GOST R 52371-2005
GOST R 52371−2005 Babbit tin and lead. Method of atomic emission spectrometry with inductively coupled plasma
GOST R 52371−2005
Group B59
NATIONAL STANDARD OF THE RUSSIAN FEDERATION
BABBIT TIN AND LEAD
Method of atomic emission spectrometry with inductively coupled plasma
Tin and lead babbits.
Method of inductively coupled plasma atomic-emission spectrometry
OKS 77.120.60
Date of introduction 2006−03−01
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. The main provisions"
Data on standard
1 DEVELOPED AND SUBMITTED by the Technical Committee for standardization TC 369 «Tin» (open joint-stock company «Central scientific-research Institute for tin «Tsniiolovo», open joint stock company «Novosibirsk tin factory NOK)
2 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology from September, 8th, 2005 N 224-St
3 INTRODUCED FOR THE FIRST TIME
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 (replacement) or cancellation of this standard a notification will be published in a monthly information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the national body of the Russian Federation on standardization in the Internet
1 Scope
This standard establishes the method of atomic-emission spectral analysis with the excitation spectrum of inductively coupled plasma for measurement of main components and impurities in tin and lead babbits.
The method is based on the excitation spectrum of inductively coupled plasma and measuring the intensity of radiation analytical spectral lines of elements determined by the photoelectric method. The sample is dissolved in a mixture of hydrochloric and nitric acids. The relationship of spectral line intensities with the concentration of the determined elements in the solution set with the help of calibration curve.
The method provides for the determination of mass fraction of elements in tin and lead babbits in the range, %:
| tin | 0.1 | to 90,0; | ||
| lead | «0,1 | «90,0; | ||
| antimony | «A 5.0 | «20,0; | ||
| copper | «0,1 | «10,0; | ||
| cadmium | «0,05 | «2,00; | ||
| arsenic | «0,03 | «0,90; | ||
| Nickel | «0,05 | «0,70; | ||
| zinc | «0,001 | «0,500; | ||
| iron | «0,01 | «0,20; | ||
| bismuth | «0,03 | «0,20; | ||
| aluminium | «0,003 | «0,020. |
2 Normative references
This standard uses the regulatory references to the following 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 12.1.004−91 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 12.1.016−79 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
GOST 12.3.019−80 standards System of labor safety. Test and measurement electrical. General safety requirements
12.4.009 GOST-83 System of standards of occupational safety. Fire fighting equipment for protection of objects. Principal. The accommodation and service
GOST 12.4.021−75 System safety standards. System ventilation. General requirements
GOST 849−97 Nickel primary. Specifications
GOST 859−2001 Copper. Brand
GOST 860−75 Tin. Specifications
GOST 1089−82 Antimony. Specifications
GOST 1320−74 (ISO 4383−91) Babbit tin and lead. Specifications
GOST 1467−93 Cadmium. Specifications
GOST 1770−74 laboratory Glassware measuring glass. Cylinders, beakers, flasks, test tubes. General specifications
GOST 3118−77 hydrochloric Acid. Specifications
GOST 3640−94 Zinc. Specifications
GOST 3778−98 Lead. Specifications
GOST 4204−77 sulfuric Acid. Specifications
GOST 4212−76 Reagents. Preparation of solutions for colorimetric and nephelometric analysis
GOST 4461−77 nitric Acid. Specifications
GOST 6709−72 distilled Water. Specifications
GOST 9849−86 iron Powder. Specifications
GOST 10157−79 Argon gaseous and liquid. Specifications
GOST 10484−78 Acid fluoride-hydrogen. Specifications
GOST 10928−90 Bismuth. Specifications
GOST 11069−2001 primary Aluminium. Brand
GOST 14919−83 electric Stoves, electric ovens and cabinets appliances. General specifications
GOST 19807−91 Titanium and titanium wrought alloys. Brand
GOST 19908−90 Crucibles, cups, glasses, flasks, funnels, test tubes and caps made of transparent quartz glass. General specifications
GOST 21877.0−76 Babbit tin and lead. General requirements for methods of 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 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions
GOST 29227−91 (ISO 835−1-81) oils. Pipettes are graduated. Part 1. General requirements
GOST 30331.3−95 (IEC 364−4-41−92)/GOST R 50571.3−94 (IEC 364−4-41−92) electrical Installations of buildings. Part 4. Requirements for security. Protection against electric shock
GOST R 8.563−96 State system for ensuring the uniformity of measurements. Methods of measurement
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) of methods and measurement results. Part 2. The basic method for the determination of repeatability and reproducibility of a standard measurement method
GOST R ISO 5725−4-2002 Accuracy (trueness and precision) of methods and measurement results. Part 4. The main methods of determining the correctness of 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 50779.10−2000 (ISO 3534.1−93) Statistical methods. Probability and fundamentals of statistics. Terms and definitions
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 national body of the Russian Federation on standardization in 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 document is replaced (modified), then the use of this standard should be guided by the replaced (modified) document. If the reference document is cancelled without replacement, then the situation in which the given link applies to the extent that does not affect this link.
