This standard specifies the pyrolysis method for the determination of carbon black content in vulcanized rubber and compounded rubber. This method is applicable to the determination of carbon black in the following vulcanized rubbers. Natural rubber; synthetic isoprene rubber; polybutadiene rubber; styrene butadiene rubber; ethylene-propylene-triethylene propylene rubber; butyl rubber; This method is not applicable to vulcanized rubbers containing halogens or nitrogen in the polymer, nor is it applicable to vulcanized rubbers containing compounding ingredients such as aluminum blocks or phenolic resins, because carbon-containing residues are formed during pyrolysis. GB/T 3515-1983 Determination of carbon black content in vulcanized rubber Pyrolysis method GB/T3515-1983 Standard download decompression password: www.bzxz.net

1 Scope of application
National Standard of the People's Republic of China
Determination of carbon black content in vulcanized rubber
Pyrolysis method
Rubber, yulcanized-determination of carbon black content-pyrolytic method This standard specifies the pyrolysis determination of carbon black content in vulcanized rubber and compounded rubber. This method is applicable to the determination of carbon black in the following various vulcanized rubbers. Natural rubber;
Synthetic isoprene rubber,
Polybutadiene rubber;
Styrene butadiene rubber;
Ethylene-propylene-blue ethylene-propylene rubber,
UDC 678.4/.7.063
GB 3515-83
Butyl rubber;
This method is not suitable for vulcanized rubber containing halogen or nitrogen in the polymer, nor for vulcanized rubber containing compounding agents such as aluminum blocks or phenolic resins, because carbon-containing residues are formed during pyrolysis. The presence of inorganic fillers that can be decomposed at pyrolysis temperature may affect the precision of this method. 2 Test method
2.1 Principle
After weighing the sample, it is extracted with solvent, dried, and the organic components are pyrolyzed in a nitrogen stream. The carbon black is then burned out in the air. The difference in the secondary mass is the carbon black content.
2.2 Reagents
Nitrogen: dry and oxygen-free (the use of commercial "oxygen-free nitrogen" requires further purification). 2.2.1
Acetone (GB686-78): chemically pure.
Chloroform (GB682-65): chemically pure. Xylene: industrial product.
2.3 Apparatus (as shown)
Pyrolysis apparatus
1-Nitrogen; 2-Deoxygenation apparatus, 3-Tube furnace, 4-Quartz tube; 5-Quartz boat, 6-Tail gas absorption apparatus National Bureau of Standards 1983-03-03 Issued
Marked Industry Free Sale
1983-12-01 Implementation
Quartz combustion tube.
Quartz combustion boat: 50-60mm long.
GB 3515-83
Tube furnace and temperature control device: can control 800～900℃. 2.3.3
2.3.4 Tail gas absorption device:
a. Condensate storage bottle.
Absorption bottle containing xylene.
2.3.5 Appropriate extraction device: see GB3516-83 "Determination of solvent extracts in vulcanized rubber" for details. 2.3.6 Dryer.
2.4 Operation steps
Weigh 0.1～0.2g (0.0002g) 1mm2 granular sample, wrap it with filter paper, extract it with acetone, if the sample contains asphalt, extract it with chloroform, extract it for at least 4h for each solvent, and dry it. Heat the tube furnace to 800-900℃ and keep the temperature constant. Place the sample in a quartz boat, place the boat in a quartz combustion tube, and place the quartz tube at the entrance of the tube furnace, plugging the tube mouth. Connect the nitrogen device through a flowmeter at the inlet of the quartz tube, and connect the gas condensation absorption device at the quartz outlet. bzxz.net
After purging the system with a nitrogen flow rate of 200cm3/min for 10 minutes, reduce the flow rate to 100cm2/min, gradually move the boat from the cold zone of the tube furnace to the hot zone within 5 minutes, and park for 5 minutes. Withdraw the boat to the cold zone of the tube furnace, cool the boat in the combustion tube for 10 minutes under continuous nitrogen flow, and close the nitrogen inlet valve. Take out the quartz boat and place it in a desiccator, cool it to room temperature, and weigh it. Put the boat back into the original tube furnace or muffle furnace, control the temperature to 800-900℃, and burn out the carbon black in the boat under air conditions. Take out the boat in a + desiccator, cool it to room temperature, and weigh it again.
2.5 Expression of results
The percentage of carbon black is calculated as follows:
Carbon black (%)=m1=m2×100
Where: mo-
Sample mass, g,
Boat and residue mass after cracking, g;
Boat and ash mass, g.
2.6 Precision
The precision of this method is expressed as the standard deviation s of the test data. The standard deviation s is calculated as follows:
Where: n -
-Number of tests;
X,—Single test value,
X—--Nth test average.
The standard deviation of this method should be less than or equal to 0.43%. Additional remarks:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and was developed by the Beijing Rubber Industry Research and Design Institute of the Ministry of Chemical Industry. This standard was drafted by the Beijing Rubber Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafter of this standard is Jia Naicheng.
This standard is entrusted to the Beijing Rubber Industry Research and Design Institute of the Ministry of Chemical Industry for interpretation.
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