ASTM E1090-08

Standard Test Method for Dicumyl Peroxide and Dicumyl Peroxide Decomposition Products in Resins (Withdrawn 2017)

SIGNIFICANCE AND USE
Knowledge of the peroxide content of uncured PE and EVA samples is required to regulate the degree of crosslinking in the cured product. As end use applications of the cured product can be affected by residual amounts of the peroxide or its decomposition products—dimethylbenzyl alcohol and acetophenone—knowledge of these levels is also important. This test method provides a procedure for determining the concentration of these compounds. A method for the HPLC assay of dicumyl peroxide is described in Test Method E 755.
SCOPE
1.1 This test method covers and is applicable to the determination of dicumyl peroxide and the decomposition products dimethylbenzyl alcohol and acetophenone in cured and uncured polyethylene (PE) and ethylene vinyl acetate (EVA) resins. These uncured polymers normally contain from 1 to 2 % dicumyl peroxide, whereas the residual peroxide level in the cured polymers is usually less than 0.1 %.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 Review the current Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.
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 hazards are given in Section 7.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, this test method was withdrawn in January 2017 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 31-Mar-2008
• Withdrawal Date: 05-Jan-2017
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E1090 − 08
Standard Test Method for
Dicumyl Peroxide and Dicumyl Peroxide Decomposition
1
Products in Resins
This standard is issued under the fixed designation E1090; 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* E682 Practice for Liquid Chromatography Terms and Rela-
tionships
1.1 This test method covers and is applicable to the deter-
2 E685 Practice for Testing Fixed-Wavelength Photometric
minationofdicumylperoxide andthedecompositionproducts
Detectors Used in Liquid Chromatography
dimethylbenzyl alcohol and acetophenone in cured and un-
E755 Test Method for Dicumyl Peroxide, Assay (Liquid
cured polyethylene (PE) and ethylene vinyl acetate (EVA)
Chromatography)
resins.Theseuncuredpolymersnormallycontainfrom1to2%
dicumyl peroxide, whereas the residual peroxide level in the
3. Summary of Test Method
cured polymers is usually less than 0.1 %.
3.1 Dicumyl peroxide and dimethylbenzyl alcohol are ex-
1.2 The values stated in SI units are to be regarded as
tracted from a cryogenically ground sample with methylene
standard. The values given in parentheses are for information
chloride. The extract is concentrated, redissolved in methanol,
only.
and analyzed by high performance liquid chromatography
1.3 ReviewthecurrentMaterialSafetyDataSheets(MSDS)
(HPLC). Acetophenone is extracted from a separate sample
for detailed information concerning toxicity, first aid
with methanol and analyzed directly by HPLC. The analyses
procedures, and safety precautions.
are performed on a reversed phase octadecylsilane (ODS)
1.4 This standard does not purport to address all of the
column using acetonitrile/water as the mobile phase and an
safety concerns, if any, associated with its use. It is the
ultraviolet detector at 254 nm. The concentration of each
responsibility of the user of this standard to establish appro-
component is determined by the internal standard technique,
priate safety and health practices and determine the applica-
using peak height ratios of the sample and standard chromato-
bility of regulatory limitations prior to use.Specifichazardsare
grams.
given in Section 7.
4. Significance and Use
2. Referenced Documents
4.1 Knowledge of the peroxide content of uncured PE and
3
2.1 ASTM Standards:
EVAsamples is required to regulate the degree of crosslinking
D1193 Specification for Reagent Water
in the cured product. As end use applications of the cured
E180 Practice for Determining the Precision of ASTM
product can be affected by residual amounts of the peroxide or
Methods for Analysis and Testing of Industrial and Spe-
its decomposition products—dimethylbenzyl alcohol and
4
cialty Chemicals (Withdrawn 2009)
acetophenone—knowledge of these levels is also important.
E300 Practice for Sampling Industrial Chemicals
This test method provides a procedure for determining the
concentration of these compounds. A method for the HPLC
assay of dicumyl peroxide is described in Test Method E755.
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
5. Apparatus
Subcommittee D16.15 on Industrial and Specialty General Standards.
Current edition approved April 1, 2008. Published May 2008. Originally
5.1 Liquid Chromatograph, equipped with a 254-nm UV
approved in 1986. Last previous edition approved in 2002 as E1090 – 96 (2002).
detector, injection valve, and an isocratic-solvent delivery
DOI: 10.1520/E1090-08.
2
Dicumyl peroxide; peroxide, bis(1-methyl-1-phenylethyl) C H O ; CAS
systemcapableofoperatingtoagagepressureof3000psi.The
18 22 2
Registry No. 80-43-3.
detector should be equipped with an attenuator switch to
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
change the sensitivity range as required. (See Practices E682
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
and E685.)
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
4
5.2 Recorder, 0 to 1 mv range,1sor less full-scale
The last approved version of this historical standard is referenced on
www.astm.org. deflection,withachartspeedof0.1in./minorotherconvenient
*A Summary of Changes section appears at the end of this standard
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E1090 − 08
6.3 Water, prepare Type II reagent water in accordance with
SpecificationD1193,ordistilldeionizedwater.Filterthrougha
7,10
0.45-µm filter and stor
...