GOST 8776-99

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  ГОСТ 8776-99

GOST 8776−99 Cobalt. Methods of chemical-atomic-emission spectral analysis

GOST 8776−99

Group B59

INTERSTATE STANDARD

COBALT

Methods of chemical-atomic-emission spectral analysis

Cobalt.
Methods of chemical-atomic-emission spectral analysis

ISS 77.040.40*

AXTU 1732
_______________
* In the index «National standards» 2006
OKS 77.040, 77.120.70. — Note the CODE.

Date of introduction 2000−07−01

Preface

1 DEVELOPED by the Russian Federation, the Interstate technical Committee for standardization MTK 502 «Cobalt"

INTRODUCED by Gosstandart of Russia

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 15−99 dated may 28, 1999)

The adoption voted:

The name of the state	The name of the national authority standardization
The Republic Of Azerbaijan	Azgosstandart
The Republic Of Belarus	Gosstandart Of Belarus
The Republic Of Kazakhstan	Gosstandart Of The Republic Of Kazakhstan
Kyrgyz Republic	Kyrgyzstandart
The Republic Of Moldova	Moldovastandart
Russian Federation	Gosstandart Of Russia
The Republic Of Tajikistan	Tajikistandart
Turkmenistan	The main state inspection of Turkmenistan
The Republic Of Uzbekistan	Standards
Ukraine	Gosstandart Of Ukraine

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated 19 October 1999 No. 352-St interstate standard GOST 8776−99 introduced directly as state standard of the Russian Federation from July 1, 2000.

4 INSTEAD OF THE GOST 8776−79

1 Scope

This standard specifies the chemical-atomic-emission spectral analysis techniques with DC arc and inductively coupled plasma as a source of excitation spectrum for determination of mass fractions of elements in cobalt GOST 123 and cobalt powder to GOST 9721.

2 Normative references

The present standard features references to the following standards:

GOST 8.315−97 State system for ensuring the uniformity of measurements. The standard samples. The main provisions, the order of development, certification, approval, registration and application

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 12.1.016−79 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 12.3.002−75 System safety standards. The process of production. 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 123−98 Cobalt. Specifications

GOST 195−77 Sodium sanitarily. Specifications

GOST 244−76 Sodium thiosulfate crystal. Specifications

GOST 804−93 primary Magnesium ingots. Specifications

The Copper GOST 859−78. Stamps*
_______________
* On the territory of the Russian Federation GOST 859−2001, hereinafter. — Note the CODE.

GOST 860−75 Tin. Specifications

GOST 1089−82 Antimony. Specifications

GOST 1467−93 Cadmium. Specifications

GOST 2789−73 surface Roughness. Parameters and characteristics

GOST 3118−77 hydrochloric Acid. Specifications

GOST 3640−94 Zinc. Specifications

GOST 3778−77 Lead. Specifications*
_______________
* Valid GOST 3778−98. — Note the CODE.

GOST 4160−74 Potassium bromide. Specifications

GOST 4198−75 Potassium phosphate odnosemjannyj. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 5494−95 aluminum Dust. Specifications

GOST 5817−77 tartaric Acid. Specifications

GOST 6008−90 metallic Manganese and nitrated manganese. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 8655−75 red Phosphorus technical. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9428−73 Silicon (IV) oxide. Specifications

GOST 9721−79 cobalt Powder. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 9849−86 iron Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 10928−90 Bismuth. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 17299−78 ethyl Alcohol technical. Specifications

GOST 18300−87 ethyl rectified technical. Specifications

GOST 19627−74 Hydroquinone (paradoxians). Specifications

GOST 19908−90 Crucibles, bowls, beakers, flasks, funnels, test tubes and caps made of transparent quartz glass. General specifications

GOST 22860−93 Cadmium high purity. Specifications

GOST 22861−93 Lead of high purity. Specifications

GOST 23148−78 Powder metal. Methods of sampling and sample preparation*
_______________
* Standards 23148−98. — Note the CODE.

GOST 24104−88 laboratory Scales General purpose and model. General specifications*
_______________
* On the territory of the Russian Federation GOST 24104−2001, hereinafter. — Note the CODE.

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

ST SEV 543−77 Number. Record rules and rounding

3 General requirements

3.1 General requirements for methods of analysis should correspond to GOST 25086.

3.2 Selection and preparation of samples is carried out in cobalt GOST 123 and cobalt powder — according to GOST 23148.

3.3 To establish the calibration according to recommended to use at least four standard samples or solutions with known concentrations of elements.

3.4 When the analysis is carried out two parallel definitions.

3.5 the value of the result of the analysis should be terminated with a figure the same category as the error is guaranteed in the application of methods of analysis (next — error analysis methods) defined in this standard.

In the preparation of quality document production on the basis of the results of the analysis allowed a test result of chemical composition to represent a number with the same number of significant figures as in the tables of chemical composition to GOST 123 and GOST 9721.

3.6 Rules for rounding of numbers shall conform to the requirements of ST CMEA 543.

4 safety Requirements

4.1 carry out All work on the appliances and electrical installations, relevant regulations for electrical [1] and requirements of GOST 12.2.007.0.

4.2 When the equipment and installations required to comply with the requirements of GOST 12.3.019 and [2], [3].

4.3 All equipment and installations should be equipped with devices for grounding in accordance with the requirements of GOST 12.2.007.0 and GOST 12.1.030. Grounding must conform to the rules of electrical devices [1].

4.4 Analysis of cobalt is carried out in rooms equipped with General dilution ventilation system according to GOST 12.4.021.

