GOST R 53198-2008
GOST R 53198−2008 Ores and concentrates of non-ferrous metals. General requirements for methods of analysis
GOST R 53198−2008
Group A39
NATIONAL STANDARD OF THE RUSSIAN FEDERATION
ORES AND CONCENTRATES OF NON-FERROUS METALS
General requirements for methods of analysis
Ores and concentrates of non-ferrous metals. General requirements for methods of analysis
OKS 77.120.01
Date of introduction 2010−01−01
Preface
The objectives and principles of standardization in the Russian Federation established by the Federal law of 27 December 2002 N 184-FZ «On technical regulation», and rules for the application of national standards of the Russian Federation — GOST R 1.0−2004 «Standardization in the Russian Federation. General provisions"
Data on standard
1 DEVELOPED Federal state unitary enterprise «State research Institute of nonferrous metals» (FSUE «Institute «GINTSVETMET»)
2 SUBMITTED by the Technical Committee for standardization TC 373 «non-ferrous metals and alloys"
3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology dated December 25, 2008 N 676-St
4 INTRODUCED FOR THE FIRST TIME
Information about changes to the present standard reports are published annually information index «National standards», and the text changes and amendments to published monthly information signs «National standards». In case of revision (replacement) or cancellation of this standard the corresponding notification will be published in published monthly information index «National standards». Relevant information, notification and lyrics are also in the information system of General use — on the official website The Federal Agency for technical regulation and Metrology in the network Internet
1 Scope
Real the standard applies to ores and concentrates of non-ferrous metals (see Appendix a), and establishes General requirements for methods of analysis and safety requirements.
The standard applies to methods of measurement used in the analysis of ores and concentrates of non-ferrous metals.
The standard does not apply to ores and concentrates light metals.
2 Normative references
This standard uses the regulatory references to the following standards:
GOST R 8.563−96 State system for ensuring the uniformity of measurements. Methods of measurement
GOST R 12.4.026−2001 The system of occupational safety standards. Color signal, signs security and marking signal. The purpose and rules of application. General technical requirements and characteristics. Test methods
GOST
GOST R ISO 5725−1-2002 Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions
GOST R ISO 5725−2-2002 Accuracy (trueness and precision) methods and results measurements. Part 2. The basic method for the determination of repeatability and reproducibility of a standard measurement method
GOST R ISO 5725−3-2002 Accuracy (trueness and precision) methods and results measurements. Part 3. Intermediate indicators the precision of a standard measurement method
GOST R ISO 5725−4-2002 Accuracy (trueness and precision) methods and results measurements. Part 4. Basic methods for determining the correctness of a standard measurement method
GOST R ISO 5725−5-2002 Accuracy (trueness and precision) methods and results measurements. Part 5. Alternative methods for determining the precision a standard measurement method
GOST R ISO 5725−6-2002 Accuracy (correctness and precision) of methods and measurement results. Part 6. The use of precision values in practice
GOST R 50779.42−99 (ISO 8258−91) Statistical methods. Shewhart charts
GOST R 50779.45−2002 Statistical methods. Control charts cumulative sums. The main provisions of the
GOST R 52361−2005 Control of the analytical object. Terms and definitions
GOST R 52599−2006 Precious metals and their alloys. General requirements for methods of analysis
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 8.395−80 State system for ensuring the uniformity of measurements. Normal conditions measurements. General requirements
GOST 12.0.001−82 standards System of labor safety. The main provisions of the
GOST 12.0.003−74 System safety standards. Dangerous and harmful production factors. Classification
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 12.1.014−84 System of standards of occupational safety. The air of the working area. Method of measuring concentrations of harmful substances indicator tubes
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 12.1.038−82 standards System of labor safety. Electrical safety. The maximum permissible values of the touch voltage and currents
GOST 12.2.003−91 System safety standards. Equipment production. General safety requirements
GOST
GOST 12.2.032−78 System safety standards. Workplace while performing work while seated. General ergonomic requirements
GOST 12.2.033−78 System safety standards. Workplace while performing work while standing. General ergonomic requirements
GOST 12.2.049−80 standards System of labor safety. Equipment production. General ergonomic requirements
GOST 12.2.062−81 System of standards of occupational safety. Equipment production. Fencing protective
GOST 12.3.002−75 System safety standards. The process of production. General safety requirements
12.3.031 GOST-83 System of standards of occupational safety. Work with mercury. 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 12.4.010−75 System safety standards. Personal protective equipment. Mittens special. Specifications
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 12.4.028−76 System of standards of occupational safety. Respirators SB-1 «Petal». Specifications
GOST 12.4.029−76 special Aprons. Specifications
GOST 12.4.034−2001 System of standards of occupational safety. Means of individual protection of respiratory organs. Classification and marking
GOST 12.4.041−2001 (EN 133−90) System of occupational safety standards. Tools personal respiratory protection filter. General technical requirements
GOST 12.4.066−79 The system of occupational safety standards. Personal protective equipment the hands from radioactive substances. General requirements and rules of application
