GOST 22025-76

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  ГОСТ 22025-76

GOST 22025−76 Alloys silicon resistive. Specifications (with Amendments No. 1, 2)

GOST 22025−76*

Group 56*
______________________

* Changed the wording, Rev. N 2.

STATE STANDARD OF THE USSR

ALLOYS OF SILICON RESISTIVE

Specifications

Resistive silicon allons. Specifications

OKP 63 9962

Date of introduction 1978−01−01

The decision of the State standards Committee of the Council of Ministers of the USSR from 1976 06.08 N 1900 the introduction of set with 01.01.78

PROVEN in 1982 by the Resolution of Gosstandart from 27.12.82 5109 N validity extended until 01.01.88**
________________
** Expiration removed by the resolution of Gosstandart of Russia from 16.04.92 N 410 (IUS N 7, 1992). — Note the manufacturer’s database.

REPLACE GOST 5.1672−72

* REPRINT August 1983, Change 1, approved in March 1983 by Decree N 5110 from 27.12.82 (IUS N 4−83).

The Change N 2 approved and put into effect by the Decree of the USSR State Committee for standards from 11.06.87 N 1988 01.01.88 with

Change No. 2 made by the manufacturer of the database in the text IUS N 9, 1987


This standard applies to resistive silicon alloys intended for manufacture by vacuum-thermal deposition of thermally stable, thin-film resistive elements and various auxiliary layers of electronic products.

1. BRAND

1.1. The resistive silicon alloys are produced by the following brands: PC-5406, PC 5402 PC-4800, PC-4400, PC-3710, PC-3001 PC-1714, PC-1004.

1.2. The chemical composition of the resistive silicon alloys shall be those specified in table.1.

Table 1

Continued

1.3. The symbol resistive silicon alloys in order and in the technical documentation should consist of the word alloy, brand (the abbreviated designation of the resistive alloy and four digits: first two digits is the nominal content of an alloying component, and the two subsequent nominal alloying content of another component) number fractions and symbols of this standard.

An example entry resistive silicon alloys:

Alloy PC-4800 FR.1 GOST 22025−76

1.1−1.3. (Changed edition, Rev. N 1).

2. TECHNICAL REQUIREMENTS

2.1. The resistive silicon alloys must be manufactured in accordance with the requirements of the present standard, using technical documentation approved in the established order.

2.2. The resistive silicon alloys produced in the form of powders dark gray or brown in color with a particle size of:

not more than 0,040 mm to fractions 1;

from 0.040 to 0,071 mm for fraction 2;

from 0,094 to 0,140 mm (only for brand PC-3710) for fraction 3.

(Changed edition, Rev. N 1).

2.3. The amount of powder resistive silicon alloys (grain size) with particle sizes beyond the limits specified in paragraph 2.2, should not exceed 5% of the mass of sample taken from middle of sample.

2.4. Powders of a resistive silicon alloys shall not contain foreign inclusions.

2.5. The expiry time of the powder resistive silicon alloy, enclosed between the upper and lower marks of the funnel (Fig.1) must not exceed:

60 — for a fraction 1;

35 — for a fraction of 2;

30 for faction 3.

Damn.1. Funnel to define the expiration time of the powders resistive silicon alloys

Funnel to define the expiration time of the powders resistive silicon alloys

Damn.1

The expiry time of the powder brand PC-4800 1st fraction should not exceed 50 C.

The expiry time of the alloy powder of the brand PC-1714 is not installed.

(Changed edition, Rev. N 1).

2.6. Powder resistive silicon alloy brand PC-1714 must be wet ethyl alcohol according to GOST 18300−72*, forming a homogeneous suspension.
_______________
* On the territory of the Russian Federation GOST 18300−87, here and hereafter. — Note the manufacturer’s database.

2.7. Data on the physical and electrical parameters of the resistive silicon alloys in the bulk state and in the form of a film in the reference Appendix 1.

2.8. The scope and methods of applying resistive silicon alloys are given in recommended Appendix 2.

3. ACCEPTANCE RULES

3.1. The resistive silicon alloys present to the acceptance of the parties. The party includes an alloy of the same brand, obtained from one or more process cycles in a single technological regime.

The weight of the batch should not exceed 10 kg.

3.2. Each batch of resistive silicon alloys subjected to acceptance tests to verify compliance of the chemical composition, flowability and wettability with the requirements of this standard.

The silicon content is determined only in case of changes in the technological process of their production. In other cases, the silicon content is determined as the difference between 100% of the chemical composition of the alloy and the sum of the content of other monitored components of the alloy, expressed as a percentage.

The particle sizes determined by sampling from one of five parties.

The test alloys on the content of impurities is carried out at the request of the consumer.

3.3. All tests resistive silicon alloys is carried out at an average sample from each batch.

3.4. If unsatisfactory results at least in one of the figures conducted a re-test new samples taken from the same batch of alloy. The results of repeated tests are final and apply to the entire party.

4. TEST METHODS

4.1. Sampling method

4.1.1. An average sample taken in the box, eliminating contamination and powder loss.

4.1.2. The entire batch of powder was poured into a square baking pan of stainless steel, which is pre-lined with polyethylene film according to GOST 10354−82, washed with distilled water by the GOST 6709−72 and pureed ethyl alcohol according to GOST 18300−72.

The mixed powder method «ring cone» chrome steel spatula and spread over the surface of the pan evenly, then divide into 25 equal squares and select the powder across the layer thickness from 13 squares in a checkerboard pattern of approximately equal portions.

The weight of the selected powder should be not less than 110 g.

Out of a sample of powder prepared in the following sample: 50 g to verify the granulometric composition, 20 g to determine the expiry time of the powder, two approximately equal mass samples from the remaining parts of powder — one for chemical analysis, another for storage during the warranty period in the event the arbitration is to test if there is disagreement in assessing the quality of the powder.

All samples fall asleep in double bags made of polyethylene film, previously wiped with ethanol. The last two samples brewed by a sealed seam.

(Changed edition, Rev. N 1, 2).

4.1.3. Between the inner and outer packages put the label where you indicate:

room of the shop of the manufacturer;

the name of the alloy;

the batch number and the sample;

the particle size of the powder;

sample mass;

date of sampling (month, year).

4.2. Determination of granulometric composition

The test is performed on the test sieve with metal wire mesh stainless steel 0040К for fraction 1, 0040К and 0071К for fraction 2 (according to normative-technical documentation approved in the established order) and 009К (GOST 6613−86) and 014К for fraction 3, installed on vibrostability (oscillation frequency 1500−3000 oscillations per minute, the vibration amplitude of 0.1−0.2 cm).

A portion of the powder with a mass of (50±0,1) g sieved for 20 min through a sieve with a mesh 0040К for alloys 1st faction or through a set of sieves with meshes 0040К and 0071К, 009К and 014К for alloys of fraction 2 and 3, respectively.

The amount of powder remaining on the sieve 0040К for the alloy fraction 1, or the total amount of powder remaining on the sieve 0071К and passed through a sieve with a mesh 0040К for alloys of fraction 2, and remaining on the sieve 014К and passed through a sieve with a mesh 009К for alloys of fraction 3, should not exceed 2.5 g.

The weighing error must not exceed 0.1 g.

(Changed edition, Rev. N 1, 2).

4.3. Determination of content of impurities

The contents of impurities in silicon alloys checked visually with the naked eye and with a microscope MBS-1, with shestnadcatiletnim increase.

4.4. The timing of the expiration of powder

4.4.1. Equipment materials:

vacuum drying oven HS-0,035;

funnel made of molybdenum glass brand С49−2 (see the devil.1);

tripod laboratory SHL;

stopwatch SDPR-1B-2 according to GOST 5072−79;

acetone according to GOST 2603−79, h;

glass IN-1−100ТС according to GOST 25336−82;

fabric cotton, art.324 according to GOST 7138−83.

(Changed edition, Rev. N 1, 2).

