GOST 9816.4-84

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  ГОСТ 9816.4-84

GOST 9816.4−84 Tellurium technical. Method of spectral analysis (with Change No. 1)

GOST 9816.4−84

Group B59

STATE STANDARD OF THE USSR

TELLURIUM TECHNICAL

Method of spectral analysis

Technical tellurium. Method of spectral analysis

AXTU 1709

Valid from 01.07.85
before 01.07.90*
__________________
* See the label «notes"

DEVELOPED by the Ministry of nonferrous metallurgy of the USSR

PERFORMERS

A. A., Babacan, E. N. Gezalov, V. N. Semavin, I. I. Lebed, N. B. Tret'yakova, E. B. Makowski, O. D. Ryabkova

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 June 27, 1984 N 2149

REPLACE GOST 9816.4−74


The Change N 1, approved and put into effect by the Decree of the USSR State Committee on management of quality and standards from 20.12.89 N c 3908 01.07.1990

Change No. 1 made by the manufacturer of the database in the text IUS N 3, 1990


This standard establishes a spectral method for the determination of impurities in technical tellurium when the mass fraction of elements:

of copper from 0.001 to 0.35%;

iron from 0.0005 to 0.2%;

of lead from 0.0005 to 1.5%;

sodium from 0.005 to 0.35%;

selenium from 0.05 to 0.5%;

silicon from 0.0005 to 0.25%;

aluminum from 0.0005 to 0.15%;

silver from 0.001 to 0.004%;

gold from 0.0005 to 0.02%;

the platinum from 0.0005 to 0.02%;

of rhodium from 0.0005 to 0.02%;

palladium, from 0.001 to 0.02%;

iridium from 0.005 to 0.2%;

of ruthenium from 0.005 to 0.2%;

tin from 0.0005 to 0.02%.

Impurities determined by the method of «three standards» with the use of the arc AC to vaporize the sample and the excitation spectrum.

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 9816.0−84.

2. APPARATUS, REAGENTS AND SOLUTIONS

Spectrograph medium dispersion of any type with being a lighting system and three-step attenuator.

Arc generator AC type IVS-28 or DG-2.

Microphotometer of any type.

Agate mortar with pestle.

Grinding machine carbon electrodes.

The infrared lamp on the other 16−87 IFMR.675000.006 TU*.
________________
* The one referred to here and hereinafter, not shown. For additional information, please refer to the link. — Note the manufacturer’s database.


Plastic jars or plastic.

Spectrographic plates of the type II sensitivity from 10 to 20 units according to GOST 10691.1−84.

Film positive type MZ-3−35 sensitivity of 0.7−1.0 units according to GOST 20945−80.

Electrodes, carbon, spectral pure helium-3, high purity 7−3 GOST 4425−72:

a crater with a diameter of 2.8 mm, a depth of 4 and 6 mm;

with a diameter of 6 mm, a length of 30−50 mm, sharpened on a cone;

a crater with a diameter of 3.5−4 mm, depth 2−2. 5 mm, shape «glass».

Graphite powder of high purity according to GOST 23463−79 or coal powder manufactured by crushing pure spectral carbon electrodes.

Developer:

metol according to GOST 25664−83 — 1 g;

sanitarily anhydrous sodium GOST 195−77 — 25 g;

hydroquinone according to GOST 19627−74 — 5 g;

potassium bromide according to GOST 4160−74 — 1 g;

the anhydrous sodium carbonate according to GOST 83−79 — 20 g;

distilled water to 1000 cm.

Fixer:

sodium thiosulfate crystal according to GOST 244−76 — 250 g;

potassium sanitarily Piro — 25 g;

distilled water to 1000 cm.

Allowed the use of other contrast working developer and fixer.

Bismuth oxide according to GOST 10216−75.

Potassium nitrate according to GOST 4144−79.

Standard samples for calibration.

(Changed edition, Rev. N 1).

