GOST 3221-85

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  ГОСТ 3221-85

GOST 3221−85 Aluminium primary. Methods of spectral analysis (with Change No. 1)

GOST 3221−85

Group B59

INTERSTATE STANDARD

ALUMINIUM PRIMARY

Methods of spectral analysis

Primary aluminium. Methods of spectral analysis

ISS 77.120.10
AXTU 1709

Date of introduction 1986−07−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

DEVELOPERS

V. P. Kiselev, Cand. tech. Sciences; Vladimir Baranovsky, PhD. tech. Sciences; L. V. Drutskaya, PhD. tech. Sciences; V. T. Lavrentiev

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 17.06.85 N 1698

3. The frequency of inspection — 5 years

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

The designation of the reference document referenced	Item number
GOST 8.315−97	1.1
GOST 8.326−89	4.2
GOST 61−75	4.1
GOST 84−76	4.1
GOST 244−76	4.1
GOST 1465−80	4.1
GOST 1770−74	4.1
GOST 3118−77	4.1
GOST 3773−72	4.1
GOST 4160−74	4.1
GOST 5556−81	4.1
GOST 6709−72	4.1
GOST 10691.0−84 — GOST 10691.4−84	4.1
GOST 11069−2001	4.7.1
GOST 12697.1−77 — GOST 12697.10−77	4.7.2
GOST 17299−78	4.1
GOST 18300−87	4.1
GOST 19627−74	4.1
GOST 25086−87	4.7.2
GOST 25664−83	4.1
GOST 28498−90	4.1

5. Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)

6. EDITION (August 2005) with amendment No. 1, approved in August 1990 (IUS 11−90)


This standard specifies the spectral methods for determination of silicon (with a mass fraction of from 0.0007 to 0.6%), iron (at mass fraction of from 0.0007 to 0.6%), copper (at a mass fraction of from 0.0007 to 0.02%), titanium (with a mass fraction of from 0.0007 to 0.02%), zinc (when the mass fraction of from 0.0007 to 0.15%), manganese (at a mass fraction of from 0.0007 to 0.02%), magnesium (at a mass fraction of from 0.0007 to 0.02%), chromium (in mass fraction of from 0.0007 to 0.01%), vanadium (with mass fraction of from 0.0007 to 0.01%), sodium (with a mass fraction of from 0.0005 to 0.03%) in the primary aluminum and high technical purity with photographic and photoelectric registration of spectrum.

Methods based on excitation of atoms of aluminum and impurities by an electric discharge, the decomposition of the radiation into a spectrum, registration of analytical signals proportional to the intensity or the logarithm of the intensity of spectral lines and subsequent determination of the mass fraction of elements in the sample, using the calibration parameters.

1. GENERAL REQUIREMENTS

1.1. Calibration characteristics establish graphical or calculation method for each element in the respective standard samples (CO), certified and applied in accordance with GOST 8.315.

1.2. The spectrum — photographic and photoelectric.

1.3. For sample preparation and analysis of high-purity aluminium should be allocated separate equipment. The laboratory needs to operate the plant for cleaning the air from dust and other contaminants, and maintained the specified temperature and humidity.

(Changed edition, Rev. N 1).

2. SAMPLING

2.1. Sampling from liquid metal

Sampling is carried out by pouring the molten metal into the graphite or cast iron tight-fitting mold. The inner surface of the chill mould and spoon sampled should exclude the possibility of sample contamination-defined elements. Design molds arbitrary. Design molds and his preparation for sampling should provide homogeneous samples of the correct shape and size without bowls, cracks and tides.

On selected samples should be embossed corresponding number.

2.1.1. For the analysis of aluminium of technical purity take samples with a diameter of 5−6 mm.

2.1.2. For the analysis of high-purity aluminium sampled with a diameter of 8−10 mm.

2.1.3. When performing analyses on quantometer with blowing argon discharge samples are taken with a diameter and a height of 30−50 mm, depending on the construction of the tripod, shapes and sizes.

2.1.4. (Deleted, Rev. N 1).