4.4.2. Preparing for the test

Funnel and the glass is pre-washed with acetone and wiped with a clean cloth.

Set the funnel in the tripod in a vertical position on a plumb, put it under glass. Distance from the funnel to the glass should not exceed 30 mm.

4.4.3. Testing

The powder from the package pour into the funnel above the upper mark and see stopwatch moments of passage of the powder surface of the upper and lower marks. Timing repeat at least five times. The measurement result should be the arithmetic mean of the measurement results.

Jet poured the powder needs to be continuous. It is not allowed to tap on the funnel at the time of testing.

4.5. The determination of chrome surround personifitsirovano method in the alloys of PC-5406, PC 5402 PC-4800, PC-4400, PC-3710 or PC-3001

4.5.1. The essence of the method

The method is based on the oxidation of chromium neccersarily ammonium sulfate in the environment prior to the dichromate ion in presence of silver nitrate. The dichromate-ion titrated with Mora salt phenylanthranilic acid as indicator.

The relative error of the measurement result must be not more than 0.5%.

4.5, 4.5.1. (Changed edition, Rev. N 1).

4.5.2. Reagents, materials:

Cup PL 118−4 according to GOST 6563−75;

cover the type of «hour glass» PTFE-4 according to GOST 10007−80;

ammonium neccersarily according to GOST 20478−75, H. h;

distilled water GOST 6709−72;

potassium dichromate, standard titer of 0.1 n. solution;

nitric acid GOST 4461−77, H. h;

sulfuric acid GOST 4204−77, H. h;

hydrofluoric acid according to GOST 10484−78, H. h;

manganese (II) sulfate 5-water according to GOST 435−77, h. e. a., A 0.4% solution;

sodium carbonate 10-water according to GOST 84−76, H. h;

sodium chloride according to GOST 4233−77, H. h, 5% solution;

silver nitrate according to GOST 1277−75, H. C., 1% solution;

salt of protoxide of iron and ammonium double sulfate (salt Mora) according to GOST 4208−72, H. h, 0,1 n. solution; prepared as follows: 40 g of Mohr salt dissolved in 200 ml of water, acidified with 30 ml of sulfuric acid, and dilute with water to volume 1000 ml. Normality of this solution was set to 0.1 n solution of potassium dichromate on the day of the titration sample;

acid N-phenylanthranilic, h. e. a., A 0.2% solution; prepared as follows: 0.2 g of N-phenylanthranilic acid are dissolved under moderate heating in 30−40 ml water containing 0.6 g of sodium carbonate, dilute with water to 100 ml Store in a dark bottle or dark place.

(Changed edition, Rev. N 1, 2).

4.5.3. Testing

0.1 g of the analyzed alloy is weighed with an accuracy of at least 0.0001 g and placed in a platinum Cup. Add 2 ml of distilled water, 5 ml of hydrofluoric acid, cover with a Teflon Cup and cover, occasionally lifting the lid, dropwise adding nitric acid to dissolve the alloy.

After the dissolution of the cap is washed with distilled water, carefully add 10 ml of sulfuric acid and evaporate the solution until copious fumes of sulphuric anhydride. The contents of the Cup is cooled, transferred to a conical flask with a capacity of 250 ml and diluted with distilled water to volume of 100 ml.

Add to the flask 1 ml of a solution of manganese sulfate, 5 ml of a solution of silver nitrate, 5 g naternicola ammonia and heat the solution to boiling. Heating was continued until the termination of allocation of small bubbles of oxygen, i.e., before the complete decomposition of ammonium naternicola. Oxidation of chromium is complete when there is a stable red-purple color of the permanganate-Jona. If this color is absent, carefully add several portions (weighing about 0.5 g) naternicola ammonium and heated until the coloring and the termination of allocation of bubbles of oxygen. Add about 10 ml of sodium chloride solution until the disappearance of the permanganate color-Yonah and leave on the warm stove to enlightenment yellow solution. The solution is cooled, add five or six drops of N-phenylanthranilic acid and titrated with a solution of salt Mora before moving dirty brown through red-purple to green.

4.5.4. Processing of the results

The chromium content in percent is calculated by the formula

,

where the caption is exactly 0.1 N. solution of salt Mora on the chrome, 0,001733 g/ml;

 — the volume of salt solution Mora, used for titration, ml;

 — the mass of the sample analyzed alloy,

For each sample spend at least two parallel definitions.

4.6. Determination of Nickel by the gravimetric method

4.6.1. The essence of the method

Nickel is precipitated from the ammonia solution in the presence of citric acid dimethylglyoxime, filtered through a glass crucible with a filter bottom, dried and weighed in the form of dimethylglyoximato Nickel. The relative error of the determination should not be more than 1%.

4.6.2. Apparatus, reagents and solutions:

the crucible TF-10-PORT-10 XC GOST 25336−82;

ammonia water according to GOST 3760−79, H. h;

distilled water GOST 6709−72;

dimethylglyoxime according to GOST 5828−77, h. e. a., 1% alcoholic solution;

nitric acid GOST 4461−77, H. h;

citric acid according to GOST 3652−69, H. h., 25% solution;

sulfuric acid GOST 4204−77, H. h;

hydrofluoric acid according to GOST 10484−78, H. h;

rectified ethyl alcohol technical, highest grade according to GOST 18300−72;

Cup PL 118−4 according to GOST 6563−75;

cover the type of «hour glass» PTFE-4 according to GOST 10007−80.

(Changed edition, Rev. N 1, 2).

4.6.3. Testing

A sample of alloy weighing about 0.25 g weighed with an accuracy of at least 0.0001 g and placed in a platinum Cup. Added 0.5 ml of distilled water, 5 ml of hydrofluoric acid, cover with a Teflon Cup with a lid and periodically, dropwise adding nitric acid to dissolve the alloy. Wash the cover with water, add 5 ml of sulfuric acid, mix thoroughly and evaporate the solution to release dense fumes of sulphuric anhydride. The solution was cooled, transferred to a beaker with a capacity of 300 ml, add 30 ml of citric acid solution, heated to a temperature of 40−45 °C, add 25 ml of a solution dimethylglyoxime and ammonia to a faint smell.

Solution and the precipitate is heated to a temperature of 60−70 °C, incubated at this temperature for 30 min and filtered through previously dried and weighed crucible with a filter bottom 3. Precipitate was washed 10−12 times with hot water and dried at a temperature of 110−115 °C to constant weight.

4.6.4. Processing of the results

The Nickel content in percent is calculated by the formula

,

where is the mass of sediment dimethylglyoximate Nickel, g;

 — the weight of the portion of the sample, g;

0,2032 — conversion factor dimethylglyoximate of Nickel on Nickel.

For each sample spend at least two parallel definitions.

4.7. Determination of the iron content photometric method in the alloy brands PC-3001 PC-5402

4.7.1. The essence of the method

The method is extended to resistive silicon alloys containing iron up to 3%.

Iron is determined by the photometric method sulfosalicylic acid after preliminary oxidation of chromium by hydrogen peroxide in ammoniacal medium and the separation of ferric hydroxide. The relative error of the determination should not be more than 2.5%.

4.7.2. Equipment and reagents:

spectrophotometer type SF-16 or the photoelectric colorimeter of the type FEK-60; allowed to use spectrophotometers and photoelectrocolorimetry other similar stamps;

ammonia water according to GOST 3760−79, H. h;

ammonium chloride according to GOST 3773−72, H. C., 20% solution;

distilled water GOST 6709−72;

hydrogen peroxide according to GOST 10929−76;

radio engineering carbonyl iron according to GOST 13610−79;

nitric acid GOST 4461−77, H. h;

sulfuric acid GOST 4204−77, H. h;

hydrochloric acid by the GOST 3118−77, H. h, the solution was diluted 1:1;

sulfosalicylic acid according to GOST 4478−78, C., 20% solution;

hydrofluoric acid according to GOST 10484−78, H. h;

methyl red h. e. a., A 0.2% aqueous-alcohol solution;

iron standard solution 10 µg/ml, prepared with a backup solution, containing 1 mg/ml, diluted 100 times;

stock solution; prepare by dissolving 1 g of iron containing 99.9% of iron, when heated in hydrochloric acid. The resulting solution was transferred to a volumetric flask with a capacity of 1000 ml and add water until full. The resulting solution contains 1 mg/ml iron;

Cup PL 118−4 according to GOST 6563−75;

filter obezdolennyh «Red tape»;

cover the type of «hour glass» PTFE-4 according to GOST 10007−80.

