ASTM D6845-2012 red 5000 Standard Test Method for Silica Precipitated HydratedCTAB (Cetyltrimethylammonium Bromide) Surface Area《沉淀的水合硅石的标准试验方法 CTAB(溴化十六烷基三甲基铵)表面积》.pdf
《ASTM D6845-2012 red 5000 Standard Test Method for Silica Precipitated HydratedCTAB (Cetyltrimethylammonium Bromide) Surface Area《沉淀的水合硅石的标准试验方法 CTAB(溴化十六烷基三甲基铵)表面积》.pdf》由会员分享,可在线阅读,更多相关《ASTM D6845-2012 red 5000 Standard Test Method for Silica Precipitated HydratedCTAB (Cetyltrimethylammonium Bromide) Surface Area《沉淀的水合硅石的标准试验方法 CTAB(溴化十六烷基三甲基铵)表面积》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation:D684502 (Reapproved 2008) Designation: D6845 12Standard Test Method forSilica, Precipitated, HydratedCTAB(Cetyltrimethylammonium Bromide) Surface Area1This standard is issued under the fixed designation D6845; the number immediately following the designation indicates the year oforiginal
2、 adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the measurement of the specific surface are
3、a of precipitated silicas exclusive of area contained inmicropores too small to admit hexadecyltrimethylammonium bromide (cetyltrimethylammonium bromide, commonly referred toas CTAB) molecules. This test method is suitable for characterizing rubber-grade silicas of all types.1.2 The values stated in
4、 SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and h
5、ealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Eva
6、luating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesPractice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practic
7、e for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Summary of Test Method3.1 The isotherm for adsorption of an aqueous solution of CTAB on silicas has a long horizontal plateau corresponding to amonolayer coverage of the substrate surface from which the adsorbate
8、 is not sterically excluded. The CTAB adsorption by silicais independent of functional groups containing hydrogen and oxygen, etc. Rapid equilibration is achieved by using mechanicalstirring. Titration with dioctyl sodium sulfosuccinate (Aerosol OT3) solution to a turbidity maximum end point is used
9、 to determinethe unadsorbed CTAB after removal of the colloidally dispersed silica by ultrafiltration.3.2 Titration of the unadsorbed CTAB with Aerosol OT solution is accomplished by automatic titration.4. Significance and Use4.1 The CTAB molecule is relatively large; so it is not adsorbed in microp
10、ores or on surface roughness. Thus, the CTAB surfacearea reflects only the surface of the silica that is available for interaction with rubber molecules.5. Apparatus5.1 Analytical Balance, 0.1 mg sensitivity.5.2 Centifuge, capable of 67 rev/s (4000 r/m).5.3 Magnetic Spinbars,4chemically resistant co
11、vered (polychlorotrifluoroethylene or TFE-fluorocarbon), 6.4- or 4.8-mm (14-or316-in.) diameter, and length nearly equal to the diameter of 50 or 100 cm3Berzelius beakers, glass vials, or other glass vessels.1This test method is under the jurisdiction of ASTM Committee D11 on Rubber and is the direc
12、t responsibility of Subcommittee D11.20 on Compounding Materials andProcedures.Current edition approved Jan. 15, 2008.1, 2012. Published February 2008.2012. Originally approved in 2002. Last previous edition approved in 20022008 as D6845 02(2008). DOI: 10.1520/D6845-02R08.10.1520/D6845-12.2For refer
13、enced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3Aerosol OT is a registered trademark of the American Cyanamid Co., P
14、rocess Chemicals Dept., Wayne, NM 07470.4Examples of suitable spinbars are Catalog No. 9235-U7, A. H. Thomas Co., Philadelphia, PA 19105, or Catalog No. S-76497-30, Sargent Welch Scientific Co., Skokie,IL 60076.1This document is not an ASTM standard and is intended only to provide the user of an AST
15、M standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published
16、by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.4 Glass Funnel, small.5.5 Glass Vials, with plastic screw caps, 28 mm in outside diameter, about 40 cm3capacity.5.6 Buret,50cm3, 0.1 c
17、m3divisions, Class A, preferably of automatic refilling and zeroing type (see Note 1) with reagentreservoir.NOTE 1Automatic burets are usually not certified to Class A tolerance. Such burets should be checked for accuracy, and if in error by more than 0.05cm3at any point, a calibration curve should
18、be prepared and used to correct observed buret readings. Burets with TFE-fluorocarbon manostat valves offersome advantage in ease of stopcock manipulation in delivering small increments of titrant.5.7 Dispenser-Type Pipet,550 cm3, attached to a suitable reservoir for CTAB solution.5.8 Pipet,10cm3, C
19、lass A.5.9 Erlenmeyer Flasks, or beakers, 50 or 100 cm3.5.10 Dropping Bottle,60cm3amber.5.11 Jar, wide-mouth, plastic screw cap, 120 or 240 cm3(4- or 8-oz) size.5.12 Gravity Convection Drying Oven, capable of maintaining 105 6 5C.5.13 Magnetic Stirrer.5.14 Containers, suitable for preparation and st
20、orage of reagent solutions.5.15 Automatic Titration Equipment with 550 nm Photoprobe,6with instruction manual.5.16 Beakers, 100 cm3Berzelius, tall form (one furnished with automatic titration equipment).5.17 Thermometer, to measure temperature in a range from 20 to 40C.5.18 Polyethylene Tubing (do n
21、ot use vinyl tubing).NOTE 2All apparatus must be kept chemically clean. Contamination of equipment, water supply, or chemicals by ionic surfactants must beparticularly avoided.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is inten
22、ded that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where suchspecifications are available.7Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without less
23、ening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType 1 in Specification D1193.6.3 Sodium Hydroxide Solution (1M)Dissolve 40.0 g NaOH ina1dm3flask containing 0.5 dm3reagent water. Afterdi
24、ssolution fill to mark.6.4 Buffer Solution of pH 9.6 (0.05 M)Prepare buffer solution by dissolving 3.101 g of orthoboric acid (H3BO4), 3.708 g ofpotassium chloride (KCl) and 36.85 cm3of sodium hydroxide (NaOH) solution ina1dm3flask containing 0.5 dm3reagent water.After dissolution fill to mark. Veri
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