GOST 9723-73
GOST 9723−73 tin Powder. Technical specifications (with Changes 1−6 N)
GOST 9723−73
Group 56
INTERSTATE STANDARD
TIN POWDER
Specifications
The Tin powder. Specifications
GST 17 9231
Date of introduction 1975−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR
DEVELOPERS
E. E. Gulyaikhin, B. A. Gosmer, A. I. Dautova
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. The standard fully complies ST SEV 6740−89
4. REPLACE GOST 9723−61
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
Item number |
GOST 12.3.009−76 |
2A.7 |
GOST 12.4.028−76 |
2A.6 |
GOST 12.4.044−87 | 2A.6 |
GOST 12.4.045−87 |
2A.6 |
GOST 860−75 |
1.1 |
GOST 2991−85 |
4.3 |
GOST 3118−77 |
3.5.1 |
GOST 3282−74 |
4.3 |
GOST 3560−73 |
4.3 |
GOST 4461−77 |
3.5.1 |
GOST 6128−81 |
4.1 |
GOST 6613−86 |
3.2, 3.6 |
GOST 9078−84 |
4.3 |
GOST 10354−82 |
4.1 |
GOST 11125−84 |
3.5.1 |
GOST 14192−96 |
4.2 |
GOST 14861−91 |
4.3 |
GOST 15483.0−78 — GOST 15483.7−78 |
3.3 |
GOST 15483.10−78 |
3.3 |
GOST 18477−79 |
4.3 |
GOST 19113−84 |
3.4.1 |
GOST 19440−94 |
3.7 |
GOST 21140−88 |
4.3 |
GOST 26663−85 |
4.3 |
GOST 29057−91 |
2A.6 |
GOST 29058−91 |
2A.6 |
6. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)
7. The re-release (Oct 1998) with Changes in N 1, 2, 3, 4, 5, 6, approved in November 1976, September 1979, June 1984, January 1987, January 1988, October 1990 (IUS 11−76, 11−79, 10−84, 5−87, 4−88, 1−91)
This standard applies to the tin powder, produced by a sputtering method and intended for the production of electric carbonic products and other metal-ceramic compositions in various industries.
The standard fully complies ST SEV 6740−89.
(Changed edition, Rev. N 3, 4, 6).
1a. BRAND
1a.1. Depending on the chemical and granulometric composition of the established brand of tin powder: PoE, PO1, PO2, PO3, PO4.
(Changed edition, Rev. N 3, 6).
1. TECHNICAL REQUIREMENTS
1.1. Tin powder must be manufactured in accordance with the requirements of this standard technological instruction, duly approved.
Tin powder shall be made of tin grades O1 and O2 according to GOST 860. The use of other brands of tin.
(Changed edition, Rev. N 3, 5, 6).
1.2. The chemical composition of the powder should conform to the standards specified in table.1.
Table 1
Chemical composition, % | |||||||||||
The brand is Rosca |
OKP code |
Tin, not less |
Impurity, not more than | Calcined residue after treatment of the powder with hydrochloric acid, no more | |||||||
Lead | Iron | Copper | Sulfur | Bismuth | Arsenic | Antimony | Oxygen | ||||
PoE |
17 9231 0004 |
99,0 |
0,25 |
0,02 |
0,03 |
0,016 |
0,05 |
0,015 |
0,05 |
0,5 |
0,02 |
PO1 |
17 9231 0001 |
99,1 |
0,15 |
0,02 |
0,03 |
0,016 |
0,05 | 0,015 |
0,05 |
0,5 |
0,02 |
PO2 |
17 9231 0002 |
99,0 | 0,25 |
0,02 |
0,03 |
0,016 |
0,05 | 0,015 |
0,05 |
0,5 |
0,02 |
PO3 |
17 9231 0003 |
99,0 |
0,25 |
0,02 | 0,03 |
0,016 |
0,05 |
0,015 | 0,05 | 0,5 | 0,02 |
PO4 |
17 9231 0005 |
98,1 |
Of 1.00 |
0,05 |
0,10 |
0,04 |
0,06 |
0,05 |
0,30 |
0,10 |
0,10 |
(Changed edition, Rev. N 3, 6).
1.3. Granulometric composition of the powder must meet the requirements specified in table.2.
Table 2
Brand powder |
Sieve residue, % | Pass through a sieve, % | |||
The numbers of nets according to GOST 6613 |
The numbers of nets according to GOST 6613 | ||||
0100 To |
0071 To |
0063 To |
0063 To |
0045 To | |
no more |
|||||
PoE |
- |
2,2 |
- |
- |
85−95 |
PO1 |
- |
2,2 |
- |
- |
85−95 |
PO2 |
- |
2,2 |
- |
- |
At least 80 |
PO3 |
- |
- |
- |
At least 100 |
Not less than 95 |
PO4 |
0,5 |
- |
2−19 |
The rest |
- |
(Changed edition, Rev. N 6).
