ASTM D5017-17
(Test Method)Standard Test Method for Determination of Linear Low Density Polyethylene (LLDPE) Composition by Carbon-13 Nuclear Magnetic Resonance
Standard Test Method for Determination of Linear Low Density Polyethylene (LLDPE) Composition by Carbon-13 Nuclear Magnetic Resonance
SIGNIFICANCE AND USE
5.1 Performance properties are dependent on the number and type of short chain branches. This test method permits measurement of these branches for ethylene copolymers with propylene, butene-1, hexene-1, octene-1, and 4-methylpentene-1.
SCOPE
1.1 This test method determines the molar composition of copolymers prepared from ethylene (ethene) and a second alkene-1 monomer. This second monomer can include propene, butene-1, hexene-1, octene-1, and 4-methylpentene-1.
1.2 Calculations of this test method are valid for products containing units EEXEE, EXEXE, EXXE, EXXXE, and of course EEE where E equals ethene and X equals alkene-1. Copolymers containing a considerable number of alkene-1 blocks (such as, longer blocks than XXX) are outside the scope of this test method.
1.3 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. See Section 8 for a specific hazard statement.
Note 1: There is no known ISO equivalent to this standard.
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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: D5017 − 17
Standard Test Method for
Determination of Linear Low Density Polyethylene (LLDPE)
1
Composition by Carbon-13 Nuclear Magnetic Resonance
This standard is issued under the fixed designation D5017; 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.
1. Scope* NMR) Spectrometers for Liquid Samples
IEEE/ASTM SI-10Standard for Use of the International
1.1 This test method determines the molar composition of
4
System of Units (SI): The Modern System
copolymers prepared from ethylene (ethene) and a second
alkene-1monomer.Thissecondmonomercanincludepropene,
3. Terminology
butene-1, hexene-1, octene-1, and 4-methylpentene-1.
3.1 Some units, symbols, and abbreviations used in this test
1.2 Calculations of this test method are valid for products
method are summarized in IEEE/ASTM SI-10 and Practice
containing units EEXEE, EXEXE, EXXE, EXXXE, and of
E386. Other abbreviations are listed as follows:
course EEE where E equals ethene and X equals alkene-1.
Copolymers containing a considerable number of alkene-1
3.2 Abbreviations:
13
blocks(suchas,longerblocksthanXXX)areoutsidethescope
3.2.1 C—carbon 13,
of this test method.
3.2.2 LLDPE—linear low-density polyethylene,
1.3 This standard does not purport to address all of the
3.2.3 T1—relaxation time, and
safety concerns, if any, associated with its use. It is the
3.2.4 TR—pulse repetition time.
responsibility of the user of this standard to establish appro-
3.3 Definitions of Terms Specific to This Standard:
priate safety and health practices and determine the applica-
3.3.1 With a few modifications, terms used to designate
5
bility of regulatory limitations prior to use. See Section 8 for a
different carbon types were suggested by Carman. Methine
specific hazard statement.
carbons are identified by CH and branch carbons are labeled
according to branch type as summarized in Table 1. Branch
NOTE 1—There is no known ISO equivalent to this standard.
carbons are numbered starting with the methyl as number one.
2. Referenced Documents
3.3.2 Backbone methylene carbons are designated by a pair
2
ofGreeklettersthatspecifythelocationofthenearestmethine
2.1 ASTM Standards:
carbonineachdirection.Forexample,α,α-methylenecarbonis
D883Terminology Relating to Plastics
+
between two methine carbons or an α,δ methylene carbon has
E177Practice for Use of the Terms Precision and Bias in
one immediate methine neighbor and the second methine
ASTM Test Methods
carbon is located at least four carbons away.
E386Practice for Data Presentation Relating to High-
Resolution Nuclear Magnetic Resonance (NMR) Spec-
3
4. Summary of Test Method
troscopy (Withdrawn 2015)
E691Practice for Conducting an Interlaboratory Study to
4.1 Polymer samples are dispersed in hot solvent and
Determine the Precision of a Test Method
analyzed at high temperatures using Carbon-13 nuclear mag-
E2977PracticeforMeasuringandReportingPerformanceof
netic resonance (NMR) spectroscopy.