GOST 12.4.103−83 System of standards of occupational safety. Special protective clothing, means of individual protection of feet and hands. Classification
12.4.120 GOST-83 System of standards of occupational safety. Collective protection against ionizing radiation. General technical requirements
GOST 12.4.155−85 System safety standards. The device of protective switching-off. Classification. General technical requirements
GOST 177−88 Hydrogen peroxide. Specifications
GOST 454−76 Bromine technical. Specifications
GOST 545−76 Iodine technical. Specifications
GOST 701−89 nitric Acid is concentrated. Specifications
GOST 1770−74 (ISO 1042−83, ISO 4788−80) Glassware volumetric laboratory glass. Cylinders, beakers, flasks, test tubes. General specifications
GOST 2184−77 the sulfuric Acid. Specifications
GOST 2228−81 Paper sack. Specifications
GOST 2263−79. caustic Soda technical. Specifications
GOST 2567−89 hydrofluoric Acid technical. Specifications
GOST 3118−77 Reagents. Hydrochloric acid. Specifications
GOST 3273−75 Sodium metal technical. Specifications
GOST 3885−73 Reagents and highly purified substances. Rules of acceptance, sampling, packing, packaging, labeling, transportation and storage
GOST 4212−76 Reagents. Methods of preparation of solutions for colorimetric nephelometric analysis
GOST 4461−77 Reagents. Nitric acid. Specifications
GOST 4517−87 Reagents. Methods for the preparation of accessory reagents and solutions used in the analysis
GOST 4658−73 Mercury. Specifications
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 6563−75 technical articles made of noble metals and alloys. Specifications
GOST 6709−72 distilled Water. Specifications
GOST 8655−75 red Phosphorus technical. Specifications
GOST 8774−75 Lithium. Specifications
GOST 8986−82 yellow Phosphorus technical. Specifications
GOST 9147−80 Glassware and equipment lab porcelain. Specifications
GOST 9285−78 (ISO 992−75, ISO 995−75, ISO 2466−73) of Potassium hydroxide technical. Specifications
GOST 13170−80 Ores and concentrates of non-ferrous metals. Method for determination of moisture
GOST 14180−80 Ores and concentrates of non-ferrous metals. Methods of sampling and sample preparation for chemical analysis and determination of moisture
GOST 19908−90 Crucibles, bowls, beakers, flasks, funnels, test tubes and caps made of transparent quartz glass. General specifications
GOST 21130−75 electrical Products. Clamps earthing and grounding. The design and dimensions
GOST 24104−2001 laboratory Scales. General technical requirements
GOST 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions
GOST 27025−86 Reagents. General instructions for testing
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
Note — When using this standard appropriate to test the effect reference standards in the information system of General use — the official website of the Federal Agency for technical regulation and Metrology on the Internet or published annually by the information the sign «National standards» published as of 1 January of this year, and according to the relevant published monthly information signs, published in the current year. If the reference the standard is replaced (changed), when using this standard should be guided by the replaced (amended) standard. If the reference standard is cancelled without replacement, the position in which it was given the link to it, is applied in part that does not affect this link.
3 Terms and definitions
3.1 this standard applies the terminology according to GOST R ISO 5725−1 and GOST R 52361, as well as additional terms and definitions:
3.1.1 the analysis of the sample: a Set of successive regulated operations to establish the mass fraction of detectable component in the sample.
3.1.2 reproducibility: Precision under conditions of repeatability.
3.1.3 measurement: determined values of the analytical signal.
3.1.4 the ratio of control : The difference between the found value of the mass fraction of the element in the standard sample and the corresponding certified value of this value in the standard sample with confidence
0,95.
3.1.5 correctness: the Degree of closeness of the average value obtained on the basis of a large series of results of the analysis to the adopted reference value.
3.1.6 repeatability: Precision under conditions of repeatability.
3.1.7 limit intermediate (inter-laboratory) precision : a Value that with a confidence level
of 0.95 is not exceeded by the absolute value of the difference between the results of two analyses
and
gained in terms of the intralaboratory precision.
3.1.8 reproducibility limit, : Value that with a confidence probability
of 0.95 is not exceeded the absolute value of the difference between the results of two determinations, obtained in conditions of repeatability.
3.1.9 limit of repeatability (convergence), : Value that with a confidence probability
of 0.95 is not exceeded by the absolute value of the difference between the largest and smallest of the
results of a single analysis, obtained in conditions of repeatability.
3.1.10 precision: the Degree of closeness to each other of independent results of measurements obtained in a particular regulated conditions.
3.1.11 accepted reference value: a Value that serves as a consensus for comparison and is obtained as:
a) a theoretical or established value based on scientific principles;
b) assigned or certified value, based on experimental works of any national or international of the organization;
in) agreed or certified value, based on the joint experimental works under the guidance of scientific or engineering group;
g) the mathematical expectation of the measured characteristics, i.e., average the value of a given set of measurements — in cases when the enumeration of a), b) and C) is not available.
3.1.12 the measurement result: the average value of a given set of measurements.
3.1.13 the result of the analysis: The value of the mass fraction of the designated component in the sample obtained by calculation based on the comparative reference values (calibration dependencies), expressed in legalized units.
3.1.14 accuracy: Degree of closeness of the result of the analysis to the adopted reference value.