3 Terms and definitions
This standard applies the following terms and definitions GOST R ISO 5725−1, GOST R 50779.10, as well as [1]:
3.1 accuracy: the Degree of closeness of measurement results to the accepted reference value. The present includes a combination of random components of error (precision) and a common systematic error (correctness).
3.2 the accepted reference value: a Value that serves as a consensus for comparison with the test result. For the purposes of this standard certified values of standard samples (co) and standard solutions coincide with the concept of «accepted reference value».
3.3 systematic error: the difference between the expectation of test results and true (in this standard — adopted by reference certified) value.
3.4 correctness: the Degree of closeness of the average value obtained on the basis of a large series of test results to the accepted reference value (in this standard — certified value of standard samples and certified mixtures).
3.5 critical difference : the Norm of the control error.
3.6 precision: the Degree of closeness to each other independent of the test results obtained in specific regulated conditions. Extreme cases of such conditions are conditions of repeatability (convergence) and reproducibility conditions.
3.7 repeatability (precision) of the results of the analysis: The degree of closeness to each other independent test results obtained under conditions of repeatability with the same method on identical objects in the same laboratory by the same operator using the same equipment within a short period of time.
3.8 the limit of repeatability (convergence) : the Value with reliable probability of 95% does not exceed the absolute value of the difference between the results of two measurements obtained in conditions of repeatability.
3.9 reproducibility of results of the analysis: the Degree of closeness to each other independent test results obtained under reproducibility by the same method, on identical objects in different laboratories with different operators using different equipment.
3.10 reproducibility limit 
3.11 source standards: Standard solutions are certified according to [2], multi-element standard solutions (MES) and solutions of the comparison (RS).
4 General requirements
4.1 General requirements for methods of analysis should correspond to GOST and GOST 25086 21877.0.
4.2 Selection and preparation of samples is carried out according to GOST 1320.
4.3 To establish the calibration based on use of at least three standard samples or standard solutions with known concentrations of elements.
5 safety Requirements
5.1 the analysis of all works in the laboratory of spectral analysis should be carried out on appliances and electrical installations, relevant [3] and requirements of GOST
5.2 When using electrical appliances and electrical installations in the process of analysis of should comply with the requirements of GOST 12.3.019, GOST 30331, [4] and [5].
5.3 All equipment and installations should be equipped with devices for grounding corresponding to GOST
5.4 Analysis of spend in buildings equipped with General dilution ventilation system according to GOST
5.5 To prevent entering the working area of harmful substances emitted in the sources of spectra excitation in quantities exceeding the maximum allowable concentration according to GOST 12.1.005, to protect from electromagnetic radiation and prevent sunburn by ultraviolet rays, each excitation source must be placed in a fixture equipped with local exhaust ventilation and protective screen according to GOST
5.6 Monitoring of content of harmful substances in the air of working zone — according to GOST 12.1.005, GOST 12.1.007, GOST
5.7 Standard solutions stored in volumetric flasks with ground stoppers. Solutions of hydrochloric, nitric and sulfuric acids and their mixtures are stored in jars with pritertymi or screw-top tubes in a fume hood at room temperature. The flasks and bottles with standard solutions and the calibration solutions (solutions) must be specified: element concentration, date of preparation, expiration date, number of solutions.
