GOST 9816.4-2014

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  ГОСТ 9816.4-2014

GOST 9816.4−2014 Tellurium technical. Method of spectral analysis

GOST 9816.4−2014

INTERSTATE STANDARD

TELLURIUM TECHNICAL

Method of spectral analysis

Tellurium technical. Method of spectral analysis

ISS 77.120.99

Date of introduction 2015−09−01

Preface

Goals, basic principles and main procedure of works on interstate standardization have been established in GOST 1.0−92 «interstate standardization system. Basic provisions» and GOST 1.2−2009 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. Rules of development, adoption, application, renewal and cancellation"

Data on standard

1 DEVELOPED by the Technical Committee for standardization TC 368 «Copper"

2 recorded by the Interstate technical Committee for standardization MTK 503 «Copper"

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol dated 30 may 2014 No. 67-P)

The adoption voted:

4 by Order of the Federal Agency for technical regulation and Metrology dated 26 November 2014 N 1776-St inter-state standard GOST 9816.4−2014 introduced as the national standard of the Russian Federation from September 1, 2015.

5 REPLACE GOST 9816.4−84


Information about the changes to this standard is published in the annual reference index «National standards», and the text changes and amendments — in monthly information index «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in the monthly information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet

1 Scope

This standard specifies the emission spectral method of measuring with a photoelectric spectra the mass fraction of copper, iron, lead, sodium, selenium, silicon, aluminum, silver, Nickel, technical tellurium in the range of mass fraction, are presented in table 1.


Table 1

Percentage

2 Normative references

This standard uses the regulatory references to the following international standards:

GOST 1770−74 laboratory Glassware measuring glass. Cylinders, beakers, flasks, test tubes. General specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 4217−77 Reagents. Potassium nitrate. Specifications

GOST 4233−77 Reagents. Sodium chloride. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 12026−76 laboratory filter Paper. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 9816.0−84 Tellurium technical. General requirements for methods of analysis

GOST 16273.0−82* Selenium technical. General requirements for method of spectral analysis

________________
* Probably, the error of the original. Should read: GOST 16273.0−85, here and hereafter. — Note the manufacturer’s database.


GOST 18300−87 ethyl rectified technical. Specifications

GOST 19908−90 Crucibles, bowls, beakers, flasks, funnels, test tubes and caps made of transparent quartz glass. General specifications

GOST 23463−79 Graphite powder of high purity. Specifications

GOST 24104−2001* laboratory Scales. General technical requirements
________________
* On the territory of the Russian Federation GOST R 53228−2008 «Scales non-automatic actions. Part 1. Metrological and technical requirements. Test».


GOST 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions

GOST 29227−91 (ISO 835−1-81) oils. Pipettes are graduated. Part 1. General requirements

GOST ISO 5725−6-2003* Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice
________________
* On the territory of the Russian Federation GOST R ISO 5725−6-2002 «Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice».

Note — When using this standard appropriate to test the effect of reference standards for the sign «National standards» drawn up as of January 1 of the current year and related information signs, published in the current year. If the reference standard is replaced (changed), when using this standard should be guided by replacing (amended) standard. If the reference standard is cancelled without replacement, then the situation in which the given link applies to the extent that does not affect this link.

3 Characteristics of measurement accuracy

The accuracy of the measurements the mass fraction of copper, silver, Nickel, lead, sodium, aluminium, iron, silicon, selenium corresponds to the characteristics given in tables 2, 3 (for P =0,95).

Limit values of repeatability and reproducibility of measurements for a confidence probability P =0.95 are shown in tables 2, 3.


