GOST 22397-77

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  ГОСТ 22397-77

GOST 22397−77 zinc Powder. Method of spectral analysis (with Amendments No. 1, 2, 3)

GOST 22397−77

Group B59

STATE STANDARD OF THE USSR

ZINC POWDER

Method of spectral analysis

The Zinc powder. Method of spectral analysis

AXTU 1709

Date of introduction 1978−01−01

INFORMATION DATA

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

DEVELOPERS

HP Garcin, N. F. Sachkov, A. A. Kopylov, V. K. Zemlyanskaya

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 22.03.77 N 678

3. INTRODUCED FOR THE FIRST TIME

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. The expiration time limit is removed by the Resolution of Gosstandart from 08.04.92 N 374

6. REPRINT (October 1996) with Amendments No. 1, 2, 3, approved in March 1983, June 1987, September 1992 (IUS 5−83, 9−87, 7−92)


This standard specifies the spectral method for determination of lead, iron, tin, copper, cadmium, antimony and arsenic in a zinc powder.

The method is based on pre-converting zinc powder into zinc oxide and subsequent determination of the impurities in the resulting zinc oxide in the arc of DC by the method of «three standards» for the calibration graphs constructed in the coordinates .

The method allows to determine the following impurities in mass fractions, %:

Note. Mass fraction of arsenic in brands of zinc powder PC1, PC2 and mass fraction of antimony in marks PC1, PC2, PC3 and PC7, respectively, determined according to GOST and GOST 19251.4 19251.6.


(Changed edition, Rev. N 1, 2, 3).

1. GENERAL REQUIREMENTS

1.1. Samples produced according to GOST 12601.

1.2. General requirements for method of analysis according to GOST 25086.

(Changed edition, Rev. N 3).

1.3. (Deleted, Rev. N 1).

1A. SAFETY REQUIREMENTS

1a.1. In the analysis of zinc powder in the laboratory of spectral analysis should be carried out on appliances and electrical installations, mass-manufactured on the drawings manufacturers, the relevant regulations for electrical installation, approved by Gosenergonadzor.

Samples of zinc powder submitted for analysis must be stored in packages of construction paper, and reagents used for the analysis in the original packaging, in cupboards or boxes made of organic glass, equipped with ventilation.

1A.2. In the use and operation of electrical appliances and electrical installations in the process of spectral analysis, one should follow safety rules of electrical installations and safety rules at operation of electrical installations, approved by Gosenergonadzor, as well as the requirements of GOST 12.3.019.

All appliances should be equipped with devices for grounding corresponding to requirements of GOST 12.2.007.0 and labeled according to GOST 2.721. Grounding shall conform to the requirements of the rules for electrical installations approved by Gosenergonadzor.

(Changed edition, Rev. N 3).

1A.3. When performing tests, it is necessary to observe the basic rules of safe work in chemical laboratories*.
________________
* On the territory of the Russian Federation the document is not valid. Acts PND f 12.13.1−03. — Note the manufacturer’s database.

1A.4. To prevent entering the working area of harmful substances emitted in the sources of spectra excitation and bad acting on the body working, in quantities exceeding maximum permissible concentration and for protection against electromagnetic radiation and prevent sunburn by ultraviolet rays, each a source of excitation spectra should be placed inside of the device, equipped with an integrated exhaust air inlet according to GOST 12.4.021 and protective screen.

1A.5. The machine is used for grinding carbon electrodes must have a built-in exhaust air inlet to prevent the ingress of carbon dust in the air, in quantities exceeding maximum permissible concentration.

1A.6. Preparation of samples for analysis (dissolution, and the collection of batches, grinding, gasket carbon electrodes) must be in the pits, equipped with built-in exhaust air terminals.

1A.7. Control of content of harmful substances in the air of working zone shall be carried out according to GOST 12.1.007 and GOST 12.1.005.

Analyses of air samples for the content of harmful substances in the air of working zone is performed according to the methods of determination of harmful substances in the air, approved by the Ministry of health of the USSR developed in accordance with GOST 12.1.016.

(Changed edition, Rev. N 3).

1A.8. Samples of zinc powder, the remainder of the analysis must be returned to the manufacturer (customer).

The recycling, disposal and destruction of zinc powder and harmful substances — waste from the production tests should be carried out in accordance with the documentation approved in the established order and agreed with the sanitary-epidemiological service of the USSR.

