ASTM D3168-85(2016)
(Practice)Standard Practice for Qualitative Identification of Polymers in Emulsion Paints
Standard Practice for Qualitative Identification of Polymers in Emulsion Paints
SIGNIFICANCE AND USE
5.1 Identification of specific acrylic polymers in emulsion paints is often difficult or impossible by infrared alone. This is particularly true when the acrylic is present in a small amount as a comonomer with vinyl acetate, or when blended with alkyds or other ester systems. If identification of an acrylic component is required in such a system, it may often be accomplished by gas-liquid chromatographic analysis of the pyrolyzed paint film. The presence of a number of other polymers may often also be confirmed by pyrolysis since they produce characteristic and reproducible pyrograms.
5.2 The pyrograms obtained from unknown samples vary in complexity according to the sample composition. It is necessary to establish the presence or absence of as many components as possible from a study of the infrared spectra obtained in the first part of this practice. The gas-liquid chromatography results may then be used to help identify any unknown components present and to confirm identifications made by infrared.
SCOPE
1.1 This practice describes a procedure for the qualitative identification in emulsion paints of most types of polymers present as major components of the paint vehicle. Limitations are discussed in Sections 5 and 10.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
General Information
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Designation:D3168 −85 (Reapproved 2016)
Standard Practice for
1
Qualitative Identification of Polymers in Emulsion Paints
This standard is issued under the fixed designation D3168; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope obtainedandcomparedwithreferencespectraforidentification
of major components.
1.1 This practice describes a procedure for the qualitative
identification in emulsion paints of most types of polymers 4.2 The paint is applied to a filament and pyrolyzed to
present as major components of the paint vehicle. Limitations depolymerizethevehicle.Aninternalstandardisaddedandthe
are discussed in Sections 5 and 10. pyrolyzate is separated into its components by gas-liquid
chromatography. Monomers are identified by comparison of
1.2 The values stated in SI units are to be regarded as the
relative retention times.
standard. The values given in parentheses are for information
only.
5. Significance and Use
1.3 This standard does not purport to address all of the
5.1 Identification of specific acrylic polymers in emulsion
safety concerns, if any, associated with its use. It is the
paints is often difficult or impossible by infrared alone. This is
responsibility of the user of this standard to establish appro-
particularly true when the acrylic is present in a small amount
priate safety and health practices and determine the applica-
as a comonomer with vinyl acetate, or when blended with
bility of regulatory limitations prior to use.
alkyds or other ester systems. If identification of an acrylic
component is required in such a system, it may often be
2. Referenced Documents
accomplished by gas-liquid chromatographic analysis of the
2
2.1 ASTM Standards:
pyrolyzed paint film. The presence of a number of other
D16TerminologyforPaint,RelatedCoatings,Materials,and
polymers may often also be confirmed by pyrolysis since they
Applications
produce characteristic and reproducible pyrograms.
D1193Specification for Reagent Water
5.2 Thepyrogramsobtainedfromunknownsamplesvaryin
D2621Test Method for Infrared Identification of Vehicle
complexity according to the sample composition. It is neces-
Solids From Solvent-Reducible Paints
sary to establish the presence or absence of as many compo-
E275PracticeforDescribingandMeasuringPerformanceof
nents as possible from a study of the infrared spectra obtained
Ultraviolet and Visible Spectrophotometers
inthefirstpartofthispractice.Thegas-liquidchromatography
results may then be used to help identify any unknown
3. Terminology
components present and to confirm identifications made by
3.1 Definitions—For definitions of terms, refer to Terminol-
infrared.
ogy D16.
6. Interferences
4. Summary of Practice
6.1 Dibutylmaleateanddibutylfumaratemonomersarenot
successfully recovered by this procedure. If their presence is
4.1 The vehicle is extracted from the dried paint and after
suspected as comonomer in a vinyl acetate copolymer system,
filtering is cast on a salt plate. The infrared spectrum is
n-butyl alcohol should be found in the pyrolyzate. This
evidence, together with the absence of butyl acrylate or butyl
methacrylate monomer peaks, is an indirect indication of the
1
This practice is under the jurisdiction of ASTM Committee D01 on Paint and
presence of one or both of these monomers.
Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
6.2 The presence of relatively low quantities of copolymer-
Current edition approved April 1, 2016. Published April 2016. Originally
ized acids may not be successfully established by this
approved in 1973. Last previous edition approved in 2011 as D3168–85(2011).
DOI: 10.1520/D3168-85R16.
procedure, due to some unavoidable decomposition of acrylate
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and methacrylate esters to acrylic or methacrylic acid and the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
corresponding alcohols during the pyrolysis. The infrared
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. spectrum and an acid number determination, both run on the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D3168−85 (2016)
polymer solids, may usually be relied upon to establish the 8.2 Purity of Water—Unless otherwise indicated
...
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: D3168 − 85 (Reapproved 2011) D3168 − 85 (Reapproved 2016)
Standard Practice for
1
Qualitative Identification of Polymers in Emulsion Paints
This standard is issued under the fixed designation D3168; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
1.1 This practice describes a procedure for the qualitative identification in emulsion paints of most types of polymers present
as major components of the paint vehicle. Limitations are discussed in Sections 5 and 10.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D16 Terminology for Paint, Related Coatings, Materials, and Applications
D1193 Specification for Reagent Water
D2621 Test Method for Infrared Identification of Vehicle Solids From Solvent-Reducible Paints
E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
3. Terminology
3.1 Definitions—For definitions of terms, refer to Terminology D16.
4. Summary of Practice
4.1 The vehicle is extracted from the dried paint and after filtering is cast on a salt plate. The infrared spectrum is obtained and
compared with reference spectra for identification of major components.
4.2 The paint is applied to a filament and pyrolyzed to depolymerize the vehicle. An internal standard is added and the
pyrolyzate is separated into its components by gas-liquid chromatography. Monomers are identified by comparison of relative
retention times.
5. Significance and Use
5.1 Identification of specific acrylic polymers in emulsion paints is often difficult or impossible by infrared alone. This is
particularly true when the acrylic is present in a small amount as a comonomer with vinyl acetate, or when blended with alkyds
or other ester systems. If identification of an acrylic component is required in such a system, it may often be accomplished by
gas-liquid chromatographic analysis of the pyrolyzed paint film. The presence of a number of other polymers may often also be
confirmed by pyrolysis since they produce characteristic and reproducible pyrograms.
5.2 The pyrograms obtained from unknown samples vary in complexity according to the sample composition. It is necessary
to establish the presence or absence of as many components as possible from a study of the infrared spectra obtained in the first
part of this practice. The gas-liquid chromatography results may then be used to help identify any unknown components present
and to confirm identifications made by infrared.
1
This practice is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved July 1, 2011April 1, 2016. Published July 2011April 2016. Originally approved in 1973. Last previous edition approved in 20052011 as
D3168 – 85 (2005).(2011). DOI: 10.1520/D3168-85R11.10.1520/D3168-85R16.
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 ----------------------
D3168 − 85 (2016)
6. Interferences
6.1 Dibutyl maleate and dibutyl fumarate monomers are not successfully recovered by this procedure. If their presence is
suspected as comonomer in a vinyl acetate copolymer system, n-butyl alcohol should be found in the pyrolyzate. This evidence,
together with the absence of butyl acrylate or butyl methacrylate monomer peaks, is an indirect indication of the presence of one
or both of these monomers.
6.2 The presence of relatively low quantities o
...
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