GOST 15483.11-78

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  ГОСТ 15483.11-78

GOST 15483.11−78 Tin. Methods for determination of bismuth, gallium, gold, cobalt, copper, Nickel, lead, silver, indium and aluminum (with Amendments No. 1, 2, 3)

GOST 15483.11−78

Group B59

INTERSTATE STANDARD

TIN

Methods for determination of bismuth, gallium, gold, cobalt, copper,
Nickel, lead, silver, indium and aluminum

Tin. Methods for determination of bismuth, gallium, gold, cobalt, copper,
nickel, lead, silver, indium and aluminium

AXTU 1709

Date of introduction 1980−01−01

INFORMATION DATA

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

DEVELOPERS

B. C. Baev, T. P. Almanova, G. M. Vlasov, C. B. Meshkova, L. V. Mishchenko, L. D. Savilov, R. D. Kresnicka

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 13.12.78 N 3300

3. REPLACE GOST 15483.10−70 in part of sec. 2

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)

6. REVISED (June 1999) with Amendments No. 1, 2, 3, approved in August 1984, October 1985, June 1989 (IUS 12−84, 1−86, 10−89)


This standard specifies the chemical-spectral method of determination of mass fractions of impurities and semi-quantitative spectral method of determining the mass fraction of aluminum and iron in tin of high purity in the range of concentrations, %:

Chemical-spectral method based on the determination of the above elements except for aluminum, the concentration of impurities by removing the foundations in the form of chloride of tin. The chlorides of the impurities adsorbed on the coal powder which is further subjected to spectral analysis.

For the determination of aluminium hitch tin metal converted into oxide, which is subjected to spectral analysis.

(Changed edition, Rev. N 3).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis and security requirements — according to GOST 15483.0.

(Changed edition, Rev. N 1).

1.2. In the course of analysis are control experiments for the correction for contamination of reagents.

2. APPARATUS, REAGENTS AND SOLUTIONS

The quartz spectrograph medium dispersion being the illumination system of the slit.

Microphotometer.

Arc generator DC or AC with high frequency ignition. The circuit shown in hell.1

1 — the source of high frequency from oscillator DT-1 or DG-2; 2 — contactor to enable the source
DC; 3 — a contactor to change the polarity of the DC arc

Damn.1

Oven muffle.

Drying Cabinet.

A horizontal tubular furnace.

An electric furnace at 120 °C (see the devil.4).

Analytical scale.

Libra torsion.

Stopwatch.

Quartz distillation apparatus for the distillation of acid and water.

Apparatus for the distillation of carbon tetrachloride.

Infrared lamp (for drying) voltage 127 volts, 500 watts.

Machine bench lathe with a set of shaped cutters.

Photographic plates of spectral types I and II according to normative-technical documentation.

Developer and fixer according to GOST 10691.6. Allowed the use of the developer of a different composition.

Graphite rods for the spectral analysis of the brand OS.h. 7−4.

Heat-resistant glasses with a capacity of 50−100 cmaccording to GOST 25336.

Boxy glass according to GOST 25336.

Caps or glass desiccators with GOST 25336.

Rack organic glass electrodes.

Cup quartz GOST 19908 or glass.

The Bulb Burza.

A drip funnel with GOST 25336.

The Flask Drexel.

Tubes, glass, with a diameter of 15−20 mm, a length of 10−12 cm.

Flask wolf size.

The quartz crucibles with a capacity of 40 cm(when selecting the preferred crucibles with the smallest diameter of the bottom) according to GOST 19908.

The agate mortar.

Powder graphite OS.h. 7−4.

Potassium permanganate according to GOST 20490.

Of phosphorus pentoxide.

Asbestos is fibrous.

Wool glass.

Hydrochloric acid according to GOST 3118.

Hydrochloric acid of high purity according to GOST 14261 and diluted 1:1.

Nitric acid according to GOST 4461, double-distilled in a quartz distiller and diluted 1:1, 1:4.

Carbon tetrachloride according to GOST 20288, distilled.

Ethylene chloride (dichloride).

The technical rectified ethyl alcohol according to GOST 18300.

Charcoal GOST 7657 or activated.

Sodium hydroxide according to GOST 4328 or potassium hydroxide according to GOST 24363.

Silicone grease type tsiatim-221 GOST 9433 or vaseline.

A mixture of hydrochloric and nitric acids in the ratio 3:1.

The calcium chloride.

Distilled water according to GOST 6709, distilled twice in a quartz distillation apparatus.

Chlorine get in the interaction of potassium permanganate and hydrochloric acid. Installation for the production and purification of chlorine is shown in hell.2.