(Changed edition, Rev. N 1, 2).

4.7.3. Testing

A sample of alloy weighing about 0.1 g is weighed with an accuracy of at least 0.0001 g and placed in a platinum Cup, add 2 ml of distilled water, 5 ml of hydrofluoric acid, PTFE cover with a lid and gently, drop by drop, add nitric acid until complete dissolution of the alloy. The cover is removed, washed with distilled water, pour 7−10 ml of concentrated sulphuric acid and evaporated until the appearance of fumes of sulphuric anhydride. The Cup is cooled, washed wall with water and again evaporated until the appearance of fumes of sulphuric anhydride. The contents of the Cup washed with water in a glass with a capacity of 300 ml, add 5 ml of hydrochloric acid, 15−20 ml of hydrogen peroxide, two or three drops of methyl red and 20−30 ml of a solution of ammonia portions with thorough stirring, heated to coagulate the precipitate of iron hydroxide and filtered through the filter «red ribbon». The precipitate is washed five or six times a hot solution of ammonium chloride containing a drop or two of ammonia in 1000 ml of solution. The washed pellet was dissolved in 10 ml of hydrochloric acid, transfer the solution into a measuring flask with volume capacity of 100 ml and adjusted to full volume with water.

Aliquot part of the solution volume of 1−10 ml, containing 15−40 µg of iron, taken in a volumetric flask with a capacity of 50 ml, add 5 ml of sulfosalicylic acid, a few drops of ammonia solution until yellow color of the solution and, in excess, 5 ml of ammonia was adjusted with water to volume, and mix.

Measure the optical density of the solution on the spectrophotometer at a wavelength of 420−450 nm or colorimeter with filter No. 3 in a cuvette with a thickness of the light absorbing layer 30 mm relative to the solution containing no iron (the zero solution). Concurrently with the tests are blank.

The content of iron in 50 ml of a solution determine from the calibration graph.

4.7.4. Construction of calibration curve

The calibration curve constructed in the coordinates: y-axis — optical density of the solution, corrected for blank, the abscissa shows the amount of iron in micrograms in 50 ml solution.

In a volumetric flask with a capacity of 50ml each placed conducted through all stages of the analysis 0,0; 0,5; 1,0; 1,5; 2,0; 3,0; 4,0; 5,0 ml of standard solution containing respectively 0; 5; 10; 15; 20; 30; 40; 50 mcg of iron.

Add 5 ml of sulfosalicylic acid solution, a few drops of ammonia solution until yellow color of the solution and, in excess, 5 ml of ammonia. Top up with water until full and stir.

Optical density of the solution is measured relative to the zero of the solution on the spectrophotometer at a wavelength of 430 nm or photoelectrocolorimeter with a filter having a maximum transmittance in the region of 420−450 nm in a cuvette with a thickness of the light absorbing layer 30 mm.

4.7.5. Processing of the results

The iron content in percent is calculated by the formula

,

where  — the amount of iron found from the calibration graph, µg/50 ml;

 — the weight of the portion of the sample corresponding to the sample,

4.8. Determination of iron content in the alloy grade PC-1004 photometric method

4.8.1. The essence of the method

Iron is determined by the photometric method sulfosalicylic acid in ammonia environment without separating it from the Nickel. The relative error of determination must be no more than 2.5%.

4.8.2. Apparatus, reagents and solutions:

spectrophotometer type SF-16 or the photoelectric colorimeter of the type FEK-60; allowed to use spectrophotometers or photoelectrocolorimetry other similar stamps;

ammonia water according to GOST 3760−79, H. h;

distilled water GOST 6709−72;

radio engineering carbonyl iron according to GOST 13610−79;

nitric acid GOST 4461−77, H. h;

sulfuric acid GOST 4204−77, H. h;

sulfosalicylic acid according to GOST 4478−78, C., 20% solution;

hydrofluoric acid according to GOST 10484−78, H. h;

Nickel chloride according to GOST 4038−79, H. C., a solution containing 0.016 mg/ml;

iron standard solution 10 µg/ml; prepared with a backup solution, containing 1 mg/ml, diluted 100 times;

stock solution; prepare by dissolving 1 g of iron containing 99.9% of iron in hydrochloric acid when heated. The resulting solution was transferred to a volumetric flask with a capacity of 1000 ml and adjusted to full volume with water. The resulting solution contains 1 mg/ml of iron.

(Changed edition, Rev. N 1).

4.8.3. Testing

A sample of alloy weighing about 0.1 g is weighed with an accuracy of at least 0.0001 g and placed in a platinum Cup. Add 2 ml of distilled water, 5 ml of hydrofluoric acid, cover with a lid and cautiously add drop by drop nitric acid until complete dissolution of the alloy. Wash the lid with distilled water, pour 3−5 ml of sulfuric acid and evaporated to fumes of sulphuric anhydride. The Cup is cooled, washed wall with water and again evaporated in a volumetric flask with a capacity of 100 ml and adjusted to full volume with water.

1−10 ml aliquote parts of a solution containing 10−40 mg of iron, taken in a volumetric flask with a capacity of 50 ml, add 5 ml of sulfosalicylic acid, a few drops of ammonia solution until yellow color and, in excess, 5 ml of ammonia adjusted to full volume with water and mix.

Optical density of the solution measured on a spectrophotometer at a wavelength of 420−450 nm or colorimeter with filter No. 3 in a cuvette with a thickness of the light absorbing layer 30 mm relative to the zero solution.

Simultaneously with the test spend idle experience with all the applied reagents.

The amount of iron determined from the calibration graph.

4.8.4. Construction of calibration curve

The calibration curve constructed in the coordinates: y-axis — optical density of the solution, corrected for blank, the abscissa shows the amount of iron in micrograms in 50 ml solution.

In a volumetric flask with a capacity of 50ml each placed conducted through all stages of the analysis 0,0; 0,5; 1,0; 1,5; 2,0; 3,0; 4,0; 5,0 ml of standard solution containing respectively 0,5; 10; 15; 20; 30; 40; 50 mcg of iron.

Add 5 ml of a solution of Nickel chloride, 5 ml of sulfosalicylic acid, a few drops of ammonia solution until yellow color of the solution and an excess of 5 ml of ammonia. Topped up to full volume with water and mix.

Optical density of the solution is measured relative to the zero of the solution on the spectrophotometer at a wavelength of 430 nm or photoelectrocolorimeter with a filter having a maximum transmittance in the region of 420−450 nm in a cuvette with a thickness of the light absorbing layer 30 mm.

4.8.5. Processing of the results

The iron content in percent is calculated by the formula

,

where  — the amount of iron found from the calibration graph, µg/ml;

 — the weight of the portion of the sample corresponding to the sample,

4.9. Determination of chromium, iron and tungsten in the alloy brand PC-1714 x-ray method

4.9.1. The essence of the method

The method is based on a linear relationship of the intensities of fluorescent x-rays from the mass concentration of the analyzed element in the sample. X-ray fluorescence spectrometer to determine the intensity of the fluorescent radiation of the analyzed and standard samples for analytical lines of chromium, iron and tungsten. Comparing the intensity for each of the identified elements, calculate their percentage in the analyzed sample.

The coefficient of variation of measurements of the alloy composition does not exceed 10% to chromium, 8% iron, 6% tungsten.