4.5 To prevent contact with the air, oxides of carbon, nitrogen and aerosols of metal oxides in quantities exceeding the maximum allowable concentration according to GOST 12.1.005, and also to protect from ultraviolet radiation of 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 grinding Machine carbon electrodes should have a suction device to prevent the ingress of coal dust in the air of working zone in quantities exceeding the maximum allowable.

4.7 Control of hazardous substances in the workplace air should be carried out in accordance with the requirements of GOST 12.1.007, GOST 12.1.005 and GOST 12.1.016.

4.8 Disposal, deactivation and destruction of hazardous wastes from the production of analyses of cobalt should be carried out in accordance with the sanitary rules approved by the Ministry of health of Russia.

4.9 the Organization of training of the working personnel to the requirements of labour safety — according to GOST 12.0.004.

4.10 Requirements for professional selection and testing of knowledge of employees — according to GOST 12.3.002.

4.11 the premises of the laboratory must comply with the fire safety requirements according to GOST 12.1.004 and have a extinguishing media in accordance with GOST 12.4.009.

4.12 laboratory Personnel must be provided with premises according to sanitary norms [4] for the group the production processes of IlIa.

4.13 laboratory Personnel must be provided with overalls, special footwear and other means of individual protection [5].

5 Chemical-atomic-emission spectral method with the DC arc as excitation source spectrum

5.1 measurement Method

The ranges defined by the mass fraction of elements, %:

— aluminium 0,0002−0,1;

— bismuth 0,00005−0,005;

— iron 0,002−1,0;

— cadmium 0,0001−0,01;

— silicon of 0.0005−0.3;the

magnesium is 0.0001−0,005;

— manganese is 0.0001−0.3 mm;

— copper of 0.00005−0.3 mm;

— arsenic 0,0003−0,01;

— Nickel 0,002−1,0;

— tin of 0.00005−0,005;

— lead 0,0001−0,01;

— antimony 0,0001−0,01;

— phosphorus 0,0003−0,005;

zinc 0,0003−0,01.

Measurement method is based on the excitation spectrum in the arc of DC, with the 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 from their mass fraction in the sample. The sample is pre-transferred to the metal oxides.

Items and options that apply only to photographic or photoelectric methods of registration of the spectrum, indicated in the text, respectively, FG and FE.

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

A multichannel photoelectric spectrometer type IFS-8 (FE) or a type spectrograph STE-1 (FG), or any other spectrometer or spectrograph for ultraviolet region of the spectrum with an inverse linear dispersion of 0.6 nm/mm.

Power source DC arc type, UGE-4, or any other, providing a voltage up to 400 V and currents up to 20 A.

Microphotometer geregistreerde of any type (FG).

Press which provides sufficient force for tabletting the crushed metal oxides.

Mold alloy steel punch with a diameter of 4−8 mm. in the manufacture of the plunger and the inner surface of the matrix, hardened, cemented and sanded. The roughness parameter of the working surfaces in the manufacture of the mold should not exceed 0,160 µm according to GOST 2789.

Muffle furnace of any type with thermostat providing temperatures up to 850 °C.

Varicellae bowls or crucibles made of quartz glass according to GOST 19908 for dissolution of samples, evaporation of the solution and calcination of a mixture of salts. Allowed for dissolution and evaporation apply flask and glasses from chemically and thermally resistant glass according to GOST 25336 and bowls, cups and glasses from glassy carbon.

Standard samples of composition of cobalt, is manufactured in accordance with the application, or another method approved in the prescribed manner.

The rods of graphite OS.CH., C-2, C-3 or C-3M with a diameter of 6 mm as the upper electrode.

The rods of graphite with a diameter of 6−15 mm as electrodes-coasters.

The machine with a set of shaped cutters for sharpening electrodes.

Photographic plates spectrographic contrast (FG).

Gas analyzers of the 2nd class of accuracy of any type with an accuracy of weighing according to GOST 24104.

Libra technical of any type, ensure the weighing masses up to 500 g.

Mortar with pestle, agate or Jasper.

Buxy according to GOST 25336 or porcelain boat type L3 by GOST 9147.

Caps glass or plastic to protect from contamination prepared for analysis of tablets of samples, standard samples and sharpened electrodes.

A pair of tweezers.

Wool.

Distilled water according to GOST 6709, further purified by distillation or otherwise.

Nitric acid according to GOST 11125 or GOST 4461, h. h. or h. d. a., further purified by distillation or otherwise, and diluted 1:1.

Hydrochloric acid according to GOST 3118, diluted 1:10.

The technical rectified ethyl alcohol according to GOST 18300 or technical ethyl alcohol according to GOST 17299, further purified by distillation or otherwise.

Sodium salitsilovaya, solution in ethyl alcohol mass concentration of 60 g/DM(FG).

The developer consisting of two solutions (FG).

Solution 1:

— metol (parameterindependent) according to GOST 25664 — 2.5 g;

— hydroquinone (paradoxians) according to GOST 19627 — 12 g;

— sanitarily anhydrous sodium GOST 195 — 55 g;

— distilled water according to GOST 6709 — 1 DM.

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 — 1 DM.

Before the manifestation of the solutions 1 and 2 merge at a ratio of 1:1.

Allowed to apply contrast working developer of a different composition.

Fixing solution (FG):

— sodium thiosulfate crystal according to 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 — 1 DM.

5.3 Preparation for assay

Weighed samples weighing 5−10 g were placed in a bowl of quartz glass or another utensil to dissolve. In the analysis of cobalt grade K0 to the sample flow 30−50 cmof hydrochloric acid diluted 1:10, and process the sample under stirring for 1 min. Acid is drained by decantation and rinsed with sample 2−3 times with water in portions of 50 cmby decantation.

The sample poured in portions of 3−5 cmof nitric acid diluted 1:1, until complete dissolution of the sample when heated. The solution was evaporated to dryness.

