1、Designation: D6143 13D6143 18Standard Test Method forIron Content of Bisphenol A (4,4 - Isopropylidenediphenol)1This standard is issued under the fixed designation D6143; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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. Scope*1.1 This test method covers the procedure to determine the iron content of bisphenol A (4,4-isopropylidenediphenol).1.2 T
3、his test method has a lower detection limit of 0.1 mg/kg, and an upper limit of 10 mg/kg of iron in bisphenol A. If theiron content is higher, it may be necessary to dilute the sample. A longer path length cell can also be used for better accuracy atlower Fe levels, as well as calibration within the
4、 range expected (for example, 0 to 1 mg/kg versus 0 to 10 mg/kg for samplesexpected to be in the 0 to 1 mg/kg range.1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be roundedoff in accordance with the rounding-off method of Practic
5、e E29.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to estab
6、lish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limits prior to use. For a specific hazard statement, see Section 9.1.6 This international standard was developed in accordance with internationally recognized principles on standar
7、dizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4297 Practic
8、e for Sampling and Handling Bisphenol A(4,4 -Isopropylidinediphenol)D4790 Terminology of Aromatic Hydrocarbons and Related ChemicalsD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE29 Practice for Using Significant Digits in Test Data t
9、o Determine Conformance with SpecificationsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.120033. Terminology3.1 See Terminology D4790 for definitions of terms used in this st
10、andard.4. Summary of Test Method4.1 Bisphenol A is dissolved in methanol, then treated with hydroxylamine hydrochloride to convert any ferric iron present toferrous iron. The ferrous iron is then complexed with FerroZine an iron reagent to form a purple/maroon chromophore that isquantified by visibl
11、e spectrophotometry at 560 nm.1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of D16.02 on Oxygenated Aromatics.Current edition approved June 1, 2013June 1, 2018. Publish
12、ed June 2013June 2018. Originally approved in 1997. Last previous edition approved in 20092013 asD6143 09.D6143 13. DOI: 10.1520/D6143-13.10.1520/D6143-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM
13、Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.3 Available 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.This document is not an ASTM sta
14、ndard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cas
15、es only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance
16、 and Use5.1 Iron may increase the color of bisphenol A and affect other properties of end-use products.5.2 High purity bisphenol A typically has less than 1 mg/kg of iron.6. Interferences6.1 No direct interferences have been observed in the use of this method.7. Apparatus7.1 Visible Spectrophotomete
17、r, capable of measuring absorbance at 560 nm.7.2 Analytical Balance, capable of weighing 100 g to the nearest 0.01 g.7.3 Glassware, 100 mL and 1 L volumetric flasks, 500 mL graduated cylinders, 10 mL volumetric pipettes, 1 cm square quartzcuvettes.7.4 All Glassware used in this test method should be
18、 dedicated and thoroughly cleaned prior to use.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specification of the Committee onAnalytical Reagents of theAmerican Chemi
19、cal Society, where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.8.2 Methanol, ACS reagent grade, 99.8 % purity.8.3 Sodium Acetate, pH
20、5.5.8.3.1 This solution may be prepared by dissolving 272.0 g 6 0.1g of reagent grade sodium acetate in 1000 mL distilled waterand adjusting to pH 5.5 with concentrated hydrochloric acid. Alternate volumes of solutions may be prepared so long as thepreparation meets the concentration specified.8.4 P
21、urity of Water, Unless otherwise indicated, references to water shall be understood to mean any reagent conforming toTypeIV of Specification D1193.8.5 Standard Iron Solution, Titrisol, 100 mg/L (ca. 98 mg/kg) iron chloride in 15 % hydrochloric acid or equivalent. Alternatevolumes of solutions may be
22、 prepared so long as the preparation meets the concentration specified.8.6 Sodium Hydroxide, 0.5 normal, ACS reagent grade.8.7 Hydroxylamine Hydrochloride, 99.999 % min.8.8 Hydroxylamine Hydrochloride SolutionMake up a 10 % by weight aqueous solution.8.9 Ferrozine Iron Reagent, 3(2Pyridyl)-5,6diphen
23、yl-1,2,4triazine-p,p-disulfonic acid, or equivalent.8.10 Ferrozine Iron Reagent Solution:8.10.1 In a 1 L volumetric flask, dissolve 1.00 6 0.01 g of ferrozine iron reagent in 20 mL of 0.5 N NaOH and dilute to 1 Lwith methanol. Alternate volumes of solutions may be prepared so long as the preparation
24、 meets the concentration specified.9. Hazards9.1 Consult current OSHAregulations, local regulations, and suppliers Material suppliers Safety Data Sheets for all materialsused in this test method.10. Sampling and Handling10.1 Sample bisphenol A (BPA) in accordance with Practice D4297.11. Calibration1
25、1.1 Weigh into separate 100 mL volumetric flasks, to the nearest 0.01 g, the following amounts of the standard iron solutionin 8.5: 0.2, 0.5, 1.0, 2.0, 4.0, 8.0, and 10.0. Dilute to volume with distilled water, stopper, and shake to mix. This will give solutionswith nominal concentrations of 0.2, 0.