Table 2 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of mass fraction of copper, silver, Nickel, lead, sodium, aluminium, iron, silicon, selenium at a confidence probability P=0.95 (at a mass fraction of tellurium from 99,95% or more)

Percentage

Table 3 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of mass fraction of copper, lead, sodium, aluminium, iron, silicon, selenium at a confidence probability P =0.95 (at a mass fraction of tellurium from 96,5% to 99.95%)

Percentage

4 measurement Means, auxiliary devices, materials, solutions

When performing measurements using the following measuring instruments and auxiliary devices:

— diffraction spectrometer type IFS with the analyzer Maes;

— drying Cabinet, providing a heating temperature of from 100 °C to 105 °C;

— special laboratory scales of accuracy class according to GOST 24104;

— device for sharpening carbon electrodes, for example, the machine model CP-35, or CCS-6;

box of organic glass;

— a mortar made of organic glass;

electrodes graphite high purity [1]*, grade not below the EU 12, with a diameter of 6 mm, a length of 35−55 mm:
________________
* See Bibliography, here and hereafter. — Note the manufacturer’s database.

1) sharpened to a cone;

2) crater with a diameter of 4 mm and a depth of 4 mm;

3) a crater with a diameter of 4 mm and a depth of 8 mm;

— stainless steel tweezers;

— volumetric flasks 2−50−2 according GOST 1770;

— flasks KN-2−100−13/23ТХС according to GOST 25336;

— a Cup of quartz according to GOST 19908;

pipettes 1−2-2−1, 1−2-2−2, 1−2-2−5, 1−2-2−10 according to GOST 29227.

When performing measurements, use the following materials, solutions:

— nitric acid of high purity according to GOST 11125 or nitric acid according to GOST 4461 (distilled);

— hydrochloric acid according to GOST 3118;

— distilled water according to GOST 6709;

— potassium nitrate according to GOST 4217;

— ethyl alcohol according to GOST 18300. Consumption of alcohol per one determination is 10 g;

sodium chloride according to GOST 4233

— graphite powder of high purity according to GOST 23463;

— aluminum oxide with a mass fraction of the basic substance of 99.9%;

— iron (III) oxide with a mass fraction of the basic substance of 99.9%;

— copper oxide with a mass fraction of the basic substance of 99.9%;

— arsenic (III) oxide with a mass fraction of the basic substance of 99.9%;

— bismuth oxide with a mass fraction of the basic substance of 99.9%;

lead oxide with a mass fraction of the basic substance of 99.9%;

— silicon (IV) oxide with a mass fraction of the basic substance of 99.9%;

— the state standard samples of composition of ion solution of silver, aluminum, copper, iron, Nickel, lead, silicon, and sodium mass concentration of 1 g/DM;

the elementary selenium [2];

— tellurium metal, high purity [3].

Notes

1 allowed the use of other measuring instruments of the approved type, auxiliary devices and materials, technical and metrological characteristics are not inferior to mentioned above.

2 allowed the use of reagents produced by other normative documents, provided that their metrological characteristics of the measurement results given in the measurement technique.

5 Method of measurement

The method is based on measuring the intensity of spectral lines of the designated components during combustion of the sample from a crater of the carbon electrode.

5.1 Preparation for measurement

5.1.1 preparation of the device for measuring

The device prepared for measurement in accordance with the requirements of the current operating instructions of the mass spectrometer. Set the operating parameters of the measurements in accordance with table 4.


Table 4

Analytical lines of the designated components, free from spectral overlaps N 1 presented in table 5.


Table 5

Analytical lines of the designated components, free from spectral overlaps N 2, are presented in table 6.


Table 6

5.1.2 Spectrometer will graduate when you create a method using samples of comparison composition of tellurium with each series of samples, building dependence of the intensity of the analytical line from the mass fraction for each component you define.

In future work adjust calibration parameters in accordance with the manual of the spectrometer.

5.1.3 Graphite electrodes with a crater and «cone» machined on the grinding machine in accordance with the operating manual.

5.1.4 sample Preparation comparison

5.1.4.1 comparison Samples prepared in accordance with Annex A.

5.1.4.2 sample Set of comparison of the composition of the tellurium N 1 (mass fraction of tellurium from of 99.95% and above)

Value of mass fraction of aluminium, iron, copper, Nickel, lead, silver, silicon, sodium, and selenium in samples of comparison composition of tellurium TL — 1−8TL — 1−1, are presented in table 7.


