ASTM D8154-24
(Test Method)Standard Test Methods for 1H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
Standard Test Methods for <sup>1</sup>H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
SIGNIFICANCE AND USE
5.1 Determination of the percentage of KEE compound in sheet roofing is of concern to many specifiers and building owners. Method A, the faster method, is best used for quality control. Method B may apply better to research and development or investigative work.
SCOPE
1.1 This test method pertains to the determination of the relative contents of ketone-ethylene-ester (KEE) and polyvinyl chloride (PVC) after their extraction from reinforced roofing membranes or fabrics. Based on proton nuclear magnetic resonance spectroscopy (1H-NMR), the method allows for the quantification of PVC with respect to an internal standard. The KEE content is then obtained by difference. The test method is not applicable to membranes or blends that contain high molecular weight polymers other than PVC and KEE.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 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.
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Standards Content (Sample)
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: D8154 − 24
Standard Test Methods for
1
H-NMR Determination of Ketone-Ethylene-Ester and
1
Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
This standard is issued under the fixed designation D8154; 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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method pertains to the determination of the
relative contents of ketone-ethylene-ester (KEE) and polyvinyl
3. Terminology
chloride (PVC) after their extraction from reinforced roofing
3.1 Definitions—Terminology D1079 and Specification
membranes or fabrics. Based on proton nuclear magnetic
1
D6754/D6754M shall apply to this test method.
resonance spectroscopy ( H-NMR), the method allows for the
quantification of PVC with respect to an internal standard. The
4. Summary of Test Method
KEE content is then obtained by difference. The test method is
not applicable to membranes or blends that contain high
4.1 Test Methods—There are two related test methods to
molecular weight polymers other than PVC and KEE.
quantify PVC and KEE in roofing fabrics. In both methods, the
polymer blend is extracted from the fabric and purified by a
1.2 Units—The values stated in SI units are to be regarded
series of dissolution, centrifugation, and precipitation. After
as standard. No other units of measurement are included in this
drying, the blend is dissolved in deuterated tetrahydrofuran
standard.
1
along with a H-NMR internal standard. In Method A, PVC
1.3 This standard does not purport to address all of the
1
content is quantified by comparing its H-NMR signal with that
safety concerns, if any, associated with its use. It is the
of the internal standard, and KEE is obtained by difference.
responsibility of the user of this standard to establish appro-
Method B adds to Method A a calibration curve the slope of
priate safety, health, and environmental practices and deter-
which providing for a correction factor. This correction factor
mine the applicability of regulatory limitations prior to use.
is applied to the polymer content obtained by Method A to
1.4 This international standard was developed in accor-
provide for greater precision on the PVC and KEE contents.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Significance and Use
Development of International Standards, Guides and Recom-
5.1 Determination of the percentage of KEE compound in
mendations issued by the World Trade Organization Technical
sheet roofing is of concern to many specifiers and building
Barriers to Trade (TBT) Committee.
owners. Method A, the faster method, is best used for quality
control. Method B may apply better to research and develop-
2. Referenced Documents
2 ment or investigative work.
2.1 ASTM Standards:
D1079 Terminology Relating to Roofing and Waterproofing
6. Interferences
D6754/D6754M Specification for Ketone Ethylene Ester
6.1 The NMR analysis of the polymer blend extracted from
Based Sheet Roofing
the sheet roofing is sensitive to impurities, including
E177 Practice for Use of the Terms Precision and Bias in
plasticizer, filler, reinforcement, and trace solvent (other than
ASTM Test Methods
the NMR solvent). The procedure here is meant to purify the
blend for proper analysis.
1
This test method is under the jurisdiction of ASTM Committee D08 on Roofing
and Waterproofing and is the direct responsibility of Subcommittee D08.18 on
7. Equipment and Apparatus
Nonbituminous Organic Roof Coverings.
Current edition approved Jan. 1, 2024. Published January 2024. Originally 7.1 Glassware. Erlenmeyer flask and stopper, 125 mL.
approved in 2017. Last previous edition approved in 2017 as D8154 – 17. DOI:
Weighing bottle, 25 mL.
10.1520/D8154-24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 7.2 Porcelain ware. Büchner funnel, 10 cm in diameter.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.3 Platform shaker. Must accept 125 mL Erlenmeyer, and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. allow for swirling at 120 to 150 rpm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D8154 − 24
7.4 Metal spatula. To stir the suspensio
...
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: D8154 − 17 D8154 − 24
Standard Test Methods for
1
H-NMR Determination of Ketone-Ethylene-Ester and
1
Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
This standard is issued under the fixed designation D8154; 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—Editorially added Research Report information in April 2019.
1. Scope
1.1 This test method pertains to the determination of the relative contents of Ketone-Ethylene-Esterketone-ethylene-ester (KEE)
and Polyvinyl Chloridepolyvinyl chloride (PVC) after their extraction from reinforced roofing membranes,membranes or fabrics.
1
Based on Proton Nuclear Magnetic Resonance Spectroscopyproton nuclear magnetic resonance spectroscopy ( H-NMR), the
method allows for the quantification of PVC with respect to an internal standard. The KEE content is then obtained by difference.
The test method is not applicable to membranes or blends that contain high molecular weight polymers other than PVC and KEE.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1079 Terminology Relating to Roofing and Waterproofing
D6754/D6754M Specification for Ketone Ethylene Ester Based Sheet Roofing
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions—Terminology D1079 and Specification D6754/D6754M shall apply to this test method.
1
This test method is under the jurisdiction of ASTM Committee D08 on Roofing and Waterproofing and is the direct responsibility of Subcommittee D08.18 on
Nonbituminous Organic Roof Coverings.
Current edition approved Nov. 1, 2017Jan. 1, 2024. Published November 2017January 2024. Originally approved in 2017. Last previous edition approved in 2017 as
D8154 – 17. DOI: 10.1520/D8154-17E01.10.1520/D8154-24.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D8154 − 24
4. Summary of Test Method
4.1 Test Methods—There are two related test methods to quantify PVC and KEE in roofing fabrics. In both methods, the polymer
blend is extracted from the fabric and purified by a series of dissolution, centrifugation, and precipitation. After drying, the blend
1
is dissolved in deuterated tetrahydrofuran along with a H-NMR internal standard. In Method A, PVC content is quantified by
1
comparing its H-NMR signal with that of the internal standard, and KEE is obtained by difference. Method B adds to Method
A a calibration curve the slope of which providing for a correction factor. This correction factor is applied to the polymer content
obtained by Method A to provide for greater precision on the PVC and KEE contents.
5. Significance and Use
5.1 Determination of the percentage of KEE compound in sheet roofing is of concern to many specifiers and building owners.
Method A, the faster method, is best used for quality control. Method B may apply better to research and development,development
or investigative work.
6. Interferences
6.1 The NMR analysis of the polymer blend extracted from the sheet roofing is sensitive to impurities, including plasticizer, filler,
reinforcement, and trace solvent (other than the NMR solvent). The procedure h
...
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