GOST 1429.14-2004

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  ГОСТ 1429.14-2004

GOST 1429.14−2004 Solders tin-lead. Methods of atomic-emission spectral analysis

GOST 1429.14−2004

Group B59

INTERSTATE STANDARD

SOLDERS TIN-LEAD

Methods of atomic-emission spectral analysis

Tin-lead solders. Methods of atomic-emission spectral analysis

ISS 25.160.50
AXTU 1709

Date of introduction 2005−07−01

Preface

1 DEVELOPED by the Russian Federation, the Interstate technical Committee for standardization MTK 500 «Tin"

2 INTRODUCED by Gosstandart of Russia

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 17 dated 1 April 2004, by correspondence)

The adoption voted:

4 by Order of the Federal Agency for technical regulation and Metrology dated October 25, 2004 N 41-St inter-state standard GOST 1429.14−2004 introduced directly as a national standard of the Russian Federation from July 1, 2005

5 REPLACE GOST 1429.14−77

1 Scope

This standard specifies the methods of atomic-emission spectral analysis with the excitation spectrum of the spark discharge and inductively coupled plasma for the determination of the elements in tin-lead solders.

2 Normative references

The present standard features 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 12.2.007.0−75 System safety standards. Products electrical. General safety requirements

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 61−75 acetic Acid. Specifications

GOST 83−79 Sodium carbonate. Specifications

GOST 195−77 Sodium sanitarily. Specifications

GOST 244−76 Sodium thiosulfate crystal. Specifications

GOST 849−97 Nickel primary. Specifications

GOST 859−2001 Copper. Brand

GOST 860−75 Tin. Specifications

GOST 1089−82 Antimony. Specifications

GOST 1429.0−77 Solders tin-lead. General requirements for methods of analysis

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 4160−74 Potassium bromide. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9849−86 iron Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 10297−94 indium. 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 18300−87 ethyl rectified technical. Specifications

GOST 19627−74 Hydroquinone (paradoxians). Specifications

GOST 19671−91 tungsten Wire for light sources. Specifications

GOST 19807−91 Titanium and titanium wrought alloys. Brand

GOST 21930−76 Solders tin-lead ingots. Specifications

GOST 21931−76 Solders tin-lead products. Specifications

GOST 22306−77 Metals of high and special purity. 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 25664−83 Metol (4-methylaminophenol). Specifications

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

3 General requirements

3.1 General requirements for methods of analysis should conform to the 1429.0 GOST, GOST GOST 25086и 22306.

3.2 Selection and preparation of samples of solders is carried out according to GOST and GOST 21930 21931.

3.3 To establish the calibration based on use of at least three standard samples or standard solutions with known concentrations of elements.

4 safety Requirements

4.1 in the analysis of tin-lead solders all work in the laboratory of spectral analysis should be carried out on appliances and electrical installations, appropriate [1] and requirements of GOST 12.2.007.0, GOST 30331.3.

4.2 the use and operation of electrical appliances and electrical installations in the process of analysis of solders should comply with the requirements of GOST 12.3.019, the rules of operation of electrical installations, approved by national inspection services and safety regulations for operation of consumers [2].

4.3 All equipment and installations should be equipped with devices for grounding corresponding to GOST 12.2.007.0, GOST 12.1.030, GOST 30331.3. The earth must be [1].

4.4 Analysis of tin-lead solders held in a room equipped with General ventilation system according to GOST 12.4.021.

4.5 To prevent contact with the air, oxides of carbon and nitrogen and metal aerosols in quantities exceeding the maximum allowable concentration according to GOST 12.1.005, to protect from electromagnetic radiation and burns to ultraviolet rays each excitation source must be placed in a fixture equipped with local exhaust ventilation and protective screen according to GOST 12.1.019.

4.6 Machine used for grinding carbon electrodes must have a built-in pulariani exhaust ventilation to prevent the ingress of coal dust in the air of working zone in quantities exceeding the maximum allowable.

4.7 Monitoring of content of harmful substances in the air of working zone — according to GOST 12.1.005, GOST 12.1.007, GOST 12.1.016.

4.8 Disposal, deactivation and destruction of hazardous wastes from the tests should be carried out in accordance with the sanitary rules approved by national health authorities.

4.9 To ensure that fire safety should comply with the requirements of GOST 12.1.004. The laboratory room must have a means of extinguishing according to GOST 12.4.009.

4.10 laboratory Personnel must be provided with premises and devices according to [3] the group IIIA of the production processes.

4.11 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 on the regulations.