1 — drip funnel with hydrochloric acid; 2 — flask production of chlorine; 3 — flask rinsing with water;
4 — column with calcium chloride and phosphorus pentoxide; 5 — quartz tube with charcoal
to remove oxygen; 6 — tubular furnace (700−800 °C); 7 — filter cotton;
8 — vial of sulfuric acid; 9 — column with phosphorus pentoxide;
10 — tap to remove the excess of chlorine; 11 — sections; 12 — tee

Damn.2

Bandwidth of chlorine is controlled visually and is 3−5 bubbles per second. All moving joints in the installation is made from vinyl chloride tubes. Rubber tube covered with glue, prepared by dissolving shavings of Plexiglas in dichloroethane (10 cmdichloroethane and 0.3 g of acrylic plastic). Cranes and sections of the flasks Drexel lubricated with silicone grease or vaseline. While providing all the safety requirements we recommend the use of chlorine from the cylinder. It is allowed to obtain chlorine by electrolysis of hydrochloric acid.

Solutions of pure standard metals (mass fraction of metal not less than 99.99%). To prepare the standard solutions using hydrochloric acid and high purity distilled nitric acid.

The tin standard solution: 10 g of tin of high purity is dissolved in 50 cmof hydrochloric acid and without hydrogen peroxide to obtain a nonvolatile chloride of tin. The resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof the solution contains 0.1 g of tin.

Solutions of gallium standard.

Solution a: 0.1 g of metal was dissolved in 50 cmof concentrated nitric acid. The resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid and stirred.

1 cmof the solution contains 1·10g of gallium.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof a solution contains 1·10g of gallium.

Solution bismuth standard.

Solution a: 0.1 g of metal was dissolved in 50 cmof concentrated nitric acid. The resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid and stirred.

1 cmof the solution contains 1·10g of bismuth.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid and stirred.

1 cmof a solution contains 1·10g of bismuth.

Solutions of lead standard.

Solution a: 0.1 g of metal was dissolved in nitric acid, diluted 1:4. The resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid, diluted 1:1, and stirred.

1 cmof the solution contains 1·10g of lead.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid, diluted 1:1, and stirred.

1 cmof a solution contains 1·10g of lead.

Solutions of copper standard.

Solution a: 0.025 g of metal was dissolved in 10 cmof nitric acid, diluted 1:1. The resulting solution was transferred to volumetric flask with a capacity of 250 cm, was adjusted to the mark with double-distilled water and stirred.

1 cmof the solution contains 1·10g of copper.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof a solution contains 1·10g of copper.

Solutions of gold standard.

Solution a: 0.05 g of the metal is dissolved in 10−15 cmof a mixture of hydrochloric and nitric acids in the ratio 3:1. The resulting solution was transferred to volumetric flask with a capacity of 50 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof the solution contains 1·10g of gold.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof a solution contains 1·10g of gold.

Solutions of cobalt and Nickel standard.

Solution a: 0.1 g of metal was dissolved in 10−15 cmof hydrochloric acid, the resulting solutions are transferred to volumetric flasks with a capacity of 100 cm, adjusted with double-distilled water to the mark and mix.

1 cmof the solution contains 1·10g of cobalt and 1·10g of Nickel.

Solution B: 10.0 cmof A solution of cobalt and 10 cmof a solution of Nickel And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof a solution contains 1·10g of cobalt and 1·10g of Nickel.

Solutions of silver standard.

Solution a: 0,0394 g of silver nitrate dissolved in double-distilled water in a volumetric flask with a capacity of 250 cm, was adjusted to the mark with double-distilled water and stirred.

1 cmof the solution contains 1·10g of silver.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof solution B contains 10·10g of silver.

Solutions India standard.

Solution a: 0.1 g of metal was dissolved in 10−15 cmof hydrochloric acid. The resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof the solution contains 1·10g India.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with double-distilled water and stirred.

1 cmof a solution contains 1·10g India.

Solutions of the aluminium standard.

Solution a: 0.02 g of metal was dissolved in nitric acid, diluted 1:1, the resulting solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid, diluted 1:1, and stirred.

1 cmof solution A contains 2·10g of aluminum.

Solution B: 10.0 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with nitric acid, diluted 1:1, and stirred.

1 cmof a solution containing 2·10g of aluminum.

Exceptionally, for the preparation of standard solutions can be used salts of the above metals qualification h. d. a. or H. h

Standard samples category SOP for determination of aluminum and iron.

(Changed edition, Rev. N 1, 2, 3).

