ASTM D1133-2013 Standard Test Method for Kauri-Butanol Value of Hydrocarbon Solvents《烃类溶剂贝壳杉脂丁醇值的标准试验方法》.pdf

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1、Designation: D1133 13Standard Test Method forKauri-Butanol Value of Hydrocarbon Solvents1This standard is issued under the fixed designation D1133; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number

2、 in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the determination of the relativeso

3、lvent power of hydrocarbon solvents used in paint andlacquer formulations. This test method is suitable for use withsolvents having an initial boiling point over 40C and a drypoint under 300C when determined in accordance with theprocedures in Note 1.NOTE 1Test Method D86 is used to determine the in

4、itial boiling pointand dry point for mineral spirits and similar petroleum solvents. TestMethod D1078 is used for pure compounds and narrow boiling range cuts.1.2 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications, test resu

5、lt(s) shall be rounded off “to the nearestunit” in the last right-hand digit used in expressing thespecification limit, in accordance with the rounding-off methodof Practice E29.1.3 For specific hazard information and guidance, consultthe suppliers Material Safety Data Sheet.1.4 The values stated in

6、 SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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 safety and heal

7、th practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD304 Specification forn-Butyl Alcohol (Butanol)D841 Specification for Nitration Grade TolueneD1

8、078 Test Method for Distillation Range of Volatile Or-ganic LiquidsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Terminology3.1 Definitions:3.1.1 kauri-butanol value, nof a solvent, the volume inmillilitres at 25C of the solvent, corrected to a

9、definedstandard, required to produce a defined degree of turbiditywhen added to 20 g of a standard solution of kauri resin innormal butyl alcohol.3.1.1.1 DiscussionThe kauri resin solution is standardizedagainst toluene, which has an assigned value of 105, and amixture of 75 % n-heptane and 25 % tol

10、uene on a volumebasis, which has an assigned value of 40.4. Significance and Use4.1 The kauri-butanol value is used as a measure of solventpower of hydrocarbon solvents. High kauri-butanol valuesindicate relatively strong solvency.5. Apparatus5.1 Water Bath, capable of being maintained at 25 6 5C.Al

11、ternatively, a temperature controlled environment main-tained at 25 6 5C may be used.5.2 Volumetric Flask, 200-mL capacity.5.3 Erlenmeyer Flask, 250-mL capacity.5.4 Sample Dispensing Device, Buret, of at least 50-mLcapacity, or equivalent, that is capable of accurately determin-ing the volume dispen

12、sed to the nearest 0.1 mL.5.5 Print SpecimenA sheet of white paper having on itblack 10 or 12 point print, No. 31 Bruce old style type.NOTE 2Text in this published standard is satisfactory to use as printspecimen.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests unle

13、ss otherwise specified. Unless otherwise1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, andApplications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved Jun

14、e 1, 2013. Published July 2013. Originally approvedin 1950. Last previous edition approved in 2010 as D1133 10. DOI: 10.1520/D1133-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info

15、rmation, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1indicated, it is intended that all reagents shal

16、l conform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society, where such specifications areavailable.3Other grades may be used, provided it is firstascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of

17、 the determi-nation.6.2 Kauri-Butanol Solution4Place in a 3-L flask 400 g ofclean, pale, bold kauri resin of Grade XXXX, XXX, or XXground to pea-size or smaller. Add, while agitating vigorously,2000 g of n-butyl alcohol, (conforming to Specification D304).Shake on a mechanical shaker until the resin

18、 goes into solution,warming to about 55C, if necessary to aid solution. If amechanical shaker is not available, fit the flask with a refluxcondenser and heat on a steam bath until all of the kauri resinis dissolved. Permit the solution to stand 48 h and then clarifyby filtering through a Bchner funn

19、el with suction, usingdouble filter paper and changing as frequently as necessary.6.3 Standard Toluene conforming to Specification D841 foruse as a high-solvency standard.6.4 Heptane-Toluene Blend consisting of 25 6 0.1 % tolu-ene and 75 6 0.1 % n-heptane on a volume basis, for use as alow-solvency

20、standard. The heptane shall be spectroscopic,HPLC, or knock test grade.NOTE 3The blend of 25 6 0.1 % toluene and 75 6 0.1 % heptane canbe prepared in any way that will give the desired accuracy. The followingtechnique is adequate: Bring the toluene and heptane and a calibrated200-mL volumetric flask

21、 to the same temperature, preferably in aconstant-temperature room or thermostat. Run 50 mL of toluene into the200-mL volumetric flask, using a buret or pipet calibrated to deliver 50mL of toluene at the chosen temperature (preferably 25C). Fill thevolumetric flask to slightly below the calibration

22、line with n-heptane,insert the ground-glass stopper of the volumetric flask, and mix carefullyby repeatedly inverting the flask. Allow to stand for a few minutes; thenbring to the 200-mL calibration mark with heptane and again carefullymix.7. Standardization7.1 Weigh or transfer 20 6 0.10 g of kauri

23、-butanol solutionin a 250-mL Erlenmeyer flask. Check that the temperature ofthe KB solution in the flask is 25 6 5C. If not, place theErlenmeyer flask and its contents in a water bath or tempera-ture controlled environment maintained at 25 6 5C and allowto equilibrate for at least 30 min. If the fla

