1、Designation: D5095 91 (Reapproved 2013)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 D5095; the number immediately following the designatio
2、n 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes a procedu
3、re 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 uni
4、ts 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 regu
5、latory limitations prior to use. For a specifichazard statement, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3980 Practice for Interlaboratory Testing of Paint andRelated Materials (Withdrawn 1998)3E145 Specification for Gravity-Convection and Force
6、d-Ventilation 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 te
7、st material 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-re
8、pellent treatments. 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
9、oven at 110 6 5C and store in a desiccator priorto use.5.2 Forced Draft Oven, Type IIAor Type IIB as specified bySpecification E145.5.3 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
10、understood to mean reagent water as definedby Type IV of Specification D1193.6.2 p-Toluenesulfonic Acid, monohydrate.46.3 Alcohol, technical grade ethanol or isopropanol.7. Hazards7.1 In addition to other precautions, provide adequateventilation, consistent with accepted laboratory practice, tolimit
11、 the accumulation of solvent vapors.1This test method is under the jurisdiction 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 June 1, 2013. Publ
12、ished June 2013. Originallyapproved in 1990. Last previous edition approved in 2007 as D5095 91 (2007).DOI: 10.1520/D5095-91R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informatio
13、n, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4The sole source of supply of the solution of pToluenesulfonic acid known tothe committee at this time is King Industries, Science Road, Norwalk, CT
14、06852. Ifyou are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C7
15、00, West Conshohocken, PA 19428-2959. United States18. 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.8.1.1 The nonv
16、olatile content of the test material can becalculated only if the same catalyst solution is used throughoutthe 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
17、.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 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
18、 in a forced draft oven for 60 min at 110 6 5C.8.2.4 Remove the dish from the oven and immediately placein 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 cataly
19、stsolution, Nc, in accordance with 9.1.8.3 Determine the percent nonvolatile content, in triplicate,of 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
20、, bydifference, of the catalyst solution into the preweighed alumi-num dish. Record the weight as W6.8.3.4 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
21、 Weighings must be done quickly to limit weight lossdue to volatilization. If there is insufficient moisture 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 swir
22、l the dish to mix the materials. Allow thematerials to stand at room temperature for 60 min.8.3.6 Heat 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 desicc
23、ator and allow the dish to cool toambient temperature.8.3.8 Reweigh the aluminum dish to 0.1 mg and record 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 follow
24、s:Nc5 W22 W1!/W3(1)where:Nc= nonvolatile matter of catalyst solution expressed as adecimal fraction,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 sp
25、eci-men as follows:Ns5 100W52 W4! 2 W6!Nc!#S(2)where:Ns= nonvolatile content of test specimen, percent,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= nonvolatil
26、e matter of catalyst solution, decimalfraction, (average of two determinations), andS = weight of 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 obtai
27、ned for the percent nonvola-tile content of the test specimen, Ns.11. Precision and Bias11.1 The 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 con
28、taining between 14 to 65 % nonvola-tiles. The results were analyzed statistically in accordance withPractice D3980. 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 devia
29、tion and coefficient of variation, the followingcriteria should be used for judging at the 95 % confidencelevel, the acceptability of results.11.1.1 RepeatabilityTwo results, each the mean oftriplicates, obtained by the same operator should be consideredsuspect if they differ by more than 0.84 % abs
30、olute.11.1.2 ReproducibilityTwo results, each the mean oftriplicates, obtained by operators in different laboratoriesshould be 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; nonvolati
31、le matter content;silanes; siloxanesD5095 91 (2013)2ASTM 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 determination of the validity of any such patent rig
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