2.2. Samples are taken from pigs and other semi-finished products from primary aluminium

2.2.1. To control the chemical composition of ingots and other semi-finished products from primary aluminium samples are taken in the form of rods, strips, disks, or other shape in accordance with the normative-technical documentation.

2.2.2. The sample must be homogeneous. On the surface of the sample intended to sparking, are not allowed shells, slag inclusions and other defects.

3. PREPARATION OF SAMPLES FOR ANALYSIS

3.1. For the analysis of used samples (after sharpening): round bars or square cross-section with a diameter of from 5 to 50 mm, length 35−120 mm, discs, strips with a minimum thickness of 5 mm. allowed to use samples of other sizes corresponding to the sizes FROM.

3.2. Ubeskrivelig the surface of the analyzed samples (AO) and standard samples (CO) sharpen on a plane, a cone or hemisphere on a lathe or milling machine (samples with a diameter of 5−10 mm are allowed to be cut by a mechanical knife or to sharpen with a file) to obtain a smooth surface without cavities and slag inclusions.

(Changed edition, Rev. N 1).

3.3. For the analysis using paired JSC or of JSC with the counter of spektralnogo coal.

3.3.1. Spectralinehandy coal protivoelektrodom 6 mm in diameter sharpened to a hemisphere with a radius of 3−4 mm, or a truncated cone with ground diameter of 1.5−2 mm, sharpening at an angle of 40−60°.

3.4. To avoid falling into the category of dirt from the lateral surface of the AO and the ends of the specimens should be wiped with ethyl alcohol.

(Changed edition, Rev. N 1).

3.4.1−3.4.2. (Deleted, Rev. N 1).

3.5. When determining the mass fraction of sodium and minimum values of the mass fraction of iron, silicon and titanium in aluminium of high purity is recommended etching of the samples for 10−15 min in a solution of hydrochloric acid (1:5) in vessels without polluting the solution defined elements.

The following etching part of the sample, previously subjected to etching, is removed.

(Changed edition, Rev. N 1).

3.5.1. (Deleted, Rev. N 1).

3.6. Preparation AO and analysis should be identical.

4. METHOD OF SPECTRAL ANALYSIS WITH PHOTOGRAPHIC REGISTRATION OF SPECTRUM

4.1. Apparatus, materials, reagents

Types spectrograph ISP-30, STE-1, DFS-452.

Generator types, IG-3, IVS-23, IVS-28, DG-2, Arkus, UGE-4.

Spectromancer types of PS-18, SP-2, DSP-2.

Microphotometer types of MF-2, MD-100, IFO-460.

The nine-damping.

Shaped carbon electrodes high purity high purity brand-7−3, brand high purity-7−4.

Photographic plates for spectrum analysis type PFS-01 (SP-1); PFS-03 (SP-2); PFS-02 (SPES); the «micro», 3−130 sensitivity units in GOST 10691.0 — GOST 10691.4 or any type for normal blackening of analytical lines and lines of comparison (belonging to a straight-line segment of the characteristic curve of the emulsion).

Fotocity or other vessels for processing photographic plates.

Oven or electropotence for drying photographic plates of any type that provides heated air to 30 °C. Room air conditioner types of a / cs-4−12B, SC-6A, BC-2500, etc.

Thermometer laboratory according to GOST 28498.

Lathes types of TV-16, TV-14, etc.

Machines for grinding samples of KP-35.

Fixture for grinding coal protivoelektrodom that allows you to sharpen them on a hemisphere or a cone.

Knives guillotine type for cutting aluminum samples onto a plane.

The manual vise and table.

Files types 2820−0016, 2820−0021, 2820−0022, 2820−0026, 2820−0027 according to GOST 1465.

Electrode holders, design and materials from which they are made, prevent hit in the analytical discharge gap controlled elements.

Baptiste for cleaning the optics; the chunk-size 200x200 mm 1 device for a period of 3 months.

Flannel for obtenci appliances and generators; the size of a piece of 300x300 mm per unit, for a period of 3 months.

