ASTM D5380-93(2014)
(Test Method)Standard Test Method for Identification of Crystalline Pigments and Extenders in Paint by X-Ray Diffraction Analysis
Standard Test Method for Identification of Crystalline Pigments and Extenders in Paint by X-Ray Diffraction Analysis
SIGNIFICANCE AND USE
4.1 The choice of pigments and extenders influences the appearance, durability, cost, and other properties of paint. This test method is a convenient way, and probably the most reliable, to identify pigments in paint.
SCOPE
1.1 This test method covers the identification of crystalline pigments and extenders in liquid paint and dry paint film. It is applicable to both water-reducible and solvent-reducible paint. It also may be used to identify pigment and extender in grind paste or alone as dry powder. It is not applicable to amorphous components such as carbon black, amorphous silica, or highly processed clay.
1.2 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 6.
General Information
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Designation:D5380 −93 (Reapproved 2014)
Standard Test Method for
Identification of Crystalline Pigments and Extenders in Paint
1
by X-Ray Diffraction Analysis
This standard is issued under the fixed designation D5380; 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 on comparison of the diffraction pattern of the sample with
3,4,5
reference patterns of standards.
1.1 This test method covers the identification of crystalline
pigments and extenders in liquid paint and dry paint film. It is
4. Significance and Use
applicable to both water-reducible and solvent-reducible paint.
4.1 The choice of pigments and extenders influences the
It also may be used to identify pigment and extender in grind
appearance, durability, cost, and other properties of paint.This
paste or alone as dry powder. It is not applicable to amorphous
test method is a convenient way, and probably the most
components such as carbon black, amorphous silica, or highly
reliable, to identify pigments in paint.
processed clay.
5. Apparatus
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
5.1 X-ray Diffractometer, suitable for collecting intensity
standard.
versus two theta (20) angle diffraction patterns in the range
from 5° to 65° 20. It is preferred that the diffractometer be
1.3 This standard does not purport to address all of the
equippedwithacoppertargetX-raytubeandamonochromator
safety concerns, if any, associated with its use. It is the
that passes only copper K-alpha radiation. If a monochromator
responsibility of the user of this standard to establish appro-
is not available, then a suitable filter may be used to remove
priate safety and health practices and determine the applica-
copper K-beta radiation from the diffracted X-ray beam. A
bility of regulatory limitations prior to use. Specific hazard
nickel filter may be used for this purpose when a copper target
statements are given in Section 6.
tube is employed.
2. Referenced Documents
NOTE 1—Follow the recommendations of the manufacturer of the
2
diffractometer used.
2.1 ASTM Standards:
D3925Practice for Sampling Liquid Paints and Related
5.2 Liquid Paint or Grind Paste:
Pigmented Coatings
5.2.1 Paint Shaker.
5.2.2 Film Applicator, that will produce a 3- to 10-mil (75-
3. Summary of Test Method
to 250 µm) wet film thickness.
5.2.3 Plastic Sheet, such as polyester film, that contains no
3.1 Every crystalline substance, in this case pigment or
crystalline components that would produce interfering X-ray
extender, has a characteristic X-ray diffraction pattern.
diffraction peaks and is not attacked by paint solvent.
Whether the substance is present alone or in a mixture, it
5.2.4 Perforated Suction Plate or other flat surface.
produces its pattern independently and can be identified by it.
An X-ray diffraction pattern of a sample is recorded. Each
5.3 Paint Chips or Pigment Powder:
crystalline substance in the sample is identified by the
5.3.1 Miniature Reciprocating Ball Mill.
Hanawalt or Fink method or other systematic procedure based
5.3.2 Stainless Steel Vials, with agitator for ball mill.
5.3.3 Powder Specimen Holders, for X-ray diffractometer.
6. Hazards
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
6.1 Precaution—As exposure to excessive quantities of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
X-radiation is injurious to health, X-ray producing equipment
CurrenteditionapprovedJuly1,2014.PublishedJuly2014.Originallyapproved
in 1993. Last previous edition approved in 2009 as D5280–93(2009). DOI:
3
10.1520/D5380-93R0914. Search Manual, (Hanawalt), “Inorganic Phases,” International Centre for
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DiffractionData,(ICDD),CatalogNo.HA42,NewtownSquareCorporateCampus,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 12 Campus Blvd., Newtown Square, PA 19073-3273.
