Astm D1363 94R01 PDF

Designation: D 1363 – 94 (Reapproved 2001)
Standard Test Method for

Permanganate Time of Acetone and Methanol1
This standard is issued under the fixed designation D 1363; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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 manufacture or contamination during distribution and to assess

1.1 This test method covers the detection in acetone and compliance with a specification.
methanol of the presence of impurities that reduce potassium 4.2 Many chemical processes that use acetone or methanol,
permanganate. or both, involve catalyst, metals, or ligand complexes that are
1.2 This standard does not purport to address all of the sensitive to oxidation. Since oxidizable contaminants may
safety concerns, if any, associated with its use. It is the affect the efficiency of these processes, this test method
responsibility of the user of this standard to establish appro- provides a comparative test for manufacturing control and
priate safety and health practices and determine the applica- assessing compliance with a specification.
bility of regulatory limitations prior to use. 5. Apparatus
1.3 For specific hazard information and guidance, consult
the supplier’s Material Safety Data Sheet. 5.1 Color Comparison Tubes—Matched 50-mL, tall form
Nessler tubes, provided with ground on, optically clear, glass
2. Referenced Documents caps.
2.1 ASTM Standards: 5.2 Constant-Temperature Bath, capable of maintaining a
D 329 Specification for Acetone2 temperature of 15.0 6 0.5°C or of 25.0 6 0.5°C. It is important
D 1152 Specification for Methanol (Methyl Alcohol)2 that the constant-temperature bath be protected from direct
D 1193 Specification for Reagent Water3 light. If a glass constant-temperature bath is employed, it
D 1209 Test Method for Color of Clear Liquids (Platinum- should be wrapped or coated with an opaque material.
Cobalt Scale)2 5.3 Pipet, capable of delivering 2.0 mL of solution.
E 180 Practice for Determining the Precision of ASTM 5.4 Interval Timer and Clock, capable of measuring a time
Methods for Analysis and Testing of Industrial and Speci- interval of 120 min or more. An alarm arrangement may be
ality Chemicals4 desirable.
E 346 Test Methods for Analysis of Methanol4 6. Reagents
3. Summary of Test Method 6.1 Reagent-grade chemicals shall be used in all tests.
3.1 Substances reacting with potassium permanganate in Unless otherwise indicated, it is intended that all reagents shall
neutral solutions reduce it to manganese dioxide which colors conform to the specifications of the Committee on Analytical
the solution yellow. In the permanganate test the time required Reagents of the American Chemical Society, where such
for the color of the test solution to change to that of a standard specifications are available.5 Other grades may be used, pro-
solution is measured. The color of the test solution changes vided it is first ascertained that the reagent is of sufficiently
from pink-orange to yellow-orange. high purity to permit its use without lessening the accuracy of
the determination.
4. Significance and Use 6.2 Unless otherwise indicated, references to water shall be
4.1 The permanganate time can be used to judge the understood to mean reagent water conforming to Type IV of
presence of oxidizable materials that may be associated with Specification D 1193.
6.3 Potassium Permanganate Solution (0.200 g/L)—
Dissolve 0.200 g of potassium permanganate (KMnO4) and
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
5
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved April 15, 1994. Published June 1994. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 1363 – 55 T. Last previous edition D 1363 – 88 (1992)e1. listed by the American Chemical Society, see Analar Standards for Laboratory
2
Annual Book of ASTM Standards, Vol 06.04. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
4
Annual Book of ASTM Standards, Vol 15.05. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
D 1363
dilute to 1 L with freshly boiled water. Clean glassware is 8. Report
essential to the stability of this solution. The solution should be 8.1 Report the following information:
stored in brown bottles and be prepared every week needed. 8.1.1 If the residual pink color of the specimen is greater
6.4 Cobaltous Chloride-Platinum Cobalt Standard than the standard, report the permanganate time as “greater
Solution—Weigh on analytical balance 175 mg of cobaltous than X minutes.” If the residual pink color of the specimen is
chloride (CoCl2·6H2O) and add 21.4 mL of 500 Pt-Co standard equal to that of the standard, report the permanganate time as
(Note 1). Transfer to a 50-mL volumetric flask, dilute to the “X minutes.” If the residual pink color of the specimen is less
mark, and mix thoroughly. This standard solution represents than the standard, report as “less than X minutes,” where “X
the color of the end point to which the sample solution fades in minutes” is the minimum time specified for the material being
the KMnO4 test. The solution is stable and should be kept in a tested (see 7.1).
50-mL glass-stoppered Nessler tube exactly the same as those 8.1.2 An estimate of the actual permanganate time may be
in which the test is run. made by closely observing the sample and reporting to the
NOTE 1—The preparation of the 500 Pt-Co standard is covered in Test nearest minute the time when the color of the specimen
Method D 1209. matches that of the standard. Duplicate determinations that
agree within 3.0 % are suitable for averaging (see Section 9).
7. Procedure
9. Precision and Bias 6
7.1 Employ the following time and temperature conditions
during the test: 9.1 Precision—These precision statements are based on an
Temperature Permanganate interlaboratory study in which three samples of methanol
of Test, °C Time, min having average permanganate times of 60, 73, and 95 min were
each analyzed by fourteen different laboratories in duplicate on
Acetone 25 30
Methanol 15 50 two different days. In this interlaboratory study, the within-
laboratory coefficient of variation was found to be 2.35 % with
NOTE 2—It is advisable to check Specifications D 329, D 1152 and Test
Methods E 346 for possible changes in acetone and methanol specifica-
40 df and the between-laboratories coefficient of variation
tions and permanganate time test conditions. 8.20 % with 12 df. Based upon these coefficients calculated in
NOTE 3—Clean test cylinders and permanganate storage and handling accordance with Practice E 180, the following criteria should
equipment with concentrated hydrochloric acid (HCl, sp gr 1.19) to be used for judging the acceptability of results at the 95 %
remove residual manganese dioxide (MnO2) which catalyzes reduction of confidence level:
KMnO4. Remove the acid with not less than ten rinsings with reagent 9.2 Repeatability—Two results, each the mean of dupli-
water. cates, obtained by the same operator on different days should
7.2 Fill a 50-mL Nessler tube beyond the mark with the be considered suspect if they differ by more than 6.7 %.
sample under test and place in the constant-temperature bath. 9.3 Reproducibility—Two results, each the mean of dupli-
Maintain the water level in the bath approximately 25 mm (1 cates, obtained by operators in different laboratories should be
in.) below the top of the tube. When the specimen has reached considered suspect if they differ by more than 25.2 %.
the specified temperature, bring the level to the 50-mL mark. 9.4 Bias—Bias cannot be determined because there is no
With a pipet, add 2 mL of the KMnO4 solution. Stopper the available material having an accepted reference value.
tube, invert once to mix the contents, return to the bath and 10. Keywords
note the time. At the end of the minimum time specified for the
material being tested, remove the tube and compare it to the 10.1 acetone; methanol; permanganate time
color standard by viewing downward through the tube against
a white background from which diffused white light is re- 6
Supporting data are available from ASTM Headquarters. Request RR:D01-
flected. 1033.
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of infringement of such rights, are entirely their own responsibility.
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Designation: D 1363 – 94 (Reapproved 2001)

Standard Test Method for

1. Scope manufacture or contamination during distribution and to assess

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