The dry residue in the bowl of quartz glass is placed in a muffle furnace, heated to a temperature of (825±25) °C and maintained at this temperature for 15−20 min the resulting oxides are cooled and pulverized in a mortar.

From the crushed material taken three sample weighing 0.200 to 1,000 g depending on the conditions of analysis and a mass fraction of detectable elements and their tableted with a press and mold.

Mold clean residue from the sample with cotton wool soaked with ethyl alcohol. Consumption of ethanol is 10 cmon the sample.

Standard samples of the composition of cobalt in the form of metal prepared for analysis in the same way as the sample. Standard samples of the composition of cobalt in the form of oxides prepared for analysis, not by swiping them through a stage of dissolution in nitric acid.

5.4 analysis

Preparing the spectrometer to the measurements carried out in accordance with the manual for operation and maintenance of the spectrometer (FE).

Recommended analytical lines and ranges of detectable concentrations of elements are given in table 1.


Table 1 — Recommended analytical lines and ranges of detectable concentrations of the elements

The designated element	Wavelength of analytical lines, nm	The range of detectable concentrations, %
Aluminium	309,27	0,0002−0,01
	257,51	0,01−0,1
Bismuth	306,77	Of 0.00005−0.005 for
Iron	271,90	0,002−0,01
	296,69	0,002−0,03
	295,39	Of 0.01−0.3
	296,53	0,05−1,0
Cadmium	228,80	0,0001−0,0003
	Of 214.44	0,0001−0,0005
	326,11	0,0003−0,01
Silicon	288,16	0,0005−0,01
	251,61	0,0005−0,01
	251,92	0,005−0,3
Magnesium	280,27	0,0001−0,005
Manganese	279,48	0,0001−0,005
	257,61	0,005−0,05
	293,31	Of 0.01−0.3
Copper	324,75	Of 0.00005−0.005 for
	296,12	0,005−0,3
	249,20	0,005−0,3
Arsenic	234,98	0,0003−0,01
	286,04	0,0005−0,01
Nickel	300,25	0,002−0,02
	310,19	0,002−0,05
	282,13	0,05−0,5
	318,44	0,1−1,0
Tin	Of 284.00	Of 0.00005−0.005 for
	286,33	0,0001−0,005
	326,23	0,0005−0,005
Lead	283,31	0,0001−0,005
	Of 217.00	0,0001−0,005
	287,33	0,001−0,01
Antimony	259,81	0,0001−0,01
	206,83	0,0001−0,01
Phosphorus	213,62	0,0003−0,005
	214,91	0,0003−0,005
Zinc	206,20	0,0003−0,01
	330,26	0,0003−0,01
Cobalt a — line comparison	257,89	Basis
	278,59
	278,70
	297,55
	205,41
	213,66
	Of 291.00
	291,02

Allowed to use other analytical lines, if they provide a determination of mass fraction of elements in the specified range with an error not exceed this standard.

Pill sample or standard sample is placed on the electrode stand. The upper electrode should be sharpened to a truncated cone.

For removal of surface contamination of the electrode pre-calcined in an arc of DC current within 20 s at a current of 6−10 A, including as the anode of the arc. The electrodes of the OS.h. not allowed to be heated up.

The shape and dimensions of the electrodes and their location during the analytical exposure is shown in figure 1.

Figure 1. The shape and dimensions of the electrodes and their location during the analytical exposition

and — before exposure; b — at the anode the polarity of the sample; in — at the cathode the polarity of the sample

Figure 1

The spectrogram is removed through a three-stage attenuator. When working in a narrow range of detectable concentrations of the elements of shooting can be performed without the attenuator (FG).

The electrode stand is placed on it a tablet of sample or standard sample is composed of the anode of the arc. The spectrum starts only after the transition of the anode spot of the arc on the melt sample.

The transition speed because after a few seconds of arc current is turned off and again turn it on, until the melt has not yet had time to cool down.

Originally established arc gap adjusted periodically throughout the exposure on a zoomed image of the arc on the screen of the objective lens of the lighting system or with a special short throw projection lens. The spectrum carried out at the following average conditions: the width of the entrance slit of the spectral device of 0.010−0.015 mm, the illumination slits being a condenser, the aperture height in the middle of the condenser lens is 5 mm, current: 5−6, exposure 40−50 C, weight pills 0,200−0,500 g. the measurements obtained in the first stage, determine the volatile elements bismuth, cadmium, arsenic, tin, antimony, lead, zinc and phosphorus.

Formed during the first stage, the Wren is placed on sweetalicious the stand and include it as the cathode of the arc. The spectrum begins after the transition of the cathode spot of the arc from the cradle to the molten portion of the bead and hold it under the same average conditions. The height of the diaphragm middle lens of the condenser is 3 mm. the measurements obtained in the second stage, determine the semi-elements — aluminum, iron, silicon, magnesium, manganese, copper and Nickel.

Allowed to carry out the second stage without removing the bead from the base at the end of the first stage, automatically changing the polarity of the electrodes and the current arc (FE).

If necessary, the lower detection limits of volatile elements analytical lines with wavelengths less than 230 nm, the additional third stage. Photographic plates are treated in a solution of sodium salicylanilide for 60 s and dried. Pill sample or standard sample is composed of the anode of the arc. Conditions of registration of the spectrum: the width of the slit of a spectrograph is 0.018−0.020 mm, the illumination slits being a condenser, the aperture height in the middle of the condenser lens is 5 mm, the current strength 18−20 And 45−60 with exposure, electrode stand with a diameter of 15 mm with a recess on the end of the 1.5 mm, weight pills 0,700−1,000 g (FG).