4.9.2. Equipment

For the test use one of the following devices:

fluorescent x-ray quantometer types of FRK-1B and CRF-11;

the x-ray apparatus of the type CRF-18;

x-ray fluorescence spectrometer of the company «Elliot», model XZ-1030 supplied with a spare x-ray tube with a tungsten anode manufacturing company «MAHLE».

4.9.3. Testing

A sample of alloy weighing not less than 16 g divide into four equal parts and placed in four cuvettes.

As a standard sample take the same alloy, were analyzed by chemical analysis. The chemical composition of the standard sample should not differ from the analyzed for each of the elements is more than 15%. Sample standard sample weighing not less than 20 g was placed in two cuvettes.

On the x-ray spectrometer to determine the intensity of fluorescence of two cuvettes with a standard sample and four cuvette with the analyzed sample.

The fluorescence intensity measured on the analytical lines, CrK, FeK, WK.

4.9.4. Processing of the results

Depending on the fluorescence intensity for each of two cuvettes with a standard sample and four cuvettes with analysable sample calculate the contents of the element in percent by the formula

,

where  — the contents of the analyzed element in the standard sample, %;

, the intensity of fluorescence from the analyzed and standard samples, respectively, imp.

For each defined element get eight concentrations. The average of these eight values gives the desired concentration of the element in the analyzed sample.

4.10. The determination of chrome surround personifitsirovano method in alloy grade PC-1714

4.10.1. The essence of the method

The method is based on the oxidation of chromium neccersarily ammonium sulfate in the environment prior to the dichromate ion in presence of silver nitrate. The dichromate-ion titrated with Mora salt -phenylanthranilic acid as indicator.

The relative error of the determination should be not more than 1%.

(Changed edition, Rev. N 1).

4.10.2. Materials, reagents:

Cup PL 118−4 according to GOST 6563−75;

ammonium neccersarily according to GOST 20478−75, H. h;

distilled water GOST 6709−72;

potassium dichromate, standard titer of 0.1 n. solution;

nitric acid GOST 4461−77, H. h;

boric acid according to GOST 9656−75, H. h, 5% solution;

sulfuric acid GOST 4204−77, H. h., diluted 1:1;

hydrofluoric acid according to GOST 10484−78, H. h;

acid N-phenylanthranilic, h. e. a., A 0.1% solution, prepared according to GOST 4919.1−77;

manganese sulfate according to GOST 435−77, h. e. a., A 0.4% solution;

sodium chloride according to GOST 4233−77, H. h, 5% solution;

silver nitrate according to GOST 1277−75, H. C., 1% solution;

salt of protoxide of iron and ammonium double sulfate (salt Mora) according to GOST 4208−72, H. C., of 0.05 n solution; prepared as follows: 20 g of Mohr salt dissolved in 500 ml of water containing 100 ml of sulfuric acid, the solution diluted with water to a volume of 1000 ml and filtered. Store in a flask with a glass stopper. The normality of the solution set on the day of consumption of 0.1 n solution of potassium dichromate in the following way: 10 ml of a solution of potassium dichromate is placed in a conical flask with a capacity of 250 ml, pour 8 ml of sulfuric acid, 4 ml of phosphoric acid, water to a volume of 150 ml, three drops of a solution of N-phenylanthranilic acid, stirred and titrated with a solution of salt Mora to the disappearance of the purple coloration of the indicator.

The coefficient of normality of salt solution Mora is calculated by the formula

,

where is the normality of a solution of potassium dichromate;

 — the volume of salt solution Mora, used for titration, ml;

 — the volume of potassium dichromate solution taken for titration, ml.

(Changed edition, Rev. N 1, 2).

4.10.3. Testing

A sample of alloy weighing about 0.1 g is weighed with an accuracy of more than 0.0001 g, placed in a platinum Cup, moisten with 2 ml of water, add 2−3 ml of hydrofluoric acid, mix and leave for 15−20 min at room temperature. Pour small portions of 1 ml of nitric acid and continue the dissolution of alloy with moderate heating. The solution was evaporated to a volume of about 2 ml. Wash the walls of the Cup with water, the solution was stirred and evaporated again to volume of 2 ml. the Treatment with water is repeated. The solution in the Cup is diluted with water and transferred to a conical flask with a capacity of 250 ml Add water to volume of 100 ml, 10 ml boric acid solution, 10 ml of sulfuric acid, 1 ml of a solution of manganese sulfate, 5 ml of a solution of silver nitrate, 5 g naternicola ammonia and heat the solution nearly to boiling. Heating was continued until the termination of allocation of small bubbles of oxygen, i.e., before the complete decomposition of ammonium naternicola. Oxidation of chromium is complete when appears stable red-purple color of the permanganate-Jona. If this color is absent, carefully add several portions (weighing about 0.5 g) naternicola ammonium and heated until the appearance of red-violet color and the termination of allocation of bubbles of oxygen.

Pour about 10 ml of sodium chloride solution until the disappearance of the permanganate color-Yonah and leave on warm stove until the enlightenment of the solution. The solution is cooled, add five or six drops of a solution of N-phenylanthranilic acid and titrated with a solution of salt Mora before moving brown color of the solution green.

4.10.4. Processing of the results

The chromium content in percent is calculated by the formula

,

where the caption is exactly 0,05 n solution of salt Mora on the chrome, 0,000867 g/ml;

 — coefficient of normality of salt solution Mora;

 — the volume of salt solution Mora, used for titration, ml;

 — the weight of the portion of alloy,

4.11. The determination of iron in alloy grade PC-1714

4.11.1. The essence of the method

The method is based on complexometrically titrate iron at pH 2−3 with sulfosalicylic acid as indicator. Iron pre-separated from the tungsten and chromium by precipitation in hydroxide sodium hydroxide in the presence of hydrogen peroxide.

The relative error of determination must be no more than 1.5%.

(Changed edition, Rev. N 1).

4.11.2. Materials, reagents:

Cup PL 118−4 according to GOST 6563−75;

filter obezdolennyh «red tape»;

ammonia water according to GOST 3760−79, H. h., 25% solution;

ammonium acetate according to GOST 3117−78, H. h;

ammonium chloride according to GOST 3773−72, H. h;

buffer solution pH 9,5−10; prepared as follows: 54 g of ammonium chloride dissolved in 200 ml of deionized water, add 350 ml ammonia solution and dilute with water to volume of 1000 ml;

deionized water grade B;

distilled water GOST 6709−72;

hydrogen peroxide according to GOST 10929−76;

potassium chloride according to GOST 4234−77, H. h;

nitric acid GOST 4461−77, H. h, concentrated and diluted 1:1;

sulfuric acid GOST 4204−77, H. h;

hydrochloric acid by the GOST 3118−77, H. h;

sulfosalicylic acid according to GOST 4478−78, H. h, 10% solution;

hydrofluoric acid according to GOST 10484−78, H. h;

sodium hydroxide according to GOST 4328−77, H. h., 25% solution;

Trilon B (Ethylenediamine-N, N, N, N'-tetraoxane acid disodium salt) according to GOST 10652−73, h. e. a., 0.025 M solution. Prepared as follows: 9.3 g of drug is dissolved in deionized water and dilute the solution with water to volume 1000 ml the Molarity of the solution Trilon B is determined by solution of zinc chloride in the following manner: 20 ml of a solution of zinc chloride is placed in a conical flask with a capacity of 250 ml, pour 15 ml of buffer solution, deionized water to a volume of 100 ml, 0.05−0.1 g of indicator mix of black eriochrome and titrated with a solution of Trilon B before the transition red-purple color of the solution blue. The coefficient of polarity of the solution Trilon B is calculated by the formula

,

where is the molarity of a solution of zinc chloride;

 — the volume of solution of zinc chloride taken for titration, ml;

 — volume of solution Trilon B, used for titration, ml;

zinc metal CV-00 GOST 3640−79*,
______________
* On the territory of the Russian Federation GOST 3640−94. — Note the manufacturer’s database.

zinc chloride, 0.025 M solution. Prepared as follows: 1,6345 g of zinc metal was dissolved in 25 ml of hydrochloric acid diluted 1:1, the solution is diluted with deionized water in a volumetric flask with a capacity of 1000 ml;

eriochrome black T, C. D. A., flat the mixture with potassium chloride 1:100.