3.1.15 characteristic error of the results of the analysis : limit of the interval in which the measurement error is with a confidence level of
0,95*.
________________
* Corresponds to the value of the expanded uncertainty. The expanded uncertainty is the amount determined by the interval around expectation the results of measurements covering a large fraction of distribution of values which reasonably can be attributed to the measurand.
4 Symbols and abbreviations
4.1 this standard applies the following designations: — mass concentration of element in solution;
— certified value of the mass fraction of the element;
— the weight of the portion of the sample;
the volume of the solution;
— mass fraction of the element;
is the number of parallel definitions;
— the number of analysis results;
the estimate of the standard deviation of repeatability;
— limit repetition;
the estimate of the standard deviation of reproducibility;
— the limit of reproducibility;
the estimate of the standard deviation intermediate precision;
— the limit of intermediate precision;
— the characteristic error of the results of the analysis;
of 0.95;
— a critical difference for probability
of 0.95.
4.2 this standard applies the following abbreviations:
GSO is the state standard sample of the composition;
WITH a standard sample of the composition;
MCHA — methods of quantitative chemical analysis;
ND — normative documentation.
5 General provisions
MCHA used in the control of the composition of ores and concentrates of nonferrous metals must comply with the requirements of GOST R 8.563, GOST R ISO 5725.1 — GOST R ISO 5725.6 with meeting the requirements security fundamental international standards: 12.0.001 GOST, GOST 12.0.003, GOST 12.0.004, GOST 12.3.002 and the requirements of this standard in the analysis of ores and concentrates of non-ferrous metals.
6 requirements for the selection and preparation of samples
6.1 Sampling and sample preparation of ores and concentrates for chemical analysis and determination of moisture is carried out according to GOST 14180 and regulatory documents for specific products.
6.2 The sample for analysis should be ground to a powder with a particle size of not more than 0.080 mm and carefully peremeshano followed test grinding.
Note — Hanging from under the crushed sample can cause discrepancies in the results of parallel measurements and analyses.
6.3 The weighing of powders should be carried out in vessels of small weight, which include glass buxy, tared aluminum scoops and cookware made of glassy carbon.
6.4 Before analysis, powdered samples of ore and concentrate should be dried at a temperature of (105±10) °C to constant weight. Determination of moisture GOST 13170.
7 Requirements for laboratory buildings
7.1 Coverage of laboratory facilities must conform to the rules [1] and [2].
7.2 Laboratory facilities should be provided with General natural and artificial ventilation, as well as local supply-and-exhaust ventilation. Ventilation system — GOST
The air content of harmful substances must meet the requirements of GOST 12.1.005 and GOST
7.3 Work tables and fume hood, designed to work with fire and explosive substances, must have bumpers and be covered fireproof materials, and when working with acids, alkalis and other chemically active substances — materials resistant to their effects.
7.4 Laboratory space, designed to work with mercury should meet the requirements of GOST
7.5 Laboratory facilities for work with sources ionizing radiation must comply with the requirements of sanitary rules [ 3].
8 hardware Requirements, its placement and arrangement of workplaces
8.1 For weighing batches of ores and concentrates, as well as the preparation of solutions and mixtures used laboratory scales according to GOST 24104. The permissible error of single weighing not more than ±0,0002 g.
8.2 For calcination batches of ores and concentrates used muffle laboratory furnaces, providing temperatures up to 1000 °C.
To dry the ores and concentrates used drying laboratory oven providing temperatures up to 250 °C.
For dissolution and evaporation of solutions used the electric oven a closed spiral, providing temperatures up to 350 °C.
8.3 For measuring time intervals less than 5 min used an hourglass stopwatches, 5 min, timers and clocks of any type.
8.4 For the analysis of used labware that meets the requirements of GOST 25336, 29227 GOST, GOST 29228, 29229 GOST, GOST 1770, 6563 GOST, GOST and GOST 9147 19908.
8.5 Allowed to use along with the measuring instruments specified in normative document on the method of analysis, other measuring tools this type providing metrological characteristics of the results analysis.
8.6 Laboratory equipment and instruments shall comply with the requirements of ND on the specific types, GOST 12.2.003 and GOST
8.7 Laboratory equipment and instruments must be placed in the working premises in accordance with the requirements of the instructions for their operation, taking into account safety requirements for GOST 12.3.002 and rules [3].
8.8 Moving parts of machinery, laboratory facilities must be fenced in accordance with the General rules security 8.7 and requirements GOST
8.9 All electrical installations and electrical equipment used in performing analyses shall conform to the requirements of GOST
8.10 Appliances used to heat flammable fluids should be with a closed coil and wires with chemically the bar insulation.
8.11 The conditions of electrical safety at workplaces should be provided in accordance with the General requirements and nomenclature of types of protection according to GOST
8.12 Safety requirements for devices used in x-ray, x-ray, x-ray fluorescence methods of analysis must comply with the safety requirements described in the operating instructions of these devices, and requirements norms [ 4] and [5].
8.13 workplace to perform work must comply with the requirements of GOST 12.2.032, GOST 12.2.033 and rules [5]. All workplaces should be provided with safety instructions for workers.
8.14 compressed and liquefied gases shall be installed in special premises in accordance with the requirements of regulation [6].