3. PREPARATION FOR ASSAY

3.1. Preparation of standard samples for calibration are given in mandatory Appendix.

3.2 Preparation buffer mixture

Sample of carbon powder or graphite powder with the weight 4,89 g, and oxide of bismuth with a mass of 0.11 g was placed in an agate mortar, thoroughly mixed. From the resulting mixture, take the sample weight of 0.5 g, transfer it to an agate mortar and triturated with 0.42 g of potassium nitrate and 4.08 g of carbon powder or graphite powder. The thus prepared buffer mixture contains 0.2% bismuth and 4% potassium.

The number of prepared buffer mixture can be doubled.

4. ANALYSIS

4.1. Technical tellurium and standard samples for calibration are mixed in an agate mortar with a buffer mixture in a weight ratio of 1:1 (200 or 400 mg technical tellurium or samples, and 200 or 400 mg of the mixture) for 30−35 min and Packed into the carbon electrodes with a crater diameter of 2.8 mm and a depth of 44 mm, pre-baked in the arc of an alternating current power (15±0,1) And for 15−20 s.

For analysis technical tellurium containing platinum metals, use electrodes shaped «glass», the film and the buffer in the form of carbon powder with a ratio of the buffer and the analyte of 1:5 (by weight).

From each analyzed sample and the standard sample: prepare four calibration electrode.

(Changed edition, Rev. N 1).

4.2. The spectra photographed using a three-step attenuator with being an illumination system and a width of slit of the spectrograph 0,015 mm. intermediate diaphragm 5 mm. allowed the photographing of the spectrum without the three-stage attenuator.

Evaporation of the sample and the excitation spectrum is carried out in the arc AC at 7−8 And exposure time (60±5) C. the Arc gap of 2.5 mm.

In the cassette placed a plate type II size 912 cm or positive film. The long-wave region of the spectrum photographed on the photographic plate «Soarta».

On the same plate or film photograph two of the spectrum of each test sample and standard sample, then photography is repeated on another plate (film).

The plate or film shown at (20±2)°C (the time of development indicated on the packaging plate), fixed, rinsed for 20−25 min in running water, rinsed with distilled water and dried.

(Changed edition, Rev. N 1).

5. PROCESSING OF THE RESULTS

5.1. When determining the mass fraction of impurities is to measure the density of blackening of the line of impurities and comparison of the following pairs of lines in nm, choosing the photometry data on the levels of attenuation at which blackening of the measured lines lie in the region of normal:

Note. Line sodium 330,20 nm used in the absence of palladium.


Calculate the difference of the blackening, finding the arithmetic mean of the two spectra of each standard sample and a test sample, build a calibration curve in the coordinates — where  — mass fraction of impurities in the standard samples for calibration in percent.

According to calculated values for each of the analyzed samples according to the schedule determine the mass percent of impurities.

(Changed edition, Rev. N 1).

5.2. The difference of greatest and least result of four parallel measurements at a confidence probability of 0.95 does not exceed the permissible values of absolute differences are given in table.1.

(Changed edition, Rev. N 1).

Table 1

6. DETERMINATION OF SELENIUM

6.1. Before analysis to prepare standard samples for calibration: mix 1.5 g of selenium with 8.5 g of tellurium-base. From the resulting mixture to take 1.5 g and mixed with 13.5 g of tellurium-basics is the primary standard sample for calibration. Subsequent samples to prepare a serial dilution of the main sample, and then each subsequent tellurium-based 2.5 times.

Mass fraction of selenium in the standard samples for calibration are given in table.2.

Table 2

Depending on the mass fraction of selenium in the analyzed samples allowed to change the content in the standard samples for calibration.

Prepare six electrodes from each sample and a standard sample and to fill in the carbon electrodes with a crater diameter of 2.8 mm and a depth of 6 mm.

6.2. To photograph spectra through a three-stage attenuator and a width of slit of the spectrograph 0,026 mm. Coverage gaps — being the condenser (two lines — nefroticescoy). Intermediate diaphragm is round. The arc gap of 2.5 mm. In the cassette (to shorter wavelengths), we put a plate of the type II sensitized. Evaporation of the sample and the excitation spectrum to be held in the arc AC (12±0,1) And exposure time (60±5) s.

To photograph one of the plates has three of the spectrum of the sample and standard samples for calibration. To repeat the survey on another plate.

(Changed edition, Rev. N 1).