(Changed edition, Rev. N 1, 2).

4.11.3. Testing

A portion of the alloy with a mass of 0.1−0.15 g, weighed with accuracy of more than 0.0001 g, placed in a platinum Cup, moistened with 1−2 ml of water, pour 2−3 ml of hydrofluoric acid, mix and leave for 15−20 min at room temperature. Added portions, while stirring with 5 ml nitric acid and heated until complete dissolution of the alloy. The solution was evaporated to moist residue. Pour 5 ml of nitric acid and again evaporated to moist residue. The last operation is repeated. To the residue poured 5 ml of the diluted 1:1 nitric acid and the contents of the Cup was transferred to a beaker with a capacity of 300−400 ml of washing a Cup of water. Adhering to the Petri dish the precipitate is dissolved with a few drops of ammonia and wash off with water in the same Cup. The solution is diluted with water to a volume of about 80 ml, pour 20−30 ml of perhydrol and the solution of sodium hydroxide until the precipitation of iron hydroxide. Pour 10−15 ml of sodium hydroxide solution and heated to coagulate the precipitate. Solution and the precipitate was filtered through a medium density filter «red ribbon», washed with hot water.

The precipitate is dissolved on the filter with 15−20 ml of hot dilute 1:1 hydrochloric acid. The filter carefully washed with hot water. The solution collected in the conical flask with a capacity of 250 ml.

To the hot solution add five drops of sulfosalicylic acid solution and ammonium acetate to pH 2−3 and titrated with a solution of Trilon B to switch the purple colour is straw-yellow. Add a small portion of acetate of ammonium. If there is the appearance of pink color, continue the titration to a straw-yellow color of the solution.

In the case of incomplete separation of chromium observed the transition of color from purple to greenish.

(Changed edition, Rev. N 1).

4.11.4. Processing of the results

The iron content in percent is calculated by the formula

,

where the caption is exactly 0.025 M solution of Trilon B at gland, 0,001396 g/ml;

 — the ratio of the molarity of the solution Trilon B;

 — volume of solution Trilon B, used for titration, ml;

 — the weight of the portion of alloy,

4.12. Determination of tungsten in alloy PC-1714 gravimetric method

4.12.1. The essence of the method

The method is based on the deposition of tungsten -nattokinaise at pH 1−6 after separation of the silicon, chromium and iron.

The coefficient of variation should not be more than 1%.

4.12.2. Materials, reagents:

scales laboratory analytical type of VLA-200g-M;

Cup PL 118−4 according to GOST 6563−75;

cover PL 101−7 according to GOST 6563−75;

the crucible PL 100−7 according to GOST 6563−75;

muffle furnace MP-2УМ. Allowed to use any muffle furnace with temperature up to 900 °C;

obezdolennyh filter «white ribbon»;

filter obezdolennyh «blue ribbon»;

distilled water GOST 6709−72;

potassium, anhydrous sodium carbonate according to GOST 4332−76, H. C., 1% solution;

nitric acid GOST 4461−77, H. h, concentrated, diluted 1:1 and 2% solution by volume;

hydrochloric acid by the GOST 3118−77, H. h;

hydrofluoric acid according to GOST 10484−78, H. h;

methyl orange h. d. a., A 0.1% aqueous solution; prepared according to GOST 4919.1−77;

-naftohinon, h. e. a., 2% solution in 2% by volume hydrochloric acid;

ammonia water according to GOST 3760−79, H. h., 25% solution.

(Changed edition, Rev. N 1, 2).

4.12.3. Testing

A sample of alloy weighing about 0.5 g, weighed with accuracy of more than 0.0001 g, placed in a platinum Cup, moisten with 2 ml of water, add 5 ml of hydrofluoric acid and leave it for 15−20 min at room temperature. Add 5 ml of nitric acid and continue the dissolution of alloy with moderate heating. The solution was evaporated to wet salts, pour 5 ml of nitric acid and again evaporated to moist salts. The last operation is repeated twice.

Pour 30−50 ml diluted 1:1 nitric acid and heat the contents of the Cup was transferred to a beaker with a capacity of 250 ml. Adhering to the Petri dish the precipitate is dissolved with a few drops of ammonia and wash off with water in the same Cup. The solution was boiled for 15−20 min. complete dissolution of salts and coagulation of the precipitate tungsten acid. The precipitate was filtered off on the filter «blue ribbon» with a small amount of filter mass. The precipitate is quantitatively transferred to the filter with the pieces obessilennaya filter, washed with 2% by volume solution of nitric acid and twice with water.

The filter with precipitate was placed in a platinum crucible, incinerated and lightly calcined in a muffle furnace at a temperature of 600−650 °C. the crucible with the precipitate of tungsten trioxide added 3 g potassium carbonate-sodium, cover the crucible with lid and fused in a muffle furnace at a temperature of 800−850 °C.

The cooled crucible was placed in a beaker with a capacity of 250 ml, pour 100 ml of hot water and boil until complete decomposition of water. The crucible is washed with hot water and removed from the glass. Solution and the precipitate was filtered through filter «white ribbon». The beaker and the filter washed with hot solution of carbonate of potassium-sodium. The filtrate and the wash solution collected in a beaker with a capacity of 400 ml, neutralized with hydrochloric acid methyl orange, cooled and added with constant stirring, 70 ml of a solution of nattokinaise. Stand at least 10 h. the Precipitate was filtered off on a tight filter «blue ribbon», washed with cold 0.5 percent sodium -nattokinaise in 1% strength by volume hydrochloric acid.

The filter with precipitate was placed in a calcined and weighed platinum crucible, carefully incinerated and calcined in a muffle furnace at a temperature of 600−650 °C to constant weight. After cooling, weigh the residue obtained tungsten trioxide.

4.12.4. Processing of the results

The tungsten content in mass percent is calculated by the formula

,

where 0,793 — the conversion factor from the mass of tungsten trioxide on the weight of the tungsten;

 — the mass of the crucible with the precipitate of tungsten trioxide, g;

 — weight of empty crucible, g;

 — the weight of the portion of the material,

4.12.3, 4.12.4. (Changed edition, Rev. N 1).

4.13. Determination of silicon content

4.13.1. The essence of the method

Silicon is determined in the form of silicon dioxide, selected after fusing the sample with sodium hydroxide, decomposition with water and evaporating the solution with sulphuric acid. The relative error of the determination should not be more than 0.5%.

4.13.2. Apparatus, reagents and solutions:

the crucible PL 100−7 according to GOST 6563−75;

crucible with lid with a capacity of 50 ml of Nickel of any brand according to GOST 6235−73*;
______________
* On the territory of the Russian Federation GOST 6235−91. — Note the manufacturer’s database.

distilled water GOST 6709−72;

sodium hydroxide according to GOST 4328−77, H. h;

sulfuric acid GOST 4204−77, H. h;

hydrochloric acid by the GOST 3118−77, H. h, a solution of 1:10;

hydrofluoric acid according to GOST 10484−78, H. h;

filter obezdolennyh red ribbon.

(Changed edition, Rev. N 1).

4.13.3. Testing

A sample of alloy weighing 0.2 g is weighed with an accuracy of at least 0.0001 g and placed in a Nickel crucible. Add a 1.5−2.0 g sodium hydroxide. The crucible closed with a lid, put in a cold muffle furnace, gradually raising the temperature to 500 °C and held at this temperature for 10 min.

Crucible is not open before the end of the process of malting. After fusing, the crucible is cooled, the melt leached with 100 ml of cold water in a glass with a capacity of 300 ml.