Vessels and apparatuses, working under pressure, must be operated in accordance with the rules [7].
8.15 Items of equipment and installations shall be painted in signal colors and is equipped with safety signs according to GOST
8.16 In the workplace when performing the measurement process when working with solutions, weighing samples, conducting operations on the filter establishing the concentration of solutions must be ensured normal conditions measurements GOST 8.395 and sanitary norms [9].
9 requirements for the application of instrumental and chemical methods of analysis
9.1 Analytical instrumentation prepared to work according to the operating instructions of these devices.
9.2 Mass concentration of elements in the sample solution determined using the calibration graphs.
9.3 For the application of instrumental analysis methods requires correct the choice of analytical spectral lines of the element. This the choice is dictated by the instrumental capabilities of equipment and the composition the analyzed samples.
9.4 With the aim of selective definition element requires the choice of the spectral analytical lines free of blending lines of the matrix chemical composition of the ore or concentrate.
9.5 In the determination of elements by atomic emission spectroscopy with inductively coupled plasma requires wavelength selection and analytical the lines of the designated element, plasma power, argon flow, speed filing solution in the plasma, the height of the recorded zone of the plasma, observance the limits of the content of acids and salts in the sample solution.
9.6 the pH and salt composition of the calibration solutions and the sample solution must support identical.
9.7 In the determination of elements by atomic absorption wavelength, the composition gas flame, which determines recovery or oxidation its action, gas flow rate, burner type and other conditions chosen in order to achieve optimal settings to ensure the required in terms of accuracy and sensitivity in the determination of the item. In the method of atomic absorption range of linear dependence «signal concentration» is much narrower than in the method of atomic emission spectroscopy with inductively coupled plasma. So when you build the calibration dependence requires multiple concentrations of an element in a narrow range. Acidity and salt composition of the sample solution and solutions for calibration it is necessary to maintain identical.
9.8 In the determination of elements by atomic-emission analysis with arc and spark excitation spectrum set operating modes devices, the wavelengths of the analytical lines and lines of comparison, working the range and nature of discharge, frequency of discharge, range current control etc.
9.9 When using x-ray methods indicate the type spectrometer with all accessories and characteristics of devices for preparation of samples for analysis.
9.10 The powdery mixtures used as models of comparison, must be certified. For each mixture, acting as a sample comparisons must include the value of error mixing.
9.11 The spectrum of the sample and each standard sample receive the same conditions. The maximum error introduced by the error calibration parameters.
9.12 When using spectrophotometric methods of analysis are required the choice of the wavelength of the element and the thickness of the absorbing light layer ditch, to ensure measurements in optimal areas optical densities.
9.13 For all of the above methods is acceptable to use analytical signals at other wavelengths, provided that the required the metrological characteristics of the analysis results.
9.14 When determining the mass fraction of elements (20% — 80%) must the use of chemical, e.g., titrimetric, gravimetric methods of analysis.
9.15 the Titer of the solutions set, hoping for at least three batches of the substance (if not MKA laid a different number of batches).
The titer is expressed in grams of ingredient per 1 cmof solution (g/cm
).
For the titer of the solution take the arithmetic mean value obtained from the three titration results. The calculated values are rounded to the fourth significant digit after the decimal point.
Error establishing titer of the solution , g/cm
, calculated by the formula:
where is the standard deviation of repeatability of the results of the titration, g/cm
;
— the student coefficient at the confidence probability of
0,95;
the number of definitions.
If we neglect the error of the titer must conform to the following inequality:
where is the limit of the absolute error of the results;
the corresponding mass fraction of the element.
10 Requirements for preparation of solutions
10.1 For the preparation of aqueous solutions and when performing analyses used distilled water according to GOST 6709 or corresponding quality deionized water. Possible more stringent requirements (bidistillate, redistilled) that should be specified in the relevant normative documents, regulating MKHA.
10.2 The degree of dilution of the solution of reagent (acid, alkali, etc.) indicate in the form And In, for example, 1:2, where A — volume part diluted substances that In large part used solvent.
Mass the concentration was expressed:
— the amount determined by the ratio of the mass of a substance to the volume occupied by them;
— the amount determined by the ratio of the mass of a substance to a certain weight (100 g) solution (mass concentration, mass fraction, which can expressed in percent);
— the amount determined by the ratio of the volume of the substance to a definite volume (100 cm) solution (volume ratio, expressed in percent);
— the amount determined by the ratio of the number of moles of a substance in solution to its volume.
10.3 the Term «warm» according to GOST 27025 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 above 75 °C.
The term «cooling» means cooling to a temperature of from 15 °C to 25 °C.
11 Requirements for major solutes, certified mixtures (solutions) and calibration chart
11.1 For the preparation of basic solutions according to GOST 4517 use a metal containing at least 99.9% of the basic substance, salt and reagents. Linkage of these substances are weighed on an analytical balance. The required accuracy of weighing and measuring the volume of lead in standards on methods of determination of mass fraction of elements indicating the number of decimal places.
