ASTM D2765-16
(Test Method)Standard Test Methods for Determination of Gel Content and Swell Ratio of Crosslinked Ethylene Plastics
Standard Test Methods for Determination of Gel Content and Swell Ratio of Crosslinked Ethylene Plastics
SIGNIFICANCE AND USE
5.1 Many important properties of crosslinked ethylene plastics vary with the gel content. Hence, determination of the gel content provides a means of both controlling the process and rating the quality of finished products.
5.2 Extraction tests permit verification of the proper gel content of any given crosslinked ethylene plastic and they also permit comparison between different crosslinked ethylene plastics, including those containing fillers, provided that, for the latter, the following conditions are met:
5.2.1 The filler is not soluble in either decahydronaphthalene or xylenes at the extraction temperature.
5.2.2 The amount of filler present in the compound either is known or will be determined by other means.
5.2.3 Sufficient crosslinking has been achieved to prevent migration of filler during the extraction. Usually it has been found that, at extraction levels up to 50 %, the extractant remains clear and free of filler.
5.3 A suitable antioxidant is added to the extractant to inhibit possible oxidative degradation at the extraction temperatures.
5.4 Before proceeding with this test method, reference shall be made to the specification of the material being tested. Any test specimen preparation, conditioning, dimensions, or testing parameters, or a combination thereof, covered in the materials specification shall take precedence over those mentioned in this test method. If there are no material specifications, then the default conditions apply.
SCOPE
1.1 The gel content (insoluble fraction) produced in ethylene plastics by crosslinking is determined by extracting with solvents such as decahydronaphthalene or xylenes. The methods described herein are applicable to crosslinked ethylene plastics of all densities, including those containing fillers, and all provide corrections for the inert fillers present in some of those compounds.
1.2 Test Method A, which permits most complete extraction in least time, is to be used for referee tests, but two alternative nonreferee Test Methods B and C are also described. Test Method B differs from the referee test method only in sample preparation; that is, it requires use of shavings taken at selected points in cable insulation, for example, rather than the ground sample required by the referee test method. Because the shaved particles are larger, less total surface per sample is exposed to the extractant, so this test method ordinarily yields extraction values about 1 to 2 % lower than the referee method. Test Method C requires that a specimen in one piece be extracted in xylenes at a constant temperature of 110°C. At this temperature and with a one-piece specimen, even less extraction occurs (from 3 to 9 % less than the referee test method), this method permits swell ratio (a measure of the degree of crosslinking in the gel phase) be determined.
1.3 Extraction tests are made on articles of any shape. They have been particularly useful for electrical insulations since specimens can be selected from those portions of the insulation most susceptible to insufficient crosslinking.
1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.
Note 1: This test method is equivalent to ISO 10147, Method B. It is not equivalent to ISO 10147 in any other measurement or section.
1.5 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 Sections 6, 9, and 24.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2765 − 16
Standard Test Methods for
Determination of Gel Content and Swell Ratio of
1
Crosslinked Ethylene Plastics
This standard is issued under the fixed designation D2765; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
not equivalent to ISO 10147 in any other measurement or section.
1. Scope*
1.5 This standard does not purport to address all of the
1.1 The gel content (insoluble fraction) produced in ethyl-
safety concerns, if any, associated with its use. It is the
ene plastics by crosslinking is determined by extracting with
responsibility of the user of this standard to establish appro-
solvents such as decahydronaphthalene or xylenes. The meth-
priate safety and health practices and determine the applica-
ods described herein are applicable to crosslinked ethylene
bility of regulatory limitations prior to use. Specific precau-
plastics of all densities, including those containing fillers, and
tionary statements are given in Sections 6, 9, and 24.
all provide corrections for the inert fillers present in some of
those compounds.