In a glass add 5 ml of hydrochloric acid and heated to dissolve the precipitate, then add 15 ml of sulfuric acid and evaporate the solution until the appearance of fumes of sulphuric anhydride. The glass is cooled, poured 100 ml of hot water containing 10 ml concentrated hydrochloric acid, heat the solution to dissolve the salts, not allowing to boil, and filtered through the filter «red ribbon». The precipitate of silicic acid on the filter is washed five or six times a hot solution of hydrochloric acid and eight to ten times with hot water.

The filtrate was evaporated until the appearance of fumes of sulphuric anhydride and secondarily emit silicic acid, as described above, filtering through a new filter.

Both the filter and the precipitate of silicic acid is placed in a platinum crucible, carefully incinerated and calcined for 1−2 hours at 1000−1200 °C to constant weight.

The calcined precipitate is moistened with two or three drops of water, add two or three drops of sulphuric acid and 2−3 ml of hydrofluoric acid. Cautiously evaporate the solution to dryness and again calcined to constant weight.

4.13.4. Processing of the results

The silicon content in percent is calculated by the formula

,

where is the mass of the crucible with the sediment before treatment with hydrofluoric acid, g;

 — weight of crucible with residue after treatment with hydrofluoric acid, g;

0,4672 — the ratio of silicon dioxide on silicon;

 — the mass of the sample analyzed alloy,

4.14. The determination of nitrogen, hydrogen and oxygen

4.14.1. The essence of the method

The analyzed material is melted in a quartz furnace with induction heating of a graphite crucible in a high vacuum with the use of an iron-Nickel-tin «baths». The oxygen dissolved in the metal and in the form of oxides, is bound into carbon monoxide and hydrogen and nitrogen are removed from the metal in the molecular state.

The entire extracted gas sample is pumped mercury diffusion pump and analyzed.

The sensitivity of the method was 1·10% by weight. The relative error of the determination should not be more than 20%.

4.14.2. Apparatus, materials and reagents:

the plant «Giredmet-911М1», you can use melograf VH-8 of the company «Heraeus»;

argon gaseous and liquid GOST 10157−79;

crucibles of graphite OS.h. 7−4;

benzene according to GOST 5955−75, h. d. a.;

Nickel tube with a diameter of 2.5−3.0 mm with a wall thickness of 0.05 mm;

carbon tool steel U12A type, a rod with a diameter of 6−12 mm according to GOST 1435−74*;
_______________
* On the territory of the Russian Federation GOST 1435−99. — Note the manufacturer’s database.

tin granulated on the other 6−09−2704−78, h;

the technical rectified ethyl alcohol according to GOST 18300−72, the highest grade.

(Changed edition, Rev. N 1, 2).

4.14.3. Preparing for the test

The analyzed alloy with a mass of 0.02−0.03 g was placed in a thin-walled sleeve length 10−11 mm, made of Nickel tube.

The casings used for the analysis, pre-calcined in a vacuum at a temperature of 1100°-1200 °C for 2−3 h.

In the installation load cases with samples analyzed before samples are placed «iron bath» (pieces of carbon steel), 0.6−0.8 g of tin and one or two empty casings.

The ratio of the weight of the analyzed alloy to the weight of the iron bath must be not less than 1:10.

4.14.4. Testing

Work on the installation is carried out in accordance with the manual.

The vacuum oven degassed at a temperature 1850−1900 °C for as long as idle outgassing of the furnace will be set at a level not more than 0.005 cmfor 10 min. After reaching the specified level of outgassing temperature of the crucible was reduced to working, 1650 °C, and drop into the crucible iron and tin, which are degassed for 15−20 min. Then the crucible dropping the empty cartridge case. Stand out from the casings of gas pumped mercury diffusion pump for 10 min, and then transferred his flow of carrier gas (argon with the addition of 0.01% by volume of benzene) in a gas chromatograph. Data obtained from the analysis of empty shells, used as a blank correction in subsequent calculations.

Analysis of the shells with powder the analyzed alloy is carried out in the same way as the analysis of the empty sleeve.

4.14.5. Calibration of the chromatograph

After the analysis of samples oven turned off and the calibrated chromatograph, which through a graduated volume produce a certain number of portions of the calibration gas as long as the chromatogram peak value of the respective components of the analyzed sample and calibration gas will not be equal. Note the temperature and pressure of calibration gas during calibration.

Calibration gas is a mixture of argon with about 25% CO, 12% N, 11−12% Nand 1.2% and 1.5% O(% by volume).

For each component of the calibration gas (CO, N, N) is constructed calibration curve in the coordinates:

peak area, mm;

the number of overlaps of the calibration mixture.

From the calibration graph to find how many lapping calibration gas equal to the determined peak component from the sample.

4.14.6. Processing of the results

The contents of oxygen , nitrogen , hydrogen percentage in the analyzed alloy powder find by the formulas:

;

;

,

where is the pressure of the calibration gas, manufactured in a graduated volume, PA;

 — graduated volume, cm;

 — the number of portions of a calibration gas at which the peak value of the designated components from the calibration and the analyzed gases is equal to the sample;

 — the number of portions of a calibration gas at which the peak value of the designated components from the calibration and the analyzed gases is equal to the empty shells;

, ,  — the content of carbon monoxide, nitrogen and hydrogen, respectively, in the calibration gas in percent of volume;

the weight of the analyzed powder, g;

 — the temperature of the calibration gas, °C;

1,924; 3,365; 0,240 — coefficients of reduction of oxygen, nitrogen and hydrogen, respectively, to normal conditions and recalculation of the volume at gra

we will.

4.15. The determination of carbon

4.15.1. The essence of the method

The determination of carbon in alloys based on the allocation of carbon in the form of a dioxide when heated, the analyzed powder in the atmosphere of purified oxygen.

Free carbon is determined by heating the powder to 600 °C, and the carbon dissolved in the alloy and bound in a carbide by fusion of powder with lead oxide at 1100−1200 °C.

The number formed during the oxidation of powder of carbon dioxide is measured by gas chromatograph.

The absolute sensitivity of the method in terms of carbon is 5·10g. the relative error of the determination should not be more than 20%.

4.15.2. Apparatus, materials and reagents:

setup for determination of carbon (Fig.2);

Damn.2. Setup for determination of carbon

Setup for determination of carbon

1 — the helium tank; 2 — oxygen; 3, 4 — oxygen scrubbers; 5 — electric resistance furnace at 1100 °C; 6 — oxidizing furnace; 7, 10 — switch gas flows; 8 — bar capacity; 9 — recorder; 11 — cumulative trap; 12 — electric resistance furnace at 300 °C; 13 — a chromatography column; 14 — a calibrated gas; 15 — detector; 16 — regulator of the gas flow rate

Damn.2

analytical scales of the 2nd class of VLA-200 g-M;

zeolite is a synthetic brand of the CAA (molecular sieve 5 ) with grain size 0.5−1.0 mm;

silica gel technical brand KSM according to GOST 3956−76;

the rate of anhydrous magnesium (anhydro);

Askari, h;

oxygen gaseous technical GOST 5583−78;

liquid nitrogen according to GOST 9292−82;

helium gas;

lead oxide according to GOST 9199−77, h. d. a.;

ampoules made of quartz, diameter 12 mm, length 45 mm;

spatula of platinum according to GOST 6563−75;

the technical rectified ethyl alcohol according to GOST 18300−72, the highest grade.

(Changed edition, Rev. N 1, 2).

4.15.3. Preparing for the test

Party quartz ampoules (6−8 pieces) pre-cleaned by annealing in flowing oxygen at 1000−1100 °C in oxidation furnace for 1−2 h.

