1、Designation: D6143 13Standard 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 last rev
2、ision. 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 theiron content of bisphenol A (4,4-isopropylidenediphenol).1.2 This test
3、method has a lower detection limit of 0.1mg/kg, and an upper limit of 10 mg/kg of iron in bisphenol A.If the iron content is higher, it may be necessary to dilute thesample. A longer path length cell can also be used for betteraccuracy at lower Fe levels, as well as calibration within therange expec
4、ted (for example, 0 to 1 mg/kg versus 0 to 10mg/kg for samples expected to be in the 0 to 1 mg/kg range.1.3 In determining the conformance of the test results usingthis method to applicable specifications, results shall berounded off in accordance with the rounding-off method ofPractice E29.1.4 The
5、values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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
6、 safety and health practices and determine the applica-bility of regulatory limits prior to use. For a specific hazardstatement, see Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4297 Practice for Sampling and Handling Bisphenol A(4,4 -Isopropylidinediphe
7、nol)D4790 Terminology of Aromatic Hydrocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE691 Practice for Condu
8、cting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 See Terminology D4790 for definitions of terms used inthis standard.4. Summary of Test Method4.1 Bisphenol A is dissolved in metha
9、nol, then treated withhydroxylamine hydrochloride to convert any ferric iron presentto ferrous iron. The ferrous iron is then complexed withFerroZine to form a purple/maroon chromophore that isquantified by visible spectrophotometry at 560 nm.5. Significance and Use5.1 Iron may increase the color of
10、 bisphenol A and affectother properties of end-use products.5.2 High purity bisphenol A typically has less than 1 mg/kgof iron.6. Interferences6.1 No direct interferences have been observed in the use ofthis method.7. Apparatus7.1 Visible Spectrophotometer, capable of measuring absor-bance at 560 nm
11、.7.2 Analytical Balance, capable of weighing 100 g to thenearest 0.01 g.7.3 Glassware, 100 mL and 1 L volumetric flasks, 500 mLgraduated cylinders, 10 mL volumetric pipettes, 1 cm squarequartz cuvettes.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Rela
12、ted Chemicals and is the direct responsibility ofD16.02 on Oxygenated Aromatics.Current edition approved June 1, 2013. Published June 2013. Originallyapproved in 1997. Last previous edition approved in 2009 as D6143 09. DOI:10.1520/D6143-13.2For referenced ASTM standards, visit the ASTM website, www
13、.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.