ASTM E755-08
(Test Method)Standard Test Method for Dicumyl Peroxide, Assay (Liquid Chromatography) (Withdrawn 2016)
Standard Test Method for Dicumyl Peroxide, Assay (Liquid Chromatography) (Withdrawn 2016)
SIGNIFICANCE AND USE
This test method provides a means for determining the percent of dicumyl peroxide in technical and refined grades of this material. This test method is specific for dicumyl peroxide. No interference is encountered from dimethylbenzyl alcohol, acetophenone, or other minor impurities normally associated with commercial dicumyl peroxide.
SCOPE
1.1 This test method covers the assay of dicumyl peroxide in commercially available refined grades of dicumyl peroxide. Technical grades can also be assayed, provided that impurities that interfere chromatographically are absent (see Note 1). These materials nominally contain approximately 99 and 92 % of dicumyl peroxide, respectively.
Note 1—In the assay of technical grade dicumyl peroxide, errors are possible if the product contains an impurity that elutes with the same retention time as the internal standard. A chromatogram obtained under the test conditions minus the internal standard will determine whether an interference situation exists in the assay of a particular technical grade product. If an impurity is noted, and its retention time is slightly different from that of the internal standard, the interference can often be eliminated by the use of a column known to have a high plate count.
1.2 Review the current material safety data sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.
1.3 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.
1.4 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. Specific precautionary statements are given in Section 7.
WITHDRAWN RATIONALE
This test method covers the assay of dicumyl peroxide in commercially available refined grades of dicumyl peroxide. Technical grades can also be assayed, provided that impurities that interfere chromatographically are absent. These materials nominally contain approximately 99 and 92 % of dicumyl peroxide, respectively.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, this test method was withdrawn in November 2016. This standard is being withdrawn without replacement due to its limited use by industry.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E755 − 08
StandardTest Method for
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Dicumyl Peroxide, Assay (Liquid Chromatography)
This standard is issued under the fixed designation E755; 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* Methods for Analysis and Testing of Industrial and Spe-
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cialty Chemicals (Withdrawn 2009)
1.1 This test method covers the assay of dicumyl peroxide
E682 Practice for Liquid Chromatography Terms and Rela-
in commercially available refined grades of dicumyl peroxide.
tionships
Technical grades can also be assayed, provided that impurities
E685 Practice for Testing Fixed-Wavelength Photometric
that interfere chromatographically are absent (see Note 1).
Detectors Used in Liquid Chromatography
These materials nominally contain approximately 99 and 92 %
E300 Practice for Sampling Industrial Chemicals
of dicumyl peroxide, respectively.
NOTE 1—In the assay of technical grade dicumyl peroxide, errors are 3. Summary of Test Method
possible if the product contains an impurity that elutes with the same
3.1 A solution of sample and internal standard in methanol
retention time as the internal standard. A chromatogram obtained under
is chromatographed on a reversed-phase ODS column using
the test conditions minus the internal standard will determine whether an
interference situation exists in the assay of a particular technical grade
85/15 methanol/water as the mobile phase and an ultraviolet
product. If an impurity is noted, and its retention time is slightly different
(UV) detector at 254 nm. The percent of dicumyl peroxide in
from that of the internal standard, the interference can often be eliminated
the sample is determined by the internal standard technique,
by the use of a column known to have a high plate count.
using the peak height ratios of standard and sample chromato-
1.2 Review the current material safety data sheets (MSDS)
grams.
for detailed information concerning toxicity, first aid
procedures, and safety precautions.
4. Significance and Use
1.3 The values stated in SI units are to be regarded as the 4.1 This test method provides a means for determining the
standard. No other units of measurement are included in this
percent of dicumyl peroxide in technical and refined grades of
standard. this material.This test method is specific for dicumyl peroxide.
No interference is encountered from dimethylbenzyl alcohol,
1.4 This standard does not purport to address all of the
acetophenone, or other minor impurities normally associated
safety concerns, if any, associated with its use. It is the
with commercial dicumyl peroxide.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. Specific precau-
5.1 Liquid Chromatograph, equipped with a 254-nm UV
tionary statements are given in Section 7.
detector, an injection valve, and an isocratic solvent delivery
2. Referenced Documents system capable of operating to a gage pressure of 3000 psi (21
3 MPa). The detector should be equipped with an attenuator
2.1 ASTM Standards:
switch to change the sensitivity range as required.
D1193 Specification for Reagent Water
E180 Practice for Determining the Precision of ASTM 5.2 Recorder, 0 to 10-mV range, or an electronic integrator
with printer-plotter, or both.
5.3 ChromatographicColumn, reversed-phase C-18, 250 by
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This test method is under the jurisdiction of ASTM Committee D16 on
4.6-mm inside diameter, containing octadecyldimethylsilane
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
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chemically bonded to spherical, 5-µm microparticulate silica.
Subcommittee D16.16 on Industrial and Specialty Product Standards.
Current edition approved Dec. 15, 2008. Published January 2009. Originally
approved in 1980. Last previous edition approved in 2003 as E755 – 94 (2003).
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DOI: 10.1520/E0755-08. The last approved version of this historical standard is referenced on
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Dicumyl Peroxide; peroxide, bis(1-methyl-1-phenylethyl) C H O ; CAS www.astm.org.
18 22 2
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Registry No. 80-43-3. The commercial guard and analytical columns found to be most satisfactory for
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or use with this test method are Zorbax Rx-18, Part Nos. 820764.914 and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 880967.9002, respectively, available from Mac Mod, 127 Commons Court, Chadds
Standards volume information, refer to the standard’s Document Summary page on Ford, PA 19317. This column was select
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