GB/T 3780.5-2017 PDF English
Search result: GB/T 3780.5-2017_English: PDF (GB/T3780.5-2017)
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Name of Chinese Standard | Status |
| GB/T 3780.5-2017 | English | 150 |
Add to Cart
|
0-9 seconds. Auto-delivery.
|
Carbon black -- Part 5: Determination of specific surface area -- CTAB test method
| Valid |
| GB/T 3780.5-2008 | English | 519 |
Add to Cart
|
3 days
|
Carbon black -- Part 5: Determination of specific surface area -- CTAB test method
| Obsolete |
| GB/T 3780.5-2002 | English | 399 |
Add to Cart
|
3 days
|
Carbon black used in rubber products -- Determination of specific surface area -- CTAB test method
| Obsolete |
| GB/T 3780.5-1991 | English | 239 |
Add to Cart
|
2 days
|
Carbon black used in rubber products Determination of specific surface area--CTAB test method
| Obsolete |
BUY with any currencies (Euro, JPY, GBP, KRW etc.): GB/T 3780.5-2017 Related standards: GB/T 3780.5-2017
PDF Preview: GB/T 3780.5-2017
GB/T 3780.5-2017: PDF in English (GBT 3780.5-2017) GB/T 3780.5-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 83.040.20
G 49
Replacing GB/T 3780.5-2008
Carbon Black - Part 5. Determination of
Specific Surface Area - CTAB Test Method
ISSUED ON. NOVEMBER 01, 2017
IMPLEMENTED ON. MAY 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative References ... 5
3 Principles ... 5
4 Test Conditions ... 6
5 Reagents and Materials ... 6
6 Apparatus ... 7
7 Sample ... 8
8 Test Procedures ... 8
9 Determination of Correlation Coefficient ... 9
10 Calibration of CTAB Solution ... 10
11 Test Data Processing ... 10
12 Precision ... 11
13 Test Report ... 11
Appendix A (Informative) Determination of Correlation Coefficient and
Calculation Example ... 12
Carbon Black – Part 5. Determination
of Specific Surface Area – CTAB Test Method
WARNINGS. Personnel using this Part shall have practical working experience
in the formal laboratory. This Part doesn’t address all the possible security
issues. The users are responsible to take appropriate safety and health
measures; and ensure the compliance with conditions set by relevant national
regulations.
1 Scope
This Part of GB/T 3780 specifies a test method for the determination of the external
surface area of carbon black using cetyltrimethylammonium bromide (CTAB).
This Part is applicable to the carbon black for rubber.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB/T 3778 Carbon Black for Use in Rubber Products
GB/T 8170 Rules of Rounding off for Numerical Values & Expression and
Judgement of Limiting Values
GB/T 9578 Industry Reference Carbon Black 4#
GB/T 12808 Laboratory Glassware – One-Mark Pipette
3 Principles
Since the CTAB molecule is quite large, it can’t be absorbed on the inner surface of
the micropores of carbon black. Therefore, the CTAB specific surface area only reflects
the effective surface of the carbon black in contact with the rubber molecules.
The adsorption isotherm of carbon black in the aqueous solution of CTAB has s flat
section of a longer single molecule adsorption layer. The adsorption of CTAB by carbon
black is not affected by the surface tar-lie substance or functional groups such as
hydrogen and oxygen; the absorption can be quickly balanced by mechanical stirring
or ultrasonic vibration. After the dispersed colloidal carbon black was filtered off, the
amount of unabsorbed CTAB can be determined by using sodium sulfosuccinate
dioctyl ester (OT). The test results were determined by industrial color reference
carbon black ITRB or industrial reference carbon black 4# (IRC4#) to determine its
CTAB specific surface area.
4 Test Conditions
Laboratory ambient temperature. (25±2) °C. The used laboratory equipment and
reagent shall be kept at the laboratory temperature for 24h.
5 Reagents and Materials
5.1 Buffer solution, pH=7, dissolve 2.722g of potassium dihydrogen phosphate
(KH2PO4), 4.260g of disodium hydrogen phosphate (Na2HPO4) and 1.169g of sodium
chloride (NaCl) into 1dm3 of water.
5.2 CTAB solution, c(C19H42BrN) = 0.01mol/L; take 3.64g of CTAB
(cetyltrimethylammonium bromide) to dissolve into 900cm3 of water; add 100cm3 of
buffer solution; heat to 27°C~37°C and dissolve; cool off to 23°C~25°C before use. If
the room temperature is lower than 23°C, it may cause the CTAB to slowly crystalize.
