This part specifies the sampling, analysis procedures, result presentation and test report for the determination of dibutyl phthalate absorption value of carbon black (compression specimen). This part is applicable to carbon black for rubber. GB/T 3780.4-2003 Carbon black Part 4: Determination of dibutyl phthalate absorption value and sample preparation (compression specimen) GB/T3780.4-2003 Standard download decompression password: www.bzxz.net

ICS 83.040.30
National Standard of the People's Republic of China
GB/T 3780.4--2003
Replaces GB/T3780.4·-1994
Carbon black--Part 4:
Deternination of dibutylphthalate absorption value and preparation of samples (compressed sample)
[ISO 6894:1991(E),Rubber compounding ingredients—Carbon black-Preparation of samples for determination of dibutylphthalateabsorptionnumber(coipressedsample),MoD)2003-10-11 Issued
People's Republic of China
General Administration of Quality Supervision, Inspection and Quarantine
2004-05-01 Implementation
GBT3780 is to be divided into the following parts: Part 1: Test method for iodine absorption value
Part 1: Dibutyl phthalate -Determination of absorption value; -Part 4: Determination of absorption value of 1-butyl phthalate and preparation of test specimens (compressed test specimens); -Part 5: Determination of specific surface area (TA method); -Part 6: Test method for tinting strength;
Part 7: Determination of H value;
Part 8: Determination of thermal loss:
-… Part 1: Determination of ash content;
-Part 11: Determination of sieve residue;
-Part 12: Inspection of impurities;
Part 14 Part: Determination of sulfur content;
Part 15: Rapid determination of transmittance of toluene extract: Part 1: Indirect determination of particles by reflectance method - Part 8; Formulation and identification methods in natural rubber: Part 20, Determination of transmittance of toluene by identification method; Part 21: Determination of sieve residue by water washing method. GB/T 3780.4-2003
This part is Part 4 of GB/T3780, corresponding to IS06894:1991 (E) Rubber compounding carbon black compression test sample determination of phthalic acid butyl ester absorption value test sample preparation. The consistency degree of this part with IS06894:1901 (F) is modified and adopted. This part replaces G13/T3780.41994 Carbon black (compression test sample) butyl phthalate absorption value determination method and test sample preparation, because the original standard is technically backward. This part is redrafted based on IS (6894): 1991 (F). For the convenience of comparison, a comparison table of the clauses of this national standard and the clauses of the international standard is listed in the informative appendix B. Due to the legal requirements of my country and the special needs of the industry, this part has been modified when adopting the international standard. These technical differences are marked with a vertical single line in the margin of the clauses they affect. In the Appendix, a table of technical differences and their causes is given for reference. For ease of use, the following editorial changes have been made to this part: the term "International Standard" is replaced by "*" in this part; the decimal point is replaced by "." in this part; the "Specifications" chapter is divided into two paragraphs. The main technical differences between this part and (G13/T 3780.4-1994): the front sound "\|tt|| is added; the sample at the bottom of the fourth shrinkage is added to pass through the 850 rm sieve (see 6.1.11 and 6.2.13); it is indicated that the absorption value of dibutyl phthalate of the compressed sample can be determined by method B of (G13/T 3780.2) (7.11 of the 1994 version, 6.2.13 of this version). 1.12 and 6.2.11) #· Removed the chapter of the 14th edition! Added informative record 'O-benzene dicarboxylic acid absorption value of compressed specimen of standard reference carbon black (see Appendix A); GB/T 3780.4-2003
- Added informative appendix "Comparison of chapter and article numbers of this part with those of ISO 6894:1991 (F) (see Appendix B): - Added informative appendix 15) Technical group differences between this part and ISO 6894:1991 (E) and their original drawings (see Appendix) Appendix A, Appendix B and Appendix C of this part are all informative records. This part was prepared by China Rubber and Chemical Industry Association. This part was prepared by the Carbon Black Sub-Technical Committee of the National Technical Committee for Standardization of Rubber and Rubber Products. Drafting unit of this part: China Rubber Group Carbon Black Industry Research and Design Institute, main contributors of this part: Dai Chuanyin, Yu Yan The previous versions of the standards replaced by this part are: GI3/T 3780, 4—1983.GB/T 3780. 4—1994. Carbon black Part 4:
Determination method of dibutyl phthalate absorption value and sample preparation (compression specimen)
GB/T 3780.4—2003
Notice that the personnel using this part should have practical experience in formal laboratory work. This part does not point out all possible safety issues. The user is responsible for taking appropriate safety and health measures and ensuring that the conditions stipulated by relevant national laws and regulations are met. 1 Scope
This part specifies the sampling, analysis steps, result expression and test report for the determination of dibutyl phthalate absorption value using dibutyl phthalate (compression specimen):
This part applies to carbon black for rubber.
