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GB/T 3780.5-2017: Carbon Black - Part 5: Determination of Specific Surface Area - CTAB Test Method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 3780.5: Historical versions
Similar standardsGB/T 3780.5-2017: Carbon Black - Part 5: Determination of Specific Surface Area - CTAB Test Method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT3780.5-2017GB 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 ContentsForeword ... 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 ScopeThis 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 ReferencesThe 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 Pipette3 PrinciplesSince 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 ConditionsLaboratory ambient temperature. (25±2) °C. The used laboratory equipment and reagent shall be kept at the laboratory temperature for 24h.5 Reagents and Materials5.1 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 Coefficient9.1 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 Precision12.1 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 ReportThe 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 full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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