1A.9. The laboratory of spectral analysis must have General dilution ventilation and local exhaust ventilation, which connect the air terminals embedded in the equipment in which dangerous substances, in accordance with the requirements of GOST 12.4.021.

1A.10. To prevent the risk of fire must comply with fire safety requirements according to GOST 12.1.004.

The laboratory must be equipped with means of fire extinguishing and fire fighting equipment according to GOST 12.4.009.

(Changed edition, Rev. N 3).

1A.11. All work in the test must be performed in a dry working clothes and safety equipment (rubber gloves, goggles) in accordance with current standard regulations of free issue of workwear, footwear and protective equipment to workers and employees of non-ferrous metallurgy approved by the state Committee for labour and social Affairs at the Council of Ministers of the USSR and GOST 12.4.011. Clothing should be stored in racks separately from your own clothes, weekly, handing it to the Laundry. Washing of workwear to implement centralized in specialized laundries with preliminary degassing and dezactiveaza. The removal of clothing and stay in it beyond the working area is not allowed.

(Changed edition, Rev. N 2, 3).

1A.12. In the analysis of zinc powder in the laboratory of spectral analysis should be provided special premises and devices according to SNiP-92−76 group III production processes.

The premises of the laboratory of spectral analysis and their illumination must comply with the requirements of SN-245 and SNiP II-4−79*.
______________
* On the territory of the Russian Federation there are SNiP 23−05−95. — Note the manufacturer’s database.

(Changed edition, Rev. N 2).

1A.13. Working in the chemical and spectral laboratories shall provide the milk in accordance with the rules of free issue of milk and other equivalent foodstuffs to the workers and employees in factories, workshops, sections and other subdivisions with harmful working conditions is approved by the state Committee for labour and social Affairs at the Council of Ministers of the USSR, which must be taken before or after work.

1A.14. To work in the spectral laboratories should be permitted to persons over the age of 18, trained in the basic techniques of working on appliances and electrical installations in accordance with the rules of safety at operation of electroinstallations of consumers, approved by Gosenergonadzor, and methods of analysis.

Coming to work and working should take place:

preliminary and periodic medical examinations;

preliminary training in the work with hazardous substances and treatment with protective means;

the safety with the corresponding registration in the prescribed manner according to GOST 12.0.004.

(Changed edition, Rev. N 3).

2. APPARATUS, MATERIALS AND REAGENTS

The diffraction type spectrograph DFS-8 (grating 600 PCs/mm) being the illumination system of the slit and the three-step attenuator.

The quartz spectrograph medium dispersion of any type with being an illumination system of the slit.

A constant current source, designed for 250−300 In 30−50 A.

Generator activated arc designed to ignite the DC arc high frequency discharge.

Microphotometer of any type, allowing to measure the density of the blackening of analytical lines.

Libra torsion bar type W with a weighing error of no more than 0.001 g.

Muffle furnace with thermostat, allowing the temperature to 600 °C.

The agate mortar.

Mortar made of organic glass.

The heat-resistant beakers with a capacity of 300 cm.

Porcelain Cup with a diameter of 50 and 100 mm.

Nitric acid ultraclean nitric acid ultraclean nitric acid or 19−4 23−4 according to GOST 11125 and solutions 1:1 and 1:2.

The technical rectified ethyl alcohol according to GOST 18300.

The graphite powder of high purity according to GOST 23463.

Graphite electrodes of high purity (in the determination of the mass fraction of arsenic and antimony is allowed to use coal brand S3 on the other 16−538−240 6 mm in diameter with a crater size 4x4 mm).

Photographic plates spectrographic type I or ES and type UPS-3.

For the manifestation of the plates of type-I and type-ES using developer of the following composition:

Before the manifestation of the solutions 1 and 2 mixed in a ratio of 1:2.

For the manifestation of plates of the type UFS-3 use developer D-19 of the following composition:

Fixer is acidic:

Lead according to GOST 3778*.
______________
* On the territory of the Russian Federation GOST 3778−98. — Note the manufacturer’s database.

Copper according to GOST 859*.
______________
* On the territory of the Russian Federation GOST 859−2001. — Note the manufacturer’s database.

Radio engineering carbonyl iron according to GOST 13610.

Tin GOST 860.

Cadmium GOST 1467.

Elementary arsenic.

Zinc GOST 3640.