11.2 Preparation of certified mixtures is carried out according to recommendations [10]. Accuracy specifications preparation of certified mixtures is calculated by the formula
where — mass fraction of the basic substance (reagent) % m;
— characteristics of the error in determining the mass fraction of basic substance, % wt;
— the weight of the portion of the reagent, g;
— the characteristic of the error of the analytical balance, g;
— the nominal volume of volumetric glassware is used, cm
;
— the characteristic error of the dosing volume, cm
.
Certified blend for metrological purpose performs the functions WITH the composition of the substance according to GOST 8.315.
11.3 The main solutions and samples for calibration (certified mix) should be stored at temperature from 15 °C to 25 °C (see GOST 27025) in sealed plastic jars or flasks with ground tubes. On tanks with basic solutions must be the label on which indicate: the name of the certified value, date cooking and shelf life under 3885 GOST and GOST 4212. The shelf life of the solutions are installed in accordance with the requirements of ND regulating of MQHA, or other relevant documents.
11.4 The calibration characteristics is obtained using the standard composition samples, samples for calibration, fundamental solutions, certified mixtures in accordance with the recommendation [ 10]. The methodology should be described the procedure of preparing basic and calibration solutions.
11.5 Calibration curve building in the system of rectangular coordinates, the axis of x lay the numerical values of the mass concentration or mass element, and the axis of ordinate the value of the analytical signal or function from him.
11.6 To build a calibration curve requires at least five calibration points, each of which is based on the arithmetic mean the results of three parallel measurements. The calibration points have to be evenly distributed across the measuring range and cover desired interval definitions.
Allowed preparation of multi-element solutions containing several elements in a single solution. The solutions should be tailored to maximum stability of the ionic forms of the existence of items entered, also allowed:
— to use for the calibration solutions with the introduction of several of the identified elements;
— change the range of the determined elements in calibration solutions while respecting the linearity of the calibration function;
— use automated build system calibration charts;
— to define multiple elements from a solution of one sample of the sample given the conformity of mass concentrations of elements in solutions for calibration charts and a mass fraction of these elements.
11.7 stability Control calibration characteristics.
The calibration characteristic to recognize is stable if the following condition is true:
where — played for the calibration feature certified the mass value, the mass concentration of the component in the calibration sample;
— certified mass value, the mass concentration of the component in the calibration sample;
— standard stability control calibration characteristics.
The values of the standard stability control calibration characteristics change in the text of the document on method of analysis.
Values should not exceed 0.5
(error analysis).
Control the stability of the calibration characteristics is carried out using calibration samples with a mass determined by the component near the bottom, upper bounds and the mid-range for plotting calibration curve.
If the condition for one calibration sample, the experiment is repeated.
Repeated failure of terms of building of the new calibration feature.
Stability control calibration characteristics is carried out when changing batches of reagents and equipment.
The frequency stability control the calibration characteristics determine for each individual method of analysis depending on the frequency analysis of work samples in the laboratory.
11.8 Preparation of solutions of indicators — according to GOST 4919.1 and buffer solutions — according to GOST 4919.2.
12 requirements for the measurement and processing of analysis results
12.1 Mass fraction of components and impurities are determined simultaneously in two the batches, if the method of analysis is not incorporated the use of more the number of parallel measurements. Simultaneously with the analysis conduct control experience to determine the contamination of reagents and the amendment in the result analysis. The number of parallel control experiments indicate the method of analysis.
12.2 Mass fraction of precious, rare and trace elements determined in three batches of samples.
12.3 the Results of parallel measurements should be obtained in conditions of repeatability in accordance with GOST R ISO 5725−1, para 3.14. The absolute discrepancy between these values is compared with a limit of repeatability :
where 
of parallel measurements, obtained in conditions of repeatability and confidence probability
of 0.95%, the values of this coefficient are given in table 1.
Table 1
| 2,0 | 3,0 | 4,0 | 5,0 | |
| 2,77 | 3,31 | 3,63 | 3,86 |
If the range of the results of four 
If the discrepancy does not exceed , the results of the parallel definitions recognize acceptable and the final result of the analysis taking the arithmetic mean value.
If the difference exceeds , hold two parallel definitions. If the range of results
of parallel measurements
If the range of results of parallel measurements exceeds
Results the analysis is a numeric value, which must end with the same number of decimal places, and values: — standard deviation of repeatability;
— limit repetition;
— standard deviation of reproducibility;
— the limit of reproducibility;
— the limit of intermediate precision;
— the limit of absolute error of the results;
— standard control, a value of the difference between the found mass fraction of the analyzed element in the standard sample and the corresponding certified value standard sample at a confidence probability
0,95.
Rounding the results of the analysis carried out in accordance with the requirements of the standard [11].
13 Control stability analysis results
Control the accuracy of the analysis results includes checking the correctness, repeatability, intermediate precision and repeatability the results of the analysis in accordance with GOST R ISO 5725−6 and recommendations [12].
13.1 Operational control of reproduction
When the control of reproduction, carried out in conditions of repeatability (results parallel definitions get the same method on identical the samples in the same laboratory by the same analyst, with using the same equipment within short time period), the absolute disparity of the two results (2) parallel measurements
and
should not exceed the limit of repeatability
, i.e., with confidence probability
of 0.95 should meet the following condition
Samples for control samples are analyzed.
