ASTM D1617-2007(2012) Standard Test Method for Ester Value of Solvents and Thinners《溶剂和稀释剂酯化值的标准试验方法》.pdf

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1、Designation: D1617 07 (Reapproved 2012)Standard Test Method forEster Value of Solvents and Thinners1This standard is issued under the fixed designation D1617; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio

2、n. A number 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

3、 estervalue of solvents and thinners used in lacquers and othercoatings.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method

4、 to relevantspecifications, test result(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 E29.1.4 This standard does not purport to address all of thesafety concerns, if any, asso

5、ciated 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. For a specifichazard statement, see 8.6.1.5 For hazard information and guidance, see the suppliersM

6、aterial Safety Data Sheet.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Summary of Test Method3.1 The specimen is reacted with a measured excess ofaqueous potassium

7、hydroxide, using isopropanol as a mutualsolvent if necessary. The amount of potassium hydroxideconsumed, which is determined by titrating the excess withstandard mineral acid, is a measure of the ester originallypresent.3.2 Since this determination is based on an acidimetrictitration, a suitable cor

8、rection should be applied if the acidity ofthe sample exceeds the limit of the specification.4. Significance and Use4.1 This test method is useful in determining the assay ofsolvents and thinners which are esters or solutions of esters ofcarboxylic acid. The ester value is calculated as percent este

9、r.This test method has its greatest application where the solventor thinner is not a pure ester. This test method may be used inassessing compliance to specification.5. Interferences5.1 Organic chlorides, nitriles, and amides may be hydro-lyzed by the reagent, particularly at 98C, and are a possible

10、source of error. Ketones interfere only slightly with thisprocedure. Aldehydes consume some alkali, but the errorintroduced by small amounts is negligible.6. Apparatus6.1 Pressure Bottle, 200 to 350-mL capacity, made fromheat-resistant glass.6.2 Container for Pressure BottleA suitable safety devicet

11、o contain the pressure bottle. A metal container with hingedtop and perforated bottom, a strong synthetic fabric or canvasbag, or a safety shield may be used.6.3 Ampoule, 1 or 2-mL capacity.6.4 Weighing Pipet, Lunge or similar type.6.5 Erlenmeyer Flasks, 250-mL glass-stoppered.6.6 Buret, 50-mL capac

12、ity.6.7 Boiling Water Bath.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,1This test method i

13、s under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved July 1, 2012. Published September 2012. Originallyapproved in

14、 1958. Last previous edition approved in 2007 as D1617 - 07. DOI:10.1520/D1617-07R12.2For 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

15、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 States1where such specifications are available.3Other grades may beused provided it is first ascertained

16、 that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type IV of Specification D1193.7.3 Hydrochloric Acid, Standard

17、 (0.5 N)Prepare 0.5 Nhydrochloric acid (HCl) and standardize to four significantfigures.7.4 Isopropyl Alcohol (99 %).7.5 Phenolphthalein Indicator SolutionDissolve1gofphenolphthalein in 100 mL of methanol, ethanol, or isopropylalcohol.7.6 Potassium Hydroxide, Standard Solution (1.0 N)Dissolve 66 g o

18、f potassium hydroxide (KOH) pellets in waterand dilute to 1 L with water (see Note 1).7.7 Sulfuric Acid, Standard (0.5 N)Prepare 0.5 N sulfuricacid (H2SO4) and standardize to four significant figures.8. Procedure8.1 Prepare a sufficient number of 250-mL, glass-stopperedErlenmeyer flasks to make all

19、blank and test determinations induplicate. Use heat-resistant pressure bottles if sealed glassampoules are required or if the reaction is conducted at 98C.8.2 Into each of the flasks or bottles, carefully introduce 25mL of 1.0 N KOH solution (Note 1) by means of a suitabletransfer pipet. Use the sam

20、e pipet for each transfer.NOTE 1Do not substitute sodium hydroxide (NaOH) solution. Thereaction conditions given in Table 1 are valid only when 1.0 N KOHsolution is used.8.3 Add the amount of isopropyl alcohol prescribed in Table1 but never add more than 40 mL. Stopper and reserve two ofthe flasks o

21、r bottles for the blank determinations.8.4 Into each of the other flasks or bottles introduce anamount of sample containing not more than 0.016 mol (16milliequivalents) of the ester. For substantially pure material,weigh the specimen to the nearest 0.1 mg, using the amountand procedure specified in

22、Table 1. Stopper the flasks afteraddition of the specimen.8.5 If a sealed glass ampoule is used, add several pieces offire-polished 8-mm glass rod to each bottle, stopper, and shakethe bottle vigorously to break the ampoule.8.6 Reaction at 98C (WarningEnclose each bottle se-curely in a suitable safe

23、ty device to restrain fragments of glassshould the pressure bottle rupture.)Place the specimens andblanks as close together as possible in a boiling water bathmaintained at least at 98C for the time prescribed in Table 1.Maintain sufficient water in the bath to just cover the liquid inthe bottles. R