2. Referenced Documents
1.2 TestMethodA,whichpermitsmostcompleteextraction
2
2.1 ASTM Standards:
in least time, is to be used for referee tests, but two alternative
D297Test Methods for Rubber Products—ChemicalAnaly-
nonreferee Test Methods B and C are also described. Test
sis
Method B differs from the referee test method only in sample
D618Practice for Conditioning Plastics for Testing
preparation;thatis,itrequiresuseofshavingstakenatselected
D883Terminology Relating to Plastics
points in cable insulation, for example, rather than the ground
D1603Test Method for Carbon Black Content in Olefin
samplerequiredbytherefereetestmethod.Becausetheshaved
Plastics
particles are larger, less total surface per sample is exposed to
D1998SpecificationforPolyethyleneUprightStorageTanks
the extractant, so this test method ordinarily yields extraction
D3351Test Method for Gel Count of Plastic Film (With-
values about 1 to 2% lower than the referee method. Test
3
drawn 2000)
MethodCrequiresthataspecimeninonepiecebeextractedin
E691Practice for Conducting an Interlaboratory Study to
xylenesataconstanttemperatureof110°C.Atthistemperature
Determine the Precision of a Test Method
and with a one-piece specimen, even less extraction occurs
2.2 ISO Standard:
(from 3 to 9% less than the referee test method), this method
ISO10147 Pipes and Fittings Made of Crosslinked Poly-
permits swell ratio (a measure of the degree of crosslinking in
ethylene (Pe-X)—Estimation of the Degree of Crosslink-
the gel phase) be determined.
ing by Determination of the Gel Content
1.3 Extraction tests are made on articles of any shape.They
have been particularly useful for electrical insulations since
3. Terminology
specimenscanbeselectedfromthoseportionsoftheinsulation
3.1 Definitions of Terms Specific to This Standard:
most susceptible to insufficient crosslinking.
3.1.1 gel content—the percentage by mass of polymer
1.4 The values stated in either SI units or inch-pound units
insoluble in a specified solvent after extraction under the
are to be regarded separately as standard. The values stated in
specified conditions.
each system may not be exact equivalents; therefore, each
3.1.2 swell ratio—the ratio of the gel volume in the swollen
system shall be used independently of the other. Combining
state to its volume in the unswollen state.
values from the two systems may result in non-conformance
3.2 Terms as shown in Terminology D883 are applicable to
with the standard.
this test method.
NOTE 1—This test method is equivalent to ISO10147, Method B. It is
1 2
These test methods are under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
PlasticsandarethedirectresponsibilityofSubcommitteeD20.15onThermoplastic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials. Standards volume information, refer to the standard’s Document Summary page on
CurrenteditionapprovedSept.1,2016.PublishedSeptember1,2016.Originally the ASTM website.
3
approved in 1968. Last previous edition approved in 2011 as D2765–11. DOI: The last approved version of this historical standard is referenced on
10.1520/D2765-16. www.astm.org.
*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. U
...
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: D2765 − 11 D2765 − 16
Standard Test Methods for
Determination of Gel Content and Swell Ratio of
1
Crosslinked Ethylene Plastics
This standard is issued under the fixed designation D2765; 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 The gel content (insoluble fraction) produced in ethylene plastics by crosslinking is determined by extracting with solvents
such as decahydronaphthalene or xylenes. The methods described herein are applicable to crosslinked ethylene plastics of all
densities, including those containing fillers, and all provide corrections for the inert fillers present in some of those compounds.
1.2 Test Method A, which permits most complete extraction in least time, is to be used for referee tests, but two alternative
nonreferee Test Methods B and C are also described. Test Method B differs from the referee test method only in sample
preparation; that is, it requires use of shavings taken at selected points in cable insulation, for example, rather than the ground
sample required by the referee test method. Because the shaved particles are larger, less total surface per sample is exposed to the
extractant, so this test method ordinarily yields extraction values about 1 to 2 % lower than the referee method. Test Method C
requires that a specimen in one piece be extracted in xylenes at a constant temperature of 110°C. At this temperature and with a
one-piece specimen, even less extraction occurs (from 3 to 9 % less than the referee test method), this method permits swell ratio
(a measure of the degree of crosslinking in the gel phase) be determined.
1.3 Extraction tests are made on articles of any shape. They have been particularly useful for electrical insulations since
specimens maycan be selected from those portions of the insulation most susceptible to insufficient crosslinking.
1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The inch-pound units in
brackets are for information only.values stated in each system may not be
NOTE 1—Method B of this test method is equivalent to ISO 10147.exact equivalents; therefore, each system shall be used independently
of the other. Combining values from the two systems may result in non-conformance with the standard.
NOTE 1—This test method is equivalent to ISO 10147, Method B. It is not equivalent to ISO 10147 in any other measurement or section.
1.5 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 Sections 6, 109, and 2524.
