1、Designation: D 1363 06Standard Test Method forPermanganate Time of Acetone and Methanol1This standard is issued under the fixed designation D 1363; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 in parentheses indicates 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 detection in acetone andmethan
3、ol of the presence of impurities that reduce potassiumpermanganate.1.2 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications, test result(s) shall be rounded off “to the nearestunit” in the last right-hand digit used in express
4、ing thespecification limit, in accordance with the rounding-off methodof Practice E 29.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 For specific hazard information and guidance, consultthe suppliers Material Safety D
5、ata Sheet.1.5 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 determine the applica-bility of regulatory limitations prior to use.2. Re
6、ferenced Documents2.1 ASTM Standards:2D 329 Specification for AcetoneD 1152 Specification for Methanol (Methyl Alcohol)D 1193 Specification for Reagent WaterD 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)E29 Practice for Using Significant Digits in Test Data toDetermine Conform
7、ance with SpecificationsE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 346 Test Methods for Analysis of Methanol3. Summary of Test Method3.1 Substances reacting with potassium permanganate inneutral solutions reduce it to
8、manganese dioxide which colorsthe solution yellow. In the permanganate test the time requiredfor the color of the test solution to change to that of a standardsolution is measured. The color of the test solution changesfrom pink-orange to yellow-orange.4. Significance and Use4.1 The permanganate tim
9、e can be used to judge thepresence of oxidizable materials that may be associated withmanufacture or contamination during distribution and to assesscompliance with a specification.4.2 Many chemical processes that use acetone or methanol,or both, involve catalyst, metals, or ligand complexes that are
10、sensitive to oxidation. Since oxidizable contaminants mayaffect the efficiency of these processes, this test methodprovides a comparative test for manufacturing control andassessing compliance with a specification.5. Apparatus5.1 Color Comparison TubesMatched 50-mL, tall formNessler tubes, provided
11、with ground on, optically clear, glasscaps.5.2 Constant-Temperature Bath, capable of maintaining atemperature of 15.0 6 0.5C or of 25.0 6 0.5C. It is importantthat the constant-temperature bath be protected from direct1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Rela
12、ted Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1955. Last previous edition approved in 2001 as D 1363 94 (2001).
13、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 page onthe ASTM website.1*A Summary of Changes section appears at the end of this sta
14、ndard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.light. If a glass constant-temperature bath is employed, itshould be wrapped or coated with an opaque material.5.3 Pipet, capable of delivering 2.0 mL of solution.5.4 Interval Time
15、r and Clock, capable of measuring a timeinterval of 120 min or more. An alarm arrangement may bedesirable.6. Reagents6.1 Reagent-grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalRe
16、agents of the American Chemical Society, where suchspecifications are available.3Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Unless otherwise indicated, references
17、to water shall beunderstood to mean reagent water conforming to Type IV ofSpecification D 1193.6.3 Potassium Permanganate Solution (0.200 g/L)Dissolve 0.200 g of potassium permanganate (KMnO4) anddilute to 1 L with freshly boiled water. Clean glassware isessential to the stability of this solution.
18、The solution should bestored in brown bottles and be prepared every week needed.6.4 Cobaltous Chloride-Platinum Cobalt StandardSolutionWeigh on analytical balance 175 mg of cobaltouschloride (CoCl26H2O) and add 21.4 mL of 500 Pt-Co standard(Note 1). Transfer to a 50-mL volumetric flask, dilute to th
19、emark, and mix thoroughly. This standard solution representsthe color of the end point to which the sample solution fades inthe KMnO4test. The solution is stable and should be kept in a50-mL glass-stoppered Nessler tube exactly the same as thosein which the test is run.NOTE 1The preparation of the 5
20、00 Pt-Co standard is covered in TestMethod D 1209.7. Procedure7.1 Employ the following time and temperature conditionsduring the test:Temperatureof Test, CPermanganateTime, minAcetone 25 30Methanol 15 50NOTE 2It is advisable to check Specifications D 329, D 1152 and TestMethods E 346 for possible ch
21、anges in acetone and methanol specifica-tions and permanganate time test conditions.NOTE 3Clean test cylinders and permanganate storage and handlingequipment with concentrated hydrochloric acid (HCl, sp gr 1.19) toremove residual manganese dioxide (MnO2) which catalyzes reduction ofKMnO4. Remove the
22、 acid with not less than ten rinsings with reagentwater.7.2 Fill a 50-mL Nessler tube beyond the mark with thesample under test and place in the constant-temperature bath.Maintain the water level in the bath approximately 25 mm (1in.) below the top of the tube. When the specimen has reachedthe speci
23、fied temperature, bring the level to the 50-mL mark.With a pipet, add 2 mL of the KMnO4solution. Stopper thetube, invert once to mix the contents, return to the bath andnote the time. At the end of the minimum time specified for thematerial being tested, remove the tube and compare it to thecolor st
24、andard by viewing downward through the tube againsta white background from which diffused white light is re-flected.8. Report8.1 Report the following information:8.1.1 If the residual pink color of the specimen is greaterthan the standard, report the permanganate time as “greaterthan X minutes.” If
25、the residual pink color of the specimen isequal to that of the standard, report the permanganate time as“X minutes.” If the residual pink color of the specimen is lessthan the standard, report as “less than X minutes,” where “Xminutes” is the minimum time specified for the material beingtested (see
26、7.1).8.1.2 An estimate of the actual permanganate time may bemade by closely observing the sample and reporting to thenearest minute the time when the color of the specimenmatches that of the standard. Duplicate determinations thatagree within 3.0 % are suitable for averaging (see Section 9).9. Prec
27、ision and Bias49.1 PrecisionThese precision statements are based on aninterlaboratory study in which three samples of methanolhaving average permanganate times of 60, 73, and 95 min wereeach analyzed by fourteen different laboratories in duplicate ontwo different days. In this interlaboratory study,
28、 the within-laboratory coefficient of variation was found to be 2.35 % with40 df and the between-laboratories coefficient of variation8.20 % with 12 df. Based upon these coefficients calculated inaccordance with Practice E 180, the following criteria shouldbe used for judging the acceptability of re
29、sults at the 95 %confidence level:9.2 RepeatabilityTwo results, each the mean of dupli-cates, obtained by the same operator on different days shouldbe considered suspect if they differ by more than 6.7 %.9.3 ReproducibilityTwo results, each the mean of dupli-cates, obtained by operators in different
30、 laboratories should beconsidered suspect if they differ by more than 25.2 %.9.4 BiasBias cannot be determined because there is noavailable material having an accepted reference value.10. Keywords10.1 acetone; methanol; permanganate time3Reagent Chemicals, American Chemical Society Specifications, A
31、mericanChemical 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. (
32、USPC), Rockville,MD.4Supporting data are available from ASTM Headquarters. Request RR:D01-1033.D1363062SUMMARY OF CHANGESCommittee D01.35 has identified the location of selected changes to this standard since the last issue(D 1363 94 (2001) that may impact the use of this standard.(1) Added referenc
33、e to Practice E29in the Scope section. (2) Added Practice E29to 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 determinati
34、on 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 or withdr
35、awn. 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 that your
36、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 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).D1363063
