GOST 26239.5-84

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  ГОСТ 26239.5-84

GOST 26239.5−84 semiconductor Silicon and quartz. Method for the determination of impurities (with Change No. 1)

GOST 26239.5−84

Group B59

STATE STANDARD OF THE USSR

THE SEMICONDUCTOR SILICON AND QUARTZ

Method for the determination of impurities

Semiconductor silicon and quartz. Method of impurities determination

AXTU 1709

Valid from 01.01.86
to 01.01.91*
________________________________
* Expiration removed
Protocol N 7−95 Interstate Council
for standardization, Metrology and certification
(IUS N 11, 1995). — Note the manufacturer’s database.

DEVELOPED by the Ministry of nonferrous metallurgy of the USSR

PERFORMERS

Y. A. Karpov, M. N. Schulepnikov, M. K. Vinnikov, G. G., Gavin, N. Gradskova, O. V. Zavialov, T. I. Zyablova, V. E., Quinn, V. A. Krylov, A. I. Kuzovlev, N. And. Marunya, V. G., Miscreants, V. M. Mikhailov, M. G. Nazarova, V. A. Orlov, A. I. Stepanov, N. With. Sysoeva, V. I. Firsov, G. I. Alexandrova

INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

Member Of The Board Of A. P. Snurnikov

APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards dated July 13, 1984 N 2490

The Change N 1, approved and in effect as of 01.01.91 by the resolution of Gosstandart of the USSR from 26.06.90 N 1847

Change No. 1 made by the manufacturer of the database in the text ICS N 10, 1990


This standard specifies neutron activation method for the determination of impurities into the undoped semiconductor silicon and quartz are within the ranges of values of mass fraction of impurities:

The method is not applicable for the analysis of silicon grades, KES-0.01 and CAM-0,01.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 26239.0−84.

2. APPARATUS, MATERIALS AND REAGENTS

Nuclear reactor with a flux of neutrons 0,5−1·10neutron/(cm·s) and a cadmium ratio for gold in the channel for irradiation of samples is equal to 2−5.

Gamma-ray spectrometer consisting of a multichannel analyzer (the number of channels of the analyzer not less than 2000), the block signal amplification, semiconductor germanium or germanium-lithium detector with photoaffinity γ-ray line With energy 1332 Kev of at least 1.5% (in the corner ). The ratio peak/Compton for not less than 30:1. The resolution of the spectrometer is not more than 3 Kev in line With with the energy of 1332 Kev.

Box protective type 1Б11−1НЖ.

Container lead transport stamps CR-10,0 wall thickness of 100 mm.

Container lead table brand KT-10 with a wall thickness of 10 mm.

Personal protective equipment against radiation and contamination by radioactive substances, according to the Basic sanitary rules OSP 72/87*.
_______________
* On the territory of the Russian Federation the document is not valid. Act SP 2.6.1.799−99. — Note the manufacturer’s database.

The aluminum canisters are made of aluminum brand 995-A.

Radiometer Tiss.

Set an exemplary standard gamma emitters (OSGI).

Filters obestochennye «blue ribbon».

Aluminum foil stamps 995-A thickness of 0.05−0.1 mm, GOST 618−73.

Volumetric flasks with a capacity of 50, 100, 1000 cm.

Measuring cylinders with a capacity of 10 and 25 cm.

Micropipettes 0.1 cm(first class).

The PTFE beakers with a capacity of 150 cm.

Glasses chemical glass with a capacity of 100 cm.

Drying oven with temperatures up to 150 °C.

Oven muffle of the type MP-2УМ.

Liquid nitrogen according to GOST 9293−74.

The mortar and pestle of agate or Jasper.

Tile electric.

Laboratory scales according to GOST 24104−88*.
_______________
* On the territory of the Russian Federation the document is not valid. Valid GOST R 53228−2008. — Note the manufacturer’s database.

Libra microanalytical type VLM-1.

Lamp infrared radiation type of ikz-220−500.

Acetone according to GOST 2603−79.

Distilled water GOST 6709−72.

Hydrochloric acid of high purity according to GOST 14261−77.

Nitric acid of high purity according to GOST 11125−78*.
______________
* On the territory of the Russian Federation the document is not valid. Standards 11125−84. — Note the manufacturer’s database.

Hydrofluoric acid according to GOST 10484−78.

Sulfuric acid of high purity according to GOST 14262−78.