6.3. To measure the density of blackening of the line of Selena at a wavelength of Komi was up RUR 207.4 nm and comparison lines of tellurium at a wavelength of nm 207,0, choosing to photometry data on the levels of attenuation at which blackening of the measured lines lie in the region of normal.

Mass fraction of selenium is determined according to claim 5.1. The difference of greatest and least result of six parallel measurements with a confidence probability of 0.95 does not exceed the permissible values of absolute differences are given in table.3.

(Changed edition, Rev. N 1).

Table 3

APP (mandatory). Preparation of standard samples for calibration

APP
Mandatory

1. Standard samples for calibration, prepared for each company according to the above method should be certified by GOST 8.315−78.

2. Allowed the preparation of standard samples for calibration of the metals, oxides of metals and solutions of metals.

3. Preparation of standard samples for calibration of the metals and metal oxides

3.1. Reagents, solutions

Sodium chloride according to GOST 4233−77.

Tellurium of high purity.

Silver GOST 6836−80

Gold GOST 6835−80.

Silicon dioxide according to GOST 9428−73.

Tin dichloride.

Iron oxide according to GOST 4173−77.

Aluminium oxide active according to GOST 8136−85.

Copper (II) oxide under GOST 16539−79.

Lead (II) oxide.

Selenium of high purity.

Platinum powder according to GOST 14837−79.

Palladium powder according to GOST 14836−82.

Rhodium powder according to GOST 12342−81.

Iridium powder according to GOST 12338−81.

(Changed edition, Rev. N 1).

3.2. Sample preparation

For preparation of the main sample for the calibration you need:

the copper oxide 0,150 g;

iron oxide — 0,171 g;

lead oxide — 0,131 g;

sodium chloride is of 0.152 g;

silica — 0,128 g;

aluminum oxide is 0,113 g;

dichloride tin — 0,105 g;

gold, silver, palladium, rhodium and platinum to 0,015 g;

iridium, ruthenium — 0,090 g;

tellurium-base — 1,796 g.

All the sample is thoroughly stirred for 2−2. 5 hours in the eraser (the type of laboratory ball mill from the material not polluting the source of the sample). Working samples for the calibration are prepared by successive dilution of the primary standard sample, and then each subsequent sample tellurium-based 2.5 times. Mass fraction of impurities determined in the standard samples given in the table.

Mass fraction of impurities in the basis determined by the method of additions and introduced the amendment in the estimated impurity content in the standard samples for calibration.

Prepared standard samples for calibration should be stored in plastic or plastic jars with tight-fitting lids for 1 year.

4. Preparation of standard samples for calibration of solutions of metals

4.1. Reagents, solutions

Barium hydroxide technical GOST 10848−79.

But hydrochloric acid GOST 3118−77 and diluted 1:1.

Nitric acid GOST 4461−77 and diluted 1:1 and 1:3.

Oxalic acid according to GOST 22180−76.

Sodium hydroxide according to GOST 4328−77.

Quartz ware (cups, glasses), GOST 19908−80.

Sodium chloride according to GOST 4233−77.

Tellurium of high purity.

Silver GOST 6836−80.

Gold GOST 6835−80.

Silicon dioxide according to GOST 9428−73.

Tin GOST 860−75.

Iron according to GOST 9849−86.

Aluminium GOST 11069−74.

Copper GOST 859−78.

Lead according to GOST 3778−77.

Selenium of high purity.

Platinum powder according to GOST 14837−79.

Palladium powder according to GOST 14836−82.

Rhodium powder according to GOST 12342−81.

Ruthenium powder according to GOST 12343−79.

Iridium powder according to GOST 12338−81.

Solutions of pure metals.

The copper solution: a sample of copper weighing 5 g was placed in a conical flask with a capacity of 250−300 cm, 45−50 cm and pour themixture of hydrochloric and nitric acids (3:1), dissolved by heating and the solution is evaporated to dryness. The residue is twice treated with 7−10 cmof hydrochloric acid, evaporating to dryness each time. The dry residue was dissolved in 60−80 cmof hydrochloric acid (1:1), cooled and placed in a measuring flask with volume capacity of 1000 cm, is diluted to the mark with water and mix.

1 cmof the solution contains 5 mg of copper.