3. DETERMINATION OF BISMUTH, GALLIUM, INDIUM, GOLD, COBALT, NICKEL, COPPER, SILVER, LEAD, INDIA

3.1. Preparation for assay

3.1.1. The preparation of calibration samples is performed on the basis of coal powder obtained from the spectral-pure carbon. Impurities in the coal powder is administered in the form of the calculated volumes of standard solutions.

Enter the volume of standard solutions (based on 50 g of carbon powder) are given in table.1.

Table 1

To the calibration samples were identical to the concentrates of the samples, they introduce a hydrochloric acid solution of tin at the rate of 2% tin to the weight of the coal powder.

With the introduction of the solutions ensure that the solution impregnating the coal powder did not reach the sidewall and bottom of the Cup. Therefore, as fluids of impurities the coal powder is dried in an oven at 100−105 °C.

After the introduction of the solutions of all the impurities and the powder completely dried, then mix thoroughly (but not ground) in an agate mortar or a mortar made of organic glass for 40 min. Prepared calibration samples stored in buksh with pritertymi covers.

3.1.2. Enrichment of the analyzed impurities from the incoming to the analysis of the average samples are taken in the form of slices or chips of five portions of 5 g. Sample is placed in the vessel for disinfection of heat-resistant glass (Fig.3) pour 10 cmof distilled carbon tetrachloride and subjected to chlorination. A portion of the chlorinated metal to the end (about 2.5−3 hours).

1 — socket; 2 — a tube hanging tin and carbon tetrachloride; 3 — trap, cooled with ice;
4 — tube rubber; 5 — a tube with calcium chloride; 6 — flask with alkali (10% solution)
to absorb the excess of chlorine

Damn.3

The resulting in vitro solutions of carbon tetrachloride, tin chloride and chlorides of the impurities is poured into a quartz crucible with portions of the spectral-pure carbon powder of 0.1 g each.

Then put the crucible on the furnace (Fig.4) heated to 120 °C; this temperature is maintained until obtaining a dry residue at the bottom of the crucible. During the distillation of perchloric tin watch that on the edges of the crucible does not accumulate crystalline chloride of tin, the remains of which can be removed with cotton wool moistened with alcohol.

1 — the furnace housing made of aluminum; 2 — heater (power of 330 W); 3 — the recess for the crucible

Damn.4

Coal powder remaining in it the chlorides of the impurities (the concentrate) the scalpel is removed from the crucible on a watch glass, gently stirred, divided into three equal weight pieces and placed in craters of the spectral-pure carbon.

The mass of the obtained concentrate ranges typically from up to 0,098 0,105 g (by weight of the concentrate control of completeness of removal of tin).

3.2. Analysis

A portion of the calibration sample with a mass of 0.03 g is placed in crater of the spectral-pure carbon electrode with a diameter of 4 mm and depth 4 mm. In the same craters placed sample concentrates.

Before applying the samples and calibration samples carbon electrodes, it is recommended to burn at a current of 10 A for 30 s. the excitation Source is an arc spectra of the DC voltage of 200−400 V and operating current 8 A.

Arc lighting is carried out by discharge from a high frequency generator (see the devil.1).

The electrode with the charge of the sample or the calibration sample is an anode, the counter is the spectral-pure carbon electrode, sharpened to a cone with ground diameter of 1.5−2 mm.

The interelectrode gap is set on the shadow projection on the intermediate aperture before the exposure begins.

Exposure 40 s. the slot Width 0.012 mm. in the Interelectrode gap of 2.5 mm is maintained throughout the exposure.

For photographing spectra in the cassette spectrograph placed photographic plates of two types. In the long-wave part of the spectrum for the determination of copper, silver, India placed the photographic plates of type I in the shortwave part of the spectrum, a photographic plate of the type II. The junction line of the plates is approximately at the site of the lengths of the waves 315,0−317,0 nm.

The spectrogram of the analyzed samples and the calibration samples should be taken on the same photographic plate. Take pictures of at least four calibration samples. For each sample removed at least three of the spectrograms. For each sample spectrograms get 15 (3 of each chlorinated sample).

Manifestation and fixation is carried out according to GOST 10691.0-GOST 10691.4.

3.3. Processing of the results

3.3.1. The resulting spectrogram photometric with microphotometry. The applied analytical lines and the intervals of concentration of the impurities are shown in table.2.

Table 2

The assessment of mass fraction of impurities to produce the absolute blackening of analytical lines.

Calibration graphs constructed in the coordinates: the absolute blackening of the impurity lines is the logarithm of the impurity concentration in the calibration sample.

Mass fraction of impurity in the sample () in percent is calculated by the formula

,

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

 — mass concentration of impurities determined in the schedule, %;

 — weight of tin,

3.3.2. The absolute discrepancies in the results of parallel measurements at a confidence probability of 0.95 should not exceed the values given in table.3.