1.4. Tin powder must not have any mechanical impurities and lumps.
1.5. The bulk density of tin powder brands PO2 and PO3 should be 3.2−4.0 g/cm.
The bulk density of tin powder brands, PoE and PO1 should be a 3.4−4.0 g/cm. Between different single packs of the same batch of powder grades PO1 and therefore, the bulk density should not vary by more than 0.2 g/cm.
The bulk density of tin powder brand PO4 should be 3.6−3.9 g/cm.
(Changed edition, Rev. N 5, 6).
1.6. Tin powder grades PO1 and therefore should have a uniform particle size distribution. Variation in the uniformity among different packages of the same batch of powder is allowed no more than 5% when sifting through a sieve with mesh N 0045 To GOST 6613.
(Changed edition, Rev. N 5).
2A. SAFETY REQUIREMENTS
2A.1. Tin powder is a substance non-toxic.
2A.2. Long-term (within 15−20 years) exposure to tin dust has a fibrogenic effect on the lungs and can cause disease running pneumoconiosis.
2A.3. Tin powder in the air and in waste water of toxic substances does not form.
2A.4. Tin powder fire and explosion hazard. The ignition temperature of the tin powder of about 440 °C, the concentration of the lower Flammability limit of 120 g/m.
2A.1−2A.4. (Changed edition, Rev. N 3).
2A.5. Tin powder may not be destroyed. In the factories-consumers of tin powder, unserviceable, should surrender in the prescribed manner for the secondary aluminum smelters.
(Changed edition, Rev. N 3, 5).
2A.6. All work with tin powder must be performed in overalls 12.4.044 according to GOST, GOST 12.4.045, GOST 29057, 29058 GOST.
For protection of respiratory organs working with tin powder must use respirators SB-1 «Petal» according to GOST
2A.7. Loading and unloading should be carried out in accordance with the requirements of GOST
2A.6 2A.7. (Changed edition, Rev. N 3).
2. ACCEPTANCE RULES
2.1. The powder was taken by the parties. The party must consist of a powder of the same brand and decorated with a single document about quality that contains:
is the trademark or name and trademark of manufacturer;
— name and brand of powder;
— the results of chemical analysis, granulometric composition, bulk density and uniformity;
— the batch number;
— the net mass, kg;
— number and numbers of cans within the party;
— date of manufacture;
— the designation of this standard.
Weight party powder brand PoE should not exceed 500 kg.
(Changed edition, Rev. N 3, 4).
2.2. To check the quality of powder with the requirements of this standard take 20% of cans from each batch, but not less than five cans.
2.3. If unsatisfactory test results of at least one of the indicators, repeat tests are carried out at twice the sample selected from the same batch. The results of repeated tests apply to the entire party.
2.2, 2.3. (Changed edition, Rev. N 3).
3. TEST METHODS
3.1. Spot samples from a controlled batch of tin powder are selected coiled probe (Fig.1). The probe is immersed in the centre of the banks to the full depth. Of all the point samples taken from one party, are a combined sample. The resulting merged sample is thoroughly mixed and subjected to reduction to obtain a representative sample weighing not less than 1000 g.
For powder grades PO1 and PoE an additional five cans a controlled party is taken spot samples weighing not less than 400 g, is intended for testing the uniformity of the granulometric composition and bulk density.
Note. On the manufacturer allowed the selection of point samples gap with a feeler gauge.
(Changed edition, Rev. N 5).
3.2. The presence of mechanical impurities and lumps determine with the naked eye in selecting the sample of the powder when sifting manually 150 g powder selected from the combined sample through a sieve with a mesh 018 To GOST 6613.
3.3. The content of lead, copper, sulphur, bismuth, iron, arsenic and antimony determined according to GOST 15483.0 — 15483.7 GOST and GOST 15483.10*.
______________
* On the territory of the Russian Federation GOST 15483.10−2004. — Note the manufacturer’s database.
Allowed to use other testing methods, providing the required accuracy.
The differences in the evaluation of the chemical composition analysis is carried out according to GOST 15483.0 — GOST 15483.7.
The tin content calculated by the difference between the 100% and the sum percentage content of impurities: iron, lead, copper, sulphur, bismuth, arsenic, antimony, oxygen, and insoluble residue.
(Changed edition, Rev. N 3, 5).
3.4. Determination of the oxygen content of the tin powder
Method involves fusion of sample powder tin with rosin when heated. Pure tin is smelted in the form of a Wren, and oxygen-containing compounds of tin are transferred to the slag. The analysis is carried out on tin goldcrest, which is separated from the slag and weighed.
