GOST 12601-76
GOST 12601−76 zinc Powder. Technical specifications (with Changes 1−5 N)
GOST 12601−76
Group 56
STATE STANDARD OF THE USSR
ZINC POWDER
Specifications
The Zinc powder. Specifications
GST 17 2132
Date of introduction 1978−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
Vakhrusheva L. Z., M. I. Zinoviev, Bendrick A. R., Maxi L. I., Lysenko V. I.
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. REPLACE GOST 12601−67
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced | The number of the paragraph, subparagraph |
GOST 12.1.004−91 |
2A.6.1 |
GOST 12.1.005−88 |
2A.3; 2A.3.1 |
GOST 12.1.010−76 |
2A.6.1 |
GOST 12.1.016−79 | 2A.3.1 |
GOST 12.3.009−76 |
2A.12 |
GOST 12.4.009−83 |
2A.6.2 |
GOST 12.4.021−75 |
2A.7 |
GOST 12.4.026−76 |
2A.6.4 |
GOST 12.4.028−76 |
2A.11 |
GOST 199−78 |
4.3.1 |
GOST 892−89 |
4.9.1 |
GOST 1277−75 |
4.8.1 |
GOST 1467−93 |
4.5.1 |
GOST 2062−77 |
4.5.1 |
GOST 2874−82 |
2A.3.2 |
GOST 2991−85 |
5.1 |
GOST 3118−77 |
4.5.1, 4.8.1 |
GOST 3640−94 |
1.1, 4.5.1 |
GOST 4204−77 |
4.3.1 |
GOST 4233−77 |
4.5.1 |
GOST 4461−77 |
4.5.1 |
GOST 4529−78 |
4.5.1 |
GOST 4658−73 |
4.5.1 |
GOST 5037−78 |
5.1 |
GOST 5799−78 |
5.1 |
GOST 6552−80 |
4.3.1 |
GOST 6613−86 |
2.2, 2.5, 4.9.1 |
GOST 6709−72 |
4.3.1, 4.8.1 |
GOST 10354−82 |
5.1 |
GOST 10929−76 |
4.5.1 |
GOST 14192−77 |
5.5 |
GOST 15102−75 |
5.7 |
GOST 18293−72 |
2A.3.2 |
GOST 19251.0−79 |
4.2 |
GOST 19251.1−79 |
4.4 |
GOST 19251.2−79 |
4.5 |
GOST 19251.3−79 |
4.6 |
GOST 19251.4−79 |
4.7 |
GOST 19251.5−79 |
4.7 |
GOST 19251.6−79 |
4.7 |
GOST 19433−88 |
5.5 |
GOST 20435−75 |
5.7 |
GOST 20490−75 |
4.3.1 |
GOST 22180−76 |
4.3.1 |
GOST 22397−77 |
4.10 |
GOST 22861−93 |
4.5.1 |
GOST 23957.1−80 |
4.5, 5.7 |
GOST 24104−88 |
4.9.1 |
GOST 24634−81 |
5.1 |
GOST 25336−82 |
4.5.1, 4.8.1 |
5. The expiration time limit is removed by the Resolution of Gosstandart No. 776 from 27.07.92
6. REPRINT (January 1997) Changes in N 1, 2, 3, 4, 5, approved in July 1980, February 1984, January 1988, October 1990, December 1992 (IUS 4−80, 1−84, 9−87, 6−90, 10−92)
This standard applies to zinc powder, applied in electrical (for the production of chemical current sources), chemical, metallurgical, pharmaceutical and other industries, designed for the needs of the national economy and exports.
(Changed edition, Rev. N 2, 3, 4).
1. BRAND
1.1. Depending on production method and particle size distribution zinc powder manufactured in two classes:
A — fine zinc powder brands PC1, PC2, PC3, PC4, produced by a method of rectification;
B — the coarse zinc powder brands PC6 and PC7, manufactured sputtering method.
Zinc powder of all grades produced from zinc grades CV, co or SMC according to GOST 3640−94.
(Changed edition, Rev. N 2, 3).
2. TECHNICAL REQUIREMENTS
2.1. Zinc powder is manufactured in accordance with the requirements of this standard for technological regulations approved in the prescribed manner.
The chemical composition of the zinc powder shall conform to the standards specified in table.1.
