GOST 1293.0-2006
GOST 1293.0−2006 lead-antimony Alloys. General requirements for methods of chemical analysis
GOST 1293.0−2006
Group B59
INTERSTATE STANDARD
LEAD-ANTIMONY ALLOYS
General requirements for methods of chemical analysis
Lead-antimony alloys. General requirements for methods of chemical analysis
ISS 77.120.60
Date of introduction 2009−01−01
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 1.2−97 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. The procedure of development, adoption, application, renewal and cancellation"
Data on standard
1 DEVELOPED by the Interstate technical Committee for standardization MTK 504 «Zinc, lead», a Subsidiary of the state enterprise «Eastern scientific-research mining-metallurgical Institute of nonferrous metals» (DGP «VNIItsvetmet») of the Republic of Kazakhstan and Republican state enterprise «Kazakhstan Institute of standardization and certification"
2 INTRODUCED by Committee on technical regulation and Metrology of the Ministry of industry and trade of the Republic of Kazakhstan
3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (minutes No. 30 dated December 7, 2006)
The standard was accepted by voting:
| Short name of the country by 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 | Intergeneratsiya |
| Belarus |
BY | Gosstandart Of The Republic Of Belarus |
| Kazakhstan |
KZ | Gosstandart Of The Republic Of Kazakhstan |
| Kyrgyzstan |
KG | Kyrgyzstandard |
| Moldova |
MD | Moldova-Standard |
| Russian Federation | EN | Federal Agency on technical regulation and Metrology |
| Tajikistan |
TJ | Tajikstandart |
| Uzbekistan |
UZ | Uzstandard |
| Ukraine |
UA | Derzhspozhyvstandart Of Ukraine |
4 by Order of the Federal Agency for technical regulation and Metrology dated January 31, 2008 N 12-St inter-state standard GOST 1293.0−2006 promulgated as the national standard of the Russian Federation from January 1, 2009
5 REPLACE GOST 1293.0−83
Information about introduction in action (termination) of this standard is published in the index «National standards».
Information about the amendments to this standard is published in the index «National standards», and the text changes — in the information sign «National standards». In case of revision or cancellation of this standard the appropriate information will be published in the information index «National standards»
1 Scope
This standard applies to lead-antimony alloys according to GOST 1292 and establishes General requirements for methods of chemical analysis and safety requirements when carrying out analysis of lead-antimony alloys.
2 Normative references
This standard uses the regulatory references to the following international standards:
GOST 8.315−97 State system for ensuring the uniformity of measurements. Standard samples of composition and properties of substances and materials. The main provisions of the
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
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 12.4.021−75 System safety standards. System ventilation. General requirements
GOST 1292−2005* lead-antimony Alloys. Specifications
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* On the territory of the Russian Federation GOST 1292−81.
GOST 4212−76 Reagents. Preparation of solutions for colorimetric and nephelometric analysis
GOST 24104−2001 laboratory Scales. General technical requirements
GOST 25086−87 non-ferrous metals and their alloys. General requirements for methods of analysis
GOST ISO 5725−3-2003 Accuracy (trueness and precision) of methods and measurement results. Part 3. Intermediate indicators the precision of a standard measurement method
GOST ISO 5725−6-2003 Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice
Note — When using this standard appropriate to test the effect of reference standards in the territory of a state index «National standards» drawn up as of January 1 of the current year and related information signs, 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.
3 General requirements
3.1 General requirements for methods of analysis GOST 25086 (1−14; 24) with additions.
3.2 Sampling and sample preparation of lead-antimony alloys is carried out according to GOST 1292.
3.3 weighing laboratory scales are used according to GOST 24104.
Sample lead-antimony alloys, metals, and reagents for the preparation of solutions of known concentration of the designated components, indicators, weighing up to 5.0 g weighed in the balance with a maximum error of 0.0002 g.
Sample lead-antimony alloys more than 5.0 g, and reagents for the preparation of auxiliary solutions are allowed to weigh in the balance with an error of not more than 0.02 g.
The required weighing accuracy given in the standard methods of analysis by specifying the category in the numeric value of the mass of sample.
3.4 For calcination used laboratory muffle furnace providing heating up to a temperature of 1000 °C. For drying use drying laboratory 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 70 °C. the Term «cool» means that the solution should have a temperature of from 15 °C to 25 °C.
3.6 For measuring time intervals less than 5 min used hourglasses and stopwatches, 5 min, timers and clocks of any type.
3.7 Mass fraction of the components and impurities determined in parallel in two or three batches (number of parallel measurements indicated in the standard methods of analysis). Simultaneously with the analysis under the same conditions performed blank contamination reagents for the amendment in the result analysis. Number of dummy experiments must match the number of parallel test portions taken for analysis.