5 the Method of atomic-emission spectral analysis with the excitation spectrum of the spark discharge

5.1 Method of analysis

The method is based on the excitation spectrum of spark discharge with subsequent registration of the radiation of spectral lines photographic, or photoelectric means. The analysis uses the dependence of the intensities of spectral lines of the elements to their content in the sample.

The method provides a quantitative determination of mass fraction of elements in tin-lead solders in the range, %:

quantitative determination of aluminum and zinc with mass fractions less than 0.002% and arsenic — less than 0.005%.

Permissible error of the results of the analysis are shown in table 1.


Table 1 — the error analysis results (at a confidence probability of 0.95)

Percentage

5.2 measurement Means, auxiliary devices, materials, reagents, solutions

The quartz type spectrograph ISP-30 or similar devices.

Spectrometer types of DFS-36 (40, 41, 51), MFS-4 (6, 8) or similar devices.

Generator spark types, IG-3, IVS-23, UGE-1 (4) or similar devices.

Microphotometer MF-2, MD-100, and other types.

Spectromancer PS-18, SP-2, DSP-2 and other types.

The machine tool for sharpening of electrodes, a file or other device for processing the analyzed surface electrodes.

Standard samples of composition of tin-lead solders: 1930−80 GSO — GSO 1938−80, 1926−80 GSO — GSO 1929−80, a standard sample of enterprises (SOP) developed by GOST 8.315.

Coals spectral brands of high purity-7−3, C-2, C-3 in the form of bars with diameter 6−7 mm.

Tungsten GOST 19671.

Crucible muffle furnace or any type of thermostat.

Crucibles of graphite or porcelain according to GOST 9147.

Mold for casting electrodes of round crosssection with a diameter of 8 mm, a length of 50−75 mm or other shape depending on the type of the used device.

The technical rectified ethyl alcohol according to GOST 18300.

Photographic plates spectrographic types of PFS-01, the SFC-02 or another type, providing a normal density of the blackening of analytical lines, of the lines of comparison and background at [4].

Fotocity or other utensils for processing of photographic plates.

A drying rack of any type for drying photographic plates, providing heating of air up to 30 °C, or room air conditioner of any type.

Distilled water according to GOST 6709.

The developer consisting of two solutions:

Solution 1:

— metol (parametermanager sulphate) according to GOST 25664 — 2.3 g;

sodium sanitarily (sodium sulfite) the crystal according to GOST 195 — 26 g;

— hydroquinone (paradoxians) according to GOST 19627 — 11.5 g;

— distilled water according to GOST 6709 — up to 1000 cm.

Solution 2:

the anhydrous sodium carbonate according to GOST 83 — 42 g;

— potassium bromide according to GOST 4160 — 7 g;

— distilled water according to GOST 6709 — 1000 cm.

Before the manifestation of the solutions 1 and 2 mixed in a volume ratio of 1:1.

Fixing solution:

— sodium thiosulfate GOST 244 — 400 g;

sodium sanitarily according to GOST 195 — 25 g;

— acetic acid according to GOST 61 — 8 cm;

— distilled water according to GOST 6709 — up to 1000 cm.

Allowed the use of developer and fixer of other compositions which do not deteriorate the quality of the photographic registration of the spectrum.

5.3 Preparation for assay

5.3.1 Samples for analysis must be in the form of cast rods with a diameter of 8 mm and a length of 35−70 mm. is allowed to change the shape of the sample of the sample depending on the type of applied device.

5.3.2 Samples received for analysis in the form of chips, is melted into bars, melting under a layer of rosin in a pre-heated graphite or porcelain crucible, and pouring the resulting melt into a mold.

5.3.3 as protivoelektrodom for standard samples (CO) use WITH corresponding, sample — electrode from a corresponding sample of the solder. Allowed as counter to use a carbon rod, sharpened on a plane or a truncated cone with ground diameter of 1−2 mm, or an electrode made of tungsten GOST 19671.

5.3.4 Before analysis the ends of the rods to be analyzed and standard samples sharpen on a plane and some rubbing alcohol. On the treated surface of the analyzed samples and must not be cavities, cracks and other defects.

5.4 analysis

5.4.1 preparation of a spectrograph or spectrometer to perform the analyses carried out in accordance with the instruction manual and device maintenance.

The source excitation spectrum is spark discharge between the terminals of analyzed samples and protivoelektrodom derived from the spark generator working in the regime of high-voltage sparks. Modes of operation of the spark generator and the parameters of the spectrograph and spectrometer choose the optimum one depending on the type of device.