5.8 Disposal, deactivation and destruction of hazardous wastes from the tests should be carried out in accordance with [6].
5.9 To ensure fire safety should comply with the requirements of GOST
5.10 laboratory Personnel must be provided with premises and devices according to [7] the group IIIA of the production processes.
5.11 laboratory Personnel must be provided with workwear and other PPE in accordance with standard industry regulations of free issue of workwear, footwear and protective equipment to workers and employees of the enterprises of nonferrous metallurgy [8].
6 measurement Means, auxiliary devices, materials, reagents, solutions
Atomic emission spectrometer with inductively coupled plasma (ICP) as the excitation source of any type.
Argon gas of the highest grade according to GOST 10157 or [9].
Dental laboratory high precision class according to GOST 24104, or any other type.
Volumetric flasks with a capacity of 100, 200, 1000 and 2000 cmaccording to GOST 1770.
Tile electrical with closed spiral according to GOST 14919.
Pipette graduated capacity 1, 2, 5 and 10 cmaccording to GOST 29227.
Conical flasks with a capacity of 100 cmaccording to GOST 25336.
Glasses with a capacity of 250 cmaccording to GOST 25336.
Beakers with a capacity of 25 and 50 cmaccording to GOST 1770.
Crucibles made of quartz glass according to GOST 19908.
Acid fluoride-hydrogen GOST 10484.
Hydrochloric acid according to GOST 3118, H. h and diluted 1:1.
Nitric acid according to GOST 4461, H. h and diluted 1:3.
The mixture of acids (hydrochloric and nitric) in the ratio of 5:1 and 3:1.
Sulfuric acid according to GOST 4204, H. h and diluted 1:4.
Distilled water according to GOST 6709.
Aluminium is not below the A95 according to GOST 11069.
Bismuth GOST 10928 brand Vi00.
The restored iron or iron powder according to GOST 9849.
Cadmium GOST 1467 grade not lower Кд0.
Copper according to GOST 859 marks M0.
Arsenic metal [10].
Nickel GOST 849 not below grade H1.
Tin GOST 860 below grade O1.
Lead at GOST brand 3778 C1.
Antimony GOST 1089 not below grade Su000.
Titan according to GOST 19807 brand VT1−00.
Zinc GOST 3640 not below grade C0.
A standard sample of enterprises (SOP) composition of tin and lead babbits, designed according to GOST 8.315 and metrological expertise.
Source standards — certified compound (standard solutions), prepared according to [2]:
— standard solution of copper mass concentration of 1000 µg/cm: linkage of copper with a mass 0,1000 g dissolved in 10 cm
of nitric acid. The solution was transferred to a volumetric flask with a capacity of 100 cm
and adjusted to the mark with water.
standard solution of lead mass concentration of 1000 µg/cm: a portion of the lead mass 0,1000 g dissolved in 5 cm
of nitric acid (1:5). The solution was transferred to a volumetric flask with a capacity of 100 cm
and adjusted to the mark with water.
— standard solution of arsenic mass concentration of 1000 µg/cm: a portion of the arsenic mass 0,1000 g was dissolved with heating in 10 cm
of the mixture of acids (5:1). The solution was transferred to a volumetric flask with a capacity of 100 cm
and adjusted to the mark with water.
