ASTM D1387-1989(2012) Standard Test Method for Saponification Number (Empirical) of Synthetic and Natural Waxes《合成和天然蜡皂化值(经验)的标准试验方法》.pdf

1、Designation: D1387 89 (Reapproved 2012)Standard Test Method forSaponification Number (Empirical) of Synthetic and NaturalWaxes1This standard is issued under the fixed designation D1387; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio

2、n, 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 covers the determination of the saponi-fication number of synthetic waxes and natural

3、waxes.1.2 This test method is applicable to Fischer Tropsche,microcrystalline, polyethylene, and Montan Ester waxes.1.3 Certain synthetic waxes, notably copolymers ofethylene, exhibit poor reproducibility when running saponifi-cation values. Reproducibility can be improved if cooking timein 7.2 is e

4、xtended from3hto1820 h.1.4 Some oxidized polyethylene and other waxes with amelt temperature above 100C may give poor reproducibility.1.5 Some dark-colored (Gardner Color 14) waxes mayobscure the color change of the indicator, resulting in poorreproducibility.1.6 The values stated in SI units are to

5、 be regarded asstandard. No other units of measurement are included in thisstandard.1.7 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

6、 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical Analysis3. Terminology3.1 Definitions:3.1.1 saponification numberthe number of mil

7、ligrams ofpotassium hydroxide required to hydrolyze1gofthesampleand is a measure of the amount of saponifiable matter present.4. Significance and Use4.1 This test method is used to determine the property ofester functionality. Ester functionality determines the utility ofthe wax as well as being a s

8、ignificant quality control test.5. Apparatus5.1 Analytical Balance.5.2 Boiling Chips, chemically resistant glass.5.3 Burets, two 50-mL capacity with 0.1-mL graduations.5.4 Erlenmeyer Flasks, 250-mL, alkali-resistant.5.5 Hot Plate.5.6 Reflux Condenser.6. Reagents and Materials6.1 Purity of ReagentsRe

9、agent-grade chemicals orequivalent as specified in Practice E200 shall be used in alltests.6.2 Hydrochloric Acid Standard (0.5 N).6.3 Phenolphthalein Indicator Solution (10 g/litre)Dissolve1gofphenolphthalein in 100 mL of USSD3Adenatured ethanol or 95 % ethanol.6.4 Potassium Hydroxide, Alcoholic Sol

10、ution (6.6 g/litre)Dissolve 6.6 g of potassium hydroxide (KOH) in USSD3Adenatured ethanol or 95 % ethanol. Dilute to 1 L with theethanol.6.5 Xylene.7. Procedure7.1 Transfer approximately1gofthesample, weighed tothe nearest 0.001 g to a 250-mL Erlenmeyer flask.7.2 Add 40 mL of xylene and a few boilin

11、g chips to theflask. Dissolve by heating on the hot plate to the boiling pointof xylene. As soon as the wax dissolves, remove from the hot1This test method is under the jurisdiction ofASTM Committee D21 on Polishesand is the direct responsibility of Subcommittee D21.02 on Raw Materials.Current editi

12、on approved Oct. 1, 2012. Published October 2012. Originallyapproved in 1955. Last previous edition approved in 2007 as D138789(2007).DOI: 10.1520/D1387-89R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of

13、ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1plate and add 50.0 mL of 0.1 N ethanolic KOH solution fromthe buret. Fit the flask with

14、a reflux condenser and reflux for 3h using the hot plate.7.3 Remove the condenser from the flask, add 5 drops of thephenolphthalein solution and titrate the sample with 0.5 N HCluntil the pink color disappears. Reheat the sample to theboiling point, and if it turns pink, resume titration until theco

15、lor once again disappears. Repeat this procedure until thepink color does not reappear on heating. Saponified waxesusually require two repetitions of heating and additionaltitration until the pink color does not reappear.8. Calculation8.1 Calculate the saponification number as follows:Saponification

16、 number 5B 2 A!N 356.1C(1)where:A = millilitres of HCl solution required for titration of thesample,B = millilitres of HCl solution required for titration of theblank,C = grams of sample used, andN = normality of the HCl solution.9. Precision and Bias9.1 Precision and bias have been established only

17、 forlight-colored waxes melting below 100C.9.1.1 Duplicate results by the same operator shall not beconsidered suspect unless they differ by more than 61.3saponification numbers (95 % confidence limits for average).9.1.2 Results reported by two laboratories shall not beconsidered suspect unless they

18、 differ by more than 63.2saponification numbers (95 % confidence limits for average).9.2 Dark-colored waxes or wax melting above 100C, orpolyethylene copolymer waxes may exhibit poorer reproduc-ibility when running saponification values. See Section 1.9.3 BiasThis test has no bias because the values

19、 producedare defined only in terms of this test method.10. Keywords10.1 natural wax; polish; polyethylene wax; saponificationnumber; synthetic wax; titration; waxASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this st

20、andard. 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 standard is subject to revision at any time by the responsible technical committee and must be rev

21、iewed 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 International Headquarters. Your comments will receive careful consideration at a meeting of theresponsi

22、ble 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 below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West C

23、onshohocken, 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/).D1387 89 (2012)2