3.8 For the results of the analysis taking the arithmetic mean value of two or three parallel measurements, obtained in conditions of repeatability (the results are obtained by the same method on identical samples in the same laboratory by the same operator using the same equipment within a short period of time), if the condition of admissibility by the formula
where 
— the values of the results of two parallel determinations;
— the value of the limit of repeatability, standardized methods of analysis.
If the discrepancy between the results of parallel measurements exceeds the value , normalized in the method of analysis studying the causes of the deviations from the technical point of view. If you need to obtain some reasonable values and in case of exceeding the limit of repeatability, act in accordance with GOST ISO 5725−6 (5.2)*.
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* On the territory of the Russian Federation GOST R ISO 5725−6-2002.
3.9 the results of the analysis obtained in conditions of repeatability (the results are obtained by the same method on identical samples (the test objects) in different laboratories by different operators using different equipment), are considered compatible if the condition
where and
— the results of the analysis;
— the value of the limit of a reproducible, standardized method of analysis.
If the difference of the analysis results exceeds the limit value reproducibility study of the causes of the deviations and act in accordance with GOST ISO 5725−6 (5.3.2, 5.3.4)*.
________________
* On the territory of the Russian Federation GOST R ISO 5725−6-2002.
3.10 the results of the analysis represent a numeric value, which must end with a digit of the same category as the numerical value of the reproducibility standards set in the standard methods of analysis.
3.11 Recommended procedure for monitoring the accuracy and stability of results in the implementation of analysis methods in the laboratory are given in Appendix A.
3.12 storage Conditions and use of the solutions determined by the components with known concentration according to GOST 4212 if the standard methods of analysis not otherwise required.
3.13 When using photometric methods of analysis the thickness of the light 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.
3.14 in the use of atomic-absorption methods of analysis set forth such conditions of measurements (for example, the flame height of the burner, gas composition of the flame, slit width), which achieved an optimal sensitivity parameters of accuracy for the corresponding component and the device.
Subject to the achievement of the metrological characteristics specified in the standard methods of analysis allowed:
— to use for the calibration solutions with the introduction of several definable components;
— change the range of content of the designated components in the solutions for grading, subject to its linearity;
— to use when measuring other resonance spectral line;
— consistently determine multiple components in one test portion of the sample after decomposition and appropriate dilution of the sample solution so that the mass of the detectable component, it was within its mass in solutions for calibration.
3.15 When using photometric and atomic absorption methods permitted to use an automated build system, calibration charts, measurements in automated mode with the results of the analysis result to the printer of the automated spectrophotometer, provided that the metrological characteristics regulated by the standard methods of analysis.
4 safety Requirements and environmental protection
4.1 Chemical analysis of lead-antimony alloys is carried out in accordance with the regulatory documents on safe conducting works in the laboratories of the analytical control, approved in the established procedure in the enterprise.
4.2 the chemical analysis of lead-antimony alloys are used reagents and materials which have a deleterious effect on the human body: ammonia, acids, alkalis, metallic mercury, inorganic and organic reagents (including organic solvents). When working with the reagents and materials necessary to fulfill the security requirements set out in the regulations for their manufacture and use.
4.3 General hygiene requirements for working zone air should correspond to GOST
Allowed to set maximum permissible concentrations of harmful substances in the air of working zone in accordance with the hygiene regulations in force on the territory of countries-members of CIS.
4.4 Monitoring of content of harmful substances in the air of working zone shall be in accordance with the requirements of GOST 12.1.005, GOST 12.1.007 and techniques developed in accordance with GOST
4.5 the premises of the laboratory must have a General ventilation according to GOST
4.6 All electrical installations and electrical equipment used in the analysis of lead-antimony alloys shall meet the requirements of GOST
4.7 Conditions of electrical safety at workplaces must comply with GOST 12.1.019, rules of technical operation of electrical installations and safety rules at operation of electrical consumers.
4.8 All equipment and installations should be equipped with devices for grounding in accordance with the requirements of GOST
4.9 the premises of the laboratory must comply with the fire safety requirements according to GOST 12.1.004 and have a extinguishing media in accordance with GOST
4.10 When working with flammable and explosive gases should comply with GOST 12.1.010, GOST 12.1.004 and safety rules in the gas sector. When you use gases in cylinders should follow the rules of safe operation of vessels working under pressure.
4.11 To prevent contamination of wastewater and air by toxic substances recycling or disposal from production tests shall be conducted in accordance with the regulations agreed with the sanitary-epidemiological service.