— working standard solution of arsenic mass concentration of 50.0 µg/cm: in a volumetric flask with a capacity of 200 cm
are 10 cm
standard solution of arsenic was added 40 cm
of hydrochloric acid and bring to mark with water;
— a standard solution of titanium mass concentration of 500 µg/cm: hitch Titan weight 0,5000 g was dissolved with heating in 10 cm
of nitric acid and 5 cm
of hydrofluoric acid in a quartz or glassy carbon crucibles. The solution is transferred into a measuring flask with volume capacity of 1000 cm
, adjusted to the mark with water and transferred for storage in plastic dishes.
Multielement standard solution of aluminium, bismuth, cadmium, iron, copper, Nickel, and zinc mass concentrations of 50 µg/cm(IEU-1): a glass with a capacity of 100 cm
placed at 0,1000 g of the above-listed metals, are dissolved in 25 cm
of a mixture of hydrochloric and nitric acids (3:1) under heating. The resulting solution was transferred to a volumetric flask with a capacity of 2000 cm
, 475 cm, add
the mixture of hydrochloric and nitric acids (3:1) and adjusted to the mark with water.
The shelf life of standard solutions — according to GOST 4212.
Allowed to use other equipment and reagents from the technical and metrological characteristics not worse the specified.
7 Preparation for assay
7.1 Preparation of solutions samples
For the analysis of selected weighed sample of babbit in the form of small particles or powder with a mass of 0.15−0.25 g when the mass fraction of lead in the babbit less than 50% (0.10 to 0.16 g for the mass concentration of lead in the babbit more than 50%) was placed in a beaker with a capacity of 50−100 cmand is dissolved by heating in 25 cm
of a mixture of acids (5:1). The resulting solution was transferred to volumetric flask with a capacity of 100 cm
, add 2 cm
of a standard solution of titanium and bring to mark with water.
7.2 Preparation of solutions the comparison (calibration solutions)
Reference solution with the mass concentration of titanium of 10 µg/cm(RS-0): in a volumetric flask with a capacity of 100 cm and
take 2 cm
of a standard solution of titanium, add 25 cm
of the mixture of acids (5:1), adjusted to the mark with water and mix. A solution of RS-0 is used as a background solution.
Reference solution with the mass concentration of 1250 µg/cm, antimony 500 µg/cm
, titanium 10 µg/cm
, copper 20 µg/cm
(RS-1): a sample of lead weighing 0,1250 g was dissolved with heating in 20 cm
of nitric acid (1:5), a portion of the antimony with a mass of 0.0500 g was dissolved with heating in 10 cm
of the mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm
, add 15 cm
of hydrochloric acid in 2 cm
of a standard solution of titanium and copper and adjusted to the mark with water.
Reference solution with the mass concentration of lead 400 µg/cm, tin 2000 µg/cm
, aluminum, bismuth, cadmium, iron, copper, arsenic, Nickel, titanium and zinc at 10 µg/cm
(RS-2): a portion of the lead mass 0,0400 g was dissolved with heating in 20 cm
of nitric acid (1:5), the weight of tin weight of 0.2000 g was dissolved with heating in 20 cm
of a mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm
, add 2 cm
of a standard solution of titanium, 20 cm
standard solutions of MES-1 and working standard solution of arsenic was adjusted to the mark with water.
Reference solution with mass concentration 1000 µg/cm, tin 1500 mg/cm
, aluminum, bismuth, cadmium, iron, copper, arsenic, Nickel, and zinc at 2 mg/cm
, titanium 10 µg/cm
(RS-3): a portion of the lead mass 0,1000 g was dissolved with heating in 20 cm
of nitric acid (1:5), the weight of tin weight 0,1500 g was dissolved with heating in 15 cm
of the mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm
, add 5 cm
of hydrochloric acid (1:1), 2 cm
of a standard solution of titanium, at 4 cm —
MES-1 and working standard solution of arsenic was adjusted to the mark with water.
