ASTM D7210-13
(Practice)Standard Practice for Extraction of Additives in Polyolefin Plastics
Standard Practice for Extraction of Additives in Polyolefin Plastics
SIGNIFICANCE AND USE
5.1 Separation and identification of additives used in the manufacture of polyolefin plastics is necessary in order to correlate performance properties with polymer composition. This practice provides guidelines for extracting phenolic antioxidants, phosphite antioxidants, UV stabilizers, antistatic agents, and slip additives, from milled polyolefin plastics .
5.2 Water bath shakers and steam-reflux Soxhlet extraction techniques have also been used to successfully remove additives from polyolefin plastics.
SCOPE
1.1 This practice covers a variety of extraction techniques for antioxidant and slip additives used in polyolefins. Typically, the extracted additives are separated and quantified using a chromatographic technique such as the procedure explained in Test Method D6953. Chromatographic analysis of the extracts is not included in this practice.
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.Note 1—There is no known ISO equivalent to this standard.
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Designation: D7210 −13
Standard Practice for
1
Extraction of Additives in Polyolefin Plastics
This standard is issued under the fixed designation D7210; 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* 3.3.2 LLDPE—Linear Low-Density Polyethylene
1.1 This practice covers a variety of extraction techniques 3.3.3 HDPE—High-Density Polyethylene
forantioxidantandslipadditivesusedinpolyolefins.Typically,
3.3.4 PP—Polypropylene
the extracted additives are separated and quantified using a
3.4 Definitions: Additives:
chromatographic technique such as the procedure explained in
Test Method D6953. Chromatographic analysis of the extracts 3.4.1 BHEB—2,6-di-t-butyl-4-ethyl-phenol or butylated hy-
droxyethyl benzene, CAS No. 4130-42-1
is not included in this practice.
1.2 This standard does not purport to address all of the
3.4.2 BHT—2,6-di-t-butyl-cresol or butylated
safety concerns, if any, associated with its use. It is the
hydroxytoluene, CAS No. 128-37-0
responsibility of the user of this standard to establish appro-
3.4.3 2-benzotriazol-2-yl-4-methylphenol, CAS No. 2440-
priate safety and health practices and determine the applica-
22-4
bility of regulatory limitations prior to use.
3.4.4 bis(3,3,5,5-tetramethyl-4-piperidyl)decanedioate,
NOTE 1—There is no known ISO equivalent to this standard.
CAS No. 91450-21-4
3.4.5 Cis-13-docosenamide or erucamide slip, CAS No.
2. Referenced Documents
112-84-5
2
2.1 ASTM Standards:
3.4.6 N,N’-diphenylbenzene-1,4-diamine, CAS No. 74-31-7
D883 Terminology Relating to Plastics
3.4.7 2,2’-ethylidene bis (4,6-di-t-butyl phenol), CAS No.
D1600 Terminology forAbbreviatedTerms Relating to Plas-
112-84-5
tics
3.4.8 Tetrakis[methylene (3,5-di-t-butyl-4-hydroxy hydro-
D6953 Test Method for Determination of Antioxidants and
cinnamate)] methane, CAS No. 98584-37-3
Erucamide Slip Additives in Polyethylene Using Liquid
3.4.9 1,3,5-trimethyl-2,4,6-tris (3,5-di-t-butyl-4-
Chromatography (LC)
hydroxybenzyl) benzene, CAS No. 99346-90-4
E131 Terminology Relating to Molecular Spectroscopy
3.4.10 Octadecyl-3,5-di-t-butyl-4-hydroxy hydrocinnamate,
3. Terminology
CAS No. 2082-79-3
3.1 Definitions: 3.4.11 Sodium Alkyl Sulfonate, CAS No. 68411-30-3
3.1.1 For definitions of plastic terms used in this practice,
3.4.12 Tris(2,4-di-t-butylphenyl) phosphite, CAS No.
see Terminologies D883 and D1600.
31570-04-4
3.4.13 Tris(2,4-di-t-butylphenyl) phosphate (oxidized
3.2 For units, symbols, and abbreviations used in this
Tris(2,4-di-t-butylphenyl) phosphite)
practice refer to Terminology E131.
3.4.14 TNPP—Tris(nonylphenyl) phosphite, CAS No.
3.3 Abbreviations:
26523-78-4
3.3.1 LDPE—Low-Density Polyethylene
3.4.15 Hydrolyzed TNPP—Nonylphenol, CAS No. 104-
40-5
1
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
3.4.16 Oxidized TNPP—Tris(nonylphenol)phosphate CAS
is the direct responsibility of Subcommittee D20.70 on Analytical Methods and
Section D20.70.01 on Physical Methods. No. 26569-53-9
Current edition approved April 1, 2013. Published April 2013. Originally
approved in 2006. Last previous edition approved in 2006 as D7210 – 06. DOI:
4. Summary of Practice
10.1520/D7210-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 The polymer sample is ground to approximately a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
0.5-mm (≈40-mesh) or 1-mm (≈20-mesh) particle size and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. extracted by one of the techniques listed in this practice.
