ASTM_D_5380_-_93_2021.pdf

Designation:D538093(Reapproved 2021)Standard Test Method forIdentification of Crystalline Pigments and Extenders in Paintby X-Ray Diffraction Analysis1This standard is issued under the fixed designation D5380;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the identification of crystallinepigments and extenders in liquid paint and dry paint film.It isapplicable to both water-reducible and solvent-reducible paint.It also may be used to identify pigment and extender in grindpaste or alone as dry powder.It is not applicable to amorphouscomponents such as carbon black,amorphous silica,or highlyprocessed clay.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific hazard statements are given in Section 6.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D3925 Practice for Sampling Liquid Paints and RelatedPigmented Coatings3.Summary of Test Method3.1 Every crystalline substance,in this case pigment orextender,has a characteristic X-ray diffraction pattern.Whether the substance is present alone or in a mixture,itproduces its pattern independently and can be identified by it.An X-ray diffraction pattern of a sample is recorded.Eachcrystalline substance in the sample is identified by theHanawalt or Fink method or other systematic procedure basedon comparison of the diffraction pattern of the sample withreference patterns of standards.3,4,54.Significance and Use4.1 The choice of pigments and extenders influences theappearance,durability,cost,and other properties of paint.Thistest method is a convenient way,and probably the mostreliable,to identify pigments in paint.5.Apparatus5.1 X-ray Diffractometer,suitable for collecting intensityversus two theta(20)angle diffraction patterns in the rangefrom 5 to 65 20.It is preferred that the diffractometer beequipped with a copper target X-ray tube and a monochromatorthat passes only copper K-alpha radiation.If a monochromatoris not available,then a suitable filter may be used to removecopper K-beta radiation from the diffracted X-ray beam.Anickel filter may be used for this purpose when a copper targettube is employed.NOTE1Follow the recommendations of the manufacturer of thediffractometer used.5.2 Liquid Paint or Grind Paste:5.2.1 Paint Shaker.5.2.2 Film Applicator,that will produce a 3-to 10-mil(75-to 250 m)wet film thickness.5.2.3 Plastic Sheet,such as polyester film,that contains nocrystalline components that would produce interfering X-raydiffraction 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 Reciprocating Ball Mill.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Feb.1,2021.Published February 2021.Originallyapproved in 1993.Last previous edition approved in 2014 as D5380 93(2014).DOI:10.1520/D5380-93R21.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Search Manual,(Hanawalt),“Inorganic Phases,”International Centre forDiffraction Data,(ICDD),Catalog No.HA 42,Newtown Square Corporate Campus,12 Campus Blvd.,Newtown Square,PA 19073-3273.4Search 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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.15.3.2 Stainless Steel Vials,with agitator for ball mill.5.3.3 Powder Specimen Holders,for X-ray diffractomet