Antimony GOST 1089.

Tartaric acid according to GOST 5817.

Oxalic acid according to GOST 22180.

Distilled water according to GOST 6709, double-distilled or obtained on ionization column.

Note. Allowed the use of devices with photoelectric registration of spectrum and other spectrographic devices and systems, the use of other materials, photographic plates and reagents, including foreign ones, providing the accuracy, regulated in this standard.


References to build calibration graphs are given in Appendix.

For the preparation of standard solutions and comparison samples used metals with a mass fraction of main substance not less than 99.99%.

The time of development of photographic plates of all types 4−5 minutes at a temperature of 18−20 °C.

(Changed edition, Rev. N 1, 2, 3).

3. ANALYSIS

3.1. Determination of lead, iron, copper, tin and cadmium.

3.1.1. From each sample taken at two sample weight 1−2 g, is converted into the oxide as well as the basis (see Annex). Obtained after calcination of zinc oxide are thoroughly ground in a mortar.

In the analysis of zinc powder brands PC1 and PC2 should use a mortar made of organic glass to avoid any contamination of samples with iron. In the analysis of the powder other brands (PC3, PC4, PC6) you can use an agate mortar.

Samples of the comparisons are mixed with graphite powder in a ratio of 2:1 and fill in the crater of a carbon electrode with a size of 4x4 mm.

As the top electrode using a carbon electrode, sharpened to a truncated cone.

3.1.2. The determination of the above impurities is carried out on diffraction spectrograph of the DFS-8 with three-lens Achromat illumination system of the slit. For the analysis of zinc powder brands PC1 and PC2 allowed to use a quartz spectrograph medium dispersion. On the slit of the instrument, establish a three-tier reliever. The slot width 0,020 mm. the Spectra are photographed on photographic plates spectrographic type 1 or ES. As a source of excitation spectra using the arc of direct current strength of 10 A. the Ignition is performed by the generator is activated the arc. The lower electrode serves as the anode. Intermediate diaphragm depends on the sensitivity of photographic plates. The distance between the electrodes 3 mm. exposure Time 60 s.

Allowed from the sample of zinc powder brands PC6 and PC7 with the press providing a pressure of 100 t/cm, to obtain a monolithic sample length less than 40 mm and a diameter of at least 10x10 mm, and perform the analysis on the content of lead, iron, copper, tin, cadmium, and arsenic GOST 17261.

3.1.1, 3.1.2. (Changed edition, Rev. N 1, 2, 3).

3.1.3. To construct the calibration graphs using the following pairs of lines:

3.2. Determination of antimony and arsenic

3.2.1. The sample for analysis is prepared according to claim 3.1.1.

In the determination of antimony and arsenic is allowed to use from clean coal S-3 or S-2.

(Changed edition, Rev. N 2).

3.2.2. Determination of antimony and arsenic is carried out using a quartz spectrograph medium dispersion being a lighting system. The width of the slit of a spectrograph 0,020 mm. intermediate diaphragm depends on the sensitivity of photographic plates. As a source of spectra excitation using arc DC power 8 A. the Ignition is carried out by high frequency discharge. The lower electrode serves as the anode. The spectra are photographed on photographic plates of the type UFS-3. The exposure time is 80 s.

(Changed edition, Rev. N 3).

3.2.3. To construct the calibration graphs using the following pairs of lines:

4. PROCESSING OF THE RESULTS

4.1. Spectra of the samples and comparison samples are photographed on the same plate three times. The blackening of analytical lines and comparison lines measured on microphotometer. The calibration graphs are built in coordinates , where is the average of the three values ,  — known mass fraction determined by impurities in the samples of the comparison in percent. The graphs determine the mass fraction of impurities in the samples using the known values . The final result of the analysis should be the arithmetic mean of two parallel definitions (each of the three spectrograms).

(Changed edition, Rev. N 3)

.

4.2. The maximum discrepancies of the results of parallel measurements () and the results of two tests (), calculated with a confidence level of 0.95, should not exceed the values calculated by the formulas

for lead, cadmium, copper and tin;

for iron and antimony;

for arsenic,

where is the arithmetic mean of the results of parallel measurements;

for lead, cadmium, copper and tin;

for iron, antimony;

for arsenic,

where is the arithmetic mean of the results of the two tests.