Sodium hydroxide according to GOST 4328−77.

The sodium sulfate Piro GOST 18344−78*.
______________
* On the territory of the Russian Federation the document is not valid. Act THAT 6−09−5404−88** (IUS N 3, 1989);
** The document is the author’s development. For additional information, please refer to the link. — Note the manufacturer’s database.

Ammonium vinocity according to GOST 4951−79*.
______________
* On the territory of the Russian Federation the document is not valid. Act THAT 6−09−08−2007−89** (IUS N 12, 1989);
** The document is the author’s development. For additional information, please refer to the link. — Note the manufacturer’s database.

The technical rectified ethyl alcohol GOST 18300−87.

Ammonium molybdate according to GOST 3765−78, H. h

Gallium metal according to GOST 12797−77.

Radio engineering carbonyl iron according to GOST 13610−79, mark PS.

Europium oxide with a purity of 99.9%.

Gold GOST 6835−80*.
______________
* On the territory of the Russian Federation the document is not valid. Standards 6835−2002. — Note the manufacturer’s database.

Indium metal according to GOST 10297−75*.
______________
* On the territory of the Russian Federation the document is not valid. Standards 10297−94. — Note the manufacturer’s database.

Potassium dichromate according to GOST 4220−75, H. h, dried to constant weight at 140 °C.

Cobalt metal according to GOST 123−78*, grades K-1.
______________
*On the territory of the Russian Federation the document is not valid. Valid GOST 123−2008. — Note the manufacturer’s database.

Semiconductor silicon, grade KP-1−6.

Lanthanum oxide with a purity of 99.9%.

Lutetium oxide with purity of 99.9%.

Copper powdered metal according to GOST 859−78*, mark M3.
______________
* On the territory of the Russian Federation the document is not valid. Valid GOST 859−2001. — Note the manufacturer’s database.

Arsenic is a metal purity of 99.9%.

Sodium volframovich 2-water according to GOST 18289−78, H. h

Sodium chloride according to GOST 4233−77, H. h, dried to constant weight.

Nickel oxide black GOST 4331−78, CH.

Silver nitrate according to GOST 1277−75, H. h, dried to constant weight at 140 °C.

Scandium oxide with purity of 99.9%.

Antimony metal according to GOST 1089−82, brand Cy-0000.

Tantalum pentoxide with purity of 99.9%.

Zinc metal according to GOST 3640−79*.
______________
* On the territory of the Russian Federation the document is not valid. Valid GOST 3640−94. — Note the manufacturer’s database.

Standard sodium solution containing 0.01 mg/cmsodium or 0.0254 g of sodium chloride, dried to constant weight, is placed in a measuring flask with volume capacity of 1000 cm, and dissolved in distilled water, adjusted to the mark, mix.

A standard silver solution containing 0.002 mg/cmsilver: 0,00315 g of silver nitrate is placed in a measuring flask with volume capacity of 1000 cmand dissolved with distilled water, bring to a label, mix.

A standard solution of molybdenum and chromium containing 0.01 mg/cmof molybdenum and 0.01 mg/cmchrome: 0,0184 g of ammonium molybdate and 0,0283 g of potassium dichromate was placed in a volumetric flask with a capacity of 100 cm, dissolved in distilled water, adjusted to the mark, mix.

Stock solution of copper and zinc containing 0.1 mg/cmcopper and 0.5 mg/cmzinc: 0,1000 g of copper and 0,5000 g of zinc is placed in a beaker with a capacity of 100 cmand dissolved by heating in 50 cmof a mixture of hydrochloric and nitric acids (1:5), after dissolution of the copper and zinc solution was cooled and transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix. From the main solution taken 10 cmand transferred to a volumetric flask with a capacity of 100 cm, adjusted with distilled water to the mark, mix. This solution, containing 0.01 mg/cmcopper, and 0.05 mg/cmzinc, used as a standard solution.

A standard solution of tungsten containing 0.005 mg/cmtungsten: 0,00897 volframovich g of sodium dissolved in distilled water in a volumetric flask with a capacity of 1000 cm, adjusted with distilled water to the mark, mix.

Stock solution of tantalum containing 0.5 mg/cmtantalum: 0610 g of tantalum pentoxide is fused in a muffle furnace with 2 g peacemaking of sodium at 900 °C until a clear melt. The fusion is dissolved by boiling in 40 cmof a 10% solution Vinokurova ammonium solution was cooled, transferred to a volumetric flask with a capacity of 100 cm, adjusted with distilled water to the mark, mix.

