1、Designation: D 1133 04Standard Test Method forKauri-Butanol Value of Hydrocarbon Solvents1This standard is issued under the fixed designation D 1133; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb
2、er in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 relativ
3、esolvent 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 D 86 is used to determine th
4、e initial boiling pointand dry point for mineral spirits and similar petroleum solvents. TestMethod D 1078 is used for pure compounds and narrow boiling rangecuts.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 The foll
5、owing applies to all specified limits in thisstandard; for purposes of determining conformance with thisstandard, an observed value or a calculated value shall berounded off “to the nearest unit” in the last right-hand digitused in expressing the specification limit, in accordance withthe rounding-o
6、ff method of Practice E 29.1.4 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 health practices and determine the applica-bility of regulatory limitations p
7、rior to use.1.5 For specific hazard information and guidance, consultthe suppliers Material Safety Data Sheet.2. Referenced Documents2.1 ASTM Standards:2D 86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 304 Specification for n-Butyl Alcohol (Butanol)D 841 Specification
8、for Nitration Grade TolueneD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsE 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Terminology3.1 Definitions:3.1.1 kauri-butanol valueof a solvent, the volume inmillilitres at 25C of th
9、e solvent, corrected to a 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 7
10、5 % n-heptane and 25 % toluene 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 bein
11、g maintained at 25 6 5C.Alternatively, a room maintained 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 dispensed t
12、o 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 unless ot
13、herwise specified. Unless otherwiseindicated, it is intended that all reagents shall conform to thespecifications of the Committee on Analytical Reagents of the1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direc
14、t responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved June 1, 2004. Published June 2004. Originallyapproved in 1950. Last previous edition approved in 2002 as D 1133 02.2For referenced ASTM standards, visit the ASTM website, www.astm.or
15、g, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C
16、700, West Conshohocken, PA 19428-2959, United States.American 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 the determi-nation.6.2
17、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 SpecificationD 304). Shake on a mechanical shaker until the resin goes intosolution, war
18、ming to about 55C, if necessary to aid solution.If a mechanical shaker is not available, fit the flask with areflux condenser and heat on a steam bath until all of the kauriresin is dissolved. Permit the solution to stand 48 h and thenclarify by filtering through a Bchner funnel with suction,using d
19、ouble filter paper and changing as frequently asnecessary.6.3 Standard Toluene conforming to Specification D 841for use 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 standard. The heptane s
20、hall 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 to the same temperatur
21、e, 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 line with n-heptane,ins
22、ert 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 out 20 6 0.10 g of kauri-butanol solution in a250-mL Er
23、lenmeyer flask. Check that the temperature of theKB solution in the flask is 25 6 5C. If not, place theErlenmeyer flask and its content in a water bath maintained at25 6 5C and allow to equilibrate for at least 30 min. Removethe flask from the water bath and titrate with the standardtoluene into the
24、 flask, with constant swirling. Gradually reducethe successive amounts of toluene added as the end point isapproached. The end point is reached when the sharp outlinesof 10-point print placed directly beneath the water bath andobserved through the liquid are obscured or blurred, but not tothe point
25、where the print becomes illegible. Check the tem-perature in the flask immediately after the end point has beenreached, and if over 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
26、 value should lie reasonably close to 105 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 out 20 6 0.10 g of the kauri-buta
27、nol solution(adjusted as described in 7.2) in a 250-mL Erlenmeyer flaskand place in the water bath. Titrate with the heptane-tolueneblend in the same manner as described in 7.1. Designate thevolume, in millilitres, of the blend used in this titration as B.NOTE 4If the composition of the blend is kno
28、wn to differ from 25 61.0 % toluene, 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
29、change in stan-dardization from day 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 20 6 0.10 g o
30、f the adjusted kauri-butanolsolution into a 250-mL Erlenmeyer flask. Check that thetemperature of the KB solution in the flask is 25 6 5C. If not,place the Erlenmeyer flask and its content in a water bathmaintained at 25 6 5C and allow to equilibrate for at least 30min. Remove the flask from the wat
31、er bath. Fill the sampledispensing device with the solvent being tested and titrate thesolvent into the Erlenmeyer flask with constant swirling.Gradually reduce the successive amounts of solvent added asthe end point is approached. The end point is reached when thesharp outlines of 10-point print (s
32、ee 5.5) placed directlybeneath the water bath and observed through the liquid areobscured or blurred, but not to the point where the printbecomes illegible. Check the temperature in the flask immedi-ately after the end point has been reached and if over 30C orunder 20C, repeat the titration. Designa
33、te the volume ofsolvent, in millilitres, to produce turbidity as C.9. Calculation9.1 Calculate the kauri-butanol value, V, as follows:V 5 65C 2 B!/A 2 B!# 1 40 (1)where:A = toluene required to titrate 20 g of kauri-butanol solu-tion (7.2), mL,B = heptane-toluene blend required to titrate 20 g ofkaur
34、i-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.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washin
35、gton, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4The sole s
36、ource of supply of prepared kauri-butanol solutions known to thecommittee at this time is the Chemical Service Laboratories, 5543 Dyer St., Dallas,TX 75206. If you are aware of alternative suppliers, please provide this informationto ASTM International Headquarters. Your comments will receive carefu
37、l consid-eration at a meeting of the responsible technical committee,1which you may attend.D113304211. 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
38、 the mean of dupli-cates, obtained by the same operator on different days shouldbe considered suspect if they differ by more than 0.01 K 0.1,where K = mean kauri-butanol value.11.1.2 ReproducibilityTwo results, each the mean of du-plicates, obtained by two laboratories should not be consideredsuspec
39、t unless they differ by more than 0.03 K + 1.0 where K= mean kauri-butanol value.11.2 BiasTest bias can 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 onl
40、y in terms of the test method.12. Keywords12.1 kauri-butanol value; hydrocarbon solvents; solvencypowerSUMMARY OF CHANGESSubcommittee D01.35 has identified the location of selected changes to this standard since the last issue(D 1133 - 02) that may impact the use of this standard.(1) Removed Test Me
41、thods D 611 from the Referenced Docu-ments list in 2.1.(2) Updated 5.4 to allow flexibility in the types of sampledispensing devices that can be used in the method.(3) Updated 6.4 regarding the heptane specifications.(4) Updated 8.1 to remove the explicit reference to the 50 mLburet size, based on t
42、he change made to 5.4.(5) Added Practice E 29 to the Scope and Referenced Docu-ments Sections.ASTM 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 determinat
43、ion 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 or withd
44、rawn. 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 that your
45、 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).D1133043
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