Table 1
Klas- Sy |
Mar Ki |
OKP code | Chemical composition, % | |||||||
Zinc metal likes- cue, not less |
Impurity, not more than | |||||||||
Iron | Lead | Cadmium | Copper | Tin | Arsenic | Antimony | ||||
And | PC1 | 17 2133 0101 10 |
96 | 0,0005 | 0,001 | 0,0015 | 0,0004 | 0,001 | 0,0005 | 0,001 |
PC2 | 17 2133 0102 09 |
95 | 0,0005 | 0,002 | 0,002 | 0,0004 | 0,001 | 0,0005 | 0,001 | |
PC3 | 17 2133 0103 08 |
95 | 0,002 | 0,006 | 0,006 | 0,001 | 0,001 | 0,001 | 0,001 | |
PC4 | 17 2133 0104 07 |
95 | 0,007 | 0,02 | 0,05 | 0,005 | 0,001 | 0,01 | 0,02 | |
B | PC6 | 17 2133 0201 07 |
98 | 0,006 | 0,014 | 0,005 | 0,001 | 0,001 | 0,001 | 0,001 |
PC7 | 17 2133 0202 06 |
95 | 0,006 | 0,014 | 0,005 | 0,001 | 0,001 | 0,001 | 0,001 |
Notes:
1., 2. (Deleted, Rev. N 3).
3. In zinc powder of all grades used in pharmaceutical industry, chemical — for the production of benzidine and its analogs and for the production of indigoid dyes, the solution obtained in the determination of insoluble residue should be colorless.
In zinc powder brand PC4 used for the production trendigen dyes, the mass fraction of copper should not be more than 0.001%.
By agreement between manufacturer and consumer in zinc powder brand PC4 used for the production of sodium hydrosulfite and rongalite, is allowed the mass fraction of cadmium not more than 0.1%.
4. Zinc powder used in pharmaceutical industry and chemical — for the production of rongalite, benzidine and its analogs, and other organic dyes, must contain the residue, insoluble in hydrochloric acid, diluted 1:1, not more than 0.1%.
2.2. Particle size distribution of the zinc powder shall conform to the standards specified in table.2.
Table 2
Classes | Brand | Granulometric composition, %, no more |
The content of fraction — Of 0.63+0.16 mm when sifting through mesh N 063К and N 016К according to GOST 6613−86, %, not less |
Mass fraction of fractions — 0,25 +0,05 mm when sifting through mesh N 025К and N 005К according to GOST 6613−86, %, not less than | |||
The residue on the mesh according to GOST 6613−86 |
|||||||
N 016К | N 008К | N 0071К | N 005К |
||||
And | PC1 | - | 0,04 |
- | 1,0 | - | - |
PC2 | Without a trace |
- | 2,0 | - | - | - | |
PC3 | 0,1 |
- | 2,5 | - | - | - | |
PC4 | 3,0 |
- | 5,0 | - | - | - | |
B | PC6 | - |
- | - | - | 94 | - |
PC7 | - |
- | - | - | - | 90 |
Notes:
1. In zinc powder brand PC4 used for the production of rongalite, the residue on the mesh N 0071К should be no more than 2%, the residue on the mesh N 016К is not standardized.
2. In the zinc powder used for the production of benzidine and its analogs, the contents of the residue on the mesh N 016К should be not more than 0.1%.
3. In zinc powder brand PC4 used for the production of rongalite, specific surface should be not less than 800 cm/g.
4. Zinc powder brand PC6 used for thermal diffusion galvanizing of tubes, allowed fraction of 1.00+0.63 mm when sifting through mesh N 1K and N 063К at least 80%.
(Changed edition, Rev. N 5).
2.3. Zinc powder should be light gray or gray.
2.4. Zinc powder should not contain impurities (pieces of metal, ceramics, ishare).
2.5. Zinc powder class And must not contain lumps, granules, pellets while sifting through the control grid N 0315К, class B — through mesh N 063К according to GOST 6613−86 on a mechanical shaker in accordance with the method stated in paragraph 4.9 of this standard.
(Changed edition, Rev. N 2, 3).
2A. SAFETY REQUIREMENTS
2A.1. Zinc powder has toxic properties. Hazard — food poisoning. Zinc dust is fed to the working body via the respiratory and gastrointestinal tract, causing catarrh of the upper respiratory tract and gastrointestinal disorders.
2A.2. (Deleted, Rev. N 5).
2A.3. General sanitary-hygienic requirements to air of working zone of production areas according to GOST 12.1.005−88.
2A.3.1. Control over the content of zinc in the air of the working zone of production areas should be carried out in accordance with the requirements of GOST 12.1.005−88.
The concentration of harmful substances in the air of working zone is determined by the techniques corresponding to GOST 12.1.016−79, or methodological instructions approved by the USSR Ministry of health.
(Changed edition, Rev. N 5).
2A.3.2. The maximum permissible concentration of zinc (Zn) in drinking water according to GOST 2874−82 — 5 mg/DM.
Drinking water analysis on the content of zinc (Zn) is carried out according to GOST 18293−72.
