ASTM D6042-04
(Test Method)Standard Test Method for Determination of Phenolic Antioxidants and Erucamide Slip Additives in Polypropylene Homopolymer Formulations Using Liquid Chromatography (LC)
Standard Test Method for Determination of Phenolic Antioxidants and Erucamide Slip Additives in Polypropylene Homopolymer Formulations Using Liquid Chromatography (LC)
SIGNIFICANCE AND USE
Separation and identification of stabilizers used in the manufacture of polypropylene is necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine erucamide slip, Vitamin E, Irgafos 168, Irganox 3114, Irganox 1010, and Irganox 1076 levels in polypropylene samples. This test method is also applicable for the determination of other antioxidants, such as Ultranox 626, Ethanox 330, Santanox R, and BHT, but the applicability of this test method has not been investigated for these antioxidants.
The additive-extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for liquid chromatographic analysis.
Under optimum conditions, the lowest level of detection for a phenolic antioxidant is approximately 2 ppm.
Note 2—Other methods that have been used successfully to remove additives from the plastics matrix include thin film, microwave, ultrasonic, and supercritical fluid extractions. Other methods have been used successfully to separate additives including SFC and capillary GC.
Irgafos 168 is a phosphite antioxidant. Phosphites are known to undergo both oxidation and hydrolysis reactions. Less Irgafos 168 may be seen in the polymer than originally added to the polymer due to oxidation during processing. The HPLC separation is capable of separating the phosphite, phosphate (oxidation product), and hydrolysis product and quantify them if standards are obtained. No significant breakdown of the phosphite antioxidant has been seen due to either extraction technique or the separation presented in this standard.
SCOPE
1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in polypropylene. These additives are extracted with a cyclohexane:methylene chloride mixture using either reflux or ultrasonic bath prior to liquid-chromatographic separation. The ultraviolet absorbence (200 nm) of the compound(s) is measured, and quantitation is performed using the internal standard method.
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. Specific precautionary statements are given in Section 9.
Note 1- There is no similar or equivalent ISO standard.
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Designation: D 6042 – 04
Standard Test Method for
Determination of Phenolic Antioxidants and Erucamide Slip
Additives in Polypropylene Homopolymer Formulations
1
Using Liquid Chromatography (LC)
This standard is issued under the fixed designation D 6042; 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* 3.3 Abbreviations:Abbreviations:
3.3.1 LC—liquid chromatography.
1.1 This test method covers a liquid-chromatographic pro-
3.3.2 PP—polypropylene.
cedure for the separation of some additives currently used in
3.4 Trade Names:
polypropylene. These additives are extracted with a cyclohex-
3.5 Vitamin E—a-Tocopherol, or 3,4-dihydro-2,5,7,8-
ane:methylene chloride mixture using either reflux or ultra-
tetramethyl-2-(4,8,12-trimethyltridecyl)-2H-1-benzopyran-6-
sonic bath prior to liquid-chromatographic separation. The
ol.
ultraviolet absorbance (200 nm) of the compound(s) is mea-
3.6 Irgafos 168—Tris(2,4 di-tert-butylphenyl) phosphite.
sured,andquantitationisperformedusingtheinternalstandard
3.7 Irganox 3114—Tris(3,5-di-t-butyl-4-hydroxybenzyl)
method.
isocyanurate.
1.2 This standard does not purport to address all of the
3.8 Kemamide-E—cis-13-docosenamide or erucamide.
safety concerns, if any, associated with its use. It is the
3.9 Irganox 1010—tetrakis[methylene(3,5-di-t-butyl-4-
responsibility of the user of this standard to establish appro-
hydroxy hydrocinnamate)]methane.
priate safety and health practices and determine the applica-
3.10 Irganox 1076—octadecyl-3,5-di-t-butyl-4-hydroxy hy-
bility of regulatory limitations prior to use. Specific precau-
drocinnamate.
tionary statements are given in Section 9.
3.11 Tinuvin P—2(28-hydroxy-58-methyl phenyl)benzotria-
NOTE 1—There is no similar or equivalent ISO standard.
zole.
2. Referenced Documents
4. Summary of Test Method
2
2.1 ASTM Standards:
4.1 The PPsample is ground to a 20-mesh particle size (850
D 883 Terminology Relating to Plastics
microns) and extracted by refluxing with a mixture of 75:25
D 1600 Terminology for Abbreviated Terms Relating to
methylene chloride:cyclohexane or placing in an ultrasonic
Plastics
bath with the same mixture.
E 131 Terminology Relating to Molecular Spectroscopy
4.2 The solvent extract is examined by liquid chromatogra-
E 691 Practice for Conducting an Interlaboratory Study to
phy.
Determine the Precision of a Test Method
4.3 Additive concentrations are determined relative to an
IEEE/ASTM SI-10 Practice for Use of the International
internalstandard(containedinthesolvent)usingreverse-phase
System of Units (SI) (the Modernized Metric System)
chromatography(C-18column)withultraviolet(UV)detection
at 200 nm.