Standard tantalum solution prepared on the day of use. From the main solution are taken 2 cm, transferred to a measuring flask with volume capacity of 1000 cmand was adjusted to the mark with 8%-s ' solution of ammonium Vinokurova, mix. Standard tantalum solution contains 0.001 mg/cmof tantalum.

Standard iron solution containing 10 mg/cmiron: 1,000 g of iron is placed in a beaker with a capacity of 100 cm, add 30 cmof concentrated hydrochloric acid and 1.5 cmof nitric acid and heated until complete dissolution of the sample, after cooling, the solution is transferred to a volumetric flask with a capacity of 100 cm, adjusted with distilled water to the mark, mix.

Standard solution of cobalt, containing 0.002 mg/cmcobalt: 0,00200 grams of cobalt was placed in a beaker with a capacity of 50 cmand dissolved in a minimum volume of nitric acid, the solution transferred to a volumetric flask with a capacity of 1000 cm, adjusted with distilled water to the mark, mix.

Standard solution of arsenic containing 0.01 mg/cmarsenic: 0,0100 g of arsenic is placed in a beaker with a capacity of 50 cmand dissolved by heating in 5 cmof sulphuric acid, after dissolution of the arsenic solution was boiled down to about 1 cm, cooled and transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix.

Stock solution of europium, lutetium and lanthanum, containing 0.01 mg/cmeuropium, 0.01 mg/cmLutetia and 0.05 mg/cmof lanthanum: 0,0116 g of europium oxide, 0,0114 g of an oxide of lutetium and 0,0596 g of lanthanum oxide placed in a beaker with a capacity of 100 cm, add 20 cmof concentrated hydrochloric acid, diluted with distilled water in the ratio 1:1, dissolved by heating, cooled, transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix. From the main solution taken 2.0 cmand transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix.

This solution containing from 0.0002 mg/cmeuropium, from 0.0002 mg/cmLutetia and 0.001 mg/cmof lanthanum, used as a standard solution.

Stock solution of scandium containing 0.1 mg/cmscandium: 0,1500 g of scandium oxide was placed in a beaker with a capacity of 100 cm, adding 25 cmof concentrated hydrochloric acid, diluted with distilled water in the ratio 1:1, dissolved by heating, after cooling, the solution is transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with distilled water, mix. This solution, containing 0.001 mg/cmscandium is used as a standard solution.

Stock solution of antimony containing 0.01 mg/cmof antimony: 0,0100 g of antimony dissolved in 5 cmof Aqua Regia (1 part nitric acid and 3 parts hydrochloric acid) when heated, after removal of the nitrogen oxides, the solution is transferred into a measuring flask with volume capacity of 1000 cm, 6M dilute hydrochloric acid to the mark, mix. From the main solution taken 10 cmand transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark 6M solution of hydrochloric acid, mix. This solution, containing 0.001 mg/cmof antimony, used as a standard solution.

Stock solution of gold, containing 0.01 mg/cmgold: 0,0100 g of gold was dissolved in 5 cmof Aqua Regia by heating, after removal of the nitrogen oxides, the solution is transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix. From the main solution taken 2.0 cmand transferred to a volumetric flask with a capacity of 100 cm, adjusted with distilled water to the mark, mix. This solution containing from 0.0002 mg/cmof gold used as standard solution of gold.

A standard solution of Nickel containing 0.5 mg/cmof Nickel: 0,0704 g of an oxide of Nickel placed in a beaker with a capacity of 50 cmand dissolved in 10 cmof dilute nitric acid, the solution transferred to a volumetric flask with a capacity of 100 cm, adjusted with distilled water to the mark, mix.

India standard solution containing 0.01 mg/cmIndia: 0,0100 g of indium is placed in a beaker with a capacity of 50 cmand was dissolved with heating in a minimum volume of Aqua Regia (1 part nitric acid and 3 parts hydrochloric acid), after cooling, the solution is transferred into a measuring flask with volume capacity of 1000 cm, adjusted with distilled water to the mark, mix.

A standard solution of gallium, containing 0.01 mg/cmgallium: 0,0100 g of gallium is dissolved in a minimum volume of Aqua Regia (1 part nitric acid and 3 parts hydrochloric acid) in a beaker with a capacity of 50 cmwhen heated, after cooling, the solution is transferred into a measuring flask with volume capacity of 1000 cm, adjusted to the mark with 1% solution of hydrochloric acid, mix.