2 Normative references
The clauses in the following documents become the clauses of this part through the application of this part. For any dated reference, all subsequent amendments (excluding errata) or revised versions are not applicable to this part. However, parties to an agreement based on this part are encouraged to study whether the latest versions of these documents can be used. For any undated reference, the latest version applies to this part. GH3778 Carbon black for rubber
GB/T378U.2 Carbon black Part 2 Determination of dibutyl phthalate absorption value (GB/T 3780.2·-2003,IS04t56-1 : 19s2( E),Rubber compouncing ingredients--Carhon black—Determination of dibutyl phthalateabsorpxion numher Pert 1:Method using absorpiometer,M(oD)GB/T3780.SDetermination of carbon black heating loss (GB/T3780.8--2002,ccVIS) 1126:1992.Rubbercompounding ingredients Carhon black Delertninatiot of loss on heating)3 Principle
A certain amount of dried carbon black is condensed 4 times under a pressure of 165MP month, and then its dibutyl phthalate (DBP) absorption value is determined according to GB/T3780.2.
4 Instruments and equipment
4.1 Balance, accuracy 0.31g
4.2 Oven, gravity convection plastic moon can control temperature (105W)4.3 Compressor and plunger, see Figures 1 and 2.4.4 Bed compressor, power head travel speed4.2 Im/s, can make the sample under pressure 165 MPa4.5 Scrape.
4.6 Stainless steel cup.
4.7 Bristle brush with bristles 38mg long.Www.bzxZ.net
4.8 Dryer,
5 Sampling
5.1 Sampling shall be carried out according to the method specified in GB3778.
5.2 Place a sufficient amount of carbon black sample in an oven (4.2) at (105±2)℃ and dry for 1h. Then place it in a dryer (4.8) for cooling. GB/T 3780.4--2003
Standby.
6 Analysis steps
6.1 Operation procedure of type A compressor
6.1.1 Place the bottom sealing plate and compression cylinder (1.3) in the specified position of the compressor (4.4), shake the bottom sealing plate handle to correct the position of the bottom sealing plate on the base plate 1:, and then rotate the compression cylinder to make it fit properly with the bottom sealing plate. Unit: mm
+31.5002k
$31. 7 g 0026
91.8±0.0127 Inner diameter
Inner coating 0.304 Buml
1·-. Plunger
2-- --Nylon lining;
3---Compression system;
1-Bottom sealing plate
Figure 1 Main components of type A compression cylinder and plunger 6.1.2 Weigh (25±0.1)g of dried carbon black sample (5.2). 6.1.3 Pour the weighed carbon black sample into the compression cylinder (4.3). 6.1.4 Put the plunger into the compression cylinder, and the end with the nylon gasket touches the sample, then gently turn the plunger by hand and press it down into the cylinder as much as possible. 6.1.5 Adjust the plunger, compression cylinder and power head to form a straight line, and keep the piston free to move. 6.1.6 Press the start button to compress the sample to 165MPa, and hold for 1s. Then release the pressure. Note: The indication of the oil pressure gauge is related to the inner diameter of the compression cylinder and the surface of the bottom end of the power head. 6.1.7 Lift the power head, remove the bottom sealing plate, and then lower the power head until the plunger and the sample are just pressed out of the compression cylinder and into the stainless steel cup (4.6).
6.1.8 Wipe the carbon black dust off the compression cylinder, plunger and bottom sealing plate, and replace the bottom sealing plate and compression cylinder on the base plate of the compressor according to the requirements of 6..1.
6.1.9 Use a scraper to break up the carbon black sample until the largest carbon black agglomerate is no larger than 0.25 cm. Ensure that no sample is lost during the operation. 6.1.10 Repeat the compression operation of 6.1.3 to 6.1.9 to compress the sample a total of 4 times. 6.1.11 Pass the sample after the 4th compression through an 850 ± m sieve, and then retain the sample for testing. GB/T 3780.4—2003
If the compression sample is not tested within 15 min after sieving, the sample should be kept in a desiccator or re-dried at (105±2) for 1 h before testing.
Unit: meter
Upper part
Plunger:
Compression cylinder,
Plunger in cylinder:
Hopper.
Main parts of type B compression cylinder and plunger in Figure 2 Weigh (20±0.02) compression sample (all kinds of carbon black are weighed in this amount), and determine its phthalate diester absorption value according to method A of GB/T3780.2; or determine its dibutyl phthalate absorption value according to method B of GB/T3780.2. It is very important to check the measured results with a standard reference carbon black with a similar value. The test results of the standard reference carbon black should be guaranteed to be within the specified range.