Reference solution with mass concentration 1000 µg/cm, aluminum, bismuth, cadmium, iron, copper, arsenic, Nickel, and zinc at 5 mg/cm
, titanium 10 µg/cm
(RS-4): a sample of lead weighing 0,1500 g was dissolved with heating in 20 cm
of nitric acid (1:5). The resulting solution was transferred to a volumetric flask with a capacity of 100 cm
, 44 cm add
hydrochloric acid (1:1), 2 cm
of a standard solution of titanium, 10 cm
of solutions of the MES-1 and working standard solution of arsenic was adjusted to the mark with water.
Reference solution with the mass concentration of tin 1000 ág/cm, antimony 250 µg/cm
, titanium 10 µg/cm
, copper of 100 µg/cm
(MS-5): a suspension of tin mass 0,1000 g of antimony mass 0,0250 g is dissolved by heating in 20 cm
of a mixture of acids (5:1). The resulting solution was transferred to a volumetric flask with a capacity of 100 cm
, add 5 cm
of hydrochloric acid (1:1), 2 cm
of a standard solution of titanium, 10 cm
of standard copper solution and adjusted to the mark with water.
Reference solution with the mass concentration of copper 500 g/cm, titanium 10 µg/cm
(RS-6): dissolve in a glass of 0.0500 g of copper in 25 cm
of nitric acid. The resulting solution was transferred to a volumetric flask with a capacity of 100 cm
, add 2 cm
of a standard solution of titanium was adjusted to the mark with water and mix.
The shelf life of calibration solutions — according to GOST 4212.
8 analysis
Preparing the spectrometer to conduct tests conducted in accordance with the manual and maintenance spectrometer. The instrument operation modes set in accordance with the recommendations of the manufacturer of the device. For a specific type of device optimal parameters of the spectrometer and the flow rate of argon is set experimentally within the range for maximum sensitivity to determine the mass fractions of elements.
Recommended analytical lines given in table 1.
Table 1 — Recommended analytical lines
| The name of the element |
Wavelength of analytical lines, nm |
| Tin |
317,505 |
| Lead |
405,782 |
| Antimony |
231,147 |
| Copper |
324,754; 510,554 |
| Cadmium |
226,502 |
| Arsenic |
234,984 |
| Nickel |
341,470 |
| Zinc |
213,856 |
| Iron |
259,940 |
| Bismuth |
306,772 |
| Aluminium |
396,152 |
| Titan — line comparison |
337,280 |
The use of other analytical lines subject to receipt of the metrological characteristics meet the requirements of this standard.
The calibration of the spectrometer is carried out when installing the device, when replacing the reagents, after the repair of the equipment, after a lengthy interruptions and other changes that affect the results of the analysis. Recalibration (adjustment of calibration curve) of the spectrometer is carried out before each measurement, the prepared samples.
Successively introduced into the plasma solutions (calibration solutions) and by using the software of the spectrometer by the method of least squares receive calibration characteristics that enter into long-term memory of the computer in the form of addiction. The mass concentration of the -th element
is determined by the formula
where the regression coefficients for
-th item, determined by the method of least squares;
— the intensity of spectral lines
-th element;
— the intensity of the line comparison.
Solutions of samples analysed successively introduced into the plasma and measure the intensity of the analytical lines of the determined elements. In accordance with the program for each solution perform at least two measurements of the intensity and calculate the average value, which using the calibration characteristics find the mass concentration of element (µg/cm) in the sample solution.
9 processing of the results
Mass fraction of the element in the sample in % is calculated by the formula
where is the mass concentration of element in sample solution, µg/cm
;
— the volume of the sample solution, cm
;
— the weight of the portion of the sample,
The mass fraction of detectable elements in the sample and their arithmetic mean values read from the screen or the tape printing device.
Records of the mass of sample, sample dilution and other variables is carried out automatically at the stage of introduction of analytical program in the computer.
The result of the analysis taking the arithmetic mean of the two results of parallel measurements
and
if the difference between them does not exceed the standard limit of repeatability (convergence)
, are shown in table 2.