Table 7

Percentage

5.1.4.3 a Set of samples comparison of composition of tellurium in N 2 (with a mass fraction of tellurium from 96,5% to 99.95%)

The values of the mass fraction of aluminum, copper, iron, lead, silicon, sodium, and selenium in samples comparison of the composition of Selena T — 2−8T — 2−1, presented in table 8.


Table 8

Percentage

5.1.5 preparation of the buffer mixture

Sample graphite powder weighing 4,889 g and bismuth oxide by weight of 0,111 g is placed in a mortar, stirred with the use of ethyl alcohol at the rate of 1.0 to 1.5 cmper 1 g of the mixture to drying and allowed to stand for 1 hour in a muffle furnace at a temperature of from 100 °C to 105 °C. From the mixture, take the sample weighing 0,500 g, placed in a mortar, add 0,517 g of potassium nitrate, 3,983 g of graphite powder and stirred with the use of ethyl alcohol at the rate of 1.0 to 1.5 cmper 1 g of the mixture to drying and allowed to stand for 1 hour in a muffle furnace at a temperature of from 100 °C to 105 °C. the Buffer mixture contains 0.2% of bismuth and 4.0% potassium. The mixture is stable for three years.

Note — change of the mass of sample components, provided the content in a buffer mixture of 0.2% of bismuth and 4.0% potassium.

5.2 performance measurement

5.2.1 General requirements for method of measurements in accordance with GOST 16273.0.

5.2.2 Mass fraction of impurities in the sample and the control sample to determine the parallel of the two batches, taking three individual measurements from each sample.

5.2.3 Measurement of the mass fraction of components in the technical tellurium with a mass fraction of tellurium from 99.95 percent and higher.

The sample is mixed with powdered graphite at a ratio of 4:1 (0.8 g sample, 0.2 g of graphite) in a mortar made of organic glass.

Prepared samples and samples of N 1 comparisons to fill the craters of graphite electrodes with a diameter of 4 mm and a depth of 8 mm by immersion.

5.2.4 Measurement of the mass fraction of components in the technical tellurium with a mass fraction of tellurium from 96,5% to 99.95%.

The sample is mixed with a buffer mixture in the ratio 1:1 (0.4 g sample, 0.4 g buffer mixture) in a mortar made of organic glass.

Prepared samples and the comparison samples No. 2 to fill the craters of graphite electrodes with a diameter of 4 mm and a depth of 4 mm by immersion.

Note — change of the mass of sample sample and buffer mixture while maintaining the ratio of 1:1.

5.2.5 Simultaneously through all stages of sample preparation to the measurements carried out control and experience on the purity of reagents and materials.

Note — the Mass fraction of the designated component of experience the idle should not exceed the lower limit of the range of the designated contents.

5.2.6 measurement of mass fractions of impurities in the samples is carried out in accordance with the manual of the spectrometer.

5.3 Processing of results

5.3.1 Processing of results of measurements carried out using a software for a given program and present them in the form of a mass fraction of the designated component.

5.3.2 measurement results take the arithmetic mean of two parallel definitions, provided that the absolute difference between them in terms of repeatability does not exceed the value (at confidence probability P=0.95) repeatability limit r given in tables 2 and 3.

If the discrepancy between the results of parallel measurements exceeds the limit value of the frequency of occurrence, perform the procedure described in GOST ISO 5725−6 (paragraph 5.2.2.1).

5.3.3 Differences between measurements obtained in two laboratories, should not exceed the limit values repeatability, are shown in tables 2 and 3. In this case, the final result can be accepted their mean value. At default of this condition can be used the procedure set out in GOST ISO 5725−6.

Annex a (recommended). Sample preparation comparison of composition of tellurium

Appendix A
(recommended)

A. 1 sample Preparation N 1 comparison of composition of tellurium

A. 1.1 For preparation of the main solution composition of selenium of selenium a hitch weight of 1,000 g was placed in a conical flask with a capacity of 100 cm, pour from 6 to 10 cmof a mixture of hydrochloric and nitric acids 3:1 and dissolved by heating, the solution was cooled, transferred to a volumetric flask with a capacity of 50 cm, adjusted to the mark with water and mix.