Photographic plates showing within 4−6 min at a temperature of 18−20 °C, fixed, washed and dried (CF).

Optimization of conditions for the analysis of a specific type or brand of products is carried out by selection of the values of variables parameters (mass of tablets, arc current, exposure, width of the entrance slit of the spectral device), selection of optimum analytical lines, of the type of photographic plates, the shape of the upper electrode, etc.

5.5 processing of the results

In the spectra of samples and standard samples to measure the intensity of the analytical lines of the elements and lines of comparison of cobalt.

While photographic registration of the spectrum in the spectrograms of the samples and standard samples to measure the blackening of analytical lines of the determined elements and lines comparison, choosing the level of attenuation with optimum values of pucherani. On the measured values calculates the difference pucherani and their average values for each standard sample and each parallel assay. Before computing the average values it is recommended to check the suitability of the measurement results in accordance with Annex B. the calculated values for the standard samples and their corresponding values of mass fraction of detectable elements to build calibration graphs in the coordinate: .

Values for samples find the mass fraction of detectable elements on the respective calibration graphs.

By the photoelectric registration of spectrum according to the obtained results of measurements of the intensity of the analytical lines of the determined elements calculate average values for each standard sample and each parallel assay. Before computing the average values it is recommended to check the suitability of the measurement results in accordance with Annex B. the calculated values for the standard samples and their corresponding values of mass fraction of detectable elements to build calibration graphs in the coordinate: or .

When working on the spectrometer with a computer the values of the mass fraction of elements in standard samples and their corresponding arithmetic means of the measurements of the intensities of the analytical lines of the determined elements introduced in the computer that generates the equation of the calibration dependence.

Values or samples to find the mass fraction of detectable elements on the respective calibration graphs.

For the results analysis be the arithmetic mean of results of parallel measurements if the difference between them does not exceed the permissible differences given in 5.6.

When the divergence of the results of parallel measurements more acceptable analysis is repeated.

If during the re-analysis of the differences between the results of parallel measurements exceeds the allowable, the sample is replaced with new, obtained upon repeated sampling.

5.6 Control of accuracy of analysis

The control accuracy of the analysis carried out in accordance with GOST 25086 at least once a quarter. As standard for the control of accuracy using error analysis method , are shown in table 2.

Standards of operational control — the permissible discrepancy between two parallel definitions and allowable discrepancies between the two analysis results are given in table 2.


Table 2 — Standards for monitoring and error analysis method (under confidence probability =0,95)

Percentage

The designated element	Mass fraction	The permissible discrepancy between two parallel definitions	The allowable discrepancy of the two results of the analysis	The error analysis method
Aluminium	0,00020	0,00013	0,00018	0,00013
	0,0005	0,0003	0,0004	0,0003
	0,0010	About 0.0006	0,0008	About 0.0006
	0,0020	0,0010	0,0015	0,0010
	0,005	0,002	0,003	0,002
	0,010	0,004	0,006	0,004
	0,020	0,008	0,012	0,008
	0,050	0,019	0,026	0,019
	0,10	0,03	0,05	0,03
Bismuth	0,00005	0,00002	0,00003	0,00002
	0,00010	0,00004	Of 0.00006	0,00004
	0,00020	0,00008	0,00011	0,00008
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
Iron	0,0020	0,0008	0,0011	0,0008
	0,0050	0,0018	0,0025	0,0018
	0,010	0,003	0,005	0,003
	0,020	0,006	0,009	0,006
	0,050	0,014	0,020	0,014
	0,10	0,03	0,04	0,03
	0,20	0,05	0,07	0,05
	0,50	0,11	0,16	0,11
	1,0	0,2	0,3	0,2
Cadmium	0,00010	0,00005	0,00007	0,00005
	0,00020	0,00010	0,00014	0,00010
	0,0005	0,0002	0,0003	0,0002
	0,0010	0,0004	About 0.0006	0,0004
	0,0020	0,0008	0,0011	0,0008
	0,0050	0,0018	0,0025	0,0018
	0,010	0,003	0,005	0,003
Silicon	0,0005	0,0003	0,0004	0,0003
	0,0010	About 0.0006	0,0008	About 0.0006
	0,0020	0,0010	0,0015	0,0010
	0,005	0,002	0,003	0,002
	0,010	0,004	0,006	0,004
	0,020	0,008	0,012	0,008
	0,050	0,019	0,026	0,019
	0,10	0,03	0,05	0,03
	0,20	0,07	0,09	0,07
	0,30	0,09	0,13	0,09
Magnesium	0,00010	0,00007	0,00010	0,00007
	0,00020	0,00013	0,00018	0,00013
	0,0005	0,0003	0,0004	0,0003
	0,0010	About 0.0006	0,0008	About 0.0006
	0,0020	0,0010	0,0015	0,0010
	0,005	0,002	0,003	0,002
Manganese	0,00010	0,00003	0,00004	0,00003
	0,00020	Of 0.00006	0,00008	Of 0.00006
	0,00050	0,00013	0,00019	0,00013
	0,0010	0,0002	0,0003	0,0002
	0,0020	0,0005	About 0.0006	0,0005
	0,0050	0,0010	0,0015	0,0010
	0,0100	0,0020	0,0028	0,0020
	0,020	0,004	0,005	0,004
	0,050	0,008	0,012	0,008
	0,100	0,016	0,022	0,016
	0,20	0,03	0,04	0,03
	0,30	0,04	0,06	0,04
Copper	0,00005	0,00003	0,00004	0,00003
	0,00010	0,00005	0,00007	0,00005
	0,00020	0,00010	0,00014	0,00010
	0,0005	0,0002	0,0003	0,0002
	0,0010	0,0004	About 0.0006	0,0004
	0,0020	0,0008	0,0011	0,0008
	0,0050	0,0018	0,0025	0,0018
	0,010	0,003	0,005	0,003
	0,020	0,006	0,009	0,006
	0,050	0,014	0,020	0,014
	0,10	0,03	0,04	0,03
	0,20	0,05	0,07	0,05
	0,30	0,07	0,01	0,07
Arsenic	0,00030	0,00014	0,00020	0,00014
	0,0005	0,0002	0,0003	0,0002
	0,0010	0,0004	About 0.0006	0,0004
	0,0020	0,0008	0,0011	0,0008
	0,0050	0,0018	0,0025	0,0018
	0,010	0,003	0,005	0,003
Nickel	0,0020	0,0005	About 0.0006	0,0005
	0,0050	0,0011	0,0015	0,0011
	0,0100	0,0020	0,0028	0,0020
	0,020	0,004	0,005	0,004
	0,050	0,008	0,012	0,008
	0,100	0,016	0,022	0,016
	0,20	0,03	0,04	0,03
	0,50	0,07	0,09	0,07
	Of 1.00	0,12	0,17	0,12
Tin	0,00005	0,00002	0,00003	0,00002
	0,00010	0,00004	Of 0.00006	0,00004
	0,00020	0,00008	0,00011	0,00008
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
Lead	0,00010	0,00004	Of 0.00006	0,00004
	0,00020	0,00008	0,00011	0,00008
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
	0,010	0,003	0,004	0,003
Antimony	0,00010	0,00004	Of 0.00006	0,00004
	0,00020	0,00008	0,00011	0,00008
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
	0,010	0,003	0,004	0,003
Phosphorus	0,00030	0,00011	0,00016	0,00011
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
Zinc	0,00030	0,00011	0,00016	0,00011
	0,00050	0,00018	0,00025	0,00018
	0,0010	0,0003	0,0005	0,0003
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0050	0,0014	0,0020	0,0014
	0,010	0,003	0,004	0,003