Cotton fabric for obtenci AO before analysis; the chunk-size 200x200 mm, 100 samples with a diameter of 5−10 mm, a size of 200x200 mm piece of 50 samples with a diameter of 30−50 mm.

Laboratory volumetric glassware (cylinders, beakers, flasks) according GOST 1770.

Rectified ethyl alcohol according to GOST 18300: in the analysis of aluminium of technical purity — 1 cmfor 5 samples with a diameter of 5−6 mm; in the analysis of high-purity aluminium — 1 cmto 1 sample with a diameter of 8−10 mm or 1 cmon one surface with a diameter of 30−50 mm; when grinding samples for milling or lathe with an alcohol cooling and lubrication — 7 cmfor one of the analyzed surface. Allowed application cleaned by distillation of technical ethyl alcohol according to GOST 17299.

Absorbent cotton wool GOST 5556.

The developer consisting of two solutions.

Solution A

metol (parameterindependent) according to GOST 25664 — 2.3 g;

sanitarily sodium (sodium sulfite) crystal — 110 g;

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

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

Solution B

sodium carbonate 10-water according to GOST 84 — 115 g;

potassium bromide according to GOST 4160 — 7 g;

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

To dissolve substances should be consistent in the manner specified above.

Before the manifestation of the mixed solutions A and B in equal volumes.

Fixer:

distilled water according to GOST 6709 — 1000 cm;

sodium thiosulfate (hyposulphite) the crystal according to GOST 244 — 300 g;

ammonium chloride according to GOST 3773 — 60

Acetic acid solution:

acetic acid according to GOST 61 — 30 cm;

distilled water according to GOST 6709 — 1000 cm.

Hydrochloric acid according to GOST 3118, diluted with distilled water 1:5.

Standard samples: state standard samples (GSO), the industry standard sample (CCA), standard samples of the enterprise (SOP).

Length used standard and analyzed samples should not be less than 35 mm in diameter 5−10 mm and less than 15 mm — with a diameter of 30−50

mm.

4.2. Allowed the use of other measuring instruments with the metrological characteristics of equipment and technical characteristics are not worse, and reagents for quality not lower than the above. Measuring instruments must be tested (public or private) or certified according to GOST 8.326*.
________________
* On the territory of the Russian Federation there are PR 50.2.009−94.

4.3. Recommended mode of processing of photoplates

Temperature fotorastvorov should be (20±1) °C.

Sequence processing: a photographic exhibit, washed with tap water, dipped for 10−15 s in a solution of acetic acid, again rinsed with water and immersed in the fixer to complete transparency, unexposed areas of the plate, after which it was thoroughly washed with water and dried.

The manifestation of the photographic plates are at a red light or in darkness, depending on the type of photographic plates. During display of the cell must gradually be shaken for mixing the developer. Recording starts under the same conditions as the manifestation, in 2−3 minutes, you can continue in normal lighting.

4.1−4.3. (Changed edition, Rev. N 1).

4.4. Analysis

4.4.1. The conditions of analysis with photographic registration of the spectrum are given in table.1, Appendix 1. Wavelengths of spectral lines and the corresponding ranges of values of the mass fraction of controlled elements are given in table.1.