4
Standards volume information, refer to the standard’s Document Summary page on Search Manual, (Fink), “Inorganic Phases,” ICDD.
5
the ASTM website. “Powder Diffraction File, Inorganic,” ICDD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5380−93 (2014)
diffracted from the substrate reach the detector, the diffraction pattern of
can be dangerous to both the operator and persons in the
the substrate.
i
...
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: D5380 − 93 (Reapproved 2009) D5380 − 93 (Reapproved 2014)
Standard Test Method for
Identification of Crystalline Pigments and Extenders in Paint
1
by X-Ray Diffraction Analysis
This standard is issued under the fixed designation D5380; 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 This test method covers the identification of crystalline pigments and extenders in liquid paint and dry paint film. It is
applicable to both water-reducible and solvent-reducible paint. It also may be used to identify pigment and extender in grind paste
or alone as dry powder. It is not applicable to amorphous components such as carbon black, amorphous silica, or highly processed
clay.
1.2 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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 6.
2. Referenced Documents
2
2.1 ASTM Standards:
D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings
3. Summary of Test Method
3.1 Every crystalline substance, in this case pigment or extender, has a characteristic X-ray diffraction pattern. Whether the
substance is present alone or in a mixture, it produces its pattern independently and can be identified by it. An X-ray diffraction
pattern of a sample is recorded. Each crystalline substance in the sample is identified by the Hanawalt or Fink method or other
3,4,5
systematic procedure based on comparison of the diffraction pattern of the sample with reference patterns of standards.
4. Significance and Use
4.1 The choice of pigments and extenders influences the appearance, durability, cost, and other properties of paint. This test
method is a convenient way, and probably the most reliable, to identify pigments in paint.
5. Apparatus
5.1 X-ray Diffractometer, suitable for collecting intensity versus two theta (20) angle diffraction patterns in the range from 5°
to 65° 20. It is preferred that the diffractometer be equipped with a copper target X-ray tube and a monochromator that passes only
copper K-alpha radiation. If a monochromator is not available, then a suitable filter may be used to remove copper K-beta radiation
from the diffracted X-ray beam. A nickel filter may be used for this purpose when a copper target tube is employed.
NOTE 1—Follow the recommendations of the manufacturer of the diffractometer used.
5.2 Liquid Paint or Grind Paste:
5.2.1 Paint Shaker.
1
This test method 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 Feb. 1, 2009July 1, 2014. Published February 2009July 2014. Originally approved in 1993. Last previous edition approved in 20032009 as
D5280 - 93 (2003).D5280 – 93 (2009). DOI: 10.1520/D5380-93R09.10.1520/D5380-93R0914.
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
Search Manual, (Hanawalt), “Inorganic Phases,” International Centre for Diffraction Data, (ICDD), Catalog No. HA 42, Newtown Square Corporate Campus, 12 Campus
Blvd., Newtown Square, PA 19073-3273.
4
Search Manual, (Fink), “Inorganic Phases,” ICDD.
5
“Powder Diffraction File, Inorganic,” ICDD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5380 − 93 (2014)
5.2.2 Film Applicator, that will produce a 3- to 10-mil (75- to 250 μm) wet film thickness.
5.2.3 Plastic Sheet, such as polyester film, that contains no crystalline components that would produce interfering X-ray
diffraction peaks and is not attacked by paint solvent.
5.2.4 Perforated Suction Plate or other flat surface.
5.3 Paint Chips or Pigment Powder:
5.3.1 Miniature Reci
...
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