ASTM D5095-1991(2007) Standard Test Method for Determination of the Nonvolatile Content in Silanes Siloxanes and Silane-Siloxane Blends Used in Masonry Water Repellent Treatments《砖.pdf

1、Designation: D 5095 91 (Reapproved 2007)Standard Test Method forDetermination of the Nonvolatile Content in Silanes,Siloxanes and Silane-Siloxane Blends Used in MasonryWater Repellent Treatments1This standard is issued under the fixed designation D 5095; the number immediately following the designat

2、ion indicates the year oforiginal adoption 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 describes a proc

3、edure for the determi-nation of the nonvolatile content (Ns) of silanes, siloxanes, andblended silane-siloxane materials used in masonry water repel-lent treatments and is applicable to both solvent- and water-borne materials.1.2 The values stated in SI units are to be regarded asstandard. No other

4、units of measurement are included in thisstandard.1.3 This standard does 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 health and safety practices and determine the applica-bility of r

5、egulatory limitations prior to use. For a specifichazard statement, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 3980 Practice for Interlaboratory Testing of Paint andRelated Materials3E 145 Specification for Gravity-Convection and Forced-Ventilati

6、on Ovens3. Summary of Test Method3.1 A designated quantity of test material is weighed into apreweighed aluminum dish containing the catalyst solution,mixed, allowed to stand for 60 min at room temperature, andthen heated in an oven at 110 6 5C for 60 min. Thenonvolatile content of the test material

7、 is calculated bysubtracting the solids of the catalyst solution from the totalsolids by weight of the test solution.4. Significance and Use4.1 This test method is used to determine the nonvolatilecontent of silanes, siloxanes, and silane-siloxane blendedmaterials used in masonry water-repellent tre

8、atments. It can beused for the purpose of calculating the volatile organic com-pound (VOC) content of these materials under specified testconditions.5. Apparatus5.1 Aluminum Dishes, 58-mm diameter by 18-mm high witha smooth (planar) bottom surface. Precondition the dishes for30 min in an oven at 110

9、 6 5C and store in a desiccator priorto use.5.2 Forced Draft Oven, Type IIAor Type IIB as specified bySpecification E 145.5.3 Syringes, 1-mL and 5-mL.5.4 Analytical Balance, capable of weighing to 0.1 mg.6. Reagents6.1 Purity of WaterUnless otherwise indicated, referencesto water shall be understood

10、 to mean reagent water as definedby Type IV of Specification D 1193.6.2 p-Toluenesulfonic Acid, monohydrate.46.3 Alcohol, technical grade ethanol or isopropanol.7. Hazards7.1 In addition to other precautions, provide adequate ven-tilation, consistent with accepted laboratory practice, to limitthe ac

11、cumulation of solvent vapors.8. Procedure8.1 Catalyst SolutionPrepare a catalyst solution contain-ing a mixture of 0.5 % p-Toluenesulfonic acid in either ethanolor isopropanol. Thoroughly mix the solution. Prepare sufficientcatalyst solution to perform all tests.1This test method is under the jurisd

12、iction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.47 on Concrete, Stone and Masonry Treatments.Current edition approved July 1, 2007. Published July 2007. Originally approvedin 1990. Last previous edition approv

13、ed in 2002 as D 5095 91 (2002).2For referenced ASTM standards, visit the 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.3Withdrawn.4The sole source of

14、 supply of the solution of pToluenesulfonic acid known tothe committee at this time is King Industries, Science Road, Norwalk, CT 06852. Ifyou are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at am

15、eeting of the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.1.1 The nonvolatile content of the test material can becalculated only if the same catalyst solution is used throug

16、houtthe test. Each time a new batch of catalyst solution is used, itsnonvolatile content must be determined.8.2 Determine the nonvolatile matter, in triplicate, of thecatalyst solution as follows:8.2.1 Weigh an aluminum dish to 0.1 mg. Record the weightas W1.8.2.2 Using a 5-mL syringe, weigh 3 6 1.0

17、 g, to 0.1 mg, bydifference, of the catalyst solution into the preweighed alumi-num dish. Record the weight of catalyst solution as W3.8.2.3 Heat the aluminum dish containing the catalyst solu-tion in a forced draft oven for 60 min at 110 6 5C.8.2.4 Remove the dish from the oven and immediately plac