Table 2 — specifications of accuracy of analysis results (at a confidence probability =0,95)
Percentage
| The name of the element | Mass fraction of element | Standards precision | The margins of error ± |
The critical difference | |
The limit of repeatability (convergence) |
The limit of reproducibility |
||||
| Tin, lead, antimony, copper | 0,100 | 0,008 | 0,010 | 0,012 | 0,006 |
| Of 1.00 |
0,05 | 0,07 | 0,05 | 0,04 | |
| Of 2.00 |
0,06 | 0,08 | 0,06 | 0,05 | |
| 5,00 |
0,10 | 0,14 | 0,10 | 0,08 | |
| 10,0 |
0,2 | 0,3 | 0,2 | 0,2 | |
| 20,0 |
0,5 | 0,5 | 0,4 | 0,3 | |
| 40,0 |
0,8 | 0,8 | 0,6 | 0,4 | |
| 60,0 |
1,2 | 1,2 | 0,9 | 0,6 | |
| 90,0 |
1,5 | 1,5 | 1,1 | 0,7 | |
| Cadmium, arsenic, Nickel, zinc, iron, bismuth, aluminum | 0,0010 | 0,0002 | 0,0002 | 0,00012 | 0,0001 |
| 0,0100 |
0,0011 | 0,0015 | 0,0012 | 0,0009 | |
| 0,0200 |
0,0021 | 0,0030 | 0,0024 | 0,0020 | |
| 0,050 |
0,006 | 0,008 | 0,006 | 0,005 | |
| 0,100 |
0,011 | 0,015 | 0,012 | 0,009 | |
| 0,200 |
0,018 | 0,025 | 0,018 | 0,015 | |
| 0,500 |
0,040 | 0,060 | 0,040 | 0,037 | |
| Of 1.00 |
0,05 | 0,07 | 0,050 | 0,04 | |
| Of 2.00 |
0,06 | 0,08 | 0,060 | 0,05 | |
Upon receipt of the results of parallel measurements with a discrepancy of more than permitted analysis of samples is repeated. The test of admissibility of repeated measurements carried out according to GOST R ISO 5725−6, paragraph 5.2.
The accuracy of the measurement result (analysis) and absolute limit of repeatability (convergence) results of the parallel measurements shall be expressed by a number containing not more than two significant digits.
10 Characteristics of errors and control the accuracy of the results of the analysis
10.1 Method provides obtaining of analysis results with an error not exceeding the values given in table 2, at a confidence level =0,95.
For intermediate values of the mass fraction of elements permitted discrepancies are calculated by using linear interpolation.
10.2 Control the accuracy of the results of the analysis carried out according to GOST 25086, GOST R 8.563, GOST R ISO 5725−1, GOST R ISO 5725−2, GOST R ISO 5725−4, GOST R ISO 5725−6 [11].
Control of accuracy of analysis results includes checking the precision and accuracy of test results.
Standards for precision — limit of repeatability (convergence) for the two results of parallel measurements and the limit of reproducibility of the two analysis results
10.3 Control of repeatability of analysis results
Control of repeatability of the results of the analysis carried out in accordance with section 9.
10.4 Control of reproducibility of analysis results
The test of admissibility analysis results, obtained in conditions of repeatability (two laboratories =2), carried out to meet the requirements of GOST R 5725−6, paragraph 5.3, with the limit of reproducibility shown in table 2.
10.5 Control of the correctness of the results of the analysis carried out using standard samples the certified mixes, by a method of additives or other methods stipulated 25086 GOST, GOST R 8.563 and [11], at least once a month, and also when replacing the reagents, solutions and equipment, after long interruptions and other changes that affect the results of the analysis.
Control of the correctness of the results of the analysis for the purposes of this standard within a single laboratory are subject to the requirements of GOST R ISO 5725−6, section 4, using as standard control error critical difference given in table 2.
When the correctness of the analysis results using standard samples and certified mixtures the control result is considered satisfactory if the condition
where is the result of the determination of the mass fraction of the element in the sample, %;
— the contents of the element in a standard sample or a certified mixture, %.