When the failure of this correlation analysis is repeated. When you re the discrepancy of the obtained results the ratio of the execution tests stop, find out the reasons of unsatisfactory results, and eliminate them.
13.2 control of the intermediate (inter-laboratory precision)
The norm control is the limit of intermediate precision . Examples of control serve as a test sample.
For control intermediate precision compare two analysis result the same samples obtained by the same method in different conditions (different equipment, different analysts, different reagents, different intervals) in one laboratory. The result of the control considered satisfactory if the condition is satisfied
where and
— the results of the analysis of one sample.
where is the estimate of the standard deviation intermediate precision.
13.3 Control of reproducibility
Control of reproducibility is carried out in the event of disputes between the two laboratories.
13.3.1 The analysis results obtained in laboratories participating in the procedure the eligibility check must accompany the Protocol, which contains:
— the name of the analysis technique;
— the value of the result of the analysis, indicating the method of its production (in the form the result of a single analysis or arithmetic averages the results of a single analysis or median of the results of a single analysis) and the number of results unit of analysis used to calculate the result for analysis.
13.3.2 results of the analysis and
obtained in two different laboratories is considered acceptable if the absolute difference between them
does not exceed the critical difference
13.3.3 calculation of the critical difference
Values the critical difference calculated depending on the production method the results of the analysis in each laboratory and the number of results the unit of analysis used to calculate the results of the analysis.
13.3.4 If a methodology is provided for receiving a result of the analysis on the basis of the results of a single analysis, and both test results were obtained as the arithmetic mean and
the results of a single analysis, respectively, the critical difference is calculated by the formula
_________________
* If ND to the method of analysis is not suitable for parallel definitions, 
where and
is the number of results unit of analysis used to calculate the result of the analysis in laboratories.
Note — If represented by each laboratory analysis results obtained in strict accordance with the regulations on the method of analysis (as the results the unit of analysis or the arithmetic mean the results of a single analysis), the critical difference is the limit of reproducibility and its value can be calculated by the formula
13.3.5 If a methodology is provided for receiving a result of the analysis on the basis of the results of single analysis, single analysis result was obtained as the arithmetic mean
and the latter as the median
of the results of a single analysis, the critical difference is calculated by the formula
where — the ratio of the standard deviation of the median to the standard deviation the arithmetic mean value.
13.3.6 If a methodology is provided for receiving a result of the analysis on the basis of the results of a single analysis, and both test results were obtained as the medians
and
the results of a single analysis, respectively, the critical difference is calculated by the formula
13.3.7 If you ND the methods of analysis are not provided in parallel definitions, the calculation of the values of limit and critical voproizvodit the difference 
1, which corresponds to formulas for the calculation of critical difference, given in GOST R ISO 5725−6 (paragraph 5.3.2).
13.3.8 If the condition (10) as final result analysis using the overall average of the results of the analysis obtained in two laboratories:
If the condition (10) both results are considered unacceptable.
13.4 Control of correctness with the use of samples for control
The control of correctness carried out using standard samples of the alternative method or by a method of additives.
The standard control is critical . Models for control are standard samples of ores and concentrates of non-ferrous metals.
Standard select the sample so that the mass fraction determined item it does not vary by more than two times in comparison with the sample.
The result of the analysis of the standard sample compared with the certified value of the designated element in the standard sample.
The control result is considered satisfactory subject to
where the result of the analyzed element in the sample for the control — arithmetic mean
results of parallel measurements, the difference between the highest and the smallest of which does not exceed the limit of repeatability;
certified value component in the standard sample.
The ratio control is calculated by the formula
where — evaluation of the standard deviation of the reproducibility;
— evaluation of the standard deviation of the repeatability;
— the results of unit definitions in the standard sample;
— uncertainty of certified value standard sample.
13.5 Control of correctness with the use of alternative (independent) method
Control the correctness is carried out by comparing the results of the analysis are identical samples obtained by the controlled and alternative methods of analysis. Selecting an alternative method of analysis is carried out in accordance with recommendations contained in the recommendations [ 12] and [13] and GOST R 52599.
The control result is considered satisfactory if the condition
where and
— the results of the analysis obtained on the controlled and control methods, respectively;
— standard control.
where is the estimate of the total standard deviation for all monitored and control methods.
The pooled standard deviation is calculated by the formula
where and
— estimation of the standard deviations of the controlled and control methods simultaneously.
The critical value is calculated by the formula
where — characteristic error of the certified value standard sample.
13.6 Control of the correctness of the results of the analysis using the method of additives
Monitoring is carried out by comparing the results of the control analysis with the normative
.
The results of the analysis taking the arithmetic mean value of results of parallel measurements.
The result of the control procedure, is calculated by the formula
where is the result of a test of measuring the mass fraction of the element in the working sample with the introduced additive;
— the result of a test of measuring the mass fraction of the element in the working sample.
The amount of the additive within the laboratory must meet the condition:
The ratio control is calculated by the formula
where 
If the result of the control procedure that satisfies the condition
the analysis confirmed to be satisfactory.
As assigned specifications of error set the boundaries of the absolute error of the results of the analysis .
