1、Designation: D 1614 08Standard Test Method forAlkalinity in Acetone1This standard is issued under the fixed designation D 1614; 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 parentheses indi
2、cates 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 in acetone ofalkalinity calculated as
3、 ammonia (NH3).1.2 For specific hazard information and guidance, consultthe suppliers Material Safety Data Sheet.1.3 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 “
4、to the nearest unit” in the last right-hand digitused in expressing the specification limit, in accordance withthe rounding-off method of Practice E29.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does no
5、t purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof whoever uses this standard to consult and establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are giv
6、en in Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for Chemi
7、calAnalysis3. 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 method provides a measurement of alkalinityin
8、 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 shall beused in all tests. Unless otherwise i
9、ndicated, 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 reagent is ofsufficiently high purity to
10、 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 D 1193.6.3 Methyl Red Indicator Solution (1 g/L)Dissolve 0.2 gof methy
11、l red in 100 mL of methanol, ethanol, or isopropanol.Prepare a fresh solution at least once a month as needed.6.4 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 E 200.NOTE 1Alternat
12、ively, 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.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Co
13、atings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved Nov. 1, 2008. Published November 2008. Originallyapproved in 1958. Last previous edition approved in 2003 as D 1614 03.2For refere
14、nced 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 page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanCh
15、emical Society, Washington, 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), Ro
16、ckville,MD.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 The reagents sulfuric acid and sodium hydroxide arehazardous as they can cause severe burns of the skin
17、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 then to the fi
18、rst 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 coloration.9.
19、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 3 0.034!/D (1)where:V =H2SO4required for titration of the specimen, mL,N = normality of the H2SO4, andD = density of the specimen at the test tempe
20、rature 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).11. Precisio
21、n 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 degrees of free
22、dom 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 mean of du-pli
23、cates, 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 more than0.00
24、02 % 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 testSUMMARY OF CHANGESCommittee D01.35 has identified the location of selected changes to this standard since the last is
25、sue(D 1614 - 03) that may impact the use of this standard. (Approved November 1, 2008.)(1) Revised 6.2.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 d
26、etermination 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
27、 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 theresponsible technical committee, which you may attend. If you feel
28、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 Conshohocken, PA 19428-2959,United States. Individual reprin
29、ts (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).4Supporting data are available from ASTM International Headquarters. RequestRR:D01-1020.D1614082
