysed and indicators methods of analysis, cost and duration analysis, etc.
Bibliography
| [1] | Guide EBRAHIM/SEATAC «a Quantitative description of uncertainty in analytical measurement"*. The translation from English. The second edition of the VNIIM im. Mendeleev, S-Pb., 2002 | |
| ________________ * Document authoring is. For additional information, please refer to the link. — Note the manufacturer’s database. | ||
| [2] | THAT 1916−027−02728846−01* | The product of glassy carbon brand SU-2000 (crucibles, bowls)** |
_______________ ** Valid on the territory of the Russian Federation. | ||
| [3] | Recommendations on the interstate standardization RMG 59−2003 |
State system for ensuring the uniformity of measurements. Verification of fitness for use in laboratory reagents with the expired period of storage method of laboratory control of precision of the measurement |
| [4] | Recommendations on the interstate standardization RMG 60−2003 |
State system for ensuring the uniformity of measurements. Mix certified. General requirements for the development |
| [5] | Recommendations on the interstate standardization RMG 76−2004 |
State system for ensuring the uniformity of measurements. Internal quality control of results of quantitative chemical analysis |
| [6] | Hygienic standards |
Chemical factors of production environment. The maximum permissible concentration (MPC) of harmful substances in the air of working zone* |
| _______________ * Valid on the territory of the Russian Federation. | ||
| [7] | PPB 01−03* | The rules of fire safety in the Russian Federation approved by the Ministry of emergency situations of Russia dated 18 June 2003 N 313** |
_______________ * On the territory of the Russian Federation the document is not valid. Rules of fire prevention regime in the Russian Federation. — Note the manufacturer’s database. ** Valid on the territory of the Russian Federation. | ||
| [8] | PB 03−576−03 | Rules of arrangement and safe operation vessels working under pressure, approved by the Resolution of Gosgortekhnadzor of the Russian Federation from June, 11th, 2003 N 91* |
| _______________ * Valid on the territory of the Russian Federation. | ||
| [9] | GOST R 51350−99 (IEC 61010−1-90) |
The system of occupational safety standards. Safety of electrical instrumentation and laboratory equipment. Part 1. General requirements* |
| _______________ * Valid on the territory of the Russian Federation. | ||
| [10] | Rules of arrangement of electrical installations, approved by the RF Ministry of energy. Order No. 204 dated July 8, 2002.* | |
| _______________ * Valid on the territory of the Russian Federation. | ||
| [11] | Building codes and rules SNiP 2.09.04−87 |
Administrative and domestic buildings |
| [12] | Recommendations on the interstate standardization RMG 61−2003* |
State system for ensuring the uniformity of measurements. Indicators of accuracy, trueness, precision methods of quantitative chemical analysis. Methods of evaluation |
| ________________ * On the territory of the Russian Federation the document is not valid. Are RMG 61−2010, here and hereafter. — Note the manufacturer’s database. | ||
| UDK 669.2/8:006.354 |
ISS 77.120.01 | B59 |
| Key words: non-ferrous metals and their alloys-selection and preparation of samples, measurement tools, indicators of accuracy | ||
