1、Designation: D4789 12Standard Test Method forSolution Color of Bisphenol A (4,4*-Isopropylidenediphenol)1This standard is issued under the fixed designation D4789; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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-Isopropylidene
3、diphenol) dissolved in methanol.1.2 This test method has been found applicable for thedetermination of Platinum-Cobalt color of bisphenol A be-tween 20 and 100 color units.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4
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. For specific hazar
5、dstatements, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D4297 Practice for Sampling and Handling Bisphenol A(4,4 -Isopropylidinediphenol)D6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydr
6、ocarbons and Related Ma-terialsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)32.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.12004NIST Letter Circular LC 1017 , Standard for Checki
7、ng theCalibration of Spectrophotometers (200 to 1000 nm)53. 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 by means of a spectrophotome
8、ter. 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 controlor for setting specifi
9、cations.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 mL, tall-formNessler tubes,
10、 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, 100 mL Nesslertubes in th
11、e direction of their longitudinal axis; and so thatwhite light is passed through or reflected off a white glass plate1This 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 Ar
12、omatics.Current edition approved Aug. 15, 2012. Published August 2012. Originallyapproved in 1988. Last previous edition approved in 2008 as D4789 08. DOI:10.1520/D4789-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For An
13、nual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail
14、Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.5Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 10
15、0 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1and directed with equal intensity through the tubes. It should beshielded so that no light enters the tubes from the sides.6.3 Spectrophotometer, equipped for liquid samples and formeasurements in the visible region.NO
16、TE 1The spectrophotometer must be clean and in excellentoperating condition. The instrument should be calibrated in accordancewith the instructions given in NIST Letter Circular LC 1017. For goodagreement with the visual method, the spectrophotometer or colorimetershould be a filter type instrument.
17、6.4 Spectrophotometer Cells, cells of different path lengthsmay be used as 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 test
18、s. 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.6Other grades may beused, provided it is first ascertained that the reagent is ofsuffic
19、iently high purity to permit its use without lessening theaccuracy of the 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 D1209.8. Hazard
20、s8.1 Consult current OSHA regulations, suppliers MaterialSafety Data Sheets, and local regulations for all materialsutilized in this test method.9. Sampling9.1 Sample the material in accordance with Practice D4297.10. Procedure10.1 Weigh 50 g of bisphenol A. Transfer to a 150-mLErlenmeyer flask.10.2
21、 Measure 70 mL of methanol. Add to the Erlenmeyerflask containing the bisphenol 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 methanolsolutio
22、n through a filter and refill the comparison tube.10.6 Visually compare the 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 devel
23、opment test is run, measure thecolor 30 min after the bisphenolAis dissolved 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
24、the standard that most nearly matchesthe specimen. If the color lies midway 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
25、 in hue between the specimensand the standards, and a definite match cannot be made, reportthe range over which an apparent match is obtained, and reportthe material as “off-hue.”12. Precision and Bias712.1 PrecisionAn interlaboratory study was conductedwhich included six laboratories analyzing thre
26、e 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 E180 was used in developing these precision esti-mates.12.1.1 Intermediate Precision, (formerly cal
27、ledRepeatability)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 differ by more than 10 units absolute.12.1.2 Reproduc
28、ibilityThe 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 by more than 35 units absolute.12.2 BiasSince there i
29、s no accepted reference materialsuitable for determining the bias in this test method bias has notbeen determined.13. Quality Guidelines13.1 Laboratories shall have a quality control system inplace.13.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sam
30、ple followingthe guidelines of standard statistical quality control practices.13.1.2 A quality control sample is a stable material isolatedfrom the production process and representative of the samplebeing analyzed.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society
31、, 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.7Su
32、pporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1010.D4789 12213.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.13.1.4 When
33、there are no QA/QC protocols established inthe testing facility, use the guidelines described in GuideD6809 or similar statistical quality control practices.14. Keywords14.1 bisphenol A; color; color test; 4,48-IsopropylidenediphenolSUMMARY OF CHANGESCommittee D16 has identified the location of sele
34、cted changes to this standard since the last issue (D4789 08) that may impact the use of this standard. (Approved August 15, 2012.)(1) Sections 1, 12, and 13 were updated to current editorialguideline verbiage and format.(2) Section 1.2 was added based on information in the Re-search Report.ASTM Int
35、ernational 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 riskof infringement of such rights, are entirel
36、y 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 this standard or for additional standardsand sh
37、ould 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 your views known to the ASTM Committee on St
38、andards, 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D4789 123