The allowable divergence is rounded up to numbers with one significant figure and the numerical values of the results of the analysis and parallel measurements — up to

two.

4.3. Control of correctness of the analysis carried out according to GOST 25086 when changing batches of samples comparison in the repair spectrographic installations, after long interruptions and other changes that affect the result of the analysis.

(Changed edition, Rev. N 3).

APP (mandatory)

APP
Mandatory

1. Sample preparation comparison

1.1. The basis for the preparation of samples of comparison is zinc oxide obtained from zinc powder brand PC2 according to GOST 12601 or zinc brand or CV CV0 according to GOST 3640. Necessary for the preparation of the samples the amount of zinc or zinc powder was placed in a Pyrex beaker and dissolved in nitric acid. The solution was transferred to a porcelain Cup and evaporated to dryness (until the termination of allocation of oxides of nitrogen) and calcined in a muffle furnace (500±20) °C for 30 min. If the present of trace elements, their content must be considered in the calculations.

Zinc oxide is stored in a plastic container with screw-caps or glass buksh.

2. Standard solutions

2.1. Standard solution of lead

0.5 g of lead metal pieces are dissolved in nitric acid solution 1:2 with moderate heating. After dissolution of the entire sample solution was cooled and quantitatively transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.005 g of lead.

2.2. Standard solution of iron

0.5 g of iron metal recovered was dissolved in 10 cmof nitric acid solution 1:1, under low heat. The solution was cooled, transferred quantitatively into a measuring flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.005 g of iron.

2.3. A standard solution of copper

0.5 g of metallic copper in the form of chips is dissolved in 10 cmof nitric acid solution 1:1, under low heat. The solution was cooled and quantitatively transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.005 g of copper.

2.4. Standard solutions of tin

0.1 g of finely divided metallic tin is placed in a beaker with a capacity of 100 cm, add 4 g of oxalic acid and 5 cmof nitric acid. The dissolution is initially at room temperature, then at low heat (50±10) °C. After the solution becomes transparent, add 10 cmof water, quantitatively transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with water.

1 cmof the solution contains 0.001 g of tin.

10 cmsolution And transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with water.

1 cmof the solution contains 0.0001 g tins

.

2.5. A standard solution of cadmium

1 g cadmium metal was dissolved in 20 cmof nitric acid solution 1:1. The solution was cooled and quantitatively transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.01 g of cadmium.

2.6. Standard solution of antimony

0.5 g of powdered metallic antimony is dissolved in 5 cmof nitric acid with the addition of 10 g of tartaric acid in low heat, quantitatively transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.005 g of antimony.

2.7. Standard solution of arsenic

0.5 g of powdered elemental arsenic is dissolved in 10 cmof nitric acid when heated. The solution was cooled, transferred quantitatively into a measuring flask with a capacity of 100 cm, adjusted to the mark with water and mix.

1 cmof the solution contains 0.005 g of arsenic.

For the preparation of solutions it is possible to use oxides, carbonates or nitrates of the above metals qualification h. d. a. or H. h

Head of the calibration sample, containing 0,06% lead, 0.04% of iron, 0.01% copper, 0.003% of tin, 0.4% cadmium, 0.03% of arsenic and antimony, is prepared as follows.

In a porcelain Cup with a capacity of 50 cmwill prevent 10 g of zinc powder or zinc of the same brands, of which prepare the base, dissolved in nitric acid solution 1:1 and add 1.2 cmof a solution of lead 0.8 cmof a solution of iron, 0.2 cmof a solution of copper, 3 cmof solution In tin, 4 cmof a solution of cadmium and 0.6 cmsolutions of arsenic and antimony. The contents of the Cup is dried under a lamp and calcined in a muffle furnace at (500±20) °C for 30 min and thoroughly mixed in a mortar for 1 h.

Working samples of comparison prepare a serial dilution 2−3 times each newly prepared sample basis.

To determine the mass fraction of lead, iron, cadmium, copper and tin are preparing a series of samples to determine the mass fraction of arsenic and antimony with the other.

Samples stored in glass buksh or plastic jars with screw lids.

The comparison samples, prepared on each enterprise according to the specified methodology shall be certified in accordance with normative-technical documentation.

The maximum allowable error value setting the values of CRM certified characteristics of the samples of the comparison does not exceed 1.5% of the certified value of the content component.

App. (Changed edition, Rev. N 2, 3).