When exceeding a critical difference to find out the cause of large deviations of the results from the certified values.
Control of the correctness of the results of the analysis by the method of additions is given in Appendix A.
10.6 the Procedures and frequency stability control of the results analysis within the laboratory are subject to the requirements of GOST R ISO 5725−6 [11] using Shewhart charts or cumulative card.
Annex a (recommended). Operational control of the correctness (uncertainty) by a method of additives
Appendix A
(recommended)
Control of the correctness of the results of the analysis carried out by additives in the working sample prepared in accordance with section 7. The volume of samples taken for monitoring should correspond to twice the volume required for analysis.
Selected volume of the working sample is divided into two parts, the first of which is analyzed in accordance with section 8 of this standard, and receive the result of the determination of the mass fraction of element in sample (%). In the second part of the working sample before bringing the volume of the flask to the mark in accordance with section 7 make Supplement of the element using standard samples and certified mixtures or solutions of comparison. The additive content should be between 50% to 200% of the element content in the sample
. The sample with the addition of analyze in accordance with section 8 of this standard, receiving the result of the determination of the mass fraction of the element in the sample with the additive
(%).
The control result is considered satisfactory if the condition
where is the result of the determination of the mass fraction of the element in the sample, %;
— the result of the determination of the mass fraction of the element in the sample with additive, %;
— the content of the item in addition to the sample, based on the value of its content in the standard sample or the certified mixture, %;
the critical difference determined by the formula
where is the critical difference corresponding to the mass fraction of the element in the sample without additive
(%) shown in table 2;
— the critical difference corresponding to the mass fraction of the element in the sample with the additive
(%) shown in table 2.
When exceeding the critical difference measurement is repeated. In the case of repeated exceeding of the standard to find out the reasons of unsatisfactory results of control and eliminate them.
Bibliography
| [1] recommendation. State system for ensuring the uniformity of measurements. MI 2336−2002 | Indicators of accuracy, trueness, precision methods of quantitative chemical analysis. Methods of evaluation |
| [2] recommendation. State system for ensuring the uniformity of measurements. MI 2334−2002 |
Mix certified. General requirements for the development |
| [3] Rules of arrangement of electrical installations (approved by Glavgosenergonadzora, 1985, 6th ed.) |
|
| [4] the Rules of operation of electrical installations (approved by Glavgosenergonadzora Russia 31.03.92, 5th ed.) |
|
| ___________________ * On the territory of the Russian Federation there are «Rules of technical operation of electrical installations», approved by order of Ministry of energy of Russia from | |
| [5] safety regulations for operation of consumers (approved by Glavgosenergonadzora 21.12.84, 4th ed.) |
|
| ___________________ * On the territory of the Russian Federation act «Interbranch Rules on labor protection (safety rules) for electrical installations» (SWEAT P M-016−2001, RD 153−34.0−03.150−00). — Note the CODE. | |
| [6] Sanitary regulations and norms SanPiN 3183−84 |
The order of accumulation, transportation, neutralization and burial of toxic industrial wastes (approved by the USSR Ministry of health 29.12.84) |
| ___________________ * On the territory of the Russian Federation act SanPiN | |
| [7] Building regulations SNiP 2.09.04−87 |
Administrative and domestic buildings |
| [8] Decree of the Ministry of labor of Russia from December 30, 1997 N 69 |
On approval of Standard regulations of free issue of special clothes, special footwear and other means of individual protection to workers of through professions and positions of all sectors of the economy |
| [9] Technical specifications TU 6−21−12−94 |
Argon gas of high purity. Specifications |
| [10] Technical specifications TU 113−12−112−89 |
Arsenic, metal, semiconductor compounds, the OS.h. |
| [11] recommendation. State system for ensuring the uniformity of measurements. MI 2335−2003 | Internal quality control of results of quantitative chemical analysis |