Download calcined in a vial of a sample of oxide of lead with a mass of 0.5 g, and calcined in oxygen at 700−750 °C for 3−4 h. the Completeness of decarburization is determined idle experience. Weigh the vial with svezhepriobretennoy oxide of lead, loaded into it 0.01−0.02 g of the analyzed powder, mix thoroughly with a platinum spatula and weighed the vial. When tested should be taken to prevent pollution of capsules and powder. Take the vial with clean forceps and stored between operations in a clean box.

4.15.4. Testing

The vial with the sample and lead oxide is placed in an oxidizing furnace, check the tightness of the furnace, set the oxygen rate of 50 ml/min and turn up the heat. Raise the furnace temperature to 600 °C for determination of free carbon and allowed to stand for 10 min. Formed during the oxidation of sample carbon dioxide, is transferred by flow of oxygen in the storage trap 11, containing 3 g of zeolite (molecular sieve having ability to adsorb carbon dioxide at room temperature and be conducted in order to when heated to 270−300 °C). Turn off the heating furnace, and after 2 minutes switch of the gas flow 10 is transferred to the helium flow (50 ml/min). Electric resistance furnace 12 is heated cumulative trap to 300 °C. Released when the carbon dioxide flow of helium is transferred to the chromatograph and recorded within 6−7 min. transfer switch the gas flow on the oxygen flow and continue the oxidation of the sample and determination method described above, but fixed carbon by heating the furnace to 1200 °C.

4.15.5. Calibration of the chromatograph

The calibration of the chromatograph is carried out by sequential overlap in the cumulative trap different amounts of the calibration gas through the switch 7 with the loop of the calibration volume (0.1−0.5 cm). Calibration gas is a known composition gas mixture of oxygen and carbon dioxide (15% volume).

The peak of carbon dioxide from the calibration gas should be equal to or slightly more than the peak of carbon dioxide from the sample.

4.15.6. Processing of the results

According to the build calibration the calibration curve in the coordinates: the area of the peaks of carbon dioxide in mm — number of inlets calibration gas.

For this curve, find what number of overlaps is equal to the peak of the calibration gas carbon dioxide from a test sample. Measure the temperature and pressure of calibration gas during the analysis.

The carbon content in percent is calculated by the formula

,

where is the atmospheric pressure, PA;

 — calibration capacity, cm;

the number of inlets for calibration gas sample;

the number of inlets calibration gas for a single experience;

 — the content of carbon dioxide in the calibration gas, % by volume;

 — the temperature of the calibration gas, °C;

 — the weight of the portion of the sample,

G.

4.16. Determination of aluminium and copper in the alloy grade PC-1714.

4.16.1. The essence of the method

The spectral analysis is carried out by a method of additives, vaporizing the sample with additives from the crater of the graphite electrode in the arc DC. The coefficient of variation should not be more than 25−30%.

4.16.2. Apparatus, materials and reagents

the quartz spectrograph medium dispersion type of ISP-30 single-lens lighting system and three-step attenuator;

microphotometer type MF-2 or IPV;

a constant current source, providing a voltage less than 200 V and is designed for loads up to 20 A;

grinding machine graphite electrodes of the type «Universal» plant «Stankokonstruktsiya»;

Libra torsion bar type W-500;

photographic plates type I, sensitivity of 4.5 units;

powder graphite OS.CH.;

coal graphite OS.CH.;

developer and fixer prepared according to GOST 10691.1−73*;
______________
* On the territory of the Russian Federation GOST 10691.1−84. — Note the manufacturer’s database.

sodium chloride for spectral analysis, H. h;

the copper oxide according to GOST 16539−79, h. d. a.;

aluminum hydroxide according to GOST 11841−76, h.d. a.

4.16.3. Preparation of control samples

Control samples are used as additives to the samples, prepared on the basis of pure graphical powder (zero baseline sample).

Head to prepare a control sample containing 1% of the identified elements, hinge oxides of detectable elements (in terms of metal) is mixed with a suspension of graphite powder.

Control samples with a smaller content of impurities is prepared from the brain by the method of successive dilution.

The composition of the used control samples (additives) shown in table.2.

Table 2

In the preparation of control samples, they administered 10% sodium chloride.

4.16.4. Preparing for the test

Four sample analyzed sample masses of 200 mg mixed with masses of test portions of 200 mg control samples 0, I, II, III (Supplement) in an agate mortar, sequentially in ascending order of concentration.

Prepared mixture is Packed tightly into the crater of the lower graphite electrode anode (depth 4.5 mm, diameter 3.5 mm).

The upper electrode-the cathode — a graphite rod 6 mm in diameter, sharpened to a truncated cone.

4.16.5. Testing

Evaporation of the mixtures is carried out in the arc of direct current strength of 10 A. the Distance between electrodes of 2 mm.

Survey spectra performed on the spectrograph slit with a width of 0.020 mm, exposure time — 60 s.

Registration of spectra is carried out in a region of wavelengths 230−340 nm.

Manifestation and fixation of photographic plates carried out according to GOST 10691.0−84 at a temperature of 20±1 °C.

Measurement of pochernenija analytical lines and the nearby background is performed on microphotometer.

Apply the following analytical lines:

copper 327,39 nm;

aluminum 308,22 nm.

(Changed edition, Rev. N 2).

4.16.6. Processing of the results

In the characteristic curve of photographic plates to find all of the measured pochernenija (lines together with the background and the line background ) the corresponding values of , .

Note. Build a response curve for a given type of photographic plates, using a three-stage attenuator supplied with the spectrograph.


Compute intensity, subtract background and calculate the contents of the determined elements () in percentage by the formula

,

where  — the value entered Supplement 1, percent by weight;

 — the ratio of the concentration of additive II additive I;

, ,  — intensity lines of the elements in the sample with additions of 0, I, II respectively.

Control sample III is used if the contents of copper and aluminum in the sample above the content elements in the second control sample.

4.17. Determination of wetting alcohol

The test powder alloy grade PC-1714 on the wettability of the alcohol is carried out by pouring 3−5 g of powder 20−25 ml of ethyl alcohol and stirring. After mixing on the surface should not be a film not soaked with alcohol.

4.18. Determination of cobalt in alloy PC-5406

4.18.1. The essence of the method

The method is based on oxidation of cobalt (II) to cobalt (III) solution relatoseroticos potassium in alkaline environment. Chrome III camouflage with a mixture of glycerol and citric acid.

The relative error in the result of the analysis should be no more than 2.5%.

4.18, 4.18.1. (Changed edition, Rev. N 1)

4.18.2. Apparatus, materials, reagents:

a potentiometer of any type galvanometer with a sensitivity of 10A;

magnetic stirrer MM-3;

the indicator electrode is (+) — wire PL IM-0.5 GOST 21007−75;

the reference electrode (—) tungsten wire brand VA with a diameter of 1 mm;

Cup PL 118−4 according to GOST 6563−75;

cover the type of «hour glass» PTFE-4 according to GOST 10007−80;

burette 1−2-5−0,or 1−2-10−0 02,05 to GOST 20292−74*;
________________
* On the territory of the Russian Federation there are 29169−91 GOST, GOST 29227−91−29229−91 GOST, GOST 29251−91-GOST 29253−91, here and hereafter. — Note the manufacturer’s database.

pipette 2−1-25 according to GOST 20292−74;

the bulb 2−100−2 according to GOST 1770−74;

glass-1−100 TC GOST 25336−82;

ammonia water according to GOST 3760−79, h. e. a., 25% solution;

ammonium sulfate according to GOST 3769−78, H. h., 25% solution;

distilled water GOST 6709−72;

ammonium citrate according to GOST odnosemjannyj 7234−79, h. d. a.;

25% ammonia solution. Prepared as follows: 250 g ammonium citrate dissolved in 500 ml of water and add 250 ml of ammonia;

potassium genesisintermedia, 0,05 n solution. Prepare standard titer* store in a dark place. 1 ml of 0.05 n solution with 0,002945 g of cobalt;
_______________
* The text matches the original. — Note the manufacturer’s database.

nitric acid GOST 4461−77, H. h;

sulfuric acid GOST 4204−77, H. h;

hydrofluoric acid according to GOST 10484−78, H. h;

citric acid according to GOST 3652−69, H. h;

glycerin according to GOST 6259−75, h.d. a.