2A.4. Zinc powder is stored in closed containers.
Scattered zinc powder is necessary to collect a scoop in the container.
Recycling, disposal and destruction of zinc powder is carried out in accordance with the requirements approved by the Ministry of health of the USSR.
2A.5. Zinc powder does not form more toxic compounds in aerial environment and waste waters in the presence of other substances or factors.
2A.6. Zinc powder fire and explosion hazard and refers to the 4th group of fire and explosion hazard substances with an ignition temperature of 600 °C and lower explosive limit it with air at a concentration of 480 g/m.
2A.6.1. The requirements of fire and explosion when working with a zinc powder — according to GOST 12.1.004−91, GOST 12.1.010−76 and common safety rules for enterprises and organizations of metallurgical industry, approved by Gosgortekhnadzor of the USSR.
2A.6.2. The item requirements types of fire equipment and fire extinguishing means — according to GOST 12.4.009−83.
2A.6.3. In bunker office should use lamps, voltage not exceeding 12 V.
2A.6.4. In places of work with zinc powder should be installed safety signs according to GOST 12.4.026−76*.
______________
* On the territory of the Russian Federation GOST R 12.4.026−2001. — Note the CODE.
2A.7. Production facilities and laboratories, which are zinc-powder must be equipped with forced ventilation according to GOST 12.4.021−75.
2A.8. Unloading zinc powder from the container and transport it by means of a pneumatic conveying should be carried out in accordance with the «General rules of explosion safety for explosive hazardous chemical, petrochemical and refining industries», approved by Gosgortekhnadzor of the USSR.
2A.7, 2A.8. (Changed edition, Rev. N 5).
2A.9, 2A.10. (Deleted, Rev. N 5).
2A.11. All work with zinc powder, you must perform a respirator type «Petal» according to GOST 12.4.028−76, dry and serviceable clothing and safety devices in accordance with «Standard industry norms of free issue to workers and employees with special shoes and other individual protection means».
2a.11. (Changed edition, Rev. N 5).
2A.12. Safety requirements for loading and unloading — according to GOST 12.3.009−76.
2A.13. Transport of zinc powder is not allowed together with inflammable substances, acids and alkalis.
Sec. 2A. (Added, Rev. N 2).
3. ACCEPTANCE RULES
3.1. Zinc powder take parties.
The party must consist of a powder of the same brand and decorated with a single document about quality that contains:
trademark or a trademark and the name of the manufacturer;
the name of the powder and its brand;
the batch number and the number of seats in the party;
the weight of the batch (gross / net, kg);
the results of the tests for compliance with the requirements of PP.2.1−2.5;
the date of manufacture;
the designation of this standard.
(Changed edition, Rev. N 2, 3).
3.2. The verification of the chemical and granulometric composition of the zinc powder in all grades Packed in special containers, and powder marks PC1, PC2 and PC3, Packed in drums, is performed on each production unit of the party.
To check the chemical and granulometric composition of zinc powder brands PC6 and PC7, Packed in jars and pouches from the party is taken every fifth unit.
The mass fraction of copper, tin, arsenic, antimony in zinc powder brands PC1, PC2, PC3, PC4 and the mass fraction of iron, lead, cadmium, copper, tin, arsenic and antimony grades PC6, PC7 are determined periodically 1 time per month.
The test of specific surface area of zinc powder brand PC4 for the production of rongalite spend every second of the party on each unit of the party.
(Changed edition, Rev. N 3, 4).
3.3. To check the appearance of the zinc powder and the absence of impurities produced in the entire production batch.
3.4. If unsatisfactory results of the analysis at least one indicator thereon, a second analysis doubled the number of samples taken from the party. Results re-analysis apply to the entire party.
4. TEST METHODS
4.1. Sampling and sample preparation
4.1.1. From each tank (container, drum, bag and jar) dipstick or tube of stainless steel, titanium or aluminium length 80 cm, diameter 10−15 mm select a single sample for the entire depth.
The probe design must ensure that the selection of powder over the entire height of the packing unit.
A sample from the container selected in two points located at a distance of 30 cm from each other.
A sample from the drums, jars and pouches taken away at one point.
The sample mass of container, shall not be less than 1 kg, of the drum and the jar is less than 200 g of the pouch — at least 100 g.
(Changed edition, Rev. N 2, 3).
4.1.2. The manufacturer is permitted to select a single sample, manual or automatic sampler for flow in the packaging of zinc powder in the container.
4.1.3. Selected samples are combined and thoroughly mixed. The average weight of the sample should be 1 kg While the mass average samples over 1 kg of her kvantovanie reduce to mass of 1 kg.