24、emove the bottles from the bath and allow themto cool to room temperature. When the bottles have cooled,remove them from the safety device and uncap them carefullyto release any pressure. Continue as described in 8.8.8.7 Reaction at Room TemperatureAllow the specimen tostand together with the blanks

25、 at room temperature for thelength of time specified in Table 1.8.8 If a white precipitate develops in the specimen flasks orbottles, add sufficient water to dissolve the salt. Add the sameamount of water to each of the blanks. Add 6 to 8 drops of thephenolphthalein indicator solution to each flask

26、or bottle andtitrate with 0.5 N H2SO4just to the disappearance of the pinkcolor. If more than 25 mL of isopropyl alcohol were added inaccordance with 8.3, titrate with 0.5 N HCl.8.9 Measure the temperature of the acid titrant. If thetemperature of the reagent at the time the ester determination isma

27、de is not the same as it was at the time the reagent wasstandardized, apply a temperature correction of 0.00014/C tothe normality.9. Calculation9.1 Calculate the percent of ester, E, as follows:E 5 B 2 V!N 3 F!/S# 3100 (1)where:V =0.5NH2SO4(or HCl) required for titration of thespecimen (8.8), mLB =

28、0.5NH2SO4(or HCl) required for titration of the blanks(8.8), avg, mL,N = normality of the H2SO4(or HCl) corrected fortemperature,F = factor specified in Table 2 for the ester beingdetermined, andS = specimen used, g.NOTE 2If the acidity of the ester exceeds the limit of the specification,it is recom

29、mended that a suitable correction be applied to the ester value.10. Report10.1 Report the following information:3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Societ

30、y, 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.TABLE 1 Specimen Size and Reaction ConditionsEster Specimen, gAIsopropylAlcoholAdded,mLMinimum ReactionCo

31、nditionsTime,minTempera-ture, CAmyl acetate 1.4 to 1.6 40 30 98Dibutyl phthalate 1.4 to 2.0 30 30 982-Ethoxyethyl acetate 1.3 to 2.1 0 30 25Ethyl acetate 0.9 to 1.4B03025Isobutyl acetate 1.2 to 1.9 25 45 25Isopropyl acetate 1.0 to 1.6B10 30 25Methyl amyl acetate 1.4 to 2.3 30 30 98Normal butyl aceta

32、te 1.2 to 1.9 25 45 25Normal propyl acetate 1.0 to 1.6B10 30 25secButyl acetate 1.2 to 1.9 25 45 98AUse a suitable weighing pipet unless otherwise specified.BUse a sealed glass ampoule.D1617 07 (2012)210.1.1 All results to the nearest 0.1 %. Duplicate determi-nations that agree within 0.38 %, absolu

33、te, are acceptable foraveraging (95 % confidence level).11. Precision and Bias11.1 PrecisionThe precision statements are based upon aninterlaboratory study in which two analysts in each of fourdifferent laboratories analyzed one sample of ethyl acetate,88 %, and one sample of dibutyl phthalate, 99 %

34、, in duplicateon three different days. The within-laboratory coefficient ofvariation was found to be 0.154 % at 40 df, and the between-laboratory coefficient of variation was found to be 0.313 % atapproximately 16 df. Based on these coefficients of variation,the following criteria should be used in

35、judging the acceptabil-ity of results at the 95 % confidence level.11.1.1 RepeatabilityTwo results, each the mean ofduplicates, obtained by the same operator on different daysshould be considered suspect if they differ by more than 0.44 %relative.11.1.2 ReproducibilityTwo results, each the mean ofdu

36、plicates, obtained by operators in different laboratoriesshould be considered suspect if they differ by more than 0.94 %relative.11.2 BiasAny material or contaminant (see Section 5 andNote 2) that will react with potassium hydroxide under the testconditions will affect the results.12. Keywords12.1 e

37、ster value; solvents; thinnerSUMMARY OF CHANGESCommittee D01.35 has identified the location of selected changes to this standard since the last issue(D1617 - 90 (2001) that may impact the use of this standard. (Approved June 1, 2007.)(1) Added reference to Practice E29 in 1.3 of the Scopesection.(2)

38、 Added Practice E29 to list of Referenced Documents.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 determination of the validity of any such patent rig

39、hts, 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 withdrawn. Your comments are invited either for

40、 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 comments have not received a fair hearing

41、 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

42、 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/).TABLE 2 Ester Fa

43、ctorsEster FactorAAmyl acetate 0.1302Dibutyl phthalate 0.13922-Ethoxyethyl acetate 0.1322Ethyl acetate 0.0881Isobutyl acetate 0.1162Isopropyl acetate 0.1021Methyl amyl acetate 0.1442Normal butyl acetate 0.1162Normal propyl acetate 0.1021secButyl acetate 0.1162AFactor = molecular weight of compound/number of reacting groups 1000.D1617 07 (2012)3