1、Designation: D 1614 03Standard 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 (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 in acetone ofalkalinity calculated a
3、s ammonia (NH3).1.2 This standard does not 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
4、to use. Specific hazardstatements are given in Section 7.1.3 For specific hazard information and guidance, consultthe suppliers Material Safety Data Sheet.1.4 The following applies to all specified limits in thisstandard; for purposes of determining conformance with thisstandard, an observed value o
5、r 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-off method of Practice E 29.2. Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2E 29 Practice for Using S
6、ignificant Digits in Test Data toDetermine Conformance with Specifications3E 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis43. Summary of Test Method3.1 The specimen is added to water previously neutralizedto the methyl red end poin
7、t. 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 acetone. The results of this measurement can be used forspecification acceptance.5. Apparatus5.1 Buret, 10-mL, graduat
8、ed 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 indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents
9、of the American Chemical Society,where such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, refer
10、encesto water shall be understood to mean reagent water conformingto Type IV of Specification D 1193.6.3 Methyl Red Indicator Solution (1 g/L)Dissolve 0.2 gof methyl red in 100 mL of methanol, ethanol, or isopropanol.Prepare a fresh solution at least once a month as needed.6.4 Sodium Hydroxide, Stan
11、dard Solution (0.05 N)Prepare and standardize a 0.05 N sodium hydroxide (NaOH)solution (Note) in accordance with Sections 12 to 17 ofPractice E 200.NOTE 1Alternatively, potassium hydroxide (KOH) solution may beused.6.5 Sulfuric Acid, Standard Solution (0.05 N)Prepare andstandardize a 0.05 N sulfuric
12、 acid (H2SO4) solution.1This test method is 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 10, 2003. Publ
13、ished August 2003. Originallyapproved in 1958. Last previous edition approved in 1995 as D 1614 95 (1999).2Annual Book of ASTM Standards, Vol 11.01.3Annual Book of ASTM Standards, Vol 14.02.4Annual Book of ASTM Standards, Vol 15.05.5Reagent Chemicals, American Chemical Society Specifications, Americ
14、anChemical 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)
15、, Rockville,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. Hazards7.1 Acetone is a highly flammable liquid.7.2 The reagents sulfuric acid and sodium hydroxide a
16、rehazardous as they can cause severe burns 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
17、 coloration with 0.05 NNaOH solution and then 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, titra
18、te it with 0.05 N H2SO4to the first pink coloration.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 VN3 0.034!/D (1)where:V =H2SO4required for titration of the specimen, mL,N = normality of the H
19、2SO4, andD = density of the specimen at the 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 acceptab
20、le for averaging (95 % confi-dence level).11. Precision and Bias611.1 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 f
21、ound to be0.00002 % absolute with nine degrees 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
22、.1.1 RepeatabilityTwo results, each the mean of du-plicates, 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
23、 be considered suspect if they differ by more 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 testSUMMARY OF CHANGESCommittee D01 has identified the location of
24、selected changes to this standard since the last issue(D 1614 - 95 (1999) that may impact the use of this standard.(1) Added Practice E 29 on significant digits to the scope.(2) Added Practice E 29 to the Referenced Documents section.(3) Changed “specific gravity” to “density” and added “g/ml”to the
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28、dmake 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).6Supporting data are available from ASTM International Headquarters. RequestRR:D01-1020.D1614032
