ASTM_D_3256_-_86_2014.pdf

Designation:D325686(Reapproved 2014)Standard Test Methods forChemical Analysis of Phthalocyanine Blue and GreenPigments1This standard is issued under the fixed designation D3256;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 These test methods cover procedures for the qualitativechemical analysis of pigments known commercially as copperphthalocyanine blue and green.1.2 The procedures appear in the following order:SectionIdentification5Moisture and Other Volatile Matter6Detection of Basic Dye Derivatives7Detection of Other Organic Coloring Matter8Detection of Ultramarine Blue9Detection of Iron Blue or Chrome Green101.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D280 Test Methods for Hygroscopic Moisture(and OtherMatter Volatile Under the Test Conditions)in PigmentsD1193 Specification for Reagent Water3.Significance and Use3.1 These test methods are suitable for determining ifimpurities are present and establishing that the required pig-ments are present.These test methods may be used formanufacturing and purchasing quality control.4.Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean Type II reagent gradewater conforming to Specification D1193.5.Identification5.1 To about 0.05 g of the sample in a 50-mL beaker,add 30mL of sulfuric acid(H2SO4,sp gr 1.84).Stir occasionally for15 min,heating if necessary to accelerate the solution of thepigment.Formation of a dark greenish yellow solution indi-cates phthalocyanine blue and a dark reddish color indicatesbrominated green pigment.Pour the solution into 250 mL ofwater and stir.The phthalocyanine pigment should immedi-ately precipitate as a flocculent mass.5.2 Filter off the precipitate,washing once or twice withwater.Scrape a small amount of the precipitate off the filter,place on a clean platinum wire moistened with hydrochloricacid(HCl),and subject it to the low flame of a bunsen burner.As the precipitate burns,a light blue-green flame should beclearly evident.This indicates organically combined copper.NOTE1Characteristic spectrophotometric absorption spectra in thenear infrared range(700 to 900 nm)are exhibited by dilute solutions ofcopper phthalocyanine pigments(2 to 50 mg/L)in H2SO4(sp gr 1.84).The absorption maxima,being sharp and well-defined,may be used forpositive qualitative identification of phthalocyanine pigments.Phthalocya-nine green has maxima at approximately 820 nm and 860 nm forbromine-free types;for the chlorinated-brominated types,the maximaappear at approximately 830 to 840 nm and 875 to 885 nm.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings,Materials,and Applications and are the directresponsibility of Subcommittee D01.31 on Pigment Specifications.Current edition approved Dec.1,2014.Published December 2014.Originallyapproved in 1973.Last previous edition approved in 2009 as D3256 86(2009).DOI:10.1520/D3256-86R14.2For 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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Moisture and Other Volatile Matter6.1 Determine moisture in accordance with Method A ofTest Methods D280.7.Detection of Basic Dye Derivatives7.1 Add to 1 g of the sample,50 mL of a mixture of equalparts of ammonium hydroxide NH4OH(sp gr 0.90)anddena