GOST 22864-83
GOST 22864−83 precious metals and their alloys. General requirements for methods of analysis (Change No. 1)
GOST 22864−83
Group B59
STATE STANDARD OF THE USSR
PRECIOUS METALS AND THEIR ALLOYS
General requirements for methods of analysis
Noble metals and alloys. General requirements for methods of analysis
OKP 175000
AXTU 1709*
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* Introduced advanced Edit. N 1.
Date of introduction 1984−07−01
The decision of the State Committee USSR on standards on March 25, 1983 N 1370 the validity period is set with
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* Expiration removed by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS No. 5/6, 1993). — Note the manufacturer’s database.
REPLACE GOST 22864−77
REPRINTING. January 1986
The Change N 1, approved and put into effect by the Decree of Gosstandart of the USSR from
Change No. 1 made by the manufacturer of the database in the text IUS N 1, 1989
This standard establishes General requirements for methods of analysis of noble metals and their alloys and safety requirements.
1. GENERAL REQUIREMENTS
1.1. The sampling is done according to normative-technical documentation on production of precious metals and alloys.
1.2 Weighing of batches is carried out with an accuracy of not more than 0.0002 g for chemical and atomic absorption methods of analysis;
0.005 g for spectral analysis;
0,00007 g for fire assay analysis method.
1.3. For analysis and preparation of solutions used reagents qualifications not lower than h. d. a., distilled water GOST 6709−72.
1.4. The reagents used in the tests of alloys containing silver as well as in the environment must be free of chlorine ions.
1.5. In the expression «diluted 1:1, 1:2», etc. the first digits indicate the volume of the acid, or any solution, the second volume of the water.
1.6. The term «hot» water (solution) means that the water (solution) has a temperature of over 70 °C.
1.7. The mass concentration of the prepared standard solution establish not less than three aliquots of this solution and expect no less than to the third significant digit.
1.8. Laboratory measuring utensils should not be below 2nd class of accuracy and correspond to GOST 1770−74 and GOST 20292−74*, GOST 25336−82, GOST 9147−80.
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* On the territory of the Russian Federation the document is not valid. There are 29169−91 GOST, GOST 29227−91−29229−91 GOST, GOST 29251−91-GOST 29253−91. — Note the manufacturer’s database.
1.9. When analysing pure metals mass fraction of the main component is calculated by the difference between the 100% and the amount of the defined impurities.
In the analysis of alloys based on noble metals mass fraction of one component is calculated by the difference between the 100% and the amount of the designated components and impurities.
1.10. Mass fraction of components in the alloys is determined not less than in two parallel batches.
The number of parallel batches in the determination of impurities indicated in the specific standard on methods of analysis.
1.11. For the results analysis be the arithmetic mean of parallel definitions.
The discrepancy between the highest and lowest results of parallel measurements with the sample analysis or the specific expertise shall not exceed the allowable differences , the values of which are given in the methods of analysis.
1.7−1.11. (Changed edition, Rev. N 1).
1.12. If discrepancies between the highest and lowest results of parallel measurements exceeds the allowable value, the analysis is repeated.
1.12. Discrepancies in the results of the analysis of the same samples obtained in two laboratories and one reference laboratory, but under different conditions, should not exceed the permissible differences given in the standard methods of analysis.
(Added, Rev. N 1).
1.13. In parallel with the analysis under the same conditions conduct control experience for the amendment of the results of the analysis. The number of parallel definitions in a control experiment it should correspond to the number of parallel measurements indicated in the particular standard on method of analysis.
1.14. Control of accuracy of analysis results is carried out according to state standard samples (GSO), the industry standard sample (CCA) or standard samples of the enterprise (SOP) reproduction of the contents defined in the component WITH the methods established in the standards.
1.15 Mass fraction of the designated component in a WITH find from among parallel definitions set a specific standard for method of analysis. The arithmetic mean value of results of parallel measurements taken for reproduced mass fraction of the designated component.
The difference between the highest and lowest results of parallel measurements in the analysis must not exceed the permissible differences given in the particular standard on method of analysis.
The results of the analysis are correct if played mass fraction of this component in different from the appraisee’s performance in the certificate WITH no more than the value 
the accuracy evaluation, shown in the certificate;
— the permissible discrepancy between the results of the analysis. If the above ratio is not fulfilled, the tests according to this method cease to ascertain and eliminate the causes of the observed deviation.
Final result for the take a result that would satisfy PP.1.12, 1.12 and 1.15.
1.14, 1.15 (Changed edition, Rev. N 1).
1.15 a. Control of accuracy of analysis results by a method of additives, is carried out by finding the mass fraction of the analyte in the test material after adding an appropriate sample of pure metal or aliquote part of a standard solution detectable component to the sample prior to analysis.
The mass of the additive (the volume of a standard solution) is chosen so that the analytical signal of the designated component would be increased in 2−3 times in comparison with the analytical signal in the absence of additives.
Determination of the mass fraction of the component in the sample with the additive is carried out from the same number of parallel measurements, and analyzing the samples. The arithmetic mean value of results of parallel measurements taken for the mass fraction of this component in the sample with the additive. The found value of additives is determined as the difference between the found mass proportions of this component in the sample with the additive and the sample without additive.
The discrepancy between the highest and lowest results of parallel measurements of the component in the sample with the additive should not exceed the value , normalized in the method of analysis.