For intermediate values of the mass fraction of elements, calculate values , and is carried out by linear interpolation.

6 Chemical-atomic-emission spectral method with inductively coupled plasma as the excitation source spectrum

6.1 measurement Method

The ranges defined by the mass fraction of elements, %:

— aluminum of 0.0005−0.3;the

— iron 0,001−1,0;

— cadmium of 0.0002−0,005;

— silicon 0,001−0,3;

— magnesium 0,0005−0,01;

— manganese of 0.0002−0.3 mm;

— copper of 0.0005−0.3;the

— Nickel 0,001−1,0;

— phosphorus 0,001−0,01;

zinc 0,0005−0,01.

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.

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

The automated spectrometer (or monochromator polychromator) atomic emission with inductively coupled plasma as the excitation source spectrum with all accessories.

Gas analyzers of the 2nd class of accuracy of any type with an accuracy of weighing according to GOST 24104.

Argon according to GOST 10157.

Nitric acid according to GOST 11125 or GOST 4461, h. h. or h. d. a., further purified by distillation or otherwise, and diluted 1:1.

Hydrochloric acid according to GOST 14261 and diluted 1:1.

A mixture of acids: 800 cmof water was added 300 cmof hydrochloric acid and 100 cmof nitric acid.

Aluminum powder according to GOST 5494.

Iron powder brand MLB-1 according to GOST 9849 or iron carbonyl, OS.CH., [6].

Cadmium GOST 1467 or GOST 22860.

Cobalt grade K0 GOST 123 with established mass proportions of the identified elements.

Sodium acid 9-aqueous.

Carbonyl Nickel powder according to GOST 9722.

Magnesium primary GOST 804.

Manganese GOST 6008.

Copper according to the GOST 859.

Potassium phosphate according to GOST 4198, dried at a temperature of (105±2) °C for 1 h.

Zinc GOST 3640.

Sodium carbonate according to GOST 83, solution of the mass concentration of 200 g/DM.

Distilled water according to GOST 6709, further purified by distillation or otherwise.

A solution of cobalt mass concentration of 200 g/DM: a portion of the cobalt with a mass of 100.00 g were placed in a glass with a capacity of 1000 cm, add 50 cmof water and in portions of 5−10 cmpour 400 cmof nitric acid. The solution was evaporated to a volume of 250−300 cm, cooled, transferred to a volumetric flask with a capacity of 500 cmand topped to the mark with water.

Solution of iron and Nickel mass concentrations of 1 g/DM: hanging iron weight 0,5000 g was dissolved with heating in 30 cmof a mixture of acids, boil for 5−10 minutes, cooled and transferred to volumetric flask with a capacity of 500 cm. The suspension of Nickel powder in a weight 0,5000 g was dissolved with heating in 25 cmof nitric acid, diluted 1:1, boiled for 5−10 min, dilute with water to 100 sm, filter the solution through a filter „red ribbon“, washed the filter 4−5 times with hot water, cooled, transferred to the same volumetric flask and topped to the mark with water.

Solution of manganese and copper mass concentration of 1 g/DMand of magnesium mass concentration of 0.1 g/DM: sample of manganese and copper for weight 0,5000 g of magnesium with a mass 0,1000 g separately dissolved by heating in 25 cmof nitric acid, diluted 1:1, boil for 5−10 minutes, cool, each solution was transferred to volumetric flasks with a capacity of 100 cmeach and topped to the mark with water. In a volumetric flask with a capacity of 100 cmis taken at 20 cmobtained solutions of manganese and copper, and 10 cmof a solution of magnesium and topped to the mark with water.