2. Referenced Documents
2
2.1 ASTM Standards:
D297 Test Methods for Rubber Products—Chemical Analysis
D618 Practice for Conditioning Plastics for Testing
D883 Terminology Relating to Plastics
D1603 Test Method for Carbon Black Content in Olefin Plastics
D1998 Specification for Polyethylene Upright Storage Tanks
3
D3351 Test Method for Gel Count of Plastic Film (Withdrawn 2000)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 ISO Standard:
ISO 10147 Pipes and Fittings Made of Crosslinked Polyethylene (Pe-X)—Estimation of the Degree of Crosslinking by
Determination of the Gel Content
1
These test methods are under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
Current edition approved Sept. 1, 2011Sept. 1, 2016. Published September 1, 2011September 1, 2016. Originally approved in 1968. Last previous edition approved in
20062011 as D2765 – 01D2765 – 11.(2006). DOI: 10.1520/D2765-11.10.1520/D2765-16.
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co
...
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: D2765 − 16
Standard Test Methods for
Determination of Gel Content and Swell Ratio of
1
Crosslinked Ethylene Plastics
This standard is issued under the fixed designation D2765; 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.
not equivalent to ISO 10147 in any other measurement or section.
1. Scope*
1.5 This standard does not purport to address all of the
1.1 The gel content (insoluble fraction) produced in ethyl-
safety concerns, if any, associated with its use. It is the
ene plastics by crosslinking is determined by extracting with
responsibility of the user of this standard to establish appro-
solvents such as decahydronaphthalene or xylenes. The meth-
priate safety and health practices and determine the applica-
ods described herein are applicable to crosslinked ethylene
bility of regulatory limitations prior to use. Specific precau-
plastics of all densities, including those containing fillers, and
tionary statements are given in Sections 6, 9, and 24.
all provide corrections for the inert fillers present in some of
those compounds.
2. Referenced Documents
1.2 Test Method A, which permits most complete extraction
2
2.1 ASTM Standards:
in least time, is to be used for referee tests, but two alternative
D297 Test Methods for Rubber Products—Chemical Analy-
nonreferee Test Methods B and C are also described. Test
sis
Method B differs from the referee test method only in sample
D618 Practice for Conditioning Plastics for Testing
preparation; that is, it requires use of shavings taken at selected
D883 Terminology Relating to Plastics
points in cable insulation, for example, rather than the ground
D1603 Test Method for Carbon Black Content in Olefin
sample required by the referee test method. Because the shaved
Plastics
particles are larger, less total surface per sample is exposed to
D1998 Specification for Polyethylene Upright Storage Tanks
the extractant, so this test method ordinarily yields extraction
D3351 Test Method for Gel Count of Plastic Film (With-
values about 1 to 2 % lower than the referee method. Test
3
drawn 2000)
Method C requires that a specimen in one piece be extracted in
E691 Practice for Conducting an Interlaboratory Study to
xylenes at a constant temperature of 110°C. At this temperature
Determine the Precision of a Test Method
and with a one-piece specimen, even less extraction occurs
2.2 ISO Standard:
(from 3 to 9 % less than the referee test method), this method
ISO 10147 Pipes and Fittings Made of Crosslinked Poly-
permits swell ratio (a measure of the degree of crosslinking in
ethylene (Pe-X)—Estimation of the Degree of Crosslink-
the gel phase) be determined.
ing by Determination of the Gel Content
1.3 Extraction tests are made on articles of any shape. They
have been particularly useful for electrical insulations since
3. Terminology
specimens can be selected from those portions of the insulation
3.1 Definitions of Terms Specific to This Standard:
most susceptible to insufficient crosslinking.
3.1.1 gel content—the percentage by mass of polymer
1.4 The values stated in either SI units or inch-pound units
insoluble in a specified solvent after extraction under the
are to be regarded separately as standard. The values stated in
specified conditions.
each system may not be exact equivalents; therefore, each
3.1.2 swell ratio—the ratio of the gel volume in the swollen
system shall be used independently of the other. Combining
state to its volume in the unswollen state.
values from the two systems may result in non-conformance
3.2 Terms as shown in Terminology D883 are applicable to
with the standard.
this test method.
NOTE 1—This test method is equivalent to ISO 10147, Method B. It is
1 2
These test methods are under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and are the direct responsibility of Subcommittee D20.15 on Thermoplastic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Sept. 1, 2016. Published September 1, 2016. Originally the ASTM website.
3
approved in 1968. Last previous edition approved in 2011 as D2765 – 11. DOI: The last approved version of this historical standard is referenced on
10.1520/D2765-16. www.astm.org.
*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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