The solution of iron: a sample of iron weighing 5 g was placed in a conical flask with a capacity of 250−300 cm, 40−45 cm pour thehydrochloric acid, is boiled and evaporated solution when heated to dry salts. Pour the 60−80 cmof hydrochloric acid (1:1), boil for 5−7 minutes, cool, put the solution into a measuring flask with volume capacity of 1000 cm, is diluted to the mark with water and mix.

1 cmof solution contains 5 mg of iron.

The solution of lead: a sample of lead weighing 5 g was placed in a conical flask with a capacity of 250−300 cm, 40−45 cm poureda solution of nitric acid (1:3) and is evaporated when heated to the wet state. Then pour 5−7 cmof nitric acid and the solution placed in a measuring flask with volume capacity of 1000 cm, is diluted to the mark with water and mix.

1 cmof the solution contains 5 mg of lead.

Silver solution: a portion of silver with a mass of 0.1 g was dissolved with heating in 15−20 cmof nitric acid (1:3) and evaporated to moist salts. Add 50−60 cmof water, place the solution in a volumetric flask with a capacity of 100 cm, is diluted to the mark with water and mix.

1 cmof the solution contains 1 mg of silver.

The solution of gold: a portion of gold weighing 0.1 g were placed in a glass (flask) with a capacity of 150−200 cm, 10−15 cm, pour themixture of hydrochloric and nitric acids (3:1) and dissolved by heating. Cooled and placed in a volumetric flask with a capacity of 100 cm, is diluted to the mark with water and mix.

1 cmof the solution contains 1 mg of gold.

Solution of aluminum: weighed aluminum weighing 0.5 g were placed in a glass (flask) with a capacity of 150−200 cm, pour 15−20 cmof nitric acid (1:1) and dissolved by heating. Cool and transfer the solution into volumetric flask with a capacity of 500 cm, is diluted to the mark with nitric acid (1:1) and stirred.

1 cmof the solution contains 1 mg of aluminium.

The solution of tin: a portion of finely divided metal with a mass of 0.1 g were placed in a glass (flask) with a capacity of 50−100 cmand add 2−3 cmof nitric acid. After the transition of the whole sample in metalogeny acid in the beaker (flask) pour 15−20 cmof water and add 2−2. 5 g of oxalic acid. Dissolve the precipitate with stirring and placed the solution in a volumetric flask with a capacity of 100 cm, washed glass (a flask) there is 2−3 cmof water and the washings are placed in the same volumetric flask, dilute to the mark with water and mix.

1 cmof the solution contains 1 mg of tin.

The solution of iridium: a sample of iridium weighing 0.5 g triturated in an agate mortar with 5−6 g of peroxide of barium. The resulting mixture is transferred to a corundum crucible N 4 and sintered in a muffle furnace at 900−920°C for 2−2,5 h. the Crucible with the cooled cake, place in a glass with a capacity of 400−500 cmand dissolved in 200−250 cmof hydrochloric acid (1:1). If the linkage is completely dissolved, a solution of residue is filtered off, the filter is dried, incinerated and sintered again. Then the combined solutions are placed in a volumetric flask with a capacity of 500 cm, is diluted to the mark with hydrochloric acid (1:1) and stirred.

1 cmof the solution contains 1 mg of iridium.

Solution of rhodium: rhodium sample weight of 0.5 g is dissolved thoroughly in an agate mortar with 5−6 g of peroxide of barium. The resulting mixture is transferred to a corundum crucible and sintered in a muffle furnace at 900−920°C for 2−2,5 hours Then sintered is cooled and dissolved in 200−220 cmof hydrochloric acid (1:1). If the linkage is completely dissolved, a solution of residue is filtered off, the filter is dried, incinerated, and repeated sintering. Then the combined solutions are placed in a volumetric flask with a capacity of 500 cm, is diluted to the mark with hydrochloric acid (1:1) and stirred.

1 cmof the solution contains 1 mg of rhodium.