*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 ----------------------
D7210 − 13
5,6
5. Significance and Use 7.2.4 Microwave Extraction Apparatus (MAE) , equipped
with 100-mL extraction vessels or equivalent.
5.1 Separation and identification of additives used in the
7.2.5 Sonication Extraction Apparatus, consisting of a suit-
manufacture of polyolefin plastics is necessary in order to
able ultrasonic cleaner such as an Aquasonic Model 75D
correlate performance properties with polymer composition.
Ultrasonic Cleaner or equivalent.
This practice provides guidelines for extracting phenolic
antioxidants, phosphite antioxidants, UV stabilizers, antistatic 7.3 Filter System, for nonaqueous solutions (pore size of
agents, and slip additives, from milled polyolefin plastics . 0.22 µm to 0.5µm).
5.2 Water bath shakers and steam-reflux Soxhlet extract
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D7210 − 06 D7210 − 13
Standard Practice for
1
Extraction of Additives in Polyolefin Plastics
This standard is issued under the fixed designation D7210; 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 Scope*
1.1 This practice covers a variety of extraction techniques for antioxidant and slip additives used in polyolefins. Typically, the
extracted additives are separated and quantified using a chromatographic technique such as the procedure explained in Test Method
D6953. Chromatographic analysis of the extracts is not included in this practice.
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.
NOTE 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
D6953 Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid
Chromatography (LC)
E131 Terminology Relating to Molecular Spectroscopy
3. Terminology
3.1 Definitions:
3.1.1 For definitions of plastic terms used in this practice, see Terminologies D883 and D1600.
3.2 For units, symbols, and abbreviations used in this practice refer to Terminology E131.
3.3 Abbreviations:
3.3.1 LDPE—Low-Density Polyethylene
3.3.2 LLDPE—Linear Low-Density Polyethylene
3.3.3 HDPE—High-Density Polyethylene
3.3.4 PP—Polypropylene
3.4 Definitions: Additives:
3.4.1 BHEB—2,6-di-t-butyl-4-ethyl-phenol or butylated hydroxyethyl benzene, CAS No. 4130-42-1
3.4.2 BHT—2,6-di-t-butyl-cresol or butylated hydroxytoluene, CAS No. 128-37-0
3.4.3 2-benzotriazol-2-yl-4-methylphenol, CAS No. 2440-22-4
3.4.4 bis(3,3,5,5-tetramethyl-4-piperidyl)decanedioate, CAS No. 91450-21-4
3.4.5 Cis-13-docosenamide or erucamide slip, CAS No. 112-84-5
3.4.6 N,N’-diphenylbenzene-1,4-diamine, CAS No. 74-31-7
3.4.7 2,2’-ethylidene bis (4,6-di-t-butyl phenol), CAS No. 112-84-5
3.4.8 Tetrakis[methylene (3,5-di-t-butyl-4-hydroxy hydrocinnamate)] methane, CAS No. 98584-37-3
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. and Section
D20.70.01 on Physical Methods.
Current edition approved March 15, 2006April 1, 2013. Published July 2006April 2013. Originally approved in 2006. Last previous edition approved in 2006 as D7210
– 06. DOI: 10.1520/D7210-06.10.1520/D7210-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 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
---------------------- Page: 1 ----------------------
D7210 − 13
3.4.9 1,3,5-trimethyl-2,4,6-tris (3,5-di-t-butyl-4-hydroxybenzyl) benzene, CAS No. 99346-90-4
3.4.10 Octadecyl-3,5-di-t-butyl-4-hydroxy hydrocinnamate, CAS No. 2082-79-3
3.4.11 Sodium Alkyl Sulfonate, CAS No. 68411-30-3
3.4.12 Tris(2,4-di-t-butylphenyl) phosphite, CAS No. 31570-04-4
3.4.13 Tris(2,4-di-t-butylphenyl) phosphate (oxidized Tris(2,4-di-t-butylphenyl) phosphite)
3.4.14 TNPP—Tris(nonylphenyl) phosphite, CAS No. 26523-78-4
3.4.15 Hydrolyzed TNPP—Nonylphenol, CAS No. 104-40-5
3.4.16 Oxidized TNPP—Tris(nonylphenol)phosphate CAS No. 26569-53-9
4. Summary of Practice
4.1 The polymer sample is ground to approximately a 0.5-mm (≈40-mesh) or 1-mm (≈20-mesh) particle size and extracted by
one of the techniques listed in this practice.
5. Significance and Use
5.1 Separation and identification of additives used in the manufacture of polyolefin plastics is necessary in order to correlate
performance properties with polymer composition. This practice provides guidelines for extracting phenolic antioxidants,
phosphite antioxidants, UV stabilizers, antistatic agents, and slip additives, from milled polyolefin plastics .
5.2 Water bath shakers and steam-reflux
...
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