18、ein a desiccator. Seal the desiccator and allow the dish to cool toambient temperature.8.2.5 Reweigh the dish to 0.1 mg. Record the weight as W2.8.2.6 Calculate the nonvolatile matter of the catalyst solu-tion, Nc, in accordance with 9.1.8.3 Determine the percent nonvolatile content, in triplicate,o

19、f the test specimen as follows:8.3.1 Thoroughly mix the test materials before use.8.3.2 Weigh an aluminum dish to 0.1 mg. Record the weightas W4.8.3.3 Using a 5-mL syringe, weigh 3 6 1.0 g, to 0.1 mg, bydifference, of the catalyst solution into the preweighed alumi-num dish. Record the weight as W6.

20、8.3.4 Using a 1-mL syringe, weigh 1.0 6 0.1 g, to 0.1 mg,by difference, of the test specimen into the weighing dishcontaining the catalyst solution. Record the weight of the testspecimen as S.8.3.4.1 Weighings must be done quickly to limit weight lossdue to volatilization. If there is insufficient m

21、oisture presentwhen testing solvent-borne silane materials, it is advisable toadd up to 0.3 g of reagent grade water to the dish containing themixture of catalyst and test solutions.8.3.5 Gently swirl the dish to mix the materials. Allow thematerials to stand at room temperature for 60 min.8.3.6 Hea

22、t the dish containing the mixture of catalyst andtest solutions in a forced-draft oven for 60 min at 110 6 5C.8.3.7 Remove the dish from the oven and immediately placein a desiccator. Seal the desiccator and allow the dish to cool toambient temperature.8.3.8 Reweigh the aluminum dish to 0.1 mg and r

23、ecord theweight as W5.8.3.9 Calculate the nonvolatile content, Ns, of the testspecimen in accordance with 9.2.9. Calculation9.1 Calculate the nonvolatile matter, Nc, in the catalystsolution as follows:Nc5 W22 W1! / W3(1)where:Nc= nonvolatile matter of catalyst solution expressed as adecimal fraction

24、,W1= weight of aluminum dish, g,W2= weight of dish plus catalyst solution after heating, g,andW3= weight of catalyst solution before heating, g.9.2 Calculate the nonvolatile content, Ns, in the test speci-men as follows:Ns5 100W52 W4! 2 W6!Nc!#S(2)where:Ns= nonvolatile content of test specimen, perc

25、ent,W4= weight of the aluminum dish, g,W5= weight of aluminum dish plus the catalyzed testmaterial after heating, g,W6= weight of catalyst solution used in test specimenbefore heating, g,Nc= nonvolatile matter of catalyst solution, decimal frac-tion, (average of two determinations), andS = weight of

26、 test specimen before heating, g.10. Report10.1 Report the following information:10.1.1 The average values obtained for the nonvolatilecontent of the catalyst solution, Nc.10.1.2 The average values obtained for the percent nonvola-tile content of the test specimen, Ns.11. Precision and Bias11.1 The

27、precision estimated for this test method is based onan interlaboratory study in which one operator in each of fivelaboratories tested in triplicate on two different days four waterrepellent materials containing between 14 to 65 % nonvola-tiles. The results were analyzed statistically in accordance w

28、ithPractice D 3980. The intralaboratory standard deviation wasfound to be 0.283 % absolute with 17 df and the interlaboratorycoefficient of variation 7.02 % relative with 16 df. Based on thestandard deviation and coefficient of variation, the followingcriteria should be used for judging at the 95 %

29、confidencelevel, the acceptability of results.11.1.1 RepeatabilityTwo results, each the mean of tripli-cates, obtained by the same operator should be consideredsuspect if they differ by more than 0.84 % absolute.11.1.2 ReproducibilityTwo results, each the mean of trip-licates, obtained by operators

30、in different laboratories shouldbe considered suspect if they differ by more than 7.02 %relative.11.2 BiasBias has not been established for this testmethod.12. Keywords12.1 masonry water repellents; nonvolatile matter content;silanes; siloxanesD 5095 91 (2007)2ASTM International takes no position re

31、specting the validity of any patent rights asserted in connection with any item 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

32、 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 or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM Inter

33、national Headquarters. Your comments will receive careful consideration at a meeting 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 b

34、elow.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 5095 91 (2007)3