A solution of aluminium mass concentration of 1 g/DM: a portion of aluminum powder with a mass of 0,4000 g was dissolved with heating in 25 cmof hydrochloric acid diluted 1:1, transferred into a volumetric flask with a capacity of 100 cmand then filled to the mark with water. In a volumetric flask with a capacity of 100 cmselect the 25 cmof this solution and topped up to the mark with water.

The solution of cadmium and zinc mass concentrations of 0.02 g/land phosphorus mass concentration of 0.04 g/DM: sample of cadmium and zinc by mass 0,1000 g separately dissolved by heating in 25 cmof nitric acid, diluted 1:1, cooled, each solution was transferred to volumetric flasks with a capacity of 500 cmeach and topped to the mark with water. Weighed potassium phosphate mass 0,4393 g dissolved in water, transferred to a volumetric flask with a capacity of 500 cmand topped to the mark with water. In a volumetric flask with a capacity of 100 cmtaken at 10 cmthe obtained solutions of cadmium and zinc, and 20 cmof a solution of phosphorus and topped to the mark with water.

A solution of a silicon mass concentration of 0.5 g/DM: suspension of silicate of sodium with a mass 2,5297 g dissolved in 50 cmof sodium carbonate solution, transferred to a volumetric flask with a capacity of 500 cmand topped to the mark with water.

For the preparation of solutions with known concentrations of elements use oxides or salts of stable composition, as well as state standard samples of solutions of metals.

Solutions of known concentrations of the elements stored in a plastic container.

6.3 Preparation for analysis

6.3.1 Preparation of graded solutions

For the preparation of the calibration solutions 1−11, the recommended composition of which is given in table 3 in volumetric flasks with a capacity of 100 cmeach taken the calculated volumes of solutions with known concentrations of elements and topped to the mark with water. If necessary, make amendments to the mass fraction of the elements in the cobalt used for the preparation of its solution.


Table 3 — Composition of the calibration mixtures

In milligrams per cubic decimeter

Item	Mass concentration of the element in the calibration solution
	1	2	3	4	5	6	7	8	9	10	11
Aluminium	-	1	5	25	50	-	0,1	0,5	5	50	100
Iron	-	5	10	50	100	-	0,2	1	10	100	200
Cadmium	-	0,2	0,4	1	5	-	1	1	1	1	1
Silicon	-	1	5	10	20	-	0,25	0,5	2,5	25	50
Magnesium	-	0,5	1	5	10	-	0,05	0,25	2,5	5	10
Manganese	-	1	5	25	50	-	0,1	0,5	5	50	100
Copper	-	1	5	25	50	-	0,1	0,5	5	50	100
Nickel	-	5	10	50	100	-	0,2	1	10	100	200
Phosphorus	-	0,4	0,8	2	10	-	2	2	2	2	2
Zinc	-	0,2	0,4	1	5	-	1	1	1	1	1

Mass concentration of cobalt in the calibration solutions 1 to 5 is 50 g/DM, 6−11 calibration solution — 20 g/DM.

6.3.2 Preparation of solutions samples

A portion of the sample with a mass of 5,000 grams are placed in a beaker with a capacity of 250 or 400 cm, dissolved in 100 cmof the mixture of acids, adding the mixture in small portions, and evaporated to a volume of 25−30 cm, transferred into a volumetric flask with a capacity of 100 cmand then filled to the mark with water. The initial solution used for the determination of cadmium, zinc and phosphorus.

In a volumetric flask with a capacity of 100 cmselect 20 cmof the primary solution and topped up to the mark with water. The solution is used for determination of Nickel, iron, copper, manganese, silicon, aluminum and magnesium.

6.4 analysis

Preparing the spectrometer to the measurements carried out in accordance with the instruction 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 and ranges of detectable concentrations are given in table 4. From the above lines choose the optimum one depending on mass fraction of elements in the samples, the type of spectrometer, the capacity of the output slots on the carriages of the device and other context-specific analysis.


Table 4 — Recommended analytical lines and ranges of detectable concentrations of the elements

The designated element	Wavelength of analytical lines, nm	The range of detectable concentrations, %
Aluminium	309,27	Of 0.0005−0.3 mm
	394,40	Of 0.0005−0.3 mm
	396,15	Of 0.0005−0.3 mm
Iron	259,94	0,001−1,0
	238,20	0,001−1,0
	234,35	0,002−1,0
Cadmium	226,50	Of 0.0002−0,005
	Of 214.44	0,0004−0,005
Silicon	251,61	0,001−0,3
Magnesium	279,55	0,0005−0,01
	280,27	0,0005−0,01
Manganese	257,61	Of 0.0002−0.3 mm
	259,37	Of 0.0002−0.3 mm
	293,31	Of 0.0002−0.3 mm
Copper	324,75	Of 0.0005−0.3 mm
	224,70	0,001−0,3
Nickel	216,56	0,001−1,0
	227,02	0,001−1,0
	351,50	0,001−1,0
	352,45	0,001−1,0
Phosphorus	178,29	0,001−0,01
	213,62	0,001−0,01
	214,91	0,001−0,01
Zinc	206,20	0,0005−0,01

Allowed to use other analytical lines, if they provide a determination of mass fraction of elements in the specified range with an error not exceed this standard.

When working at the monochromator position check of the analytical lines, using the calibration solution of 5 or 10.

The calibration dependence for cadmium, zinc and phosphorus is found using the calibration solutions 1 to 5, and for Nickel, iron, manganese, copper, magnesium, aluminum and silicon — calibration solutions 6−11.

For each calibration solution perform at least 5 measurements of the intensities of the analytical lines of the determined elements. By calculating the average of the values of the intensities define the parameters of the calibration graphs, which are introduced into the computer memory at the stage of creating analytical programs.

Before the beginning of measurements and after every 2 hours of operation of the device adjust the calibration graphs for the two calibration solutions of 2 and 5 or 7 and 11.