3.4.1. Apparatus, materials and reagents
Analytical scale.
Libra technical.
Crucibles porcelain low N 6 forms.
Drying oven with the temperature heating up to 300 °C.
Tongs crucible.
The scalpel.
Mortar porcelain.
Rosin GOST 19113 brands and crushed to fine powder.
Thermometer with scale up to 300 °C.
(Changed edition, Rev. N 5).
3.4.2. Analysis
In a porcelain crucible 6 is placed N the weight of rosin, approximately 15 grams, weighed on a technical scale. In the crucible, quantitatively transfer the suspension of tin powder 30 g, taken with an error of not more than 0.01 g. the Contents of the crucible are thoroughly stirred with a glass rod, which is then removed from the crucible. The mixture in the crucible from the top and carefully around the walls covered with rosin, taken in an amount of 2−3 g. Then spend the melting of the test powder with rosin. To do this, the crucible with the mixture was placed in a drying Cabinet preheated to 275 °C, and maintained at a temperature of from 260 to 275 °C to until the tin powder is completely melted.
During the melting process every 30 min starting from the moment of heating, the crucible is removed from the oven crucible tongs and carefully stirred its contents with a rotary motion to the liquid mass of captured particles of tin powder from the walls of the crucible to better merge with the main ingot.
After the last stirring, the crucible is kept in the closet for another 30 minutes, and then removed from the oven and allow it to cool. The contents of the crucible carefully separated from the walls with a scalpel, the crucible is turned upside down and tapping on the bottom of the crucible contents are extracted to a sheet of glossy paper. Then carefully separate the bead from the slag and weighed.
1 — the outer spiral; 2 — spiral internal; 3 — outer palukanos;
4 — internal palukanos; 5 — clamp; 6 — pin; 7 — lever; 8 — the handle
Damn.1
3.4.3. Processing of the results
The oxygen content () in percent is calculated by the formula
,
where is the mass of the bead, g;
— the ratio of tin dioxide to oxygen;
— suspension of tin powder,
The analysis is carried out in two parallel batches. The oxygen content is calculated as the arithmetic average of the two determinations. The maximum discrepancy between the results of parallel measurements in oxygen content to 0.5% incl. shall not exceed 0.05%.
3.5. Determination of insoluble residue in the tin powder
The method is based on the solubility of tin in a mixture of nitric and hydrochloric acids. The undissolved part is determined quantitatively.
3.5.1. Apparatus, materials and reagents
Analytical scale.
A glass with a capacity of 250 cm.
Glass coverslip.
Tile electric.
Filters with a white ribbon.
Funnel.
Crucibles porcelain.
Oven muffle.
Nitric acid according to GOST 4461, a density of 1.37−1.40 g/cm, H. h
Nitric acid of high purity according to GOST 11125.
Hydrochloric acid according to GOST 3118, density of 1.19 g/cm.
Hydrochloric acid according to GOST 3118, diluted 1:1.
3.5.2. Analysis
A portion of the tin powder with a mass of 10 grams, taken with an error of less than 0.0002 g, placed in a beaker with a capacity of 250 cmand dissolved without heating, priliva 70 ml of hydrochloric acid density of 1.19 g/cm, and then dropwise add 15 cmof nitric acid. The glass is covered with a cover glass. At the end of the reaction the solution was heated and boiled for 10−15 min. the Solution was diluted with distilled water and filtered. The residue on the filter is washed 15−20 times with a hot solution of hydrochloric acid diluted 1:1. The filter with residue placed in a porcelain crucible previously calcined and weighed, and calcined to constant weight at 800−850 °C. the Crucible with the calcined residue is cooled in desiccator and weighed.
3.5.3. Processing of the results
The content of calcined balance () percentage calculated by the formula
,
where — the mass of the ignited insoluble residue, g;
— a charge of powder,
Definition of calcined insoluble residue is produced in two parallel batches and the result of the determination taking the arithmetic average of the two determinations. The maximum divergence between two parallel definitions should not exceed 0.01% when the content of insoluble residue up to 0.02% incl.
3.6. Determination of granulometric composition
Particle size distribution of the tin powder grades, PoE, PO1, PO2, PO3, PO4 define sieve analysis on mechanical shaker type 028М and 029М with the rotation speed of eccentric shaft 300±15 per minute, number of strokes of the lever 180±10 per minute, the lift rod from the top of the connecting rod 35−45 mm, stroke 20 to 23 mm mechanical shakers or other types, providing the specified conditions of test. Screened powder is carried out with a set of mechanical sieves, with the mesh according to GOST 6613, listed in the table.2 of this standard. Sieves should be round with a diameter of 200 mm and depth 30 mm. the average Number of samples of powder of all grades should be 100 g, time sifting 20 min.