Recommended operating conditions analysis and technical characteristics of the instrument are given in Appendix A.

Recommended analytical lines and lines of comparison are shown in table 2.


Table 2 — Recommended analytical lines and lines comparison

In nanometers

Allowed to use other analytical lines subject to receipt of the metrological characteristics meet the requirements of this standard.

5.4.2 analysis with photographic registration of spectrum

In the cassette of the spectrograph placed photographic plates of two types.

In the long-wave part of the spectrum is placed photographic plates of type SFC-01, in the shortwave part of the spectrum — type PFS-02.

The spectrogram of the analyzed samples and standard samples should be obtained on the same plate.

For each sample and receive at least two spectrograms.

Exposed photographic exhibit, fixed and dried. Photographic plates obtained with spectrograms mounted on microphotometer and measure the density of the blackening of analytical lines of the determined elements and lines of comparison. As a comparison, using a line of tin.

For semi-quantitative determination of aluminium and zinc at mass fractions less than 0.002% and arsenic — less than 0.005% visually compare the density of the blackening of analytical lines of aluminum, zinc, and arsenic in standard samples (SOP) and samples.

5.4.3 analysis with photoelectric registration of spectrum

Instrumental parameters of the spectrometer set within the range for maximum sensitivity to determine the mass fractions of elements.

For each defined element output measuring device, take readings of registered values of intensity of radiation in the spectrum of the standard samples to construct calibration curve and samples for the assessment of the identified elements according to this schedule. In the spectrometer control computer readings registered values of the intensity of radiation is administered in long-term memory of the computer.

For each sample and record at least two measurements.

When semi-quantitative determination of aluminium, zinc or arsenic was compare the readings of the intensities of analytical lines of aluminum, zinc, and arsenic in a sample and a standard sample of enterprises (SOP), making the semi-quantitative evaluation of the presence of these elements in the sample.

5.5 processing of the results

The mass fraction of elements in the analyzed samples is determined by the calibration graphs. To construct the calibration graphs used methods of the three standards solid calibration curve, a test standard. In processing the results of the analysis on a computer calibration charts can be in the form of polynomial equations of different degrees.

The analysis of the photographic method of calibration graphs constructed in the coordinates: or where is the difference of the blackening of analytical lines of the designated element and the comparison lines (background);  — mass fraction of the element in; and the intensity of the analytical line of the element and comparison lines or background area of the element.

The analysis of the PV method, calibration graphs are built in coordinates: where is the average output of the measuring device;  — mass fraction of the element.

In the spectrometer control computer calibration of the spectrometer and receiving the results of the analysis carried out in accordance with the technical description attached to the spectrometer software. The results of parallel measurements and the arithmetic mean of the values read from the screen or printing device.

The result of the analysis taking the arithmetic mean of the two results of parallel measurements if the difference between them does not exceed the value of the standard operational control of convergence , are given in table 3.


Table 3 — Standards for operational quality control of analysis results (at a confidence probability of 0.95)

Percentage

Upon receipt of the results of parallel measurements with a discrepancy of more than permitted analysis of samples is repeated.

With repeated exceeding of the standard operational control of convergence find out the reasons of unsatisfactory results of the analysis, and eliminate them.

5.6 quality Control of analysis results

Quality control of the results of the analysis carried out according to GOST 25086 and other regulatory documents.

Control of accuracy of analysis results is carried out at least once a month, and after prolonged breaks and other changes that affect the results of the analysis.

As standard in the operational monitoring of accuracy of analysis results use the values of the norm of the control error , given in table 3.

Standards of operational control of convergence for the two results of parallel measurements and the reproducibility of the two analysis results are shown in table 3.

6 the Method of atomic-emission spectral analysis with the excitation spectrum of inductively coupled plasma

6.1 Method of analysis

The method is based on the excitation spectrum of inductively coupled plasma and subsequent radiation of spectral lines photoelectric method. The analysis uses the dependence of the intensities of spectral lines of the elements from their mass fraction in the sample. The sample is dissolved in a mixture of hydrochloric and nitric acids.

The method provides for the determination of mass fraction of elements in tin-lead solders in the range, %:

Use this method for the analysis of alloys of tin and lead. Permissible error of the results of the analysis are given in table 4.


Table 4 — the error analysis results (at a confidence probability of 0.95)

Percentage

For intermediate values of the mass fraction of the element error bound calculated using linear interpolation.

6.2 measurement Means, auxiliary devices, materials, reagents, solutions

Automated atomic emission spectrometer with inductively coupled plasma as the excitation source with all accessories.