4.1.4. An average sample is divided into two parts, one of which is subjected to the tests and the other is Packed in a sealed container, which is applied to the brand of powder, batch number, and date of sampling, and stored for three months in case of differences in the assessment of quality.
4.2. General requirements for methods of chemical analysis according to GOST 19251.0−79, with the following additions.
4.2.1. To determine the chemical composition of zinc powder brands PC1 and PC2 are used reagents on the degree of purity not lower than H. h, brands PC3, PC4, ПЦ5, PC6 and PC7 — not below h.d. a.
(Changed edition, Rev. N 2).
4.3. Determination of metallic zinc in zinc powder using the phase chemical analysis.
The method is based on extraction of zinc metal selective solvent and subsequent permanganatometricly defining it in the mass fraction range of 92−98%.
(Changed edition, Rev. N 3).
4.3.1. Reagents and solutions
Oxalic acid according to GOST 22180−76, 0,1 n solution, fixanal.
Sulfuric acid GOST 4204−77, diluted 1:3 and 1:20 (by volume).
Orthophosphoric acid according to GOST 6552−80.
Potassium permanganate according to GOST 20490−75, 0.1 N. solution.
Setting the coefficient of normal
Pipetted 25 cmof a solution of oxalic acid was placed in a conical flask with a capacity of 250 cm, adding 25 cmof sulphuric acid diluted 1:3, about 100 cmof water and heat the solution to 70 °C, then titrated solution of potassium permanganate.
The coefficient of normality () is calculated by the formula
,
where is the number of solution of oxalic acid, cm;
— the quantity of potassium permanganate solution consumed for titration, sm.
Alum salesonline on the other 6−09−5359−88.
Sodium acetate according to GOST 199−78.
Distilled water GOST 6709−72.
Selective solvent of zinc metal with a pH of 2.4 to 2.6; prepared as follows: 400 g gentoomaniac alum dissolved in 1 DMof water is added 150 g sodium acetate was dissolved and filtered.
4.3.2. Analysis
For powder marks PC1, PC2, PC3, PC6, PC7.
0.15 g of zinc powder is weighed with an error not exceeding 0.0002 g, placed in a conical flask with a stopper with a capacity of 500 cm, add 50 cmof the selective solvent and continuously shake the contents of the flask on a mechanical vibrator until complete dissolution of zinc powder (40 min). Then the solution was poured 200 cmof sulphuric acid, diluted 1:20, 5 cmof phosphoric acid to obtain a more precise titration and titrated with potassium permanganate solution until the appearance of stable for 2 min slightly pink color.
For powder brands PC4 and ПЦ5
1 g of zinc powder is weighed with an error not exceeding 0.0002 g, placed in a conical flask with a capacity of 500 cm, add 100 cmof the selective solvent and continuously shake the contents of the flask for 40 min. Then, washing the walls of the bulb, add another 75 cmof the selective solvent and continued to stir 20 min. Then the entire solution was transferred to volumetric flask with a capacity of 200 cmand was adjusted to the mark with water. For titration pipetted 20 cmof the solution in a flask with a capacity of 500 cm, 200 cm pouredsulphuric acid, diluted 1:20, 5 cmof phosphoric acid for more precise titration and titrated with potassium permanganate solution until the appearance of stable for 2 min slightly pink color.
At the same time carried out a control experiment under the same conditions with the same amount of trouble.
tivov.
4.3.3. Processing of the results
Mass fraction of zinc metal (a) in percent is calculated by the formula
,
where — the amount of potassium permanganate solution consumed for titration, cm;
— the quantity of potassium permanganate solution consumed for titration of the solution in the reference experiment, cm;
— the coefficient of the normality of solution of potassium permanganate;
— the amount of zinc corresponding to 1 cmexactly 0.1 N. solution of potassium permanganate, g;
— the weight of zinc powder, g, which powder brands PC4, ПЦ5 is calculated by the formula
,
where is the mass of the original sample of zinc powder, g;
— number aliquote part, taken from the volumetric flask, cm;
— capacity volumetric flasks, cm.
For the results analysis be the arithmetic mean of results of three parallel measurements allowed the differences between them should not exceed in the analysis of zinc powder class A — 1 abs.%, class B — 0,8 abs.% (=0,95).
4.4. Determination of the mass fraction of iron is carried out according to GOST 19251.1−79.
By photometric determination from the 0.0003 to 0.001% of iron take a suspension of zinc powder with a mass of 2 g, is decomposed in 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 8−10 cm. Transfer the solution into a measuring flask with a capacity of 50 cmand then conduct analysis 19251.1 GOST-79.
Calibration curve constructed in the concentration range 5−50 µg of iron 50 cmof the solution.
