1、Designation: D6740 10Standard Test Method forSilanes Used in Rubber Formulations(bis-(triethoxysilylpropyl)sulfanes): Residue on Ignition1This standard is issued under the fixed designation D6740; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 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 determination of the residueon ignition of silanes of the type b
3、is-(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 does not purport to ad
4、dress 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. Referenced Documents2.1 ASTM Standards:2E177 Practic
5、e for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 In this test method, a sample of the silane is treated withhydrochloric acid and then ignited in a muffle furnace
6、at1000C. The mass retained after this procedure is called theresidue on ignition. It is expressed in percentage of the initialmass.4. Significance and Use4.1 The residue on ignition, which consists essentially ofSiO2, is related to the silicon content of the silane and may beused to verify the compo
7、sition of the silane.5. Apparatus5.1 Analytical Balance, accuracy 60.1 mg.5.2 Simon-Mueller Oven, or equivalent (850C).5.3 Muffle Oven, (1000C).5.4 Porcelain Crucible (High-Form), capacity 25 cm3.5.5 Beaker, 500 cm3.5.6 Graduated Pipet,20cm3.5.7 Graduated Cylinder, 250 cm3.5.8 Glass Rod.5.9 Desiccat
8、or.6. Reagents6.1 Hydrochloric Acid, 37 %, analytical grade.6.2 Sulfuric Acid, 96 %, analytical grade.6.3 Deionized Water.6.4 Silica Glass Wool.7. Preparation of 90 % Sulfuric Acid7.1 Pipet 20 cm3of deionized water into 500 cm3beakercontained in an ice-water bath.7.2 While stirring with a glass rod,
9、 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.7.3 Cool to room temperature.7.4 Transfer the mixture into a suitable glass bottle.8. ProcedureNOTE 2Preheat porcel
10、ain 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.8.1 Liquid Silanes:8.1.1 Weigh (tare) a predried crucible and glass wool plug.Remove the glass wool and tare the crucible alone.8.1.2
11、 Weigh approximately1goftheliquid silane into thepre-treated crucible to the nearest 0.1 mg.8.1.3 Add 2 cm3of 90 % sulfuric acid and homogenize bycareful agitation.8.1.4 Cover the mixture with pre-treated silica glass wool.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberan
12、d is the direct responsibility of Subcommittee D11.20 on Compounding Materialsand Procedures.Current edition approved June 1, 2010. Published July 2010. Originally approvedin 2001. Last previous edition approved in 2006 as D6740 01 (2006). DOI:10.1520/D6740-10.2For referenced ASTM standards, visit t
13、he ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
14、 United States.8.1.5 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.8.1.6 When most of the acid has been evaporated (usuallyafter 1 h),
15、 transfer the crucible into a muffle furnace, previouslybrought to 1000C.8.1.7 Heat for2hat1000C.8.1.8 If the ash is gray or black, continue heating for anadditional2hinthemufflefurnace at 1000C.8.1.9 Allow to cool in a desiccator and weigh to the nearest0.1 mg.8.2 Admixtures of Silanes and Carbon B
16、lack:8.2.1 Weigh (tare) a pre-dried crucible and glass wool plug.Remove the glass wool and tare the crucible alone.8.2.2 Weigh approximately1gofthesilane/carbon blackadmixture into the pre-treated crucible to the nearest 0.1 mg.8.2.3 Add 2 cm3of 37 % hydrochloric acid and homogenizeby careful agitat
17、ion.8.2.4 Cover the contents with the respective glass woolplug.8.2.5 Place the crucible into a Simon-Mueller oven,mounted in a fume-cupboard, and raise the temperature to125C.NOTE 4The Simon-Mueller oven may be replaced by an electricalheating plate if the former is not available.8.2.6 When the maj
18、or part of the acid has been evaporated(usually after 1 h), transfer the crucible into a muffle furnace,previously brought to 1000C.8.2.7 Heat for2hat1000C.8.2.8 If the ash is gray or black, continue to heat the cruciblefor an additional2hinthemufflefurnace at 1000C.8.2.9 Allow to cool in a desiccat
19、or and weigh to the nearest0.1 mg.9. Calculation9.1 Calculate the residue on ignition to the nearest 0.01 % asfollows:Residue on ignition 5C A!B A!3 100 (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 g
20、lass wool plus the residue onignition, g.10. Report10.1 Report the following information:10.1.1 Proper identification of the sample, and10.1.2 The average of two single determinations, reported tothe nearest 0.01 %.11. Precision and Bias311.1 The precision of this test method is based on aninterlabo
21、ratory study conducted in 2008. Seven laboratoriesparticipated in this study. Each of the labs reported fourreplicate test results for a single material. Every “test result”reported represents an individual determination. Except for theuse of only a single material, Practice E691 was followed forthe
22、 design and analysis of the data.11.1.1 Repeatability limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more than the “r” value for that material; “r”istheinterval representing the critical difference between two testresults for the same material
23、, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.11.1.1.1 Repeatability limits are listed in Table 1.11.1.2 Reproducibility limit (R)Two test results shall bejudged not equivalent if they differ by more than the “R” valuefor that material; “R” is the inte
24、rval representing the criticaldifference between two test results for the same material,obtained by different operators using different equipment indifferent laboratories.11.1.2.1 Reproducibility limits are listed in Table 1.11.1.3 The above terms (repeatability limit and reproduc-ibility limit) are
25、 used as specified in Practice E177.11.1.4 Any judgment in accordance with statement 11.1.1 or11.1.2 would have an approximate 95 % probability of beingcorrect.11.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testmethod, therefore
26、no statement on bias is being made.11.3 The precision statement was determined through sta-tistical examination of 28 results, from six laboratories, on onematerial. Due to the small number of participating labs, nooutliers were removed. This material was described as follows:Material A is a commerc
27、ially available bis-(triethoxysilylpropyl)tetra sulfane.12. Keywords12.1 ash; organosilanes; silanes3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1102.TABLE 1 Residue on Ignition (%)Material AverageARepeatabilityStandardDe
28、viationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitx SxSrSRrRA 22.86 0.17 0.12 0.20 0.35 0.57AThe average of the laboratories calculated averages.D6740 102ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item
29、mentionedin this standard. Users of this standard are expressly advised that determination 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 commit
30、tee and must be reviewed every five years andif not revised, either reapproved or 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 mee
31、ting of theresponsible technical committee, which you may attend. If you feel that 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,
32、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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D6740 103
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