5.3 OT (sodium sulfosuccinate dioctyl ester) solution, c(C20H37NaO7S) = 0.0022mol/L;
take 1.000g of 100% OT into 1dm3 of water containing 2.5cm3 of formaldehyde solution
(mass fraction of 37%); use magnetic stirrer to vigorously stir for 48h; after tightening
the lid, place into a cool and dry place for 12d then it can be used. The unsealed OT
reagent shall be stored in a desiccator. OT solution is prone to degradation and its
concentration change shall be noted during the use period.
5.4 Emulsifier OP (octyl phenyl polyoxyethylene ether, Triton × -100) solution, mass
fraction of 0.015%; completely dissolve 0.15g of OP in 1dm3 of water with a magnetic
stirrer.
5.5 Industry tint reference black (ITRB with specific surface area of 83.0×103m2/kg) or
industry reference carbon black 4# (IRC 4# with specific surface area of
78.5×103m2/kg), and conform to GB/T 9578.
b) Plug the stopper after adding the magnetic stirring bar; place into the ultrasonic
electromagnetic disperser; soaking depth shall be at least 50mm; keep the water
bath temperature at 23°C~25°C; sonicate in the water bath for 1min; then stir for
1min; repeat the operation for twice; the total time is 6min.
8.4 Place the dry filter membrane into the sample filter cartridge; install it according to
the installation requirements of filter cartridge of the pressured filtration device.
8.5 Dry the water droplets outside the conical flask; thoroughly pour the mixture of
carbon black sample and CTAB solution into the sample filter cartridge; tighten the
upper lid; install on the pressure filtration device; turn on the compressed gas; adjust
he gas pressure to 0.4MPa ~ 0.7MPa; it is better to filter out the liquid into a quick drop.
Discard the initially discharged about 10cm3 filtrate; COLLECT all the filtrate flowing
out before the foam at the lower end outlet of the sample filter cartridge is formed INTO
50cm3 conical flask; plug the stopper, shake for testing. If the filtrate of carbon black is
diafiltered, the sample shall be discarded, and can’t be re-filtered.
8.6 Install and debug the carbon black specific surface area tester or potentiometric
titrator according to the instrument manual; drain all bubbles on the pipeline and
interfaces of the titrator.
8.7 TRANSFER 5cm3 of filtrate from the to-be-tested filtrate in the 50cm3 conical flask
INTO a clean quartz cup; after adding 15cm3 of OP solution and magnetic stirring bar,
place the quartz cup into the instrument measuring tank (hand can’t touch the
transparent surface of the quartz cup). Press the “Titration” button; the titration shall
start automatically and the titration volume (cm3) shall be shown on the digital display
at the same time; after it stops automatically, record the consumed volume of OT
solution, V; accurate to 0.01cm3.
9 Determination of Correlation Coefficient
9.1 Separately take 5 parts of dry industry tint reference black (ITRB) or industry
reference carbon black (IRC4#) for the amount of 0.2g, 0.3g, 0.4g. 0.5g, 0.6g; accurate
to 0.1mg.
9.2 Measure as per the procedures from 8.3 to 8.7.
9.3 Draw a standard curve with OT solution consumption volume Vi (cm3) as the
ordinate, sample mass mi (g) as the abscissa; calculate the slope b (cm3/g) and the
intercept V0 (cm3) by the least squares; obtain the regression equation. Calculate the
specific surface area as per the Formula (1) in 11.1; the difference between the
calculated result and the standard value shall be no more than 1.5×103m2/g; otherwise,
repeat the steps from 9.1 to 9.3.
average value; then perform the data rounding-off as per the report requirements or
the provisions of GB/T 3778 through the GB/T 8170.
12 Precision
12.1 Repeatability – the absolute difference between two independent test results
obtained under the repeatability conditions shall be no greater than 1.9% of its average
value.
12.2 Reproducibility – the absolute difference between two independent test results
obtained under the reproducibility conditions shall be no greater than 5.1% of its
average value.
13 Test Report
The test report shall at least give the following contents.
a) Sample name and mark;
b) Reference standard of this test;
c) The selected standard reference carbon black and its specified specific surface
area during the solution calibrating period;
d) V0 and b values used to calibrate the solution;
e) Sample quality;
f) Volume of OT solution consumed by titration of sample;
g) Test results (average value, median value, number of tests);
h) The difference from the analysis procedures; and the anomaly in the test;
i) Test date.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
|