6.2 Operation procedures of type B compressor (Figure 2) 6.2.1 Weigh (25=0.1) dried carbon black sample (5.2), 6.2.2 Pour the weighed carbon black sample into the compression cylinder (4.3). 6.2.3 Start the right control valve to move the power head downward to compress the sample until the pressure indicated by the equipment is 103 MPa, then immediately release the pressure. 6.2.4 Use the right control valve to lift the power head until the power head is about 4 cm away from the compression valve, that is, flush with the edge of the hopper 1. GB/T 3780.4--2003
6.2.5 Use the left control valve to raise the plunger in the cylinder to push the sample out of the compression cylinder. At the same time, it is squeezed by the power head on the back and then put into the hopper. 6.2.6 Use a scraper to break up the sample until the largest carbon agglomerate is no larger than 0.25 cm1. Ensure that no sample is lost during the operation. 6.2.7 Lower the plunger in the cylinder to allow the carbon black sample to fall back into the compression cylinder. Use a brush to sweep all the carbon black in the hopper into the compression cylinder. 6.2.8 Repeat the operations of 6.2.3 to 6.2.7 twice. 6.2.9 Remove the hopper and repeat the operation of 6.2.3 again. 6.2.10 Raise the power head with the right control valve. 6.2.11 Raise the plunger in the cylinder with the left control valve. Push the sample out of the compression cylinder. 6.2.12 Reset the plunger in the cylinder with the left control valve. 6.2.13 Pass the sample after the fourth compression through a &50 μr1 sieve and retain the sample for testing. If the compressed sample is not tested within 15m after compression, the sample shall be kept in a desiccator or re-dried at (1052)℃ for 1h before testing. 6.2.14 Weigh (20-0.02)g of compressed sample (this amount is used for all kinds of carbon black) and determine its absorption value of dibutyl phthalate according to Method A of GB/T3780.2 or its absorption value of monobutyl phthalate according to Method B of GB/T3780.2. It is very important to verify the measured results with a standard reference carbon black with a similar value, and the test results of the standard reference carbon black should be guaranteed to be within the specified range. 7 Result expression According to GE /T3780.2 requirements for the expression of results
8 Test report
The test report shall include the following contents:
0) Type and number of the test sample;
b) Number of the standard on which the test is based;
Type of compression derivative used; Method for measuring the absorption value of phthalate esters; d) Test results;
e) Differences from the specified analytical procedures;
Abnormal phenomena observed during the test:
, Test date.
Appendix A
(Informative Appendix)
Absorption value of tributyl phthalate of compression specimen of standard reference carbon black Absorption value of dibutyl phthalate of compression specimen of standard reference carbon black See Table A.1. Table A.1 Dibutyl phthalate absorption values ​​of compression specimens of standard reference carbon Standard reference carbon black
(N135)
(N22C)
(N762)
(NG6C)
(N683)
Standard value!
(10-n\/kg)
J18. 111.23
86.8:1.20
98. 4 - 1. 20
57. 8 =1. 74
72. 3 -1.23
88.4±2.01
Standard reference carbon black
(N134)
(V326)
(N762)
(NSGO)
(N683)
GB/T3780.4—2003
Standard value!
(10m/sg)
101.0_2.46
98. 5= 1. 30
68. ​​1-.1. 59
60.2-1.59
76.012. 49
88. 6±2. 58
GB/T3780.4—2003
Appendix B
(Informative)
Comparison table B.1 of the chapter and article numbers of this part with those of IS06894:1991(E) gives a comparison table of the chapter and article numbers of this part with those of IS06894:1991(E). Table B.1 Correspondence between the abbreviations of this part and the chapter numbers of ISO 06894: 1991 (E) Chapter and clause numbers of this part
5.1.1 to 6.1.9
6, 1.11, paragraph 1
6, 1.11, paragraph 2
6.2.1 to 6.2.12
6.2.13, paragraph 1
6.2.13, paragraph 2
Appendix A
Appendix B
Appendix C
Corresponding chapter and clause numbers of the international standard
2, paragraph 4.5
7.1.1 to 7.1.9
7.1.10, paragraph 1 7.1.10, the second paragraph, 7.2.1 to 7.2, 12, the second paragraph of 7.2.13. General Note: The numbers of the other clauses of this part other than the clauses in the table are alternate with the numbers of other clauses of ISO 6894:1991(E) and the contents are corresponding. Appendix (informative) Technical differences between this part and ISO 6894:1991(E) and their causes Table C.1 gives a list of the technical differences between this part and ISO 6894:1991(F) and their causes. Table C.1 Technical differences between this part and IS0 6894:1991 (E) and their reasons Article number of this part
4. 2, 5, 2,
6. 1, 11, 6, 2, 13
6. 1. 11, 6. 2. 13
6. 1. 12, 6. 2.14
Technical differences
Quotes Chinese standards based on international standards instead of international standards
Added reference G3778. Deleted 50 689:9(), paragraph 1
1S0 4656:2:1981, paragraph 5150 6809:1389Deleted 4.2.57.1.11 and 7.2, 13 of ISO 6894:1991(F) Dryness (125±2)℃. Added sampling section,
Added that the sample after the first compression should be sieved through 55 1μm sieve. Added? GR/T 378(2) method (technical method) for measuring DBP absorption value: GB/T 3780.4—2003 is not suitable for my country's situation. There are some contents in this standard. It is not suitable for my country's situation. It is more complete with other standards in the carbon black industry. It is convenient for the dry weight of samples and the determination of DBP absorption value. It is not suitable for my country's situation.
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