In atomic absorption the determination of from 0.0004 inch to 0.001% of iron take the weight of zinc powder weight of 5 g and prepare a calibration solution with a mass concentration of iron of 0.20, 0.5 and 1.0 µg/cmbased on the solution of zinc (mass concentration of zinc should be 50 g/DM). When calculating the mass fraction of iron is necessary to consider the contributions made by solution of zinc in calibration solutions of iron.
Permissible discrepancies in the results of parallel definitions should not exceed 0,0002% in the range of mass fraction 0,0003−0,001%.
4.5. The definition of a mass fraction of lead and cadmium is carried out according to GOST 19251.2−79 or GOST 23957.1−80*.
________________
* On the territory of the Russian Federation GOST 23957.1−2003. — Note the CODE.
For atomic absorption determination 0.0008 to 0.002% lead take a sample of zinc powder weight of 5 g and prepare a calibration solution with a mass concentration of lead at 0.4, 1.0 and 2.0 µg/cmbased on the solution of zinc (mass concentration of zinc should be 50 g/DM).
When calculating the mass fraction of lead is necessary to consider the contributions made by solution of zinc in calibration solutions of lead.
4.4, 4.5. (Changed edition, Rev. N 3).
4.5.1. Equipment and reagents
Polarograph oscilloscope DC or AC polarograph.
Funnel filter type VF-1−32-THEN, 100 TCS or VF-1−40-THEN, 100 of TCS according to GOST 25336−82.
Hydrogen peroxide according to GOST 10929−76, 30% solution.
Hydrochloric acid by the GOST 3118−77, diluted 2:1 and 1:3.
Bromatologia acid according to GOST 2062−77.
Nitric acid GOST 4461−77 diluted 1:3.
Cadmium brand KDO according to GOST 1467−93.
Sodium chloride according to GOST 4233−77.
Hydrazine hydrochloric acid.
Background electrolyte; prepared as follows: into a flask with a capacity of 1 DMare placed 200 g of sodium chloride, 5 g of hydrazine hydrochloric acid, poured 10 cmof hydrochloric acid, diluted to a volume of 1 DMwater and stirred.
Mercury GOST 4658−73.
Lead brand S00 GOST 22861−93.
Chloride solution; prepared as a background electrolyte, without adding hydrochloric acid hydrazine.
Standard solution A, is prepared as follows: a sample mass of 0.2 g of finely chopped lead and a sample weight of 1 g of cadmium is placed in a beaker with a capacity of 1 DM, is dissolved by heating in 30 cmof nitric acid, diluted 1:3, and evaporated to a moist residue. Add 10 cmof hydrochloric acid and again evaporated almost to dryness. Evaporation with 10 cmof hydrochloric acid repeated two more times. To the residue is added 600 cmchloride solution, heated to dissolve the salts, cooled, transferred to a volumetric flask with a capacity of 1 DM, dilute to the mark with this same solution and mix.
1 cmstandard solution A contains 0.2 mg of lead and 1 kg* cadmium.
________________
* The text matches the original. — Note the CODE.
Standard solution B is prepared as follows: 0.1 g of finely chopped lead, and 0.1 g of cadmium is placed in a conical flask with a capacity of 250 cm, was dissolved with heating in 20 cmof nitric acid, diluted 1:3, and further receives, as described in section 4.5.1 in the preparation of a standard solution As lead and cadmium. The solution was diluted in a volumetric flask with a capacity of 1 DMchloride solution.
1 cmstandard solution B contains 0.1 mg of lead and 0.1 mg of cadmium.
Zinc chloride according to GOST 4529−78, anhydrous.
Zinc brand of front wheel drive or C0 according to GOST 3640−94 in the form of chips or powder.
Zinc solution containing 200 g/lof zinc; prepared from the anhydrous salt of zinc chloride or of zinc.
A solution of zinc chloride salt; prepared as follows: 750 g of zinc chloride are dissolved with stirring in 500 cmof water, being careful (the solution is strongly heated), add 20cmof hydrochloric acid, 35−40 g of metallic zinc and stirred for 30 min. (cleaning of impurities of lead and cadmium). The solution was filtered through the filter funnel, to which is added about 2 g of zinc powder without creating a vacuum. The filtrate is collected in a polyethylene bottle with a capacity of 2 DM. Then 5 cmof the filtrate was evaporated as described in section 4.5.2, and determine the lead and cadmium. When these elements are present in the solution, the filtrate is poured into a flask, which was performed cementation of impurities, add 10 cmof hydrochloric acid and treated with zinc again. After cleaning and filtering the zinc solution is diluted with water to a volume of 2 DMand mixed.
