1、Designation: D 6740 01 (Reapproved 2006)Standard Test Method forSilanes Used in Rubber Formulations(bis-(triethoxysilylpropyl)sulfanes): Residue on Ignition1This standard is issued under the fixed designation D 6740; the number immediately following the designation indicates the year oforiginal adop
2、tion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the residueon ignition of
3、silanes of the type bis-(triethoxysilylpropyl)sulfane, or of admixtures of these silanesand solid carriers, such as carbon black, waxes, or organicpolymers.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard d
4、oes not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Summary of Test Method2.1 In th
5、is test method, a sample of the silane is treated withhydrochloric acid and then ignited in a muffle furnace at1000C. The mass retained after this procedure is called theresidue on ignition. It is expressed in percentage of the initialmass.3. Significance and Use3.1 The residue on ignition, which co
6、nsists essentially ofSiO2, is related to the silicon content of the silane and may beused to verify the composition of the silane.4. Apparatus4.1 Analytical Balance, accuracy 60.1 mg.4.2 Simon-Mueller Oven, or equivalent (850C).4.3 Muffle Oven, (1000C).4.4 Porcelain Crucible (High-Form), capacity 25
7、 cm3.4.5 Beaker, 500 cm3.4.6 Graduated Pipet,20cm3.4.7 Graduated Cylinder, 250 cm3.4.8 Glass Rod.4.9 Desiccator.5. Reagents5.1 Hydrochloric Acid, 37 %, analytical grade.5.2 Sulfuric Acid, 96 %, analytical grade.5.3 Deionized Water.5.4 Silica Glass Wool.6. Preparation of 90 % Sulfuric Acid6.1 Pipet 2
8、0 cm3of deionized water into 500 cm3beakercontained in an ice-water bath.6.2 While stirring with a glass rod, add, very slowly, inseveral steps, 250 cm3of 96 % sulfuric acid.NOTE 1Adding acid too fast will generate excessive heat in themixture and may result in acid splashes. Handle carefully.6.3 Co
9、ol to room temperature.6.4 Transfer the mixture into a suitable glass bottle.7. ProcedureNOTE 2Preheat porcelain crucibles and silica glass wool used for thetest for 2 h at 1000C in a muffle furnace. Cool to room temperature andstore in a desiccator until needed for the test.7.1 Liquid Silanes:7.1.1
10、 Weigh (tare) a predried crucible and glass wool plug.Remove the glass wool and tare the crucible alone.7.1.2 Weigh approximately1goftheliquid silane into thepre-treated crucible to the nearest 0.1 mg.7.1.3 Add 2 cm3of 90 % sulfuric acid and homogenize bycareful agitation.7.1.4 Cover the mixture wit
11、h pre-treated silica glass wool.7.1.5 Place the crucible into a Simon-Mueller oven,mounted in a fume-cupboard, and raise the temperature to125C.NOTE 3The Simon-Mueller oven may be replaced by an electricalheating plate if the former is not available.7.1.6 When most of the acid has been evaporated (u
12、suallyafter 1 h), transfer the crucible into a muffle furnace, previouslybrought to 1000C.7.1.7 Heat for2hat1000C.7.1.8 If the ash is gray or black, continue heating for anadditional2hinthemufflefurnace at 1000C.7.1.9 Allow to cool in a desiccator and weigh to the nearest0.1 mg.1This test method is
13、under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.20 on Compounding Materialsand Procedures.Current edition approved Oct. 1, 2006. Published November 2006. Originallyapproved in 2001. Last previous edition approved in 2001 as D 6740 01.1Copyri
14、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 Admixtures of Silanes and Carbon Black:7.2.1 Weigh (tare) a pre-dried crucible and glass wool plug.Remove the glass wool and tare the crucible alone.7.2.2 Weigh approximately1gofthesilane/
15、carbon blackadmixture into the pre-treated crucible to the nearest 0.1 mg.7.2.3 Add 2 cm3of 37 % hydrochloric acid and homogenizeby careful agitation.7.2.4 Cover the contents with the respective glass woolplug.7.2.5 Place the crucible into a Simon-Mueller oven,mounted in a fume-cupboard, and raise t
16、he temperature to125C.NOTE 4The Simon-Mueller oven may be replaced by an electricalheating plate if the former is not available.7.2.6 When the major part of the acid has been evaporated(usually after 1 h), transfer the crucible into a muffle furnace,previously brought to 1000C.7.2.7 Heat for2hat1000
17、C.7.2.8 If the ash is gray or black, continue to heat the cruciblefor an additional2hinthemufflefurnace at 1000C.7.2.9 Allow to cool in a desiccator and weigh to the nearest0.1 mg.8. Calculation8.1 Calculate the residue on ignition to the nearest 0.01 % asfollows:Residue on ignition 5C A!B A!3 100 (
18、1)where:A = mass of crucible and silica glass wool, g,B = mass of crucible, silica glass wool plus the sample, g,andC = mass of crucible, silica glass wool plus the residue onignition, g.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample, and9.1.2 The average of
19、two single determinations, reported tothe nearest 0.01 %.10. Keywords10.1 ash; organosilanes; silanesASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that det
20、ermination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved o
21、r withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel th
22、at your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 6740 01 (2006)2