(Changed edition, Rev. N 1).

3. PREPARATION FOR ASSAY

3.1. Preparation of samples analysed samples and comparison to irradiation

Pencil case for radiation and aluminum foil for wrapping samples and comparison samples are washed with acetone, then alcohol.

From each test portion is taken for two sample 2−3 mm thick, weighing 4−6 grams, put each portion into an aluminum package, the package label.

The total mass of analyzed samples is in the pencil box should not exceed 30 g.

From each standard solution was taken at 0.1 cmand nakatyvaet on separate strips of filter paper of «blue ribbon» size 1x3 cm, dried under an infrared lamp, then the strip is folded in three layers to a size of 1x1 cm and wrapped in aluminum foil, labeled. In a container for irradiation is placed simultaneously with the samples for two sample comparisons for each defined element. Each reference sample contains: tungsten 0.0005 mg, 0.001 mg of gallium, europium 0,00002 mg, iron 1.0 mg, gold 0,00002 mg, 0.001 mg India, cobalt 0.002 mg, 0.0001 mg lanthanum, lutetium 0,00002 mg copper 0.001 mg, 0.001 mg molybdenum, arsenic 0.001 mg, 0.005 mg sodium, Nickel 0.5 mg, 0.0001 mg scandium, silver of 0.0002 mg 0.0001 mg antimony, tantalum 0.0001 mg, 0.001 mg of chromium, zinc of 0.005 mg.

In each case for the radiation is placed one strip of filter paper is prepared and packaged as described above, but without dripped on it standard solutions.

Pencil case with the analyzed samples and comparison samples are irradiated in a nuclear reactor during:

100 h if the expected mass fraction of impurities to be determined, is less than 10% by weight;

10 h if the expected mass fraction of impurities, which must be determined is more than 10% by weight.

Irradiated samples are transported to the laboratory in a lead transport container TC-10,0.

(Changed edition, Rev. N 1).

4. ANALYSIS

4.1. Processing the analyzed samples and comparison samples after irradiation

Pencil case with irradiated analyte samples and comparison samples are placed in a protective box type 1Б11−1НЖ. 25−30 h after irradiation of the analyzed samples free from aluminum packets and placed in Teflon beakers and thrice etched in a freshly prepared mixture of nitric and hydrofluoric acids (5:1). Each etching 20−40 with no heat. After acid etching, the sample is treated with 10% alkali solution for 40−80 s. After each etching, the samples are washed with water, and after alkaline etching is dried under an infrared lamp, weighed on an analytical balance, Packed in aluminum foil, labeled.

Samples of comparison and a strip of filter paper without dripped on it standard solutions recovered from aluminum packets and placed in non-irradiated aluminum packages.

The analyzed samples and the comparison samples placed in different security containers of the type CT.

4.2. Preparation of a gamma-ray spectrometer to the measurement of activity and measurement of the activity of the analyzed samples and the samples of comparison

The measurement of the activity of the analyzed samples and the samples of the comparison is preceded by the calibration of the spectrometer energy by using the set OSGI. During calibration select this amplification of signals, in which channel 1 of the analyzer had to 0.7−1.0 Kev.

Before measuring activity of samples measured within 30−40 min the natural background level of the detector. If in the spectrum there are gamma lines of the radionuclides that can be identified as artificially radioactive substances, take measures to decrease the background to the natural background level of the detector, caused by naturally-radioactive elements in the materials surrounding the detector (wall, defense, etc.).

When measuring the activity of samples and sample comparisons download of the spectrometer should not lead to distortion of the shape of the amplitude distribution of more than 10%.

If you want to reduce the load of the spectrometer from the bremsstrahlung radiation caused by the radionuclides that are formed from silicon and from low-energy gamma rays of the radionuclides impurity elements, applying the filter radiation — a layer of aluminium of 3 mm and a iron layer with a thickness of 3−4 mm.

If you want to reduce the load of the spectrometer only from low-energy radiation of radionuclides impurity elements, applying the filter radiation — a layer of aluminium of 2 mm and a layer of lead of 2−3 mm.

In an analytical use of gamma lines of the radionuclides given in table.1.

