1、Designation: D 3256 86 (Reapproved 2009)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 () 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 a
3、s 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 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 the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate s
5、afety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Conditions) in PigmentsD 1193 Specification for Reagent Water3. Significance
6、 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 t
7、ests. 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 ofsuf
8、ficiently 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 D 1193.5. Identification5.1 To about 0.05 g of the sample in
9、 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
10、 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 hydrochlorica
11、cid (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.NOTE 1Characteristic spectrophotometric absorption spectra in thenear infrared range (700 to 900 nm) are exhibited by
12、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 for1These test
13、 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, 2009. Published June 2009. Originallyapproved in 1973. Last previous
14、edition approved in 2004 as D 3256 86 (2004).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 Chemica
15、ls, 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 F
16、ormulary, 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.bromine-free types; for the chlorinated-brominated types, the maximaappear at approximately 830 to 840 nm and 875 to 8
17、85 nm.6. Moisture and Other Volatile Matter6.1 Determine moisture in accordance with Method A ofTest Methods D 280.7. Detection of Basic Dye Derivatives7.1Addto1gofthesample, 50 mL of a mixture of equalparts of ammonium hydroxide NH4OH (sp gr 0.90) anddenatured ethyl alcohol (95 %). Warm gently and
18、filter. Neu-tralize the filtrate with tartaric acid solution (200 g/L) untilslightly acid to litmus. If the solution is colorless, 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
19、) solution(Note 2). If a basic dye is present, the color will lightensignificantly. If no basic dye is present, no significant 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
20、 0.1 N. Protect from oxidation.8. Detection of Other Organic Coloring Matter8.1 ProcedureWeigh about 0.05 g of the sample 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 f
21、ew minutesand let stand for about 2 h. Filter through two thicknesses ofmedium-texture, qualitative filter paper. The presence 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 abov
22、e reagents are notlikely to be in phthalocyanine pigments but, if desired, proce-dures given in standard references can be followed to establishif they are present.9. Detection of Ultramarine Blue9.1 ProcedureWarm gently about 1 g of the sample withabout 5 mL of HCl (1 + 1). Decomposition of the ult
23、ramarineblue takes place with evolution of H2S. This may be detectedby either its odor or a brown coloration appearing on a strip 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). Bo
24、il for about 1 min. Dilute toapproximately 40 mL and filter.10.1.2 Add HCl (1 + 1) to the filtrate until faintly acid tolitmus. 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 chrome
25、green in the original pigment. For amounts around 0.05 % ironblue, the color may take 2 to3htodevelop.11. Precision and Bias11.1 No precision or bias information are available for thesetests.12. Keywords12.1 chrome green; detection of; iron blue; detection of;phthalocyanine blue; analysis of; phthal
26、ocyanine green; analy-sis of; pigment; ultramarine blue; detection ofASTM International takes no position respecting the validity 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 an
27、y such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject 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 i
28、nvited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. 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 receiv
29、ed a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard 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 (2009)2