Control the repeatability of parallel measurements, intermediate precision and the reproducibility of the results of the analysis carried out when changing reagents, the replacement of equipment and unacceptable results of the analysis, but not less than one times a month.
13.7 Control of the stability of analysis results
Control within the same lab should be done by check precision and correctness of the result in support of these indicators the required level for a long time.
The stability control indicator intermediate precision is carried out using control charts cumulative amounts in accordance with GOST R 50779.45.
Stability control indicators of correctness carried out using Shewhart charts and GEO 50779.42 according to GOST and GOST R ISO 5725−6.
The frequency inspection specified in the laboratory documents, as well as is chemicals replacement, professionals, replacement, equipment, change of other conditions of performance tests.
14 safety Requirements when working with reagents and source materials
14.1 The reagents and other raw materials used in the analyses of the samples of non-ferrous products, as well as safety requirements for working with them must comply with ND for these materials are approved in the prescribed manner.
14.2 When working with acids and salts must meet the following security requirements:
— when working with nitric acid according to GOST and GOST 4461 701 it is necessary to use individual means of protection (respirators, rubber gloves, goggles, overalls), and observe good personal hygiene. Tests should be carried out in the fume cupboard of the laboratory;
— should avoid the contact of nitric acid with turpentine, carbides, powders of metal salts of chloric and picric acids, and also with combustible materials. When hit acids on the skin and mucous membranes the eyes need first aid: rinse thoroughly with water the diseased organ, and then a solution of sodium bicarbonate mass fraction 2%, and to immediately take the victim to a medical facility. When irritation of the mucous membrane of the respiratory tract is necessary to drink warm milk, apply oxygen inhalation and to provide medical assistance;
— all types of work with hydrochloric acid according to GOST 3118 should be in cloth clothing, rubberized apron, rubber boots, acid gloves, safety glasses;
— in contact with hydrochloric acid on the skin should wash immediately with abundant running water and if splashed in the eyes rinse them with water and treat with a solution of sodium bicarbonate a mass fraction of 2%. If exposed to vapours of hydrochloric acid on the organs breathing require immediate medical attention;
— working with sulfuric acid according to GOST 2184 should be provided with special clothing and footwear, and also means personal protection. In case of burns with sulfuric acid, rinsed the affected organ with water, then with sodium bicarbonate solution mass a share of 5% or a solution of ammonium carbonate mass fraction of 10%. When storage acid isolated from metallic powders, carbides, salts nitric, chloric, picric acids and combustible materials. When the ignited substances in the presence of acid should be extinguished with sand. When extinguishing unacceptable use of water;
— hydrofluoric acid (hydrofluoric acid) according to GOST 2567 and its vapors, and smoke generated in the presence of ammonia, extremely poisonous. Acid has a destructive effect on glass and other substances, not valid for platinum. If hydrofluoric acid has been found in the area fire, when extinguishing is possible to use water. To uncover cookware with a hydrofluoric acid must be very careful not damage the container. When you open the tube the throat of the cookware should be kept in direction. Burns from hydrofluoric acid is necessary the affected area wash immediately with plenty of water until until whitened the surface of the skin gets red. Then impose a freshly prepared suspension of magnesium oxide in glycerol mass fraction 20%;
— anhydrous perchloric acid may explode upon contact with organic substances such as wood, coal, paper, air and. When working with perchloric acid should not use rubber gloves. Vessel (beaker or flask), you need to take metal forceps. For mass analyses, involving the use of perchloric acid, you should often be washed with water and the inner walls of the exhaust channels Cabinet. In contact with the skin of perchloric acid should be rinsed with plenty water. Avoid contact of perchloric acid with organic and flammable substances;
— salt perchloric acid, potassium chlorate (potassium Chornovetsky, potassium chlorate salt), sodium chlorate, is dangerous if ingested, as are strong blood poison. They are dangerous in case of fire, in contact with flammable substances can explode. When extinguishing use water. Store the reagents should be isolated from combustible substances, acids and sulphur.
14.3 safety Requirements when working with lye
All work with sodium hydroxide (see GOST 2263) and potassium hydroxide (see GOST 9285) should be carried out only in protective clothing: costumes from cotton fabric, rubber boots and gloves from alkali-resistant rubber and protective glasses. In case of contact with skin and clothing the affected area should immediately be washed with water or saline solution, then make gadgets from solutions acetic, tartaric, hydrochloric or citric acid mass fraction of 5%. In case of contact with eyes, immediately flush them with water or physiological solution and consult a doctor.
14.4 safety Requirements when working with the Halogens
Work with bromine (see GOST 454) should be under the hood in rubber gloves. Bromine is stored in a special the dark glass jars small containers with a tightly sealing plug. When poisoning pairs of bromine needed fresh air, inhalation of water vapor with small amounts of ammonia, inhalation soda solution, inhalation of oxygen.
Work with iodine (see GOST 545) should be under the hood in rubber gloves. Iodine is stored in the banks of dark glass with a glass stopper.
14.5 Acid and alkali should be poured by using a glass siphon with a pear or other injection devices.
Shed acid and alkali except hydrofluoric acid, should be poured sand, and after it is cleaning the seats against spills of acids should be treated lime or soda. Spilled hydrofluoric acid must to neutralize the sodium hydroxide in the form of powder or solution.