24、sk was placed in awater bath, remove the flask from the water bath. Titrate thecontents of the flask with the standard toluene. Swirl thecontents of the flask during titration, periodically stopping toobserve the clarity of the print beneath the flask. Graduallyreduce the successive amounts of tolue

25、ne added as the endpoint is approached. The end point is reached when the sharpoutlines of 10-point print placed directly beneath the Erlen-meyer flask and observed through the liquid are first perceivedto be obscured or blurred. The point where the print becomesillegible is past the end point. Chec

26、k the temperature in theflask immediately after the end point has been reached, and ifover 30C or under 20C, repeat the titration.7.2 The volume of toluene used, in millilitres, represents theactual titer for the particular kauri-butanol solution at hand.This value should lie reasonably close to 105

27、 mL, but not over110 nor under 100 mL. If these limits are exceeded, adjust theconcentration of the kauri-butanol solution to bring the totalvolume of toluene within them. Designate the final value usingtoluene as A.7.3 Weigh or transfer 20 6 0.10 g of the kauri-butanolsolution (adjusted as describe

28、d in 7.2) in a 250-mLErlenmeyerflask and place in the water bath. Titrate with the heptane-toluene blend in the same manner as described in 7.1. Desig-nate the volume, in millilitres, of the blend used in this titrationas B.NOTE 4If the composition of the blend is known to differ from 25 61.0 % tolu

29、ene, but is within the range from 22 to 28 % toluene, theconstant in the blend factor equation will differ from 40.0 by 0.60 units foreach 1 % toluene. For example, at 28 % toluene, the constant is 41.8instead of 40.0.NOTE 5Freshly prepared kauri-butanol solution may change instandardization from da

30、y to day. It is, therefore, desirable to permit thesolution to age before initial standardization and, in any case, thestandardization should be rechecked on successive days until the toluenefactor and blend factor remain constant.8. Procedure8.1 Weigh or transfer 20 6 0.10 g of the adjusted kauri-b

31、utanol solution into a 250-mL Erlenmeyer flask. Check thatthe temperature of the KB solution in the flask is 25 6 5C. Ifnot, place the Erlenmeyer flask and its contents in a water bathor temperature controlled environment maintained at 25 6 5Cand allow to equilibrate for at least 30 min. If the flas

32、k wasplaced in a water bath, remove the flask from the water bath.Fill the sample dispensing device with the solvent being tested.Titrate the contents of the flask with the solvent. Swirl thecontents of the flask during the titration, periodically stoppingto observe the clarity of the print beneath

33、the flask. Graduallyreduce the successive amounts of solvent added as the endpoint is approached. The end point is reached when the sharpoutlines of 10-point print (see 5.5) placed directly beneath theErlenmeyer flask and observed through the liquid are firstperceived to be obscured or blurred. The

34、point where the printbecomes illegible is past the end point. Check the temperaturein the flask immediately after the end point has been reachedand if over 30C or under 20C, repeat the titration. Designatethe volume of solvent, in millilitres, to produce turbidity as C.9. Calculation9.1 Calculate th

35、e kauri-butanol value, V, as follows:V 5 65C 2 B!/A 2 B!#140 (1)3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals,

36、 BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4The sole source of supply of prepared kauri-butanol solutions known to thecommittee at this time is the Chemical Service Laboratories, 5543 Dyer St., Da

37、llas,TX 75206. If you are aware of alternative suppliers, please provide this informationto ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technical committee,1which you may attend.D1133 132where:A = toluene required to titrate 20 g

38、 of kauri-butanol solution(7.2), mL,B = heptane-toluene blend required to titrate 20 g of kauri-butanol solution (7.3), mL, andC = solvent under test required to titrate 20 g of kauri-butanol solution (Section 8), mL.10. Report10.1 Report the calculated kauri-butanol value to the nearest0.5 KB unit.

39、11. Precision and Bias11.1 The following criteria should be used for judging theacceptability of the results in the range from 30 to 90 at the95 % confidence level.11.1.1 RepeatabilityTwo results, each the mean ofduplicates, obtained by the same operator on different daysshould be considered suspect

40、 if they differ by more than 0.01K 0.1, where K = mean kauri-butanol value.11.1.2 ReproducibilityTwo results, each the mean ofduplicates, obtained by two laboratories should not be consid-ered suspect unless they differ by more than 0.03 K + 1.0 whereK = mean kauri-butanol value.11.2 BiasTest bias c

41、an result if the kauri-butanol solutionis not carefully standardized and adjusted (see 7.2 and 7.3).Thetest method has no definitive bias statement because the valueof the test result is defined only in terms of the test method.12. Keywords12.1 kauri-butanol value; hydrocarbon solvents ; solvencypow

42、erSUMMARY OF CHANGESCommittee D01 has identified the location of selected changes to this standard since the last issue (D1133-10)that may impact the use of this standard. (Approved June 1, 2013.)(1) Updated 7.1, 7.3, and 8.1 adding “or transfer” after Weigh.ASTM International takes no position resp

43、ecting 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 s

44、tandard 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 Interna

45、tional 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 bel

46、ow.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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1133 133