A. 1.2 For preparing a mixture composition of graphite powder G-1 And with a mass fraction of aluminum, iron, copper, Nickel, lead, silver and 0.02%, silicon, selenium and sodium 0.2% in quartz Cup is placed a portion of the graphite and aliquote part of the certified reference material of composition of the solution of aluminum ions, iron, copper, Nickel, lead, silver and silicon and the basic solution of the composition of selenium in accordance with table A. 1. The resulting mixture is dried, placed in a mortar, add sodium chloride (table A. 1) and stirred with application of ethyl alcohol at the rate of 1.0 to 1.5 cmper 1 g of the mixture before drying and kept in a desiccator for one hour at a temperature of from 100 °C to 105 °C.


Table A. 1

A. 1.3 sample Preparation comparison of composition of tellurium TL — 1−8TL — 1−1 is carried out in two stages.

— prepare a mixture composition of graphite Gr-8Gr-1;

— each of the prepared mixtures in the composition of the graphite is mixed with four times by weight the amount of tellurium.

A. 1.3.1 a Series of mixtures of the composition of graphite Gr-8Gr-1 is prepared by the method of successive dilution of the primary mixture of Gr — 1 graphite powder. Sample of the mixture taken for the bulk and graphite powder*, according to table A. 2, placed in a mortar and stirred with the use of ethyl alcohol at the rate of 1 to 1.5 cmper 1 g of the mixture before drying and kept in a desiccator for one hour at a temperature of from 100 °C to 105 °C. the Values of mass fraction of aluminium, iron, copper, Nickel, lead, silver, silicon, sodium, selenium in a series of mixtures of the composition of graphite powder GRS-8GRS-1 is presented in table A. 2.
___________________
* The text of the document matches the original. — Note the manufacturer’s database.


Table A. 2

A. 1.3.2 a Series of samples of comparison composition of tellurium TL — 1−8 TL — 1−1 prepared by dilution method from each of the prepared mixtures in the composition of graphite four times by weight the amount of tellurium. The sample mixture composition of graphite and tellurium (in accordance with table A. 3) placed in a mortar and stirred with the use of ethyl alcohol at the rate of 1 to 1.5 cmper 1 g of the mixture before drying and kept in a desiccator for one hour at a temperature of from 100 °C to 105 °C.

Value of mass fraction of aluminium, iron, copper, Nickel, lead, silver, silicon, sodium, selenium in samples of comparison composition of tellurium TL — 1−8 TL — 1−1 is presented in table A. 3.


Table A. 3

Mass fraction of components in the tellurium was determined by additives and added to the calculated content of impurities in the samples comparison.

A. 2 Preparation of the samples the N 2 comparison of composition of tellurium

A. 2.1 For preparation of the main sample of tellurium TL — 2 with a mass fraction of aluminum, copper, iron, lead, silicon, sodium and selenium 1.0% in a mortar put the hitch components and aliquot part of the solution of selenium, according to table A. 4. The mixture was stirred with the use of ethyl alcohol at the rate of 1.0 to 1.5 cmper 1 g of the mixture before drying and kept in a desiccator for one hour at a temperature of from 100 °C to 105 °C.


Table A. 4

The expiration date of the basic sample structure of tellurium TL — 2 And one year.

A. 2.2 a Series of samples of comparison composition of tellurium TL — 2−8TL — 2−1 prepare by the method of successive dilution of the sample TL — 2-metal tellurium. Sample reference sample (considered as primary) and tellurium, according to table A. 5, placed in a mortar and stirred with the use of ethyl alcohol at the rate of 1.0 to 1.5 cmper 1 g of the mixture before drying and kept in a desiccator for one hour at a temperature of from 100 °C to 105 °C.


Table A. 5

Shelf life of samples comparisons of one year.

Bibliography