In case of a spill of an alkali solution to neutralize it, spraying the spill site with plenty of water.
When solid alkali spillage it should be collected in a dustpan and place spillage wash with plenty of water.
14.6 Working with alkali metals (lithium GOST 8774 and sodium GOST 3273) must be performed in a fume hood lined with a sheet steel with asbestos gasket away (not closer than 5 m) from sources of fire and water, with use for heating oil, air or sand baths. When work with alkaline metals, use tweezers.
14.7 Work with concentrated hydrogen peroxide according to GOST 177, inorganic and organic peroxides must be carried out in the protection of personnel using protective goggles or masks from organic glass, cotton bathrobes and rubber gloves.
14.8, Works with phosphorus (yellow to red 8986 GOST and GOST 8655) should be carried out in a fume hood when working ventilation. For carrying phosphorus in the reaction vessel should use a tweezers.
Working with red phosphorus should be provided with personal protective equipment in accordance with GOST
14.9 Work carried out extremely and highly hazardous and radioactive substances should be conducted in specially equipped the cabinets of «Isotope» in accordance with the safety requirements set out in the ND’s work with these substances.
14.10 Accounting, expenditure, and work with radioactive substances should be in accordance with the requirements of regulation [4] and [5].
4.11 Work with mercury according to GOST 4658 should be carried out in accordance with GOST and sanitary 12.3.031 rules [14].
15 requirements for the storage of reagents, samples analyzed products and raw materials
15.1 Storage facilities for reagents, samples analyzed products and other the source materials used in the analyses must meet requirements [ 15] and be equipped with ventilation systems according to GOST
15.2 storage of radioactive substances shall be equipped in accordance with the rules [3].
15.3 Storage space for gases in the compressed and gaseous pollutants and cooling of gas mixtures shall be equipped according to the rules [ 6].
15.4 Sample analyzed products and raw materials should be stored in a respective sealed glass container at 3885 GOST, GOST 25336 or in packages of thick paper according to GOST 2228.
15.5 storage of chlorine must comply with the rules [15].
16 fire safety Requirements when conducting analyses
16.1 Laboratory facilities and their equipment must comply with the General fire safety requirements according to GOST
16.2 All work with flammable liquids (flammable liquids) and combustible liquids (combustible liquids) must be carried out in a fume hood when working ventilation off heating devices. Heating flammable liquids and combustible liquids should be conducted on a pre-heated baths filled a heat carrier (e.g. sand). The coolant must have temperature not exceeding the flash point of flammable liquids and combustible liquids. Not allowed heated in a water bath of substances which can react with water with a possible explosion or release of gases.
17 Requirements for personnel permitted to participate in the tests
17.1 Staff training in safe working practices in the laboratory and rules handling of protective equipment and a safety briefing labor with appropriate design conducted in the prescribed manner according to GOST
17.2 Choice of collective protection of the personnel shall be subject to the requirements of GOST 12.3.002, GOST
17.3 laboratory Personnel must be provided with premises according to the norms [16] for the group of production processes, depending on the process analyses of harmful substances.
17.4 Working with sources of ionizing radiation shall be provided with means of protection according to GOST and GOST 12.4.120
17.5 Protection against high voltages in the electric circuit, a circuit which can pass through the human body, needs to provide a protective, insulating, safety devices, automatic control and alarm, automatic disconnect, grounding, earthing devices and remote control systems, lighting rods and arrestors, insulating coatings, safety signs, PPE according to 12.1.019 GOST, GOST 12.1.030, GOST 12.4.155, GOST 12.1.038, GOST
17.6 Providing laboratory personnel with means of individual protection must comply with the standard [17].
17.7 Types used in the analyses of individual means of protection must comply with GOST
Annex a (informative). The list of ores and concentrates of non-ferrous metals
Appendix A
(reference)
A. 1 List of ores and concentrates of non-ferrous metals are given in table A. 1.
Table A. 1
| Non-ferrous metal ores |
Concentrates of non-ferrous metals |
| Copper; |
Copper; |
| copper-zinc; |
copper and molybdenum; |
| copper-lead; |
molybdenum; |
| copper-Nickel; |
copper-Nickel; |
| copper and molybdenum; |
pyrrhotite; |
| copper-lead-zinc; |
lead; |
| copper-cobalt; |
zinc; |
| lead; |
bismuth; |
| lead-zinc; |
tungsten; |
| lead-barium; |
antimony; |
| lead-zinc-barite; |
tin; |
| lead-zinc-tin; |
Nickel; |
| lead-copper-cobalt-Nickel; |
barite; |
| lead-copper-cobalt; |
gold; |
| lead and molybdenum; |
platinum group metals; |
| molybdenum; |
flotation of gold; |
| molybdenum-bismuth; |
gravitational gold-bearing; |
| tungsten; |
zolotorevskii |
| tungsten-molybdenum; |
|
| cobalt; |
|
| tin; |
|
| antimony; |
|
| arsenic; |
|
| mercury; |
|
| gold; |
|
| gold placer; |
|
| Sands |
|
| Note Depending on exploration, mining and processing of other names elementoorganic ores and concentrates of non-ferrous metals. | |
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