1、Designation: D1614 09 (Reapproved 2017)Standard Test Method forAlkalinity in Acetone1This standard is issued under the fixed designation D1614; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in
2、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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination in acetone ofalka
3、linity calculated as ammonia (NH3).1.2 The following 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 specif
4、ication limit, in accordance withthe rounding-off method of Practice E29.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 For specific hazard information and guidance, consultthe suppliers Safety Data Sheet.1.5 This stand
5、ard 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific haza
6、rd statements are given in Section 7.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Tr
7、ade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE200 Practice for Preparation, Standardization, and Storageof
8、Standard and Reagent Solutions for Chemical Analysis3. Summary of Test Method3.1 The specimen is added to water previously neutralizedto the methyl red end point. If alkalinity is detected, it is titratedwith 0.05 N H2SO4and reported as weight percent of NH3.4. Significance and Use4.1 This test meth
9、od provides a measurement of alkalinityin acetone. The results of this measurement can be used forspecification acceptance.5. Apparatus5.1 Buret, 10-mL, graduated in 0.05-mL subdivisions.5.2 Erlenmeyer Flask, 250-mL capacity.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shal
10、l 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,where such specifications are available.3Other grades may beused, provided it is first ascertained that the
11、 reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type IV or higher purity of Specification D1193.6.3 Methyl Red Indicato
12、r Solution (1 g/L)Dissolve 0.1 gof methyl red in 100 mL of methanol, ethanol, or isopropanol.Prepare a fresh solution at least once a month as needed.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsi
13、bility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved Dec. 1, 2017. Published December 2017. Originallyapproved in 1958. Last previous edition approved in 2009 as D1614 09. DOI:10.1520/D1614-09R17.2For referenced ASTM standards, visit the ASTM we
14、bsite, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For su
15、ggestions 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.Copyright ASTM Internationa
16、l, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides
17、and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16.4 Sodium Hydroxide, Standard Solution (0.05 N)Prepare and standardize a 0.05 N sodium hydroxide (NaOH)solution (Note 1) in accordance with Sections 12 to 17 ofPractice E200.NOTE 1Alternatively,
18、potassium hydroxide (KOH) solution may beused.6.5 Sulfuric Acid, Standard Solution (0.05 N)Prepare andstandardize a 0.05 N sulfuric acid (H2SO4) solution.7. Hazards7.1 Acetone is a highly flammable liquid.7.2 The reagents sulfuric acid and sodium hydroxide arehazardous as they can cause severe burns
19、 of the skin or eyes.8. Procedure8.1 To a 250-mL Erlenmeyer flask, add 50 mL of water and3 drops of methyl red indicator solution. If the water is basic,neutralize to the first faint pink coloration with 0.05 N H2SO4.If acidic, neutralize to the first yellow coloration with 0.05 NNaOH solution and t
20、hen to the first faint pink coloration with0.05 N H2SO4solution. Now add 50 mL of sample to theneutralized water. If there is no change in the color of thesolution, the sample may be considered free of alkalinity. If,however, the solution turns yellow, titrate it with 0.05 N H2SO4to the first pink c
21、oloration.9. Calculation9.1 When it is necessary to titrate the solution with the 0.05N H2SO4calculate the percent of alkalinity as ammonia (NH3)as follows:NH3,%5 VN 30.034!/D (1)where:V =H2SO4required for titration of the specimen, mL,N = normality of the H2SO4, andD = density of the specimen at th
22、e test temperature in g/ml.10. Report10.1 If the solution does not turn yellow, report alkalinity aszero.10.2 If the solution is alkaline, report the percent of ammo-nia to the nearest 0.0001 %. Duplicate runs that agree within0.00007 % absolute are acceptable for averaging (95 % confi-dence level).
23、11. Precision and Bias411.1 Precision:11.1.1 On the basis of an interlaboratory study of this testmethod in which operators in eleven laboratories analyzed onesample of acetone with a mean alkalinity of 0.0009 %, thewithin-laboratory standard deviation was found to be0.00002 % absolute with nine deg
24、rees of freedom and thebetween-laboratories standard deviation 0.00007 % absolutewith eight degrees of freedom. Based on these standarddeviations, the following criteria should be used for judging theacceptability of results at the 95 % confidence level:11.1.1.1 RepeatabilityTwo results, each the me
25、an ofduplicates, obtained by the same operator on different daysshould be considered suspect if they differ by more than0.0001 % absolute.11.1.1.2 ReproducibilityTwo results, each the mean ofduplicates, obtained by operators in different laboratoriesshould be considered suspect if they differ by mor
26、e than0.0002 % absolute.11.2 BiasBias cannot be determined for this test methodbecause there is no available material having an acceptedreference value.12. Keywords12.1 acetone; alkalinity testASTM International takes no position respecting the validity of any patent rights asserted in connection wi
27、th 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 standard is subject to revision at any time by the responsible tech
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29、ion 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 below.This standard is copyrighted by ASTM International, 100 Barr Ha
30、rbor 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(ww
31、w.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1020. ContactASTM CustomerService at serviceastm.org.D1614 09 (2017)2
