ASTM D1832-04
(Test Method)Standard Test Method for Peroxide Number of Petroleum Wax
Standard Test Method for Peroxide Number of Petroleum Wax
SIGNIFICANCE AND USE
The magnitude of the peroxide number is an indication of the quantity of oxidizing constituents present. Deterioration of petroleum wax results in the formation of peroxides and other oxygen-carrying compounds. The peroxide number measures those compounds that will oxidize potassium iodide.
SCOPE
1.1 This test method covers the determination of the peroxide number of petroleum wax.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Technical Association of Pulp
Designation:D1832–04 and Paper Industry Standard Method T 659 su-67
Standard Test Method for
1
Peroxide Number of Petroleum Wax
This standard is issued under the fixed designation D1832; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope* tee on Analytical Reagents of the American Chemical Society,
2
where such specifications are available. Other grades may be
1.1 This test method covers the determination of the perox-
used, provided it is first ascertained that the reagent is of
ide number of petroleum wax.
sufficiently high purity to permit its use without lessening the
1.2 This standard does not purport to address all of the
accuracy of the determination.
safety concerns, if any, associated with its use. It is the
6.2 Purity of Water—Unless otherwise indicated, references
responsibility of the user of this standard to establish appro-
to water shall be understood to mean distilled water or water of
priate safety and health practices and determine the applica-
equal purity.
bility of regulatory limitations prior to use.
6.3 Acetic Acid Solution—Mix 4 mLof concentrated hydro-
2. Terminology chloric acid (HCl, sp gr 1.19) with 996 mL of ACS special
reagent grade glacial acetic acid (CH CO H). The acetic acid
2.1 Definitions: 3 2
1
must pass the ⁄2-h test for substances reducing K Cr O .
2 2 7
2.1.1 peroxide number—the milliequivalents of constituents
6.4 Xylenes,(Warning—Flammable liquid. Vapor harm-
per 1000 g of wax that will oxidize potassium iodide.
ful.) Treated to remove oxidizing impurities. One way to do
3. Summary of Test Method
this is to pass the xylenes through an activated alumina column
shortly prior to use.
3.1 A quantity of sample is dissolved in xylenes and
6.5 Potassium Dichromate, Standard Solution (0.1 N)—
acidified with acetic acid solution. A solution of potassium
Recrystallize potassium dichromate (K Cr O ) twice from an
iodide is added and, after a reaction period, the solution is 2 2 7
aqueous solution and dry at about 325°F (164°C) to constant
titrated with sodium thiosulfate solution to the end point
weight. Dissolve 2.452 g of the purified K Cr O in water and
indicated by the color change of added starch solution. 2 2 7
dilute to 500 mL in a volumetric flask.
4. Significance and Use
6.6 Potassium Dichromate, Standard Solution (0.01 N)—
Dilute 100 mL of 0.1 N K Cr O solution with water to 1000
4.1 The magnitude of the peroxide number is an indication
2 2 7
mL in a volumetric flask.
of the quantity of oxidizing constituents present. Deterioration
6.7 Potassium Iodide Solution—Dissolve 120 g of potas-
of petroleum wax results in the formation of peroxides and
sium iodide (KI) in 100 mLof water. Discharge any color from
other oxygen-carrying compounds. The peroxide number mea-
this solution as follows: put 1 mL of KI solution, 50 mL of
sures those compounds that will oxidize potassium iodide.
water, and 5 mL of starch solution in a 300-mL flask and
5. Apparatus
blanket with nitrogen or carbon dioxide. If a blue color
develops, add 0.005 N Na S O solution from a microburet
5.1 Iodine Flask, borosilicate glass, 250-mLcapacity, glass-
2 2 3
until color just disappears. Calculate and add sufficient
stoppered.
Na S O solution to the main KI solution to convert all free
2 2 3
6. Reagents and Materials
iodine to iodide. When starch solution is added to 1 mL of KI
6.1 Purity of Reagents—Reagent grade chemicals shall be solution a blue color should not develop, but upon the addition
of 1 drop of 0.01 N K Cr O solution and 2 drops of
used in all tests. Unless otherwise indicated, it is intended that
2 2 7
all reagents shall conform to the specifications of the Commit- concentrated hydrochloric acid (HCl, sp gr 1.19), a blue color
1 2
This test method is under the jurisdiction of the ASTM Committee D02 on Reagent Chemicals, American Chemical Society Specifications, American
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
D02.10 on Properties of Petroleum Wax. listed by the American Chemical Society, see Annual Standards for Laboratory
Current edition approved Nov. 1, 2004. Published November 2004. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1961. Last previous edition approved in 1999 as D1832–87(1999). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D1832-04. MD.
*A Summary of Changes section appears at the end of this standard.
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