Zinc solution made of metal; prepared as follows: 400 g of zinc metal is placed in a flask with a capacity of 3 DMand dissolved first in 50 cmof hydrochloric acid, diluted 2:1, then at least reduce the rate of dissolution of zinc are added in portions of 25−30 cmof concentrated hydrochloric acid with frequent stirring. After the bottom of the flask will have about 25−30 grams of zinc, add 25−30 g of zinc powder, 20 cmof hydrochloric acid and continue cleaning until dissolved, approximately half of the zinc. The solution is filtered and checked for purity as described above. The filtrate was diluted to a volume of 2 DMwater.
Calibration solutions of lead and cadmium; prepared as follows: 19 in conical flasks with a capacity of 100 cmmeasured in accordance with the table.3 standard solutions A and B and evaporated zinc solution until crystals of zinc chloride. Then pour in 45−50 cm, background electrolyte, heated up to dissolve the salt, cooled, quantitatively transferred to volumetric flasks with a capacity of 200 cm, is diluted to the mark and the background electrolyte and stirred.
Table 3
Room calibration solution | The number of solution of zinc chloride, see |
The number of standard solution, cm |
Mass fraction in the calibration solution, cm | ||
And | B |
lead | cadmium | ||
1 | 20* |
- | - | - | - |
2 | 20* |
- | 0,5 | 0,25 | 0,25 |
3 | 20* |
- | 1 | 0,50 | 0,50 |
4 | 20* |
- | 2 | 1 | 1 |
5 | 10 |
- | - | - | - |
6 | 10 |
- | 4 | 2 | 2 |
7 | 10 |
- | 6 | 3 | 3 |
8 | 10 |
- | 8 | 4 | 4 |
9 | 10 |
- | 10 | 5 | 5 |
10 | 10 |
- | 12 | 6 | 6 |
11 | 10 |
- | 16 | 8 | 8 |
12 | 10 |
- | 20 | 10 | 10 |
13 | 10 |
- | 25 | 12,5 | 12,5 |
14 | 5 |
- | - | - | - |
15 | 5 |
5 | - | 5 | 25 |
16 | 5 |
10 | - | 10 | 50 |
17 | 5 |
15 | - | 15 | 75 |
18 | 5 |
20 | - | 20 | 100 |
19 | 5 |
25 | - | 25 | 125 |
________________
* In the determination of 0.0005% of the total mass fraction of lead and cadmium (sample masses of 2 and 2.5 g, the dilution of the sample solution 50 cm) in the calibration solutions 1−4 in the process of their preparation is administered, respectively, 40 or 50 cmzinc solution.
Mass fraction of lead and cadmium in the calibration solutions are shown in table.3.
In the analysis of zinc powder brands PC1 and PC2 used the calibration solutions 1−4, brands PC3, PC6 and PC7 — calibration solutions 5−13, brands and PC4 ПЦ5 — calibration solutions 14−19. Calibration solutions of 1, 5, 14 serve to hold the reference experiment.
4.5.2. Analysis
In a conical flask with a capacity of 100−250 cmis placed a suspension of zinc powder (tab.4), add small portions of hydrochloric acid, diluted 2:1, and lead the dissolution of the cold and then when heated. At the end of the dissolution add about 0.5 cmof hydrogen peroxide and evaporated to a volume of 8−10 cm. Pour 5 cmbromatological acid and continue to evaporate until crystallization of the salt of zinc chloride.
Table 4
Brand | The weighed sample, g | The amount of hydrochloric acid, see |
Capacity volumetric flasks, cm |
PC1 and PC2 |
1−2,5 | 20−60 |
50 |
PC3, PC6 and PC7 |
1 | 20 | 100 |
PC4 and ПЦ5 |
0,5 | 15 | 100 |
Simultaneously, control experiments carried out in the following way: in four conical flasks with a capacity of 100 cm, respectively, measured every 2.5 cm(weight mass 0.5 g), 5 cm(weight mass 1 g), 10 cm(weight mass 2 g), 12.5 cm(weight mass 2.5 g) solution of zinc chloride, poured 20 cmof hydrochloric acid, diluted 2:1 add 0.5 cmof hydrogen peroxide and evaporated to a volume of 8−10 cm. Then pour 5 cmbromatological acid, and continue the evaporation until crystallization of the salt of zinc chloride. To the residue poured 25 or 50 cmbackground electrolyte, heated to dissolve the salts, cooled and transferred to volumetric flask with a capacity of 50 or 100 cm(see table.4).