Argon gas of the highest grade according to GOST 10157.

Laboratory analytical scale of high precision or of any type with an accuracy of weighing according to GOST 24104.

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.

Hydrochloric acid according to GOST 3118, H. h and diluted 1:1.

Nitric acid according to GOST 4461, H. h and diluted 1:3, 1:5.

The mixture of acids (hydrochloric and nitric) in the ratio of 5:1.

Sulfuric acid according to GOST 4204, H. h and diluted 1:4.

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.

Indium GOST 10297 brand Ин00.

Cadmium GOST 1467 grade not lower Кд0.

Copper according to GOST 859 marks M0.

Arsenic metal [5].

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.

Standard samples of composition of tin-lead solders: 1930−80 GSO — GSO 1938−80, 1926−80 GSO — GSO 1929−80, a standard sample of enterprises (SOP) developed by GOST 8.315.

India standard solution mass concentration of 1000 µg/cm: linkage India mass 0,1000 g dissolved in 5 cmof hydrochloric acid. The solution was transferred to a volumetric flask with a capacity of 100 cmand then filled 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 cmof the mixture of acids (5:1). The solution was transferred to a volumetric flask with a capacity of 100 cmand then filled to the 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 100 cmof sulphuric acid (1:4). The solution is transferred into a measuring flask with volume capacity of 1000 cm, a few drops of nitric acid to the bleaching solution and topped up to the mark with water.

A standard solution of copper mass concentration of 1000 µg/cm: linkage of copper with a mass 0,1000 g dissolved in 10 cmof nitric acid. The solution was transferred to a volumetric flask with a capacity of 100 cmand then filled to the mark with water.

Multi-element standard solution (MES-1) of aluminium, bismuth, cadmium, iron, copper, Nickel, and zinc mass concentrations of 50 µg/cm: linkage of cadmium and zinc by mass 0,1000 g dissolved in 10 cmof nitric acid (1:3), linkage of aluminum and iron weighing 0,1000 g was dissolved with heating in 15 cmof the mixture of acids (5:1), the sample of bismuth, copper and Nickel mass 0,1000 g was dissolved with heating in 20 cmof nitric acid. The resulting solutions are transferred to volumetric flask with a capacity of 2000 cm, add 50 cmof hydrochloric acid and topped up to the mark with water.

Multi-element standard solution (MES-2) arsenic, indium mass concentrations of 50.0 µg/cm: in a volumetric flask with a capacity of 200 cmis injected at the 10 cmstandard solutions of indium, arsenic, added 40 cmof hydrochloric acid and topped up to the mark with water.

For the preparation of solutions with known concentrations of elements allowed to use the state standard samples of solutions of metals.

6.3 Preparation for analysis

6.3.1 Preparation of solutions samples

For the analysis of selected weighed sample of the solder in the form of small particles or powder with a mass of 0,15−0,25 g (0.10 to 0.16 g for the mass concentration of lead in solders for more than 50%) was placed in a beaker with a capacity of 50−100 cmand is dissolved by heating in 25 cmof a mixture of acids (5:1). The resulting solution was transferred to volumetric flask with a capacity of 100 cm, add 2 cmof a standard solution of titanium and topped to the mark with water.

6.3.2 Preparation of solutions comparison

Reference solution (RS-0) with a mass concentration of titanium of 10 µg/cm: in a volumetric flask with a capacity of 100 cm andtake 2 cmof a standard solution of titanium, add 25 cmof the mixture of acids (5:1) and topped to the mark with water. A solution of RS-0 is used as a background solution.

Reference solution (RS-1) with the mass concentration of 1250 µg/cm, antimony 500 µg/cm, titanium 10 µg/cm, copper 20 µg/cm: linkage of lead weight 0,1250 g was dissolved with heating in 20 cmof nitric acid (1:5), a portion of the antimony with a mass of 0.0500 g was dissolved with heating in 10 cmof the mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm, add 15 cmof hydrochloric acid (1:1), 2 cmof a standard solution of titanium and copper and topped to the mark with water.

Reference solution (RS-2) with the mass lead concentration of 400 micrograms/cm, tin 2000 µg/cm, aluminum, bismuth, cadmium, iron, indium, copper, arsenic, Nickel, titanium and zinc at 10 µg/cm: linkage of lead weight 0,0400 g was dissolved with heating in 20 cmof nitric acid (1:5), the weight of tin weight of 0.2000 g was dissolved with heating in 15 cmof the mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm, add 2 cmof a standard solution of titanium, 20 cmstandard solutions of MES-1 and MES-2 and topped to the mark with water.