Table 1

The designated element	The wavelength of the element, nm	Preventing elements	The range of values of the mass fraction of element, %
Vanadium	437,92	Iron	0,003−0,01
	318,54	«	0,001−0,01
	318,40	«	0,001−0,01
Iron	371,99	-	0,0005−0,5
	302,06	Chrome	0,0003−0,3
	275,40	«	0,1−1,0
	274,32	Nickel	0,1−1,0
	259,94	-	0,03−1,0
	248,33	-	0,0005−1,0
	239,56	-	0,1−1,0
Silicon	390,55	Iron	0,1−1,0
	298,76	-	0,5−1,0
	288,16	-	0,0005−1,0
	251,61	Titan	0,001−1,0
	250,69	-	0,01−1,0
Magnesium	518,36	-	0,001−0,02
	285,21	Iron	Of 0.0005 to 0.02
	280,27	Manganese	0,001−0,02
	279,55	Iron	0,001−0,02
	279,08	-	0,003−0,02
Manganese	482,35	-	0,001−0,02
	403,08	Gallium, iron	From 0.0002 to 0.02
	294,92	Tungsten, titanium	0,001−0,02
	293,30	-	0,005−0,02
	280,11	Magnesium, iron	From 0.0002 to 0.02
	260,57	-	0,001−0,02
	259,37	Iron	0,001−0,02
Copper	510,55	Iron	0,001−0,03
	327,40	-	0,0003−0,03
	324,75	Iron, titanium	0,0003−0,03
		-	0,0003−0,03
Sodium	589,59	-	0,001−0,03
	Of 589.00	-	Of 0.0003 to 0.02
Titan	365,35	Iron	0,002−0,03
	337,28	-	0,003−0,03
	334,90	-	0,0001−0,03
	323,45	Iron	0,005−0,03
Chrome	425,43	-	0,0001−0,005
	359,35	Iron	0,001−0,01
	357,87	Strip CN	0,003−0,01
	301,48	Iron	0,003−0,01
Zinc	636,23	-	0,001−0,1
	481,05	-	0,001−0,1
	334,50	-	0,0002−0,1
Line comparison:
1) aluminium	396,153	-
	394,403	-
	308,216	-
	305,993	-
	305,008	-
	293,6	-
	266,92	-
	265,249	-
	266,039	-
	237,841	-
2) background near analytical lines	-	-

Notes:

1. From the above lines for specific analytical methods to choose the optimal line, depending on their intensity, overlay lines («nuisance items»), the spectral type of installation, the sensitivity of photographic plates or photomultipliers, the possibility of placing the output slots on the carriages of the device.

2. Allowed to use other spectral lines, subject to obtaining the metrological characteristics are not worse than specified in this standard.

4.4.2. For construction of calibration characteristics choose at least four FROM covering a certain range of values of the mass fraction of this element. It is unacceptable to extrapolate the calibration characteristics for the range of values of the mass fraction of the controlled element in the appropriate WITH on the basis of which were established calibration characteristics.

Spectra AO and photographed on the same photographic plate at the desired testing conditions, a series of spectra WITH should be placed between the spectra of AO to average the possible heterogeneity of the emulsion. For each co and AO photographed at least two spectra independently from the sharpened surfaces. For example, if AO represent bars with a diameter of 5−10 mm, the spectra get them from different ends.

When determining the values of the mass fraction of impurities in aluminum of high purity and the determination of the mass fraction of sodium in all brands of primary aluminium take pictures of at least three spectra from each co and AO.

4.4.3. After you run the phototreatment dry clean plate photometric on microphotometer. Measure the blackening of analytical lines and lines of comparison (proportional to the logarithm of the light intensity of the wavelength falling on a photographic plate), calculate the difference of pochernenija for the analytical line pairs, and the arithmetic mean of two or three spectra. Building calibration characteristics in the coordinates for each item, where  — mass fraction of the controlled element. This feature is suitable for determining the mass fraction of the element in those joint-stock companies, which photographed the spectra together with the spectrum FROM on one photographic plate.

The blackening of analytical lines must be in the region of the straight portion of the characteristic curve for a given emulsion and the wavelength. If blackening of analytical lines are outside the linear region of the characteristic curve, it is necessary to adjust exposure when photographing spectra or photographic plates to use a different sensitivity.

To determine the minimum grade, when the small black and small the difference between pochernenija lines and the background, moving from pochernenija to intensities by using the characteristic curve drawn in the field of neoteric.

The calibration characteristics in this case are built in coordinates

,

where is the intensity of the line of the designated element;

 — the intensity of the comparison lines or background area of the controlled element.

(Changed edition, Rev. N 1).

4.4.4. When performing Express analysis of allowed to use the method of «continuous graphics».

The bulk of the calibration characteristic is established during the implementation of specific techniques for this spectral installation.