A solution of ruthenium: a portion of the ruthenium in a weight of 0.5 g triturated in an agate mortar with 5−6 g of peroxide of barium. The resulting mixture is transferred to a corundum crucible and sintered in a muffle furnace at 900−920°C for 2−2,5 hours Then sintered is cooled and dissolved in 200−220 cmof hydrochloric acid (1:1). If the linkage is completely dissolved, a solution of residue is filtered off, the filter is dried, incinerated, and repeated sintering. Then the combined solutions are placed in a volumetric flask with a capacity of 500 cm, is diluted to the mark with hydrochloric acid (1:1) and stirred.

1 cmof the solution contains 1 mg of ruthenium.

The platinum solution: a sample of platinum weighing 0.1 g were placed in a glass (flask) with a capacity of 100−150 cm, 10−15 cm, pour themixture of hydrochloric and nitric acids (3:1), covered with a cover glass and dissolve in low heat. After dissolution of the sample remove the glass, wash it with water over the glass (bulb), put the beaker in a water bath and evaporate the solution to 3−5 cm. Cool, the solution is placed in a volumetric flask with a capacity of 100 cm, is diluted to the mark with hydrochloric acid 2 mol/land stirred.

1 cmof the solution contains 1 mg of platinum.

A solution of palladium: a sample of palladium weighing 0.1 g were placed in a glass (flask) with a capacity of 50−100 cm, 10−15 cm, pour themixture of hydrochloric and nitric acids (3:1), covered with a cover glass and heated to remove the main mass of oxides of nitrogen. Remove the glass, wash it with water over the glass (bulb) and the solution was evaporated to 5−7 cm. Cooled, placed in a volumetric flask with a capacity of 100 cm, is diluted to the mark with hydrochloric acid 2 mol/land stirred.

1 cmof the solution contains 1 mg of palladium.

A sodium solution: a sample of sodium chloride mass 0,2543 g is placed in a volumetric flask with a capacity of 100 cm, 30−40 cm pouredwater, stirred to dissolve the sample, dilute to the mark with water and mix again.

1 cmof the solution contains 1 mg of sodium.

A solution of silicon: a portion of the silicon dioxide mass 0,1875 g placed in the beaker (flask) with a capacity of 50−100 cm, 10−15 cm pour thesolution of sodium hydroxide and heated to dissolve sample. Cool the resulting solution, placed in a volumetric flask with a capacity of 100 cm, is diluted to the mark with a solution of sodium hydroxide and stirred.

1 cmof the solution contains 1 mg of silicon.

For the preparation of solutions it is possible to use oxides or nitrate salts of metals.

Solution a: in a volumetric flask with a capacity of 100 cmplaced at 10 cmof solutions of iridium, ruthenium, platinum, palladium, rhodium, dilute to the mark with water and mix.

1 cmof solution A contains 0.1 mg of the indicated metals.

(Changed edition, Rev. N 1).

4.2. Preparation of standard samples for calibration

For the preparation of the primary standard sample with a mass fraction of copper, iron, lead 4%, sodium, silicon, aluminum, tin 0.8% each, of iridium, ruthenium, gold, silver, platinum, palladium, rhodium, 0.5% is necessary to prepare mixtures A and B.

Mixture A: in a quartz (or other) Cup with a capacity of 50 cmis placed 5 cmof solution A and 4 g of graphite powder. The mixture is dried under a lamp, injected with 0.8 cmof solutions of copper, iron, lead, sodium, silicon, aluminium and tin. Again carefully dried under a lamp to remove the smell of nitric acid. The resulting mixture was thoroughly stirred for 1−1,5 hours.

Mixture B: in a quartz (or other) Cup with a capacity of 50 cmis placed 0.5 cmof the solution of gold and 1 g graphite powder, carefully dried at a temperature not above 70 °C. Then the dried residue is moistened with 3−5 drops of nitric acid and again dried. Repeated wetting and drying to remove the smell of nitric acid.

Both mixtures are combined, thoroughly mixed in an agate mortar within 1−1,5 hours.

Working standard samples for calibration prepare a serial dilution of the main sample, and then each subsequent sample tellurium-based 2.5 times.

The mass fraction of the designated impurities shown in the table.

Depending on the composition of tellurium entering the analysis allowed to reduce the content of a particular impurity in the standard samples or completely eliminate it with the appropriate recalculation of the composition of the samples.