The sample solution and the solution in the reference experiment is poured into the cell and polarographic lead and cadmium, respectively, in the peak potentials from minus minus 0.45 to 0.65 In relative to the saturated calomel electrode with the use of oscilloscope polarograph at an initial voltage minus 0.30 In, end — minus 0.9 volts, the speed voltage of 0.25−0.5 In/s, the period of dripping of mercury 4−6 with a latency of 3−5 s, the scheme «differential — 2−3» and the optimal values of the current range. In similar conditions polarographic calibration solutions. Polarographically using polarography AC is carried out at a dripping period of mercury from the capillary of 1−2. 5 s and the optimal values of the current range.
Of wave heights determined elements subtracted the value of the wave heights in the reference experiment and calculate the results of the analysis of lead and ka
dmia.
4.5.3. Processing of the results
Mass fraction of lead or cadmium (a) in percent is calculated by the formula
,
where the wave height of the element of the test sample solution, mm;
— the volume of the original solution of the sample, cm;
— weight of sample, g;
— the ratio of the wave height of an element to its concentration in the calibration solution in mg/DM.
The allowable divergence between the extreme results of the analysis shall not exceed the values given in table.5.
Table 5
Mass fraction of element, % | The allowable divergence between the extreme results of the analysis, abs. | |
lead | cadmium | |
From 0.0005 to 0.001 |
0,0002 | 0,0002 |
SV. Of 0.001 «to 0.002 |
0,0003 | 0,0003 |
«To 0.002» 0.004 s |
0,004 | 0,0004 |
«0,004» 0,006 |
About 0.0006 | About 0.0006 |
«Of 0.006» to 0.01 |
0,001 | 0,001 |
«0,01» 0,02 |
0,002 | 0,002 |
«0,02» 0,03 |
0,003 | 0,003 |
«0,03» 0,06 |
0,005 | 0,005 |
«Of 0.06» to 0.1 |
0,008 | 0,008 |
«0,1» 0,2 |
- | 0,01 |
«0,2» 0,3 |
- | 0,015 |
«0,3» 0,5 |
- | 0,04 |
«0,5» 1,0 |
- | 0,06 |
«1,0» 2,0 |
- | 0,12 |
4.6. Mass fraction of copper is determined according to GOST 19251.3−79.
For the photometric determination from 0,0003 to 0,0005% copper take a suspension of zinc powder with a mass of 2 g and the definition of lead from the entire sample.
For atomic absorption definition from 0,0003 to 0,0005% copper take a suspension of zinc powder weight of 5 g and prepare a calibration solution with a mass concentration of 0.125; 0.25 and 0.5 µg/cmbased on the solution of zinc (mass concentration of zinc should be 50 g/DM).
When calculating the mass fraction of copper is necessary to consider the contributions made by solution of zinc in calibration solutions of copper.
(Changed edition, Rev. N 3).
4.7. Mass fraction of tin, arsenic and antimony determined according to GOST 19251.4−79 — 19251.6 GOST-79.
4.8. Determination of the mass fraction of residue insoluble in a dilute 1:1 hydrochloric acid
4.8.1. Reagents, solutions and devices
Distilled water GOST 6709−72.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
The filter crucible according to GOST 25336−82, TF-40-PORT 100 XC or TF-32-PORT 100 KHS.
Silver nitrate according to GOST 1277−75, a 1.5% solution.
(Changed edition, Rev. N 2).
4.8.2. Analysis
A suspension of zinc powder with a mass of 10 g is weighed with an accuracy of at least 0.01 g, placed in a conical flask with a capacity of 250 cm, 120 cm addhydrochloric acid, close the neck of the bulb watch glass or glass bulb and boiled to dissolve the zinc (15−60 min). The solution was cooled and filtered through pre-dried at a temperature of (105±2) °C to constant weight glass crucible with a porous bottom. The residue on the filter and flask washed with distilled water until a negative reaction to the chloride ion in the washing water (test with solution of nitrate of silver). The crucible with the residue is dried at 105±2 °C to constant weight.
4.8.3. Processing of the results
Mass fraction of residue insoluble in hydrochloric acid, () percentage calculated by the formula
,
where is the mass of sample of zinc powder, g;
is the mass of insoluble solids,
The analysis result should be the arithmetic mean of two parallel definitions, allowable differences between them should not exceed 0,015 abs.% (=0,95).
4.9. Determination of granulometric composition and the presence of lumps, granules and pellets
4.9.1. Equipment
Mesh N 063К, 0315К, 016К, 008К, 0071К and 005К according to GOST 6613−86.
A set of sieves with meshes, with lid and pan. Sieves should be round with dimensions not less than: diameter 100 mm, depth 25 mm, height of sides 40 mm.
Mechanical scrambler brand 162Т-G or type «Rotap». It is possible to use other types of mechanical shakers with a speed of (300±15) rpm, while shaking with a uniform rate of 180±10 per minute.