Table 1

______________
* Conversion factor 1 Kev=1,602·10erg


The time of measurement of the activity of the analyzed samples depends on the content of determined elements and is 1−6 h. the Time of measuring the activity of samples comparisons and strips of filter paper, which is not dripped a standard solution that is 1−3 min. exposure Time of a sample depends on the mass fraction and the ratio of trace elements in the analyzed samples. For the samples with the mass fraction of vysokozastyvayuschih impurity elements (sodium, scandium, cobalt, copper, gallium, arsenic, bromine, antimony, rare earth elements, hafnium, tantalum, tungsten, rhenium, iridium, and gold) not more than (1−3)·10%, tungsten, gallium, europium, lanthanum, copper, arsenic, sodium, and zinc determined by the exposure time equal to 20−30 h, and other elements — when the exposure time of 60−100 h. If the mass fraction listed above vysokozastyvayuschih elements less (1−3)·10%allowed the simultaneous determination of all elements after aging for 25−30 h

Spectra of samples decode the energies of most intense gamma-lines of radionuclides detectable elements with the use of the spectrometer at the energy and position of the analytical gamma lines in the spectra of samples comparison.

4.1, 4.2. (Changed edition, Rev. N 1).

5. PROCESSING OF THE RESULTS

5.1. The mass fraction of detectable elements () in percent is calculated by the formula

,

where is the number of pulses in the analytical peak of the radionuclide of the element in the spectrum of a test sample, imp;

, is the number of pulses in the analytical peak in the spectrum of the samples of comparison 1 and 2, respectively, of imp;

, ,  — the measurement of the spectrum of the analyzed sample and the comparison samples 1 and 2, respectively, min;

 — weight of sample, mg;

 — the content of the element in the reference sample, mg;

is the correction factor due to difference in the geometrical dimensions of sample and sample comparison; is set experimentally for each detector (1);

 — the half-life of the radionuclide;

,  — the period of time between the measurement of the spectrum of reference sample 1 and reference sample 2 and the middle of-time measurement of the spectrum of the analyzed sample.

Correction for the decay of radionuclides can be factored into , where is or , i.e. as a rule when calculating the mass fraction of scandium, chromium, cobalt, iron, silver, lutetium, indium, tantalum and antimony. In this case

.

The correction factor that takes into account different shapes of analyzed samples and comparison samples, determined experimentally. Irradiate a portion of the silicon (quartz) according to mass and shape similar to the analyzed samples. This linkage should contain the impurity elements, which produce radionuclides with energies of gamma-lines in the region of 0.1−0.2 MeV, 0.4 to 0.5 MeV, and 1−1. 3 MeV. Such elements can be, for example, tungsten and tantalum, hafnium, and cobalt, etc. these elements can be introduced as additives (mass fraction 10-10%) in the silicon or quartz, crushed to a powder in an agate mortar under a layer of alcohol, or can be used in silicon, alloy of these elements. After irradiation the measured specific intensity of the respective gamma lines (pulse/min·mg) for the whole sample and of the sample (1x1 cm mass 100−200 mg) . The ratio gives the value of the correction factor for the energy of the corresponding gamma lines. Values for intermediate values of the analytical gamma lines, find using linear interpolation.

In determining the copper line annihilating radiation of Cu (511 Kev) necessary to consider the possibility of the contribution of gamma-ray lines of W (511,6 Kev) and lines annihilating radiation from radionuclides Na, Ga, and Zn. With this purpose, measure the activity of the test sample and establish the presence in the spectrum of radionuclides of tungsten, gallium, sodium and zinc. If any of these elements present in the analyzed sample, the samples of comparison data items to measure not only the intensity of the analytical gamma lines, but the intensity of the lines with an energy of 511 Kev, for tungsten 511,6 Kev.

When calculating the mass fraction of copper in the analyzed sample of silicon the number of pulses in the analytical peak of Cu () is determined by the formula

,

where is the number of pulses in gamma-ray line with an energy of 511 Kev and 511,6, due to radiation is Cu radiation and radionuclides of the elements, interference, pulse;

 — number of pulses in an analytical gamma line of the radionuclide element, interference in the spectrum of a test sample, imp (Na — 1368 Kev, Zn 1115 Kev, Ga — 834 Kev W — 686 Kev);

 — the count rate in the gamma lines 511 Kev (tungsten 511,6 Kev) in the spectrum of the reference sample pulse/min;

 — the rate of pulses in an analytical gamma line of the radionuclide element, interference in the spectrum of the reference sample, pulse/min;

 — the number of radionuclides-interference taken into consideration.