(Changed edition, Rev. N 3, 5, 6).
3.6.1. Analysis
Clean and dry the sieve stack on the increasing size of cells one above the other, the pallet is placed under the lower sieve set. The test sample is poured into the top sieve and cover it with a lid.
The thus prepared system of sieves placed on the shaker and turn it on.
At the end of the screening the individual fractions poured from the sieves, starting with the sieve with the largest cell. The contents on the sieve gently shake to one side and pour on the smooth paper. The powder adjacent to the grid and the frame of the sieve, gently sweep a soft brush through the sieve into another sieve with smaller cells. After this operation, the remaining on the sieve, the powder attached to the appropriate fraction.
Thus, the separated fraction is weighed with an error not more than 0.1 g. Such operations are performed with each sieve. The fraction collected on the pan, weigh. The sum of the portions of all fractions shall not be less than 98% of the mass of the test sample. The difference between the sample mass and the sum of the portions of all the fractions added when writing to the mass fraction collected on the pan.
Mass fraction of individual fractions () in percent calculated with an error of not more than 0.1% by the formula
,
where is the mass of this fraction, g;
— mass of test sample, g.
(Changed edition, Rev. N 3).
3.7. The bulk density of the powder is determined on volumemeter according to GOST 19440 on a sample prepared by PP.2.2 and 3.1.
(Changed edition, Rev. N 6).
3.7.1−3.7.4. (Deleted, Rev. N 6).
4. PACKING, MARKING, TRANSPORTATION AND STORAGE
4.1. Tin powder is Packed in bags of polyethylene film of a thickness of 0,060−0,080 mm according to GOST 10354. Bags closed hermetically and placed in metal cans manufactured according to GOST 6128. No need to varnish or paint the outer surface of the cans.
By agreement with the consumer allowed to pack the powder in metal cans, made working drawings, approved in the prescribed manner. Capacity and dimensions of cans shall be as specified in table.3.
Table 3
Capacity, cm |
Diameter, mm |
Height, mm | ||||
internal |
exterior |
pred. off. |
internal |
exterior |
pred. off. | |
8092 |
215 |
218 |
±5 |
223 |
232 |
±5 |
7104 |
195 |
198 |
±5 |
238 |
245 |
±5 |
2984 |
140 |
143 |
±5 |
194 |
200 |
±5 |
1671 |
110 |
113 |
±5 |
176 |
182 |
±5 |
For sealing the connection point of the lid with the jar and the side seams must be sealed or rolled up. Net weight cans should be no more than 30 lbs. For easy loading and unloading banks can be equipped with a handle.
(Changed edition, Rev. N 3, 4).
4.2. In each jar put in the document as stating:
a) the trademark or name and trademark of manufacturer;
b) the names and brand of powder;
C) the batch number;
g) numbers of banks;
d) net mass;
e) date of manufacture;
g) the designation of the present standard;
h) (Deleted, Rev. N 5).
Each Bank needs to be glued paper label, indicating the name and brand of powder, batch number, numbers, banks, weight, manipulation of the sign «Sealed package» according to GOST 14192.
(Changed edition, Rev. N 2, 3, 5, 6).
4.3. Cans powder transporterowych in universal containers according to GOST 18477 or metal containers according to GOST 14861, type 1, performance 1, size 1200х800х750 mm, with a gross mass of not more than 1 T.
Small shipments powder transporterowych in planked boxes, the type II-1 according to GOST 2991размерами according to GOST 21140, with a gross mass not exceeding 50 kg.
The form boxes on wooden pallets according to GOST 9078 into transport packets according to GOST 26663 with strapping in the longitudinal and transverse directions of the metal tape not less than 0,3х30 mm according to GOST 3560 or wire with diameter at least 3 mm according to GOST 3282. The gross mass of the package is not more than 1.0 T.
(Changed edition, Rev. N 3, 6).
4.3. Transport marking — according to GOST 14192 with the application of manipulation sign «Sealed package».
(Changed edition, Rev. N 3, 6).
4.4. The powder transported by all kinds of transport in covered vehicles in accordance with cargo carriage regulations applicable to transport of this species.
(Changed edition, Rev. N 3).
4.5. Powder should be stored in packaging manufacturer in a dry warehouse premises at temperature not below 12 °C in the absence of environmental oxidants.
5. MANUFACTURER’S WARRANTY
5.1. (Deleted, Rev. N 3).
5.2. The manufacturer must ensure that the quality of the tin powder with the requirements of this standard, subject to consumer storage conditions specified in this standard.
5.3. The warranty storage period is set for six months from the time of issue of tin powder.
(Changed edition, Rev. N 3).