For each of the sample solution and carry out three measurements of intensity of analytical lines of the determined elements.

6.5 processing of the results

The mass fraction of detectable elements in the sample and their average values read from the screen or the tape printing device.

Records of the mass of sample dilution solutions of the sample and other variables is performed automatically at the stage of introduction of analytical program in the computer.

For the results analysis be the arithmetic mean of results of parallel measurements if the difference between them does not exceed the permissible differences given in 6.6.

When the divergence of the results of parallel measurements more acceptable analysis is repeated.

If during the re-analysis of the differences between the results of parallel measurements exceeds the allowable, the sample is replaced with new, obtained upon repeated sampling.

6.6 accuracy Control analysis

The control accuracy of the analysis carried out in accordance with GOST 25086 at least once a quarter. As standard for the control of accuracy using error analysis method And shown in table 5.

Standards of operational control — the permissible discrepancy between two parallel definitions and allowable discrepancies between the two analysis results are given in table 5.


Table 5 — Standards for monitoring and error analysis method (under confidence probability =0,95)

Percentage

The designated element	Mass fraction	The permissible discrepancy between two parallel definitions	The allowable discrepancy of the two results of the analysis	The error analysis method
Aluminium	0,00050	0,00023	0,00028	0,00020
	0,0010	0,0005	About 0.0006	0,0004
	0,0020	0,0007	0,0009	About 0.0006
	0,0050	0,0015	0,0019	0,0014
	0,010	0,003	0,004	0,003
	0,020	0,005	0,006	0,004
	0,050	0,012	0,015	0,011
	0,100	0,022	0,028	0,020
	0,30	0,06	0,08	0,06
Iron	0,0010	0,0004	0,0005	0,0004
	0,0030	0,0009	0,0012	0,0008
	0,0050	0,0015	0,0019	0,0014
	0,010	0,003	0,004	0,003
	0,030	0,007	0,009	0,006
	0,100	0,018	0,022	0,016
	0,200	0,028	0,030	0,021
	0,50	0,06	0,07	0,05
	Of 1.00	0,11	0,14	0,10
Cadmium	0,00020	0,00008	0,00010	0,00007
	0,00030	0,00017	0,00020	0,00014
	0,00050	0,00026	0,00030	0,00021
	0,0010	0,0004	0,0005	0,0004
	0,0020	About 0.0006	0,0007	0,0005
	0,0050	0,0014	0,0017	0,0012
Silicon	0,00050	0,00025	0,00030	0,00021
	0,0010	About 0.0006	0,0007	0,0005
	0,0050	0,0015	0,0019	0,0014
	0,010	0,003	0,004	0,003
	0,030	0,007	0,009	0,006
	0,050	0,011	0,014	0,010
	0,100	0,024	0,030	0,021
	0,30	0,07	0,09	0,06
Magnesium	0,0005	0,0004	0,0005	0,0004
	0,0010	0,0007	0,0009	About 0.0006
	0,0050	0,0015	0,0019	0,0014
	0,0100	0,0028	0,0030	0,0021
Manganese	0,00020	0,00007	0,00009	Of 0.00006
	0,00050	0,00016	0,00020	0,00014
	0,0010	0,0003	0,0004	0,0003
	0,0050	0,0009	0,0011	0,0008
	0,0100	0,0019	0,0024	0,0017
	0,030	0,004	0,005	0,004
	0,050	0,006	0,007	0,005
	0,100	0,010	0,012	0,008
	0,300	0,025	0,030	0,021
Copper	0,00050	0,00015	0,00019	0,00014
	0,0010	0,0003	0,0004	0,0003
	0,0020	About 0.0006	0,0007	0,0005
	0,0050	0,0011	0,0014	0,0010
	0,0100	0,0022	0,0027	0,0019
	0,020	0,004	0,005	0,004
	0,030	0,006	0,007	0,005
	0,050	0,008	0,010	0,007
	0,100	0,015	0,019	0,014
	0,30	0,04	0,05	0,04
Nickel	0,0010	0,0003	0,0004	0,0003
	0,0050	0,0009	0,0011	0,0008
	0,0100	0,0019	0,0024	0,0017
	0,050	0,006	0,007	0,005
	0,100	0,010	0,012	0,008
	0,300	0,025	0,030	0,021
	0,50	0,04	0,05	0,04
	Of 1.00	0,06	0,07	0,05
Phosphorus	0,0010	0,0004	0,0005	0,0004
	0,0020	0,0008	0,0010	0,0007
	0,0030	0,0011	0,0014	0,0010
	0,0050	0,0015	0,0018	0,0013
	0,010	0,003	0,004	0,003
Zinc	0,00050	0,00026	0,00030	0,00021
	0,0010	0,0004	0,0005	0,0004
	0,0020	About 0.0006	0,0009	About 0.0006
	0,0030	0,0008	0,0010	0,0007
	0,0050	0,0012	0,0014	0,0011
	0,0100	0,0024	0,0030	0,0021

For intermediate values of the mass fraction of elements, calculate values , and is carried out by linear interpolation.

APPLICATION (recommended). The method of preparation of the calibration standard samples

APPENDIX A
(recommended)

Standard samples for the calibration represent a crushed cobalt oxide additions introduced with the identified elements. The composition of the standard samples to develop a given mass fraction of elements in the analyzed products. Metrological characteristics of standard samples is set in accordance with the requirements of GOST 8.315.

A. 1 measurement Means, auxiliary devices, materials, reagents, solutions

Gas analyzers of the 2nd class of accuracy of any type with an accuracy of weighing according to GOST 24104.

Muffle furnace of any type with thermostat providing temperatures up to 850 °C.