Laboratory scales lever according to GOST 24104−88* or any other type with a weighing error of no more than 0.001 g.
________________
* Standards 24104−2001. — Note the CODE.
Tracing GOST 892−89.
(Changed edition, Rev. N 2, 3).
4.9.2. Analysis
Clean and dry the sieve stack on the increasing size of cells one above the other; the tray is placed under the lower sieve.
A sample weight of 100 g, weighed with accuracy of more than 0.1 g, poured on the top sieve and cover it with a lid.
The thus prepared set of sieves placed on the shaker and turn it on. The sieving time of 20 min.
At the end of the screening the individual fractions poured from sieves, beginning with a sieve with large cells. The contents on the sieve gently shaken to one side and pour on the tracing paper or glass of the weighted buxy with light tapping on the wall of the sieve. The resulting fraction is weighed with an error of not more than 0.001 g.
This operation is repeated for each sieve and pan. The mass of all fractions in the sum must be at least 99% of the mass of the test sample.
4.9.3. Processing of the results
The content of individual fractions () in percent is calculated with a relative error to 0.1% by the formula
,
where is the mass of this fraction, g;
— mass of test sample, g.
4.10. Allowed to determine the chemical composition of the zinc powder in the spectral method according to GOST 22397−77.
(Changed edition, Rev. N 2).
4.11. Color of zinc powder checked by comparison with the samples agreed upon by the manufacturer and consumer.
4.12. Control in the absence of impurities is carried out by visual inspection.
4.13. The specific surface area of zinc powder is determined according to the procedure agreed between the manufacturer and the consumer.
(Added, Rev. N 3).
5. PACKING, MARKING, TRANSPORTATION AND STORAGE
5.1. Zinc powder is Packed in special hermetically sealed containers: metal containers (Fig.1), drums (damn.2) manufactured according to normative-technical documentation, and jar for GOST 5799−78 type FS or FSTS or GOST 5037−78 type FA or FL.
Damn.1
Damn.2
Zinc powder for the production of chemical current sources is packaged in galvanized metal drums (damn.2) with sealed seams and zinc-coated flasks according to GOST 5799−78 or GOST 5037−78. By agreement with consumer it is permitted to pack the zinc powder in non-metallic drums (damn.2) the flask according to GOST 5799−78 or GOST 5037−78 providing the tightness of the packing and preservation of products.
Zinc powder intended for export, Packed in polyethylene bags according to GOST 10354−82 with subsequent packing of pouches brewed in wooden boxes according to GOST 24634−81 or GOST 2991−85.
(Changed edition, Rev. N 3, 5).
5.2. Containers for the packaging of zinc powder is filled to the brim, to the surface of the powder had less air.
Can be applied returnable packaging according to normative-technical documentation.
5.3. The gross mass of zinc powder in the container should not be more than 1500 kg, in drums of 65 kg, jars, 100 kg, plastic bags — 15 kg. container Capacity should be 0.36 mdrum — 0,01−0,015 m, jar — 0.03 m, 0.04 m.
5.2, 5.3. (Changed edition, Rev. N 2, 3).
5.4. It is not allowed to fill the caps of containers with bitumen or other organic substance which can get into zinc powder when resuorce.
5.5. Transport marking under GOST 14192−77* with application of manipulation sign «Protect from moisture».
________________
* Valid GOST 14192−96. — Note the CODE.
Markings representative of the transport of dangerous goods, according to GOST 19433−88 with the application of the label (Fig.4B/4B), classification code group 4372, serial numbers 1436 and UN shipping name of the cargo — «zinc powder».
(Changed edition, Rev. N 5).
5.6. (Deleted, Rev. N 2).
5.7. Zinc powder is Packed in special containers, transporterowych rail, river and sea transport in covered vehicles in accordance with the rules of transportation of dangerous goods, operating on transport of the species.
Zinc powder in drums and flasks are additionally placed in universal metal containers according to GOST 20435−75 or GOST 15102−75, transportyour on the open rolling stock, vehicles, river and sea vessels.
(Changed edition, Rev. N 3).
5.8. Zinc powder stored in the manufacturer’s packaging in covered warehouses in the absence of acids, alkalis and other aggressive substances.
Powder, Packed in containers, may be stored under a canopy.
(Changed edition, Rev. N 2).
6. MANUFACTURER’S WARRANTY
6.1. The manufacturer must guarantee the conformity of zinc powder with the requirements of this standard if the purchaser respects the conditions for transport and storage specified by the standard.
6.2. Warranty period of storage of the zinc powder is set six months from the date of manufacture.
(Changed edition, Rev. N 2, 3, 4).
Sec. 7 (Deleted, Rev. N 2).
The App (Deleted, Rev. N 3).