1、Designation: D1363 06 (Reapproved 2011)Standard Test Method forPermanganate Time of Acetone and Methanol1This standard is issued under the fixed designation D1363; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. A number in 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 Department of Defense.1. Scope*1.1 This test method covers the detection in ac
3、etone andmethanol 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
4、used in expressing thespecification limit, in accordance with the rounding-off methodof Practice E29.1.3 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 Mat
5、erial Safety Data 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 prio
6、r to use.2. Referenced Documents2.1 ASTM Standards:2D329 Specification for AcetoneD1152 Specification for Methanol (Methyl Alcohol)D1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)E29 Practice for Using Significant Digits in Test Data toDetermi
7、ne Conformance with SpecificationsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals3E346 Test Methods for Analysis of Methanol3. Summary of Test Method3.1 Substances reacting with potassium permanganate inneutral solutions redu
8、ce it to 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 permang
9、anate time 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
10、 that aresensitive 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,
11、provided 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 Pain
12、tand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved Feb. 1, 2011. Published February 2011. Originallyapproved in 1955. Last previous edition approved in 2006 as D1363
13、06. DOI:10.1520/D1363-06R11.2For 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.3Withdrawn. The last approved ver
14、sion of this historical standard is referencedon www.astm.org.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.light. If a glass constant-temperature bath is employed,
15、itshould be wrapped or coated with an opaque material.5.3 Pipet, capable of delivering 2.0 mL of solution.5.4 Interval Timer 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.Unles
16、s otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.4Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyh
17、igh purity to permit its use without lessening the accuracy ofthe determination.6.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to Type IV ofSpecification D1193.6.3 Potassium Permanganate Solution (0.200 g/L)Dissolve 0.200 g of potassium perman
18、ganate (KMnO4) anddilute to 1 L with freshly boiled water. Clean glassware isessential to the stability of this solution. 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 cobal
19、touschloride (CoCl26H2O) and add 21.4 mL of 500 Pt-Co standard(Note 1). Transfer to a 50-mL volumetric flask, dilute to themark, 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 ke
20、pt in a50-mL glass-stoppered Nessler tube exactly the same as thosein which the test is run.NOTE 1The preparation of the 500 Pt-Co standard is covered in TestMethod D1209.7. Procedure7.1 Employ the following time and temperature conditionsduring the test:Temperatureof Test, CPermanganateTime, minAce
21、tone 25 30Methanol 15 50NOTE 2It is advisable to check Specifications D329, D1152 and TestMethods E346 for possible changes in acetone and methanol specifica-tions and permanganate time test conditions.NOTE 3Clean test cylinders and permanganate storage and handlingequipment with concentrated hydroc
22、hloric acid (HCl, sp gr 1.19) toremove residual manganese dioxide (MnO2) which catalyzes reduction ofKMnO4. Remove the 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 th
23、e water level in the bath approximately 25 mm (1in.) below the top of the tube. When the specimen has reachedthe specified 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
24、. At the end of the minimum time specified for thematerial being tested, remove the tube and compare it to thecolor standard 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 residua
25、l pink color of the specimen is greaterthan the standard, report the permanganate time as “greaterthan X minutes.” If 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 standa
26、rd, report as “less than X minutes,” where “Xminutes” is the minimum time specified for the material beingtested (see 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 th
27、at of the standard. Duplicate determinations thatagree within 3.0 % are suitable for averaging (see Section 9).9. Precision and Bias59.1 PrecisionThese precision statements are based on aninterlaboratory study in which three samples of methanolhaving average permanganate times of 60, 73, and 95 min
28、wereeach analyzed by fourteen different laboratories in duplicate ontwo different days. In this interlaboratory study, 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
29、 calculated inaccordance with Practice E180, the following criteria should beused for judging the acceptability of results 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 diffe
30、r by more than 6.7 %.9.3 ReproducibilityTwo results, each the mean of dupli-cates, obtained by operators in different 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
31、.10. Keywords10.1 acetone; methanol; permanganate time4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd.,
32、 Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1033.D1363 06 (2011)2SUMMARY OF CHANGES
33、Committee D01.35 has identified the location of selected changes to this standard since the last issue(D1363 94 (2001) that may impact the use of this standard.(1) Added reference to Practice E29 in the Scope section. (2) Added Practice E29 to list of Referenced Documents.ASTM International takes no
34、 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 determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own respons
35、ibility.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 withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed t
36、o 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 comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the add
37、ress 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1363 06 (2011)3
