1、Designation: D 4789 08Standard Test Method forSolution Color of Bisphenol A (4,4*-Isopropylidenediphenol)1This standard is issued under the fixed designation D 4789; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、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. Scope*1.1 This test method describes the procedure for determina-tion of the Platinum-Cobalt Color of bisphenol A (4,48-Isopropylid
3、enediphenol) dissolved in methanol.1.2 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 limit
4、ations prior to use. For a specifichazard statement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D 4297 Practice for Sampling and Handling Bisphenol A(4,48 -Isopropylidinediphenol)D 6809 Guide for Quality Control and Q
5、uality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals2.2 Other Documents:OSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.12003NIST Letter Circular L
6、C 1017, Standard for Checking theCalibration of Spectrophotometers (200 to 1000 nm)43. Summary of Test Method3.1 Bisphenol A is dissolved in methanol. This solution isthen transferred to a color comparison tube and the colorcompared to that of the Platinum-Cobalt Color Standards,either visually or b
7、y means of a spectrophotometer. The coloris reported as that closest to the applicable standard.4. Significance and Use4.1 Color is caused by impurities in the bisphenol A. Theacceptable amount of color depends on the end-use of thebisphenol A.4.2 This test method can be used for internal quality co
8、ntrolor for setting specifications.5. Interferences5.1 The presence of any turbidity or haze will affect thecolor reading.5.2 AbisphenolAcolor that is off-hue, or tinted with respectto the color standards, may interfere with proper color com-parison.6. Apparatus6.1 Color Comparison TubesMatched 100
9、mL, tall-formNessler tubes, provided with ground-on, optically clear, glasscaps. Tubes should be selected so that the height of the 100-mLgraduation mark is 275 to 295 mm above the bottom of thetube.6.2 Color Comparator, constructed to permit visual com-parison of light transmitted through tall-form
10、, 100 mL Nesslertubes in the direction of their longitudinal axis; and so thatwhite light is passed through or reflected off a white glass plateand directed with equal intensity through the tubes. It should beshielded so that no light enters the tubes from the sides.6.3 Spectrophotometer, equipped f
11、or liquid samples and formeasurements in the visible region.NOTE 1The spectrophotometer must be clean and in excellent oper-ating condition. The instrument should be calibrated in accordance withthe instructions given in NIST Letter Circular LC 1017. For goodagreement with the visual method, the spe
12、ctrophotometer or colorimetershould be a filter type instrument.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.02 on Oxygenated Aromatics.Current edition approved Jan. 1, 2008. Publis
13、hed January 2008. Originallyapproved in 1988. Last previous edition approved in 2003 as D 4789 03.2For 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 Docu
14、ment Summary page onthe ASTM website.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gai
15、thersburg, MD 20899-1070, http:/www.nist.gov.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.4 Spectrophotometer Cells, cells of different path lengthsmay be used as
16、 long as the equipment is calibrated with thesame length cells as the sample solution.6.5 Filter Paper, glass fiber filter, 1.2-m pore retention.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall confo
17、rm to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the
18、determination.7.2 MethanolCheck for color against deionized water; ifthe methanol is not water white, redistill in an all-glass system.7.3 Platinum-Cobalt Color StandardsPrepared in accor-dance with Test Method D 1209.8. Hazards8.1 Consult current OSHA regulations, suppliers MaterialSafety Data Shee
19、ts, and local regulations for all materialsutilized in this test method.9. Sampling9.1 Sample the material in accordance with PracticeD 4297.10. Procedure10.1 Weigh 50 g of bisphenol A. Transfer to a 150-mLErlenmeyer flask.10.2 Measure 70 mL of methanol. Add to the Erlenmeyerflask containing the bis
20、phenol A.10.3 Stir until all the bisphenol A is dissolved.10.4 Transfer the methanol solution to a color comparisontube, fill to the 100-mL mark, and cap the tube.10.5 If there is any visible turbidity, pass the methanolsolution through a filter and refill the comparison tube.10.6 Visually compare t
21、he methanol solution comparisontube with the color standards.Aspectrophotometer can be usedto determine the transmittance at a wavelength of 436 nm,which would be an indication of the color intensity.10.7 If a timed color development test is run, measure thecolor 30 min after the bisphenolAis dissol
22、ved in the methanol.(WarningUse of a spectrophotometer may provide valueswhich are higher or inconsistent with those obtained by usingcolor comparison tubes.)11. Report11.1 Report the following information:11.1.1 The number of the standard that most nearly matchesthe specimen. If the color lies midw
23、ay between two standards,report the darker of the two.11.1.2 The result to the nearest 5 units. Duplicate runs thatagree within 10 units absolute are acceptable for averaging(95 % confidence level).11.2 If there is a difference in hue between the specimensand the standards, and a definite match cann
24、ot be made, reportthe range over which an apparent match is obtained, and reportthe material as “off-hue.”12. Precision and Bias612.1 PrecisionThe following criteria should be used tojudge the acceptability at the 95 % probability level of theresults obtained by this test method. The criteria were d
25、erivedfrom an interlaboratory study conducted on three specimens ofbisphenol A from three different sources. One analyst in eachof six laboratories performed duplicate determinations andrepeated on a second day, for a total of 72 determinations.Practice E 180 was used in developing these precision e
26、sti-mates.12.1.1 Intermediate Precision, (formerly calledRepeatability)The standard deviation of results (each theaverage of duplicate determinations), obtained by the sameanalyst on different days, was estimated to be 2.0 units absoluteat 18 df. Two such averages should be considered suspect ifthey
27、 differ by more than 10 units absolute.12.1.2 ReproducibilityThe standard deviation of results(each the average of duplicate determinations), obtained byanalysts in different laboratories has been estimated to be 9.0units absolute at 5 df. Two such averages should be consideredsuspect if they differ
28、 by more than 35 units absolute.12.2 BiasSince there is no accepted reference materialsuitable for determining the bias in this test method formeasuring solution color, bias has not been determined.13. Quality Guidelines13.1 Refer to Guide D 6809 for suggested QA/QC activitiesthat can be used as a p
29、art of this test method. It is recom-mended that the operator of this test method select and performrelevant QA/QC activities like the ones in Guide D 6809 tohelp ensure the quality of the data generated by this testmethod.14. Keywords14.1 bisphenol A; color; color test; isopropylidenediphenol5Reage
30、nt 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
31、National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1010.D4789082SUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to thi
32、s standard since the last issue(D 4789 - 03) that may impact the use of this standard. (Approved January 1, 2008.)(1) Section 2 Reference to Guide D 6809 was added.(2) Section 13 Numbering and some verbiage was changedper Editorial Guidelines.(3) Section 14 Quality Guidelines was added and thefollow
33、ing Sections renumbered accordingly.ASTM 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 any such patent rights, and the ris
34、kof 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 invited either for revision of thi
35、s 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 received a fair hearing you shouldmake
36、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).D4789083