1、Designation: D 3256 86 (Reapproved 2004)Standard Test Methods forChemical Analysis of Phthalocyanine Blue and GreenPigments1This standard is issued under the fixed designation D 3256; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、as copperphthalocyanine blue and green.1.2 The procedures appear in the following order:SectionIdentification 5Moisture and Other Volatile Matter 6Detection of Basic Dye Derivatives 7Detection of Other Organic Coloring Matter 8Detection of Ultramarine Blue 9Detection of Iron Blue or Chrome Green 101
4、.3 This standard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1
5、ASTM Standards:2D 280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Conditions) in PigmentsD 1193 Specification for Reagent Water3. Significance and Use3.1 These test methods are suitable for determining ifimpurities are present and establishing that the required pig
6、-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
7、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 otherw
8、ise indicated, referencesto water shall be understood to mean Type II reagent gradewater conforming to Specification D 1193.5. 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 accele
9、rate 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
10、 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 bec
11、learly evident. This indicates organically combined copper.NOTE 1Characteristic 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 an
12、d 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 tes
13、t 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 June 1, 2004. Published June 2004. Originallyapproved in 1973. Last previous
14、 edition approved in 1999 as D 3256 86 (1999).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 Chemic
15、als, 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
16、Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Moisture and Other Volatile Matter6.1 Determine moisture in accordance with Method A ofTest Methods D 280.7. Detec
17、tion of Basic Dye Derivatives7.1 Addto1gofthesample, 50 mL of a mixture of equalparts of ammonium hydroxide NH4OH (sp gr 0.90) anddenatured ethyl alcohol (95 %). Warm gently and filter. Neu-tralize the filtrate with tartaric acid solution (200 g/L) untilslightly acid to litmus. If the solution is co
18、lorless, discountinga slight yellow tinge, no basic dye is present.7.2 If the solution is colored beyond a slight yellow tinge,add about 5 mL of 0.1 N titanium trichloride (TiCl3) solution(Note 2). If a basic dye is present, the color will lightensignificantly. If no basic dye is present, no signifi
19、cant colorchange will occur.NOTE 2Titanium trichloride is marketed as a 16 % solution in HCl.Mix 7 mL of this solution with 90 mL of HCl (1 + 12) to obtain a reagentapproximately 0.1 N. Protect from oxidation.8. Detection of Other Organic Coloring Matter8.1 ProcedureWeigh about 0.05 g of the sample
20、into eachof two 50-mL beakers. Add 25 mL (at room temperature) ofdenatured ethyl alcohol (95 %) to one beaker and about 25 mLof acetone to the other. Stir each thoroughly for a few minutesand let stand for about 2 h. Filter through two thicknesses ofmedium-texture, qualitative filter paper. The pres
21、ence of morethan an extremely slight pink, yellow, or blue tint in eitherfiltrate indicates other organic coloring matter is in the pig-ment. Organic colors resistant to the above reagents are notlikely to be in phthalocyanine pigments but, if desired, proce-dures given in standard references can be
22、 followed to establishif they are present.9. Detection of Ultramarine Blue9.1 ProcedureWarm gently about1gofthesample withabout 5 mL of HCl (1 + 1). Decomposition of the ultramarineblue takes place with evolution of H2S. This may be detectedby either its odor or a brown coloration appearing on a str
23、ip ofmoistened lead acetate paper.10. Detection of Iron Blue and Chrome Green10.1 Procedure:10.1.1 To1gofthesample in a 100-mL beaker, add 25 mLof NaOH solution (50 g/L). Boil for about 1 min. Dilute toapproximately 40 mL and filter.10.1.2 Add HCl (1 + 1) to the filtrate until faintly acid tolitmus.
24、 Add 2 mL of a ferric iron solution ferric sulfate orferric alum (20 g/L). The development of a blue color revealsthe presence of ferrocyanide, and hence iron blue or chromegreen in the original pigment. For amounts around 0.05 % ironblue, the color may take 2 to3htodevelop.11. Precision and Bias11.
25、1 No precision or bias information are available for thesetests.12. Keywords12.1 chrome green; detection of; iron blue; detection of;phthalocyanine blue; analysis of; phthalocyanine green; analy-sis of; pigment; ultramarine blue; detection ofASTM International takes no position respecting the validi
26、ty of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subjec
27、t to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarte
28、rs. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard
29、is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 3256 86 (2004)2