For this photograph at least three spectra, each WITH five different photos. Calculate the arithmetic average of the 15 measurements (for 15 spectra). Define a straight line segment calibration curve and choose FROM two, located on the borders of the straight portion.

In the analysis of the AO on the working plate three times taking pictures of spectra selected FROM two AO. The results of electrophoretic spectrum determines the angle of rotation of the work schedule and the magnitude of the parallel displacement relative to the main schedule.

For the calibration characteristic in the form of a graph or table determine the value of the mass fraction of a monitored item in stock.

4.5. Processing of the results

4.5.1. Parallel (unit) definition of () believe the value of the mass fraction of the component in the analyzed material, calculated on the analytical signal in one spectrogram, obtained on the plate with photographic registration of spectrum on the photovoltaic installation.

For the results analysis be the arithmetic mean of two parallel definitions

, (1)

provided that at 0,95

, (2)

where is the absolute maximum divergence between two parallel definitions of the mass fraction of characterizing the convergence of analysis results; values are given in table.2.

If condition (2) is not satisfied, then the analysis should be repeated by setting the required number of parallel measurements (based on two measurements) according to the formula

, (3)

where divergence parallel to the definitions obtained in the analysis. The resulting value is rounded up to higher whole number.

The final result should be the arithmetic mean of parallel definitions of confidence interval, the corresponding confidence interval of the arithmetic mean that would be obtained if according () to the standards table.2.

Table 2

Permissible differences that characterize the repeatability and reproducibility of the results
when the photographic method

Impurity	The range of mass fraction, %	Allowable absolute differences of two parallel definitions of the mass fraction of impurities (%) characterizing the rate of convergence of parallel measurements (p = 0.95)	Allowable absolute differences of two parallel definitions of mass fraction of impurity (%) characterizing the measure of the reproducibility of the results of the analysis (0,95)
Iron, silicon	From 0,003 to 0,010 incl.	0,002	0,004
	SV. 0,010 «0,030 «	0,006	0,010
	«To 0.03» to 0.10 «	0,01	0,02
	«To 0.10» to 0.30 «	0,03	0,05
	«Of 0.30» to 0.60 «	0,04	0,06
Copper	To from 0,0005 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0050 «	0,0007	0,0015
	«0,005» 0,010 «	0,001	0,002
	«0,010» 0,020 «	0,002	0,003
Magnesium	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0050 «	0,0007	0,0015
	«0,005» 0,020 «	0,002	0,003
Titanium, manganese	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0050 «	0,0007	0,0015
	«0,005» 0,010 «	0,001	0,002
	«0,010» 0,020 «	0,002	0,003
Zinc	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0050 «	0,0007	0,0015
	«0,005» 0,010 «	0,002	0,003
	«0,010» 0,100 «	0,007	0,015
Chromium, vanadium	From 0,0010 to 0,0020 incl.	0,0004	0,0008
	SV. 0,002 «0,010 «	0,001	0,002
Sodium	From 0.0007 to 0,0010 incl.	0,0010	0,0020
	SV. 0,001 «0,004 «	0,002	0,003
	«0,004» 0,010 «	0,004	0,006
	«0,010» 0,020 «	0,008	0,015

4.5.2. When determining the mass fraction of the controlled elements in aluminium of high purity and mass fraction of sodium performing three parallel detection (three spectra). For the results analysis be the arithmetic mean of three parallel measurements , and with confidence probability of 0.95

, (4)

provided that

, (5)

where and  — maximum and minimum values of the results of three parallel measurements.

If the condition (5) is not satisfied, then the analysis is repeated by defining the required number of parallel measurements (including done) by the formula (3), where the discrepancy between the highest and lowest results of parallel measurements obtained in the analysis.

The final result of the analysis be the arithmetic mean of parallel definitions; the confidence interval corresponds to the confidence interval of the arithmetic mean that would be obtained if according () to the standards table.2.