(Changed edition, Rev. N 1, 2).

4.18.3. Testing

A portion of the sample weighing 0.5 g is weighed to ±0.0001 g, placed in a platinum Cup, add 2−3 ml of water, 5 ml of hydrofluoric acid, cover Cup lid and carefully lifting the lid, add drop by drop nitric acid until complete dissolution of the alloy. The cover is removed, washed with water, in a Cup add 2−3 ml of sulfuric acid, gently stirred, the solution is evaporated until the sulphuric acid fumes. The Cup is cooled, washed walls 2−3 ml of water and again evaporated to fumes of sulfuric acid. The contents of the Cup is cooled, diluted with water, poured into a measuring flask with volume capacity of 100 ml, made up to the mark with water and mix.

In a glass with a capacity of 250 ml is poured 2.5 ml of a solution of ammonium sulfate, 13.5 ml of ammonia solution, 25 ml of glycerol and add 1.5 g citric acid. The resulting solution was thoroughly stirred with a magnetic stirrer and slowly the jet is injected with a pipette 25 ml of the analyzed solution. The side of the Cup washed with water, after which the total volume of solution should not exceed 100 ml.

In the thus-prepared solution are immersed the electrodes, turn the agitator switch potentiometer «titration» and added to a solution of zhelezovanadievoj of potassium from the burette first 0.2−0.5 ml, and then 0.1 ml to the titration end — of 0.05 ml to a sharp jump of potential. An equivalent volume of solution relatoseroticos potassium consumed in the titration of cobalt , ml, is calculated by the formula

,

where  — volume of potassium relatoseroticos at the time of spike potential, ml;

 — the difference between the volume of the solution relatoseroticos potassium is added in the region of the spike potentials, ml;

 — the potential difference before the maximum potential difference, mV;

 — the potential difference subsequent to the maximum potential difference, mV.

4.18.4. The content of cobalt in the sample sample of the alloy in mass % is calculated by the formula

,

where  — the weight of the portion of alloy, suitable aliquote part of the solution, ml.

The result of the analysis consider the arithmetic mean of the number of parallel measurements (at least three).

4.18.3, 4.18.4. (Changed edition, Rev. N 1).

5. MARKING, PACKAGING, TRANSPORTATION AND STORAGE

5.1. Powders of silicon alloys with weight from 100 to 200 grams Packed in double bags made of polyethylene film according to GOST 10354−82 or PET film; batch sizes are determined by the mass of the Packed powder.

At the request of customers allowed the packaging of powders of alloys in packages weighing 50 g.

It is allowed to pack the powder in a glass or plastic banks B-5P, Bo-5P, B-6 GOST 3885−73, the mass of the powder should be from 250 to 400 g.

Packing powder produced with an error of no more than 1 year

(Changed edition, Rev. N 2).

5.2. Packages are pre-wiped with coarse calico cloth moistened with ethyl rectified technical alcohol of the highest grade according to GOST 18300−72.

(Changed edition, Rev. N 1).

Banks before filling washed powder «Lotus» and wiped with coarse calico cloth moistened with ethyl alcohol.

5.3. After packing the powder packs brew a sealed seam between the inner and outer packages pre-put label.

When packaging to cans for extra sealing the lid with the jar should be covered with adhesive tape of a width not less than 20 mm. On the jar and label.

5.4. Labels must include:

trademark of the manufacturer;

name and grade;

batch number;

net weight of powder in the package;

the number fraction of the powder;

date of manufacture (month, year);

the designation of this standard;

stamp of technical control Department.

(Changed edition, Rev. N 1).

5.5. Packets of powder resistive silicon alloys is placed in a polystyrene box. In each box are placed the packages of powder in one batch.

The box should contain:

trademark of the manufacturer;

name and grade.

Each jar of powder is wrapped in a corrugated cardboard according to GOST 7376−84* in one or two layers.
______________
* On the territory of the Russian Federation GOST 7376−89**;
** On the territory of the Russian Federation GOST R 52901−2007. — Note the manufacturer’s database.

(Changed edition, Rev. N 2).

5.6. Polystyrene boxes, glass or plastic cans are placed in cardboard boxes according to GOST 22637−77 or plywood boxes according to GOST 22638−77*, lined inside with a polyethylene film according to GOST 10354−82. Banks should be interleaved corrugated cardboard in horizontal and vertical planes.
______________
* On the territory of the Russian Federation GOST 22638−89. — Note the manufacturer’s database.

Allowed to use wooden boxes according to GOST 22638−77*.
______________
* On the territory of the Russian Federation GOST 22638−89. — Note the manufacturer’s database.

(Changed edition, Rev. N 1, 2).

5.7. In each polystyrene box or a box with the banks investing a certificate that must contain the following information:

trademark of the manufacturer;

name and grade;

the number fraction of the powder;

the results of analyses;

batch number;

the date of manufacture (month, year);

a lot of the packaged material;

the mark of the technical control Department of the manufacturer;

the designation of this standard.

(Changed edition, Rev. N 1).

5.8. Labeling of the boxes should be performed according to GOST 14192−77*.
_______________
* On the territory of the Russian Federation GOST 14192−96. — Note the manufacturer’s database.

5.9. (Deleted, Rev. N 2).

5.10. The resistive silicon alloys in the manufacturer’s packaging stored in heated rooms at an ambient temperature of from 10 °to 40 ° C and the absence of vapors of acids or other corrosive substances.

5.11. Silicon alloys transporterowych any mode of transport at any temperature.

(Changed edition, Rev. N 1).

6. APPLICATION NOTES

6.1. All operations with resistive silicon alloys to prevent contamination should be carried out in dust-free conditioned space subject to the rules of electronic hygiene.

(Changed edition, Rev. N 1).

6.2. Primary packaging of the manufacturer should be opened only immediately prior to use of silicon alloys. Unused powder should be stored in boxe or jar with a glass stopper, not pouring out of the package, or in a desiccator with silica gel within the stipulated warranty period.

6.3. After a long storage period (over three months) powder resistive silicon alloys, it is recommended to dry in a drying Cabinet at a temperature of 100−120 °C for 1 h with the aim of improving their yield.

(Changed edition, Rev. N 1).

6.4. Additional processing of the powders of the alloy before use is not required. Allowed to wash the powder in pure ethyl alcohol according to GOST 5962−67* with subsequent drying according to claim 6.3.
_______________
* On the territory of the Russian Federation GOST R 51652−2000. — Note the manufacturer’s database.

7. MANUFACTURER’S WARRANTY

7.1. The manufacturer guarantees the resistive silicon alloys with the requirements of this standard, subject to consumer storage conditions specified in this standard.

7.2. Warranty storage time resistive silicon alloys — 2 years from date of manufacture.

ANNEX 1 (reference). Physical and electrical parameters of resistive silicon alloys

ANNEX 1
Reference

Notes:

1. Bulk samples obtained in the smelting resistive silicon alloys.

2. The parameters of the films obtained at the following technological parameters of their receipt by the method of explosive VacuumTechExpo application on the installation UVN-2M-2:

Changing technological processes of film deposition parameters of the films can vary significantly. For example, the temperature coefficient of resistance of films of alloy PC-3710 can have a positive or negative value, irreversible changes in surface resistance can be reduced to 0.1−0.01 percent.

APPENDIX 2 (recommended). The scope and methods of applying resistive silicon alloys

ANNEX 2
Recommended

Note. To obtain resistive and intermediate layers can be used as the evaporator of carbon-graphite fabric coated with pyrographite, but the properties of the films will differ slightly from those described in the background Annex 1. The applicability properties of these films should be determined by the consumer.

Manufacturer of resistors, is possible with the method and mask of the photolithography.