Reference solution (RS-3) with mass concentration 1000 µg/cm, tin 1500 mg/cm, aluminum, bismuth, cadmium, iron, indium, copper, arsenic, Nickel, and zinc at 2 mg/cm, titanium 10 µg/cm: a portion of the lead mass 0,1000 g was dissolved with heating in 20 cmof nitric acid (1:5), the weight of tin weight 0,1500 g was dissolved with heating in 15 cmof the mixture of acids (5:1). The resulting solutions are transferred to volumetric flask with a capacity of 100 cm, add 5 cmof hydrochloric acid (1:1), 2 cmof a standard solution of titanium, at 4 cm —MES-1 and MES-2 and topped to the mark with water.

Reference solution (PC-4) with mass concentration 1000 µg/cm, aluminum, bismuth, cadmium, iron, indium, copper, arsenic, Nickel, and zinc at 5 mg/cm, titanium 10 µg/cm: linkage of lead weight 0,1500 g was dissolved with heating in 20 cmof nitric acid (1:5). The resulting solution was transferred to a volumetric flask with a capacity of 100 cm, 22 cm addhydrochloric acid (1:1), 2 cmof a standard solution of titanium, 10 cmof solutions of the MES-1 and MES-2 and topped to the mark with water.

Reference solution (RS-5) with the mass concentration of tin 1000 ág/cm, antimony 250 µg/cm, titanium 10 µg/cm, copper of 100 µg/cm: linkage of tin mass 0,1000 g of antimony mass 0,0250 g is dissolved by heating in 20 cmof a mixture of acids (5:1). The resulting solution was transferred to a volumetric flask with a capacity of 100 cm, add 5 cmof hydrochloric acid (1:1), 2 cmof a standard solution of titanium, 10 cmof standard copper solution and topped up to the mark with water.

6.4 analysis

Preparing the spectrometer to perform the tests conducted in accordance with the manual and maintenance spectrometer. Instrumental parameters of the spectrometer and the flow rate of argon is set within the range for maximum sensitivity to determine the mass fractions of elements.

Recommended analytical lines given in table 5.


Table 5 — Recommended analytical lines

The use of other analytical lines subject to receipt of the metrological characteristics meet the requirements of this standard.

Successively introduced into the plasma solutions and comparison with the help of a special program 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 elements , µ g/cm, determined by the formula

, (1)

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.

6.5 processing of the results

Mass fraction of the element in the sample in % is calculated by the formula

, (2)

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 are 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 if the difference between them does not exceed the value of the standard operational control of convergence , are given in table 6.


Table 6 — Standards for operational quality control of analysis results (at a confidence probability of 0.95)

Percentage

For intermediate values of the mass fraction of element permissible differences calculated using linear interpolation.

Upon receipt of the results of parallel measurements with a discrepancy of more than permitted analysis of samples is repeated.

With repeated exceeding of the standard operational control of convergence find out the reasons of unsatisfactory results of the analysis, and eliminate them.

6.6 quality Control of analysis results

Quality control of the results of the analysis carried out according to GOST 25086 and other regulatory documents.

Control of accuracy of analysis results is carried out at least once a month, and after prolonged breaks and other changes that affect the results of the analysis.

As standard in the operational monitoring of accuracy of analysis results use the values of the norm of the control error , given in table 6.

Standards for internal operational control of convergence for the two results of parallel measurements and the reproducibility of the two analysis results are shown in table 6.

Annex a (recommended). The conditions of analysis and specifications of the devices

APPENDIX A
(recommended)

Table A. 1

ANNEX B (informative) Bibliography

APPENDIX B
(reference)

[1] Rules of arrangement of electrical installations, approved by the Glavgosenergonadzora, 1985, 6th ed.

[2] safety regulations for operation of consumers, approved by the Glavgosenergonadzora 21.12.84, 4th ed.

[3] SNiP 2.09.04−87 Administrative and domestic buildings

[4] THE spectrographic Plates 6−17−678−84

[5] THE 113−12−112−89 Arsenic, metal, semiconductor compounds, the OS.h.

ANNEX b (informative). Normative documents in force in the territory of the Russian Federation

THE APP
(reference)

1 the Rules of operation of electrical installations, approved by the Glavgosenergonadzora Russia 31.03.92, 5th ed.

2 Decree of the Ministry of labor of Russia from December 30, 1997 No. 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"

3 MI 2335−95 Internal quality control of results of quantitative chemical analysis