Table 3

4. DETERMINATION OF ALUMINIUM

4.1. Preparation for assay

4.1.1. For preparation of calibration samples using a metal tin, spectral-pure aluminium. The sample tin is placed in a quartz Cup and dissolved in distilled concentrated nitric acid while stirring with a glass rod. After dissolution of the sample the resulting mush metalbands acid was evaporated under an infrared lamp to obtain a dry residue. The dry residue over a 40 min calcined in muffle at 800 °C. the Resulting tin oxides are transferred into an agate mortar, triturated and then poured into a glass boxy. Sample of tin oxide in 10.0 g is placed in a quartz Cup, introduced at 1,0; 2,5; 5,0 and 15.0 cmto the standard solution of aluminium was mixed thoroughly and evaporated under an infrared lamp to obtain a dry residue. The dry residue over a 40 min calcined in muffle at 800 °C. the resulting standards are transferred into an agate mortar and ground for 30−40 min, then poured into glass buxy for storage.

4.1.2. Sample preparation: from average samples are taken in the form of chips of thin plates two sample weighing 1 g of Sample was dissolved in quartz cups with a capacity of 100−150 cmin distilled concentrated nitric acid. Mush metalbands acid was evaporated under an infrared lamp to obtain a dry residue. The residue for 20 min calcination in muffle at 800 °C. the Resulting oxide powder is ground in an agate mortar.

4.2. Analysis

4.2.1. A portion of the calibration sample or analyte sample with a mass of 0.03 g is placed in crater of the spectral-pure carbon electrode with a diameter of 3 mm and a depth of 2 mm. the excitation Source is the arc of a DC voltage of 200−400 V and a current of 8 A. the Electrode with the charge of the sample or the calibration sample is the anode, and spectral-pure charcoal, sharpened to a cone with an area of diameter 1.5−2 mm, the cathode.

When photographing spectra in the cassette spectrograph placed photographic plates of type I. the Width of the slit of a spectrograph 0.012 mm. in the Interelectrode gap equal to 2.5 mm in the arc (as the combustion of the electrodes) is adjusted by a projection on the diaphragm. Precalcination required to burn the bulk of tin, equal to 40 C, operating exposure — 60 s.

Spectra of unknown samples and calibration samples should be taken on the same photographic plate. For each calibration sample receive at least three spectrograms for a sample of four spectrograms (two from each expansion).

Manifestation and fixation is carried out according to GOST 10691.0-GOST 10691.4.

4.3. Processing of the results

4.3.1. In the resulting spectrograms photometric line of aluminium 309,2 nm and line tin 322,3 nm. Calculate the difference of pochernenija and find .

The calibration graphs are built in coordinates , where the aluminium concentration in the calibration samples. Largest samples in the calibration schedule to determine the concentration of impurities in the sample.

4.3.2. Allowable absolute discrepancies in the results of parallel measurements at a confidence probability of 0.95 does not exceed the values given in table.4.

Table 4

5. SEMI-QUANTITATIVE SPECTRAL METHOD FOR THE DETERMINATION OF ALUMINIUM AND IRON

5.1. The essence of the method

The method is based on photographing the spectra of standard samples of the enterprise (SOP) and samples excited by a spark discharge and a visual comparison of pochernenija analytical lines of the determined elements obtained by the spectrogram.

5.2. Apparatus, reagents and solutions — sec. 2.

5.3. Analysis

5.3.1. As the standard samples of the enterprise for determination of aluminum and iron use samples of tin metal with a known mass fraction of aluminum 3·10% and iron 1·10%.

Standard samples of the enterprise is prepared in the form of rods with diameter 7−8 mm and a length of 70−80 mm by casting pewter into a mold.

5.3.2. Before shooting the ends of the analyzed and standard samples sharpen on the plane.

The excitation source is alternating current arc force 3−3,5 A.

5.3.3. Survey samples and standard samples is carried out on the spectrograph. Intermediate diaphragm and the slot width are selected optimum from the type of device and records. Exposure — not less than 20 s.

5.3.4. In the cassette of the spectrograph in wavelength part of the spectrum is placed a plate type SP-2.

For the standard sample is removed at least two spectrograms for each sample at least three.

5.3.5. A photographic plate obtained with spectrograms mounted on spectromancer and visually compare the blackening of analytical lines of aluminum and iron in a standard sample of the enterprise and in the samples.

Recommended analytical lines: Fe — 358,1 nm; Al — 396,1 nm.

Section 5. (Added, Rev. N 3).