4.5.3. When determining the values of the mass fraction of controlled elements near the boundary marks the result of the analysis is calculated as the average of the two or more definitions. The required number of definitions () is calculated by the formula

, (6)

where  — coefficient characterizing the limiting error analysis for the accepted confidence probability of 0.95 (1,64);

 — the price of a unit in the last decimal the maximum value of mass fraction of the controlled element according to GOST 11069;

factor Pearson (2,77).

The resulting value is rounded up to higher whole number.

4.5.1, 4.5.2. (Changed edition, Rev. N 1).

4.6. Control the reproducibility of the results of the analysis

4.6.1. Control the reproducibility of the spectral analysis is carried out at least once a quarter.

(Changed edition, Rev. N 1).

4.6.2. The number of repeated definitions set depending on the total number of incoming samples, but not less than 0.5% of all samples of commercial products received in the laboratory during the quarter.

4.6.3. Control the reproducibility of the analysis results (calculated as an arithmetic mean of parallel definitions, 2) is performed by comparing previously obtained and reproduced according to this method, the analysis result for selected samples.

The discrepancy between the results of the initial and re-analyses are compared with the standard where  — allowable absolute difference of results of two parallel measurements (obtained in different shifts) that characterize the reproducibility of the results (values are given in table.2).

If the difference between the results of the initial and re-analyses of the same samples exceed the value of the ratio is not more than 5% of cases, the reproducibility of spectral analysis were satisfactory.

4.7. Control the accuracy of the results of spectral analysis

4.7.1. Control the accuracy of the results of spectral analysis carried out according to GSO through the entire course of the analysis. Use to control the accuracy of the CCA and SOP is valid in the case, if not released, the corresponding set of GSO for the analytical range or detectable component, not covered by GOST 11069.

The difference between a single result of determining the mass fraction of impurity in the GSO used for the control of accuracy of analysis spectra each time photographing the spectra of the analyzed samples and the certified values of mass fractions of impurities should not exceed the values given in table.2.

. (7)

To control the accuracy of analysis results using at least two of GSO certified values of mass fractions of components are close to the upper and lower boundaries of the range of the mass fraction of the designated component.

If the condition (7) is not satisfied, then the analysis is repeated by setting the rejection reason.

4.7.2. Besides the control of accuracy of analysis results with the use of notes, carried out as control data obtained by chemical methods according to GOST and GOST 25086 12697.1 — GOST 12697.10 or other methods at least once per quarter.

The number of results of spectral analysis, controlled by chemical or other methods, depends on the total number of incoming samples, but should not be less than 0.1% of all samples received in the laboratory for a specified period.

4.7.3. The coincidence of the two methods can be considered satisfactory if the observed condition

, (8)

where ,  — indicators of convergence for the spectral and reference methods given in the relevant standards;

, is the number a single results when calculating and ;

factor Pearson; 0,95

2,77	2
3,31	3
3,63	4

When

. (9)

Control the accuracy of the results of the analysis should also be conducted after a long break in work, repair of equipment.

(Changed edition, Rev. N 1).

5. METHOD OF SPECTRAL ANALYSIS WITH PHOTOELECTRIC REGISTRATION OF SPECTRUM

5.1. Apparatus, materials, reagents

Photovoltaic plant types, MFS-4, MFS-6, MFS-8, FSPA. the Rest of equipment: the materials, the reagent according to claim 4.1 and 4.2, with the exception of specifically related to the photographic method.

5.1.1. (Deleted, Rev. N 1).

5.2. Preparation for assay

5.2.1. Training photovoltaic installation measurements carried out according to the instructions of the manufacturer for maintenance and operation of the facility.

5.2.2. The establishment of calibration parameters for each PV plant is carried out when implementing the techniques of measurements using certified reference material of composition. Kit GSO should fully cover the whole range of determined values of the mass fraction of each of the controlled elements.

5.2.3. In the initial calibration, perform at least five series of measurements on different days of the photovoltaic installation. In a series of for each carried out WITH two pairs of parallel measurements (performed one after the other on the same surface). Allowed if the size of the analyzed surface does not allow two measurements (spot sparking overlap), use the required number of copies of the same.