In determining India on gamma-ray lines In Kev 192 the contribution of gamma-ray lines of Fe into account similarly to that described above for copper.

The presence of detectable elements (most often sodium, copper, and scandium) in the strips of filter paper, which nakatyvaet the standard solutions, take into account according to the formula

,

where is the speed pulse counting analytical gamma line of the radionuclide of the element, due to the content of this element, dripped from the reference sample, pulse/min;

 — count rate analytical gamma line of the radionuclide of the element obtained in the measurement of the reference sample, pulse/min;

the count rate of the gamma line of the radionuclide of the element due to the presence of this element in filter paper, pulse/min.

For each of the designated impurities in the result of the analysis take the average of the two results of parallel measurements conducted by each of the individual sample in PP.3.1; 4.1; 4.2; 5.1.

5.2. The difference between the larger and the smaller of the two results of the parallel definitions should not exceed the allowable absolute values of the differences for a confidence probability of 0.90 as shown in table.2.

5.3. To check the correctness of the results of analysis of the prepared artificial mixtures (N 1−4) based on semiconductor silicon, powdered in an agate mortar to a powder, which is administered defined elements of the introduction of the previously prigotovleny standard solutions (sect.2). Powdered silica pre-check neutron-activation method on the content of all determined elements. Mass fraction of detectable elements in a powdery silicon should be not more than 20% of the content of the items introduced in Supplement form from solutions.

The mass fraction of each of the additives shall be not less than three times the value of the lower boundary of the designated contents of elements according to the method and not more than the upper boundary of the designated contents of elements.

Table 2

Powdered silicon was placed in an agate mortar, impose solutions determined elements, then under a layer of alcohol triturated with a mixture of 2.5−3 h and the mixture is dried under an infrared lamp to constant weight.

A mixture of 1: to 10.0 g of powdered silicon are added in a 0.1 cmsolutions containing sodium, lanthanum, europium, lutetium and scandium. Mass fraction of sodium in the resulting mixture is 1.0·10%, Lantana 1,0·10%, europium 2,0·10%, lutetium 2,0·10%, scandium 1,0·10%.

A mixture of 2: to 10.0 g of powdered silicon is added to 0.05 cmsolutions containing silver and chromium, 0.1 cm insolutions containing antimony and molybdenum. Mass fraction of silver in the resulting mixture is 1.0·10%, chromium of 5.0·10%, antimony of 1.0·10% molybdenum 5,0·10%.

A mixture of 3: to 10.0 g of powdered silicon is added to 0.05 cmsolutions containing cobalt and tantalum, 0.02 cmof a solution containing iron, and 0.1 cmsolutions containing arsenic and gallium. Mass fraction of cobalt in the mixture is 1.0·10%, tantalum 5,0·10%, iron of 1.0·10%, arsenic of 1.0·10%
and gallium 1,0·10%.

A mixture of 4: 10.0 g of powdered silicon is added 0.05 cmof a solution containing copper and zinc, 0.1 cmof a solution containing gold, 0,02 cmof a solution containing Nickel, and 0.1 cmof a solution containing indium. Mass fraction of copper in the resulting mixture is 1.0·10%, zinc 5,0·10%, gold 2,0·10%, tungsten 5,0·10%, Nickel of 1.0·10% India, 5.0, and·10%.

From each of the prepared mixtures selected three sample 2.0 g and analyzed PP.3.1−4.3 and sec. 5.

The time of exposure of batches of artificial formulas when defining the elements given in table.3.

Table 3

For each user-defined impurities get the result of the analysis (minus the mass fraction of element into a powdered silicon prior to the introduction of additives) as the arithmetic average of the three results of parallel measurements carried out from each sample 2.0 g of the Analysis is considered correct if found at the same value of mass fraction of impurity (%) within: tungsten 5,0·10±0,8·10, gallium is 1.0·10±0,2·10, EU-2·10±0,4·10, gold of 2.0·10±0,4·10, cobalt of 1.0·10±0,2·10, lutetium 2,0·10±0,4·10, molybdenum 5,0·10±1,0·10, sodium of 1.0·10±0,2·10, scandium 1,0·10±0,2·10, antimony of 1.0·10±0,2·10, chrome 5,0·10±1,0·10.

Allowable differences for intermediate values of mass fraction find by linear interpolation.

(Changed edition, Rev. N 1).