4.12 To work in chemical laboratories are open to persons under the age of 18.
Coming to work and working should take place:
— preliminary and periodic medical examinations;
— advanced training in working with hazardous substances and the rules for the treatment of the protective means;
— safety with appropriate design according to GOST
4.13 Working in the laboratory should be provided with premises according to [1] the group IIIA of production processes.
4.14 Working in the laboratory should be provided with means of individual protection according to the rules of issuance of special clothing, special footwear and other means of protection, approved in the prescribed manner.
Annex a (recommended). Control accuracy and stability of analysis results
Appendix A
(recommended)
A. 1 Operational control of accuracy of analysis results
Control the accuracy of the results of the analysis of lead-antimony alloy includes control of the accuracy, reproducibility, intermediate precision and repeatability.
The frequency of inspection is installed in each laboratory, depending on the number of running definitions of each component and the status of analytical work (change of reagents, solutions, equipment, long break from work, etc.).
When unsatisfactory results of the inspection control procedure the accuracy of the analysis is repeated. When you re obtaining negative results to investigate the cause of unsatisfactory results of control and eliminate them.
A. 1.1 Operational control of reproduction
Samples for control samples are analyzed.
The ratio of control — limit of repeatability .
For control of reproduction compare differences of results of parallel measurements obtained by analysis of the sample.
The control result is considered satisfactory if the condition
where 
— the values of the maximum and minimum results of parallel measurements, respectively;
— the value of the limit of repeatability, normalized in the method of analysis.
A. 1.2 Operational control of intermediate indicators for precision
Samples for control samples are analyzed.
The standard control value calculated by the formula
where — an indicator of the precision (standard deviation of results of measurements) set by the laboratory for specific regulated conditions (in terms of variability of one or more factors: time, calibration, operator and equipment) according to GOST ISO 5725.3*.
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* On the territory of the Russian Federation GOST R ISO 5725−3-2002.
To monitor intermediate indicators of precision of comparing two results of the analysis of the same sample obtained in one laboratory by the same method under different conditions.
The control result is considered satisfactory if the condition
where and
— the results of the analysis of samples;
— the ratio of control computed according to the formula (A. 2).
A. 1.3 Operational control reproducibility
Samples for control samples are analyzed.
The ratio of control — the limit of a reproducible , standardized method of analysis.
To control the reproducibility of the compare two results of the analysis of the same samples obtained by the same method in different laboratories by different operators using different equipment.
Control of reproducibility is carried out at occurrence of disputable situations:
— between the two laboratories;
— when checking the compatibility of the result obtained in the comparative tests (for accreditation of laboratories and inspection control).
The control result is considered satisfactory if the condition
where and
— the test results obtained in conditions of repeatability;
— the value of the limit of a reproducible, standardized method of analysis.
If the limit of repeatability is exceeded, you must determine the cause of differences from a technical point of view (the difference of the test sample, systematic error, etc.).
A. 1.4 Operational control of the correctness
The control of correctness carried out using standard samples of composition of lead-antimony alloys or alternative (independent) method.
The standard control is a critical value of (
or
).
A. 1.4.1 Operational control of the correctness of the standard samples
Models for control are standard samples developed in accordance with GOST 8.315.
Simultaneously with the analysis of samples in accordance with standard methods of analysis carry out analysis of standard sample of lead-antimony alloys. The contents of the designated component in the standard sample and the sample must not vary by more than two times.
The result of the analysis of a standard sample are compared to the certified value of the standard characteristics of the sample.
The control result is considered satisfactory if the condition
where the result of the designated component in the standard sample, obtained from the results
of single determinations;
— the value of the certified characteristics of a standard sample;
the critical value calculated according to the formula
where is the standard deviation of reproducibility;
— standard deviation of repeatability;
— the number of results unit definition certificated characteristics of the standard sample;
— evaluation of the standard deviation of the values of certified characteristics of a standard sample.
A. 1.4.2 Operational control of the correctness of alternative (independent) method
Samples for control samples are analyzed.
Compare the results of the analysis of the same samples, obtained by two fundamentally different methods set out in standard methods of analysis, or standardized and any other certified method with error not exceeding the error of the standardized method.
The control result is considered satisfactory if the condition
where and
— the results of the analysis obtained on the controlled and control methods, respectively;
the critical value calculated according to the formula
where is the estimate of the total standard deviation of the controlled and control methods
where and
— evaluation of the standard deviations of the controlled and control methods accordingly:
where and
— the standard deviation of reproducibility of the controlled and control methods, respectively;
and
— standard deviation of repeatability of the controlled and control methods, respectively;
and
— the results of a single controlled definitions and control methods respectively.
A. 2 Control stability analysis results in the laboratory
Stability control indicators precision and accuracy of the results of the analysis in the laboratory is carried out according to GOST ISO 5725−6 (section 6)*.
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* On the territory of the Russian Federation GOST R ISO 5725−6.