26、5, 1.0, 2.0, 4.0, 8.0, and 10 mg/kg, respectively.11.2 Prepare and analyze two 10.0 6 0.1 g aliquots of each of the above calibration standard solutions and two blanks inaccordance with the instructions given in Section 12.4 Reagent Chemicals, American Chemical Society Specifications, American Chemi
27、cal Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rock
28、ville, MD.D6143 18211.3 Calibrate the instrument in accordance with manufacturers instructions.11.4 If manual calibration is required, calculate the average of the replicate measurements of each of the calibration and blanksolutions.11.5 Plot the nominal concentrations versus the average absorbance
29、measurement for each of the calibration standards.11.6 Using linear regression, determine the slope and intercept of the calibration curve according to Eq 1:C 5mA1b (1)where:C = concentration of iron in the solution in mg/kgm = slope of the calibration curve, mg/kg per absorbency unitsA = absorbance
30、 of the solution in absorbency unitsb = intercept of the calibration curve in mg/kg12. Procedure12.1 Weigh 10.0 g of the BPA sample to be analyzed to the nearest 0.1 g into a 100mL volumetric flask.12.2 Label a second, clean, empty, 100 mL volumetric flask as a blank.12.3 Add 40 mL of methanol to ea
31、ch of the above flasks.12.4 Gently swirl until all of the sample is dissolved.12.5 Add 30 mL of the sodium acetate solution to each of the flasks.12.6 Gently swirl then allow to stand for approximately 10 min.12.7 Add 2 mL of the 10 % aqueous hydroxylamine hydrochloride solution.12.8 Gently swirl th
32、en allow to stand for approximately 10 min.12.9 Add 4 mL of ferrozine iron reagent solution to each of the flasks.12.10 Dilute the contents of each flask to the mark with methanol, cap and shake the flasks to thoroughly mix the contents.12.11 Set a timer for 10 min to allow the color complex to beco
33、me stable.NOTE 1The color is somewhat unstable and care should be taken to adhere to this development time as closely as possible.12.12 Transfer a portion of each of the above solutions to a 1 cm quartz cuvette and read the absorbance using thespectrophotometer set to 560 nm.D6143 183NOTE 2It is cru
34、cial, especially for low levels of iron, that the windows of the cuvette be absolutely clean. Carefully wiping the windows with a papertowel wetted with water followed by one wetted with methanol and then drying with a clean paper towel after the sample has been added to the cuvetteis strongly recom
35、mended.13. Calculation and Report13.1 If manual calculations are required, calculate the concentration of iron in each of the samples as follows:C15mAS 2AB!1b (2)where:C1 = concentration of iron in the sample in mg/kg,m = slope of the calibration curve from Section 11, mg/kg per absorbency units,AS
36、= absorbance of the sample solution in absorbency units,AB = absorbance of the blank solution in absorbency units,b = intercept of the calibration curve from Section 11, in mg/kg.13.2 Report iron in the bisphenol A to the nearest 0.1 mg/kg. Results less than 0.1 mg/kg should be reported as 0.1 mg/kg
37、.14. Precision and Bias514.1 The criteria in Table 1 should be used to judge the acceptability at the 95 % probability level of the results obtained bythis test method (95 % confidence level). The criteria were derived from an interlaboratory study of five samples in triplicatebetween three laborato
38、ries. Practice E691 was followed for the design and analysis of the data; the details are given in ASTMResearch Report RR:D16-1034.14.2 RepeatabilityIntermediate Precision (formerly called Repeatability)Results in the same laboratory should not beconsidered suspect unless they differ by more than th
39、e amounts listed in Table 1. Results differing by less than “r” have a 95 %probability of being correct.14.3 ReproducibilityResults submitted by two laboratories should not be considered suspect unless they differ by more thanthe amounts listed in Table 1. Results differing by less than “R” have a 9
40、5 % probability of being correctcorrect.14.4 BiasSince there is no accepted reference material suitable for determining the bias in this test method for measuring theseimpurities, iron in Bisphenol-A, bias has not been determined.15. Quality Guidelines15.1 Laboratories shall have a quality control s
41、ystem in place.15.1.1 Confirm the performance of the test instrument or test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.15.1.2 Aquality control sample is a stable material isolated from the production process and representat
42、ive of the sample beinganalyzed.15.1.3 When QA/QC protocols are already established in the testing facility, these protocols are acceptable when they confirmthe validity of test results.15.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines described in Guid
43、e D6809 orsimilar statistical quality control practices.16. Keywords16.1 bisphenol A; iron5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D16-1034. Contact ASTM CustomerService at serviceastm.org.TABLE 1 Summary of Precision D
44、ataPrecision, characterized by repeatability, Sr, r,and reproducibility, SR, R for analysis of Fe in BPASample # mg/kgAverage Sr SR r R1 0.29 0.09 0.10 0.26 0.272 0.02 0.00 0.04 0.00 0.113 7.30 0.32 0.65 0.90 1.834 0.51 0.15 0.17 0.41 0.495 3.30 0.15 0.91 0.42 2.55D6143 184SUMMARY OF CHANGESCommitte
45、e D16 has identified the location of selected changes to this standard since the last issue(D614309)13) that may impact the use of this standard. (Approved June 1, 2013.)2018.)(1) Brought all Sections up-to-date with Minor tweaks per current D16 Editorial Guidelines.Guidelines in Sections 8, 9, 13,
46、and14.(2) Section 3 added and all subsequent sections re-numbered.All references toTitrisol and Ferrozine were made generic in Sections4, 8, and 12.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
47、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 subject to revision at any time by the responsible technical committee and must be reviewed every fi
48、ve 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 Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical c
49、ommittee, 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 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(w