Mortar with pestle, agate or Jasper.

Bowl varicellae quartz glass according to GOST 19908 or glassy carbon.

The technical rectified ethyl alcohol according to GOST 18300 or technical ethyl alcohol according to GOST 17299, further purified by distillation or otherwise.

Nitric acid according to GOST 11125 or GOST 4461, h. h. or h. d. a., further purified by distillation or otherwise, and diluted 1:1 and 1:2.

Sulfuric acid according to GOST 4204, diluted 1:2.

Hydrochloric acid according to GOST 3118, diluted 1:10.

Tartaric acid according to GOST 5817.

Aluminum powder according to GOST 5494.

Bismuth GOST 10928.

Iron powder brand MLB-1 according to GOST 9849 or iron carbonyl, OS.CH., [6].

Cadmium GOST 1467 or GOST 22860.

Cobalt grade K0 GOST 123 with established mass proportions of the identified elements.

Silicon (IV) oxide according to GOST 9428, crushed and sifted through a sieve with cell size 0,074 mm, or tetraethyl ester of silicic acid solution in ethyl alcohol.

Magnesium primary GOST 804.

Manganese GOST 6008.

Copper according to the GOST 859.

Arsenic [7].

Carbonyl Nickel powder according to GOST 9722.

Tin GOST 860.

Lead at 3778 or GOST GOST 22861.

Antimony GOST 1089.

Red phosphorus according to GOST 8655 or potassium phosphate according to GOST 4198, dried at a temperature of (105±2) °C for 1 h.

Zinc GOST 3640.

Distilled water according to GOST 6709, further purified by distillation or otherwise.

For the preparation of solutions of the input elements use oxides or nitrate salt of stable composition, as well as state standard samples of solutions of metals.

A. 2 Production of material of standard samples

Before preparation of a solution of the basis cathode plate cobalt pre-treated with hydrochloric acid diluted 1:10, washed with water, then with ethanol and dried with filter paper.

A portion of the estimated mass of cobalt is dissolved by heating in nitric acid, diluted 1:1.

Sample calculation mass of Nickel powder, iron, copper, magnesium, manganese, aluminum powder, zinc, lead, bismuth, cadmium, and phosphorus is dissolved by heating in nitric acid, diluted 1:1.

When using a phosphate of potassium for the introduction of phosphorus dissolved in water. Antimony is dissolved in the presence of tartaric acid at a weight ratio of antimony and tartaric acid 1:5. Arsenic is dissolved in hot nitric acid. The solutions were transferred to volumetric flasks and topped up to the mark with nitric acid, diluted 1:2.

Tin dissolves in sulphuric acid, the solution was transferred to volumetric flask and topped to the mark with sulfuric acid diluted 1:2.

The estimated volumes of solutions with known content of elements added to a solution of cobalt.

Silicon injected in the form of an aqueous slurry of silicon oxide or solution tetrachloro ester of silicic acid in ethyl alcohol.

The resulting solutions evaporated to dry salts and calcined in a muffle furnace at a temperature of (825±25) °C. the Calcined mixture of oxides is cooled, crushed to a powder in a mortar or other method eliminating contamination of material from the standard samples. The material is mixed and used to determine the metrological characteristics.

Material of standard samples stored in tightly closed cans or buksh under conditions that exclude contamination and moisture.

APPENDIX B (recommended). The procedure for verifying the suitability of the results of the parallel measurements with the calculation result of the determination

APPENDIX B
(recommended)

Three values of the differences pochernenija (or intensities) of the analytical spectral lines find the mass fraction of the determined elements in the calibration schedule. Suitable considered three dimensions for which the condition

, (B. 1)

where , and are the values on the mass fraction of the element corresponding to highest, lowest and average of the three difference values of pucherani (or intensity);

 — relative value allowable discrepancies between and , the recommended value for aluminum, bismuth, cadmium, silicon, copper, arsenic, magnesium =0.50 mm, for the rest of the items =0,33.

If this condition is not met, it is allowed to exclude the result, the most remote of the average. The remaining two dimensions are considered suitable, if the condition

, (B. 2)

where , and are the values on the mass fraction of the element corresponding to highest, lowest and average of the two remaining values of the difference of pochernenija (or intensity).

If this condition is not met, the analysis is repeated on the new tablets of the same sample.

ANNEX b (informative). Bibliography

THE APP
(reference)

[1]		Rules of arrangement of electrical installations, approved by the Glavgosenergonadzora, 1985, 6th ed.
[2]		The rules of operation of electrical installations, approved by the Glavgosenergonadzora Russia 31.03.92, 5th ed.*
_______________ * Rules of technical operation of electrical consumers., approved by order of Ministry of energy of Russia from 13.01.2003 No. 6. — Note the CODE.
[3]		Safety regulations for operation of consumers, approved by the Glavgosenergonadzora 21.12.84, 4th ed.*
_______________ * Apply cross-industry Rules on labor protection (safety rules) for electrical installations» (SWEAT P M-016−2001, RD 153−34.0−03.150−00). — Note the CODE.
[4]	SNiP 2.09.04−87	Administrative and domestic buildings
[5]		Typical branch norms of free issue to workers and employees with special clothes, special footwear and other individual protection means, approved by the Resolution of USSR state Committee and the Presidium of the all from 01.08.79 N 344/P-7 and augmented 21.08.85 N 289/P-8*
_______________ * There are Standard norms 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 (as amended on 17 December 2001). — Note the CODE.
[6]	THAT 6−09−05808009−262−92	Carbonyl iron, OS.h. 13−2 OS.h. 6−2
[7]	THAT 113−12−112−89	Arsenic, metal, semiconductor compounds, the OS.h.