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ASTM D8154-17

(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.

General Information

Status
Historical
Publication Date
31-Oct-2017
ICS
91.100.50 - Binders. Sealing materials
Technical Committee
D08 - Roofing and Waterproofing
Drafting Committee
D08.18 - Nonbituminous Organic Roof Coverings
Current Stage
Ref Project

Relations

Replaced By
ASTM D8154-17e1 - Standard Test Methods for <sup>1</sup>H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
Effective Date
01-Nov-2017

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ASTM D8154-17 - Standard Test Methods for <sup>1</sup>H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing FabricsASTM D8154-17 - Standard Test Methods for <sup>1</sup>H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
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ASTM D8154-17 - Standard Test Methods for <sup>1</sup>H-NMR Determination of Ketone-Ethylene-Ester and Polyvinyl Chloride Contents in KEE-PVC Roofing Fabrics
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Standards Content (Sample)

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:D8154 −17
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
3.1 Definitions—Terminology D1079 and Specification
1.1 This test method pertains to the determination of the
D6754/D6754M shall apply to this test method.
relative contents of Ketone-Ethylene-Ester (KEE) and Polyvi-
nyl Chloride (PVC) after their extraction from reinforced
4. Summary of Test Method
roofing membranes, or fabrics. Based on Proton Nuclear
1
Magnetic Resonance Spectroscopy ( H-NMR), the method
4.1 Test Methods—There are two related test methods to
allowsforthequantificationofPVCwithrespecttoaninternal
quantify PVC and KEE in roofing fabrics. In both methods the
standard.The KEE content is then obtained by difference.The
polymer blend is extracted from the fabric and purified by a
test method is not applicable to membranes or blends that
series of dissolution, centrifugation, and precipitation. After
contain high molecular weight polymers other than PVC and
drying, the blend is dissolved in deuterated tetrahydrofuran
1
KEE.
along with a H-NMR internal standard. In Method A, PVC
1
contentisquantifiedbycomparingits H-NMRsignalwiththat
1.2 Units—The values stated in SI units are to be regarded
of the internal standard, and KEE is obtained by difference.
asstandard.Nootherunitsofmeasurementareincludedinthis
Method B adds to Method A a calibration curve the slope of
standard.
which providing for a correction factor. This correction factor
1.3 This standard does not purport to address all of the
is applied to the polymer content obtained by Method A to
safety concerns, if any, associated with its use. It is the
provide for greater precision on the PVC and KEE contents.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
5. Significance and Use
mine the applicability of regulatory limitations prior to use.
5.1 Determination of the percentage of KEE compound in
1.4 This international standard was developed in accor-
sheet roofing is of concern to many specifiers and building
dance with internationally recognized principles on standard-
owners. Method A, the faster method, is best used for quality
ization established in the Decision on Principles for the
control. Method B may apply better to research and
Development of International Standards, Guides and Recom-
development, or investigative work.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
6. Interferences
6.1 The NMR analysis of the polymer blend extracted from
2. Referenced Documents
the sheet roofing is sensitive to impurities, including
2
2.1 ASTM Standards:
plasticizer, filler, reinforcement, and trace solvent (other than
D1079Terminology Relating to Roofing and Waterproofing
the NMR solvent). The procedure here is meant to purify the
D6754/D6754MSpecification for Ketone Ethylene Ester
blend for proper analysis.
Based Sheet Roofing
7. Equipment and Apparatus
7.1 Glassware. Erlenmeyer flask and stopper, 125 mL.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD08onRoofing
Weighing bottle, 25 mL.
and Waterproofing and is the direct responsibility of Subcommittee D08.18 on
Nonbituminous Organic Roof Coverings. 7.2 Porcelain ware. Büchner funnel, 10 cm in diameter.
Current edition approved Nov. 1, 2017. Published November 2017. DOI:
7.3 Platform shaker. Must accept 125 mL Erlenmeyer, and
10.1520/D8154-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or allow for swirling at 120 to 150 rpm.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.4 Metal spatula.Tostirthesuspensionduringtheprecipi-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tation step.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8154−17
7.5 Pasteur pipettes. To transfer solubilized polymer and details. Centrifugation flasks must be resistant to the fluid
solvent from one flask to another. being used and must not swell.
9.3 Magnetic Fields—NMR spectroscopy involves strong
7.6 Centrifuge. Capable of 10 000 RPM.
magnetic fields. Analysis by NMR requires safety and equip-
7.7 Centrifuge tubes. 50 mL. Must be resistant to THF, for
ment training. Follow local laboratory gu
...

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