The sample analysis results are considered accurate if the found value differs from the additive input value by no more than 
and
— the permissible discrepancy of the two results of the analysis for the sample and the sample with the additive, respectively.
For the final result of the analysis of samples take result of satisfying the PP.1.12, 1.12 a and 1.15 a.
1.15 b. Control the accuracy of the results of the analysis of samples for synthetic compounds is carried out by reproducing are introduced into the mixture, the mass fraction of the designated component according to the method of analysis.
Requirements for preparing synthetic mixtures and normative-technical documentation regulating the method of their preparation and the appraisal of the accuracy of establishing the values of the mass fractions of components mixture — according to GOST 8.505−84*.
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* On the territory of the Russian Federation the document is not valid. Valid GOST R 8.563−2009, here and hereafter. — Note the manufacturer’s database.
Determination of the mass fraction of a component in synthetic mixture carried out simultaneously with the analysis of samples from the same number of parallel definitions prescribed by the method of analysis.
The discrepancy between the highest and lowest results of parallel measurements of this component in the analysis of the synthetic mixture should not exceed the value , normalized in the method of analysis.
The sample analysis results are considered accurate if played mass fraction of this component in the synthetic mix is different from the one entered in the mixture mass fraction of not more than the value of 0.71, which is the method of analysis.
For the final result of analysis accept the result that satisfies PP.1.12, 1.12 a and 1.15 b.
1.15 Monitoring the accuracy of the results of the analysis of samples carried out by their comparison with the results of the analysis of the same samples obtained with a different methodology, are included in the standard for the method of analysis or certified according to GOST 8.505−84 and with the error not exceeding the error-controlled method.
The tests are considered accurate when the ratio of the absolute value of the difference of analysis results from both methods with a probability of 0.95 does not exceed
and
— the permissible discrepancy of the two results of the analysis, the numerical value of which is regulated in a controlled and specific control methods of analysis.
For the final result of analysis accept the result that satisfies PP.1.12, 1.12 a and 1.15 B.
1.15 a-1.15 V. (Introduced later, Rev. N 1).
1.16. For analysis it is possible to use equipment of the same type to ensure the required accuracy of the analysis.
(Changed edition, Rev. N 1).
2. SAFETY REQUIREMENTS
2.1. Concentrated acids (nitric, sulfuric, hydrochloric) must be kept in thick-walled glass container with a capacity not exceeding 2 DMin cabinets with exhaust ventilation in accordance with GOST 12.4.021−75.
2.2. Bottles of acids, alkalis and ammonia must carry serviceable in baskets or slatted crates or transported on special trolleys.
2.3. When using source materials that have hazardous properties should comply with the safety requirements regulated by normative-technical documentation for the respective reagents.
2.4. Laboratory areas in which analyses are performed, shall be equipped with a system of supply and exhaust ventilation in accordance with GOST 12.4.021−75.
2.5. Jobs must have lighting in accordance with sanitary norms and rules approved by the Gosstroy of the USSR.
2.6. Electrical appliances must conform to the rules of electrical devices, their operation must be conducted in accordance with the rules of technical operation of electrical installations and safety rules at operation of electrical installations* approved by Gosenergonadzor.
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* On the territory of the Russian Federation the document is not valid. There are «Interbranch Rules on labor protection (safety rules) for electrical installations» (SWEAT P M-016−2001, RD 153−34.0−03.150−00). — Note the manufacturer’s database.
2.7. Devices for carrying out spectral analysis shall be equipped with locks in an arc generator, local exhaust ventilation from the arc source of spectrum excitation, a glass screen on a tripod generator for protection from ultraviolet radiation, a protective earthing connection on the alternator and the tripod.
2.8. The analysis by atomic absorption method using a gas mixture, all works shall be carried out in accordance with the rules of safety in the gas sector, approved by Gosgortekhnadzor of the USSR.
2.9. The maximum permissible concentration of harmful substances in the air of working zone and hazard class of these substances — according to GOST 12.1.005−76.
2.10. Selected acids and bases should be collected separately in special containers; after neutralizing, drain into the sewer or in accordance with local conditions in the designated place.
Solutions containing noble metals should be collected in special containers for further disposal.
2.11. To work in analytical laboratories is open to persons under 18 years of age, passed the preliminary medical examination and be approved for health reasons to work with hazardous substances.
2.12. Working in the lab undergo a periodic medical examination in accordance with the instructions of the Ministry of health of the USSR.
2.13. Every employee should be trained and specific training in occupational safety in accordance with GOST 12.0.004−79*.
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* On the territory of the Russian Federation the document is not valid. Valid GOST 12.0.004−90. — Note the manufacturer’s database.
2.14. Working in the chemical and special laboratories should be provided with PPE according to current standards of issue of clothing, footwear and protective equipment.
2.15. The analysis needs to be taken that prevent the release of acids and alkalis on the skin and to apply individual means of protection according to GOST 12.4.011−87*, and also observe measures of personal hygiene. Protective dermatological means — according to GOST 12.4.068−79.
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* On the territory of the Russian Federation the document is not valid. Valid GOST 12.4.011−89. — Note the manufacturer’s database.
(Changed edition, Rev. N 1).
2.16. Laboratory spaces must be equipped with primary fire extinguishing means in accordance with GOST 12.4.009−83. Fire safety laboratory spaces shall be provided in accordance with the requirements of GOST 12.1.004−85*.
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* On the territory of the Russian Federation the document is not valid. Valid GOST 12.1.004−91. — Note the manufacturer’s database.