3. Terminology
3.1 For definitions of plastic terms used in this test method,
5. Significance and Use
see Terminologies D 883 and D 1600.
5.1 Separation and identification of stabilizers used in the
3.2 For the units, symbols, and abbreviations used in this
manufactureofpolypropyleneisnecessaryinordertocorrelate
test method, refer to Terminology E 131 or Practice IEEE/
performance properties with polymer composition. This test
ASTM SI-10.
method provides a means to determine erucamide slip,Vitamin
E, Irgafos 168, Irganox 3114, Irganox 1010, and Irganox 1076
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
levels in polypropylene samples. This test method is also
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
applicable for the determination of other antioxidants, such as
Current edition approved July 1, 2004. Published July 2004. Originally approved
Ultranox 626, Ethanox 330, Santanox R, and BHT, but the
in 1996. Last previous edition approved in 1996 as D 6042 - 96.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or applicability of this test method has not been investigated for
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
these antioxidants.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
*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.
1
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D6042–04
5.2 The additive-extraction procedure is made effective by
the insolubility of the polymer sample in solvents generally
used for liquid chromatographic analysis.
5.3 Under optimum conditions, the lowest level of detection
for a phenolic antioxidant is approximately 2 ppm.
NOTE 2—Other methods that have been used succes
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D6042–96 Designation: D 6042 – 04
Standard Test Method for
Determination of Phenolic Antioxidants and Erucamide Slip
Additives in Polypropylene Homopolymer Formulations
1
Using Liquid Chromatography (LC)
This standard is issued under the fixed designation D 6042; 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*
1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in
polypropylene. These additives are extracted with a cyclohexane:methylene chloride mixture using either reflux or ultrasonic bath
priortoliquid-chromatographicseparation.Theultravioletabsorbeance(200nm)ofthecompound(s)ismeasured,andquantitation
is performed using the internal standard method.
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. Specific precautionary statements are given in Section 9.
NOTE 1—There is no similar or equivalent ISO standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics
D 1600 Terminology for Abbreviated Terms Relating to Plastics
E 131 Terminology Relating to Molecular Spectroscopy
E380Practice for Use of the International System of Units (SI) (the Modernized Metric System) Terminology Relating to
Molecular Spectroscopy
4
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method Practice for Conducting
an Interlaboratory Study to Determine the Precision of a Test Method
IEEE/ASTM SI-10 Practice for Use of the International System of Units (SI) (the Modernized Metric System)
3. Terminology
3.1 For definitions of plastic terms used in this test method, see Terminologies D 883 and D 1600.
3.2 For the units, symbols, and abbreviations used in this test method, refer to Terminology E 131 or Practice E380or Practice
IEEE/ASTM SI-10.
3.3 Abbreviations:Abbreviations:
3.3.1 LC—liquid chromatography.
3.3.2 PP—polypropylene.
3.4 Trade Names:
3.5 Vitamin E—a-Tocopherol, or 3,4-dihydro-2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-2H-1-benzopyran-6- ol.
3.6 Irgafos 168—Tris(2,4 di-tert-butylphenyl) phosphite.
3.7 Irganox 3114—Tris(3,5-di-t-butyl-4-hydroxybenzyl) isocyanurate.
3.8 Kemamide-E—cis-13-docosenamide or erucamide.
3.9 Irganox 1010—tetrakis[methylene(3,5-di-t-butyl-4-hydroxy hydrocinnamate)]methane.
3.10 Irganox 1076—octadecyl-3,5-di-t-butyl-4-hydroxy hydrocinnamate.
3.11 Tinuvin P—2(28-hydroxy-58-methyl phenyl)benzotriazole.
1
This test method is under the jurisdiction of ASTM Committee D-20 D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
.
Current edition approved Nov. 10, 1996. Published April 1997.
Current edition approved July 1, 2004. Published July 2004. Originally approved in 1996. Last previous edition approved in 1996 as D 6042 - 96.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 08.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
1
---------------------- Page: 1 ----------------------
D6042–04
4. Summary of Test Method
4.1 The PP sample is ground to a 20-mesh particle size (850 microns) and extracted by refluxing with a mixture of 75:25
methylene chloride:cyclohexane or placing in an ultrasonic bath with the same mixture.
4.2 The solvent extract is examined by liquid chromatography.
4.3 Additive concentrations are determined relative to an internal standard (contained in the solvent) using reverse-phase
chromatography (C-18 column) with ultraviolet (UV) detection at 200 nm.
5. Significance and Use
5.1 Separation and identification of stabilizers used in the manufacture of polypropylene is necessary in order to correlate
performance properties with polymer composition. This test method provides a means to determine erucamide slip, Vitamin E,
Irgafos 168, Irgan
...
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