Fourier-Transform Nuclear Magnetic Resonance (FT-
4.2 Spectra are recorded under conditions such that the
response of each chemically different carbon is identical.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
Integrated responses for carbons originated from the different
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
comonomers are used for calculation of the copolymer com-
Current edition approved March 1, 2017. Published March 2017. Originally
ε1 position.
approved in 1991. Last previous edition approved in 2009 as D5017–96(2009) .
DOI: 10.1520/D5017-17.
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
4
Standards volume information, refer to the standard’s Document Summary page on Available from ASTM International Headquarters, 100 Barr Harbor Drive,
the ASTM website. C700, West Conshohocken, PA 19428.
3 5
The last approved version of this historical standard is referenced on Carman,C.J.,Harrington,R.A.,andWilkes,C.E., Macromolecules1977,Vol
www.astm.org. 10, p. 536.
*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 ----------------------
D5017 − 17
−1
TABLE 1 Designations for Different Carbon Types
9.8 Pulse width, <[4×sweep width Hz]
Monomer Branch Type
...
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.
´1
Designation: D5017 − 96 (Reapproved 2009) D5017 − 17
Standard Test Method for
Determination of Linear Low Density Polyethylene (LLDPE)
1
Composition by Carbon-13 Nuclear Magnetic Resonance
This standard is issued under the fixed designation D5017; 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
ε NOTE—Reapproved with editorial changes in April 2009.
1. Scope Scope*
1.1 This test method determines the molar composition of copolymers prepared from ethylene (ethene) and a second alkene-1
monomer. This second monomer can include propene, butene-1, hexene-1, octene-1, and 4-methylpentene-1.
1.2 Calculations of this test method are valid for products containing units EEXEE, EXEXE, EXXE, EXXXE, and of course
EEE where E equals ethene and X equals alkene-1. Copolymers containing a considerable number of alkene-1 blocks (such as,
longer blocks than XXX) are outside the scope of this test method.
1.3 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. See Section 8 for a specific hazard statement.
NOTE 1—There is no equivalent ISO known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E386 Practice for Data Presentation Relating to High-Resolution Nuclear Magnetic Resonance (NMR) Spectroscopy
3
(Withdrawn 2015)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2977 Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR)
Spectrometers for Liquid Samples
4
IEEE/ASTM SI-10 Standard for Use of the International System of Units (SI): The Modern System
3. Terminology
3.1 Some units, symbols, and abbreviations used in this test method are summarized in IEEE/ASTM SI-10 and Practice E386.
Other abbreviations are listed as follows:
3.2 Abbreviations:
13
3.2.1 C—carbon 13,
3.2.2 LLDPE—linear low-density polyethylene,
3.2.3 T1—relaxation time, and
3.2.4 TR—pulse repetition time.
3.3 Definitions of Terms Specific to This Standard:
5
3.3.1 With a few modifications, terms used to designate different carbon types were suggested by Carman. Methine carbons
are identified by CH and branch carbons are labeled according to branch type as summarized in Table 1. Branch carbons are
numbered starting with the methyl as number one.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved April 1, 2009March 1, 2017. Published June 2009March 2017. Originally approved in 1991. Last previous edition approved in 20032009 as
ε1
D5017 – 96(2003)(2009) . DOI: 10.1520/D5017-96R09E01.10.1520/D5017-17.
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.
4
Available from ASTM International Headquarters, 100 Barr Harbor Drive, C700, West Conshohocken, PA 19428.
5
Carman, C. J., Harrington, R. A., and Wilkes, C. E., Macromolecules 1977, Vol 10, p. 536.
*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 ----------------------
D5017 − 17
TABLE 1 Designations for Different Carbon Types
Monomer Branch Type Label
Propene (P) methyl M1
Butene-1 (B) ethyl E1–E2
Hexene-1 (H) butyl B1–B4
4-Methylpentene-1 (MP) isobutyl IB1–IB3
Octene-1 (O) hexyl H1–H6
3.3.2 Backbone methylene carbons are designated by a pair of Greek letters that specify the location of the nearest methine
+
carbon in each direction. For example, α,α-methylene carbon is between two methine carbons or an α,δ methylene carbon has one
immediate methine neighbor and the second methine carbon i
...
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