Order parallel measurements are chosen randomly (changing in each series).

Calculate the arithmetic mean value of analytical signals for the five series of measurements each WITH (20 measurements).

The calculated or graphically set the calibration characteristics that are expressed in the form of a graph, table or formula.

The calibration characteristics are used to determine the mass fraction of the controlled elements in the AO.

5.2.4. Stability control calibration parameters is performed not less than 4 hours of photovoltaic installation. Allowed to exercise control for the upper and lower limit of the measuring range.

For control purposes, choose two with the corresponding values of the mass fraction of this element (or group elements),andanalyze them at least four times. Calculated for a series of measurements each WITH (and ).

Correction of the calibration characteristics is required if the bias exceeds the standard deviation of four measurements FROM one of the limits, i.e. when

,

where  — the number of concurrent measurements of co, which is controlled by the position of the calibration parameters (4);

 — the value of the mass fraction of the element in m WITH (1 or 2);

 — the relative standard deviation of the four measurements corresponding WITH.

5.2.5. Re-calibrating photovoltaic installation in accordance with clause 5.2.3 at least once a month, at the same time allowed the reduction of the number of measurements.

5.3. Analysis

5.3.1. The conditions of analysis are given in table.2 of Annex 1.

5.3.2. Wavelengths of spectral lines and the corresponding ranges of values of mass fraction are given in table.1.

5.3.3. Perform two parallel denitions for each controllable element of AO (two spectra).

5.3.4. When determining the values of the mass fraction of controlled elements in aluminium of high purity grades A995 and the A99 and the determination of the mass fraction of sodium performing three parallel detection (three spectra).

5.3.3, 5.3.4. (Changed edition, Rev. N 1).

5.4. Processing of the results

5.4.1. Processing of the results of the analysis performed in accordance with clause 4.5. Value , for the PV method are given in table.3.

Table 3

Permissible differences that characterize the repeatability and reproducibility
the results of the analysis by the photoelectric method

Impurity	Range mass fraction, %	Allowable absolute differences of two parallel definitions of the mass fraction of impurities (%) characterizing the rate of convergence of parallel measurements (p = 0.95)	Allowable absolute differences of two parallel definitions of the mass fraction of impurities (%) characterizing the measure of the reproducibility of the analysis (0,95)
Iron, silicon	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0030 «	0,0004	About 0.0006
	«0,003» 0,010 «	0,001	0,002
	«0,010» 0,030 «	0,003	0,005
	«0,030» 0,100 «	0,007	0,010
	«To 0.10» to 0.30 «	0,01	0,02
	«Of 0.30» to 0.60 «	0,02	0,03
Copper, magnesium, manganese, titanium	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0050 «	0,0007	0,0010
	«0,005» 0,010 «	0,001	0,002
	«0,010» 0,020 «	0,002	0,003
Vanadium, chromium	From 0.0007 to 0,0010 incl.	0,0002	0,0004
	SV. 0,0010 «0,0020 «	0,0004	About 0.0006
	«0,0020» 0,0050 «	0,0007	0,0010
	«0,005» 0,010 «	0,001	0,002
Zinc	From 0.0007 to 0,0010 incl.	0,0003	About 0.0006
	SV. 0,0010 «0,0030 «	About 0.0006	0,0010
	«0,003» 0,007 «	0,001	0,002
	«0,007» 0,010 «	0,002	0,003
	«0,010» 0,070 «	0,005	0,008
	«0,07» a 0,15 «	0,01	0,02
Sodium	To from 0,0005 0,0010 incl.	0,0005	0,0008
	SV. 0,0010 «0,0040 «	0,0010	0,0015
	«0,004» 0,010 «	0,002	0,003
	«0,010» 0,020 «	0,004	0,006

(Changed edition, Rev. N 1).

5.5. Control of reproducibility of results of analysis made in accordance with clause 4.6.

5.6. Control of the correctness of the results of the analysis performed in accordance with clause 4.7.

ANNEX 1 (recommended). The conditions of analysis

ANNEX 1
Recommended

Table 1

The conditions of analysis with photographic registration of spectrum

Controlled parameter	The values of the mass fraction of controlled elements, %
	The iron, silicon less than 0.03; copper, manganese, magnesium, titanium, zinc less than 0.005	Vanadium, chromium, manganese, titanium — less than 0.01; zinc — less than 0.1	The iron, silicon less than 1.0; copper, manganese, magnesium, titanium — less than 0,03	Sodium less than 0.02
Spectrograph	ISP-30	ISP-30	ISP-30	STE-1
The width of the slit of a spectrograph, mm	0,010−0,030	0,010−0,025	0,020−0,040	0,007−0,015
Generator, character of discharge	DG-2; TDF-28; UGE-4	DG-2; TDF-28; UGE-4	IG-3; IVS-23; UGE-4	DG-2; TDF-28; UGE-4.
	The arc is AC or DC	The arc is AC or DC	High voltage condensed spark. The scheme is simple or complex (controllable)	The arc is AC or DC
Inductance, mH	-	-	0; 0,01; 0,05; 0,15; 0,55	-
Capacitance, µf	-	-	0,005; 0,01; 0,02	-
The analytical gap, mm	1,5−2,0	1,5−2,0	2−3	1,5
The strength of the current, And	5−9	7−9	1,5−4,0	7−8
The roasting	3−10	2−5	20−40	Without firing
The polarity of the co and AO in the arc of DC	The anode	The anode	-	The anode
Photographic plates, type	1,2,S, slide, micro	1,2,S, slide, micro	1,2,S, slide, micro	Film wide latitude sensitivity, pangram
Coordinate system	;	;		;

Notes:

1. In addition to the paired samples allowed the use of coal counter, sharpened a plane, a hemisphere or a truncated cone.

2. The exposure time is set depending on the sensitivity of the photographic plates. The blackening of analytical lines must be located at the straight portion of the characteristic curve.

3. Allowed to use other conditions of the analysis (depending on the available equipment, materials, reagents) subject to obtaining the metrological characteristics are not worse than specified in this standard.

Table 2

The conditions of analysis with photoelectric registration of spectrum

Controlled parameter	The values of the mass fraction of controlled elements, %
	The iron, silicon less than 1.0; copper, manganese, magnesium, titanium — less than 0,03	The iron, silicon less than 0.03; copper, manganese, magnesium, titanium, zinc less than 0.005	Vanadium, chromium, manganese, titanium — less than 0.01; zinc — less than 0.1	Sodium — less than 0.02
Photovoltaic installation	MFS-4, 6, 8	MFS-4, 6, 8	MFS-4, 6, 8	FSPA-
The voltage, V	220±20	220±20	220±20	220±20
Width of the input gap, mm	0,01−0,06	0,01−0,06	0,01−0,06	0,01−0,06
Width of output slit, mm	0,030−0,200	0,030−0,200	0,030−0,200	0,030−0,200
Generator, character of discharge	IG-3; IVS-23; UGE-4 high-voltage condensed spark. The scheme is simple or complex (controllable)	DG-2; TDF-28, UGE-4 — arc AC, DC or intermittent arc width modulation
The strength of the current, And	1,5−4,0	3−9	3−9	7−8
The analytical gap, mm	1,5−3,0	1,5−2,0	1,5−2,0	1,5−2,0
The roasting	20−40	3−5	3−5	Without firing
Inductance, mH	0; 0,01; 0,05; 0,15; 0,55	-	-	-
Capacitance, µf	0,005; 0,01; 0,02	-	-	-
The polarity of the co and AO in the arc of DC	-	The anode	The anode	The anode
Coordinate system	;	;

Notes:

1. In addition to the paired samples allowed the use of a carbon counter, sharpened to a hemisphere or truncated cone.

2. Allowed to use other conditions of the analysis (depending on equipment) subject to obtaining the metrological characteristics are not worse than specified in this standard.


APPENDIX 1. (Changed edition, Rev. N 1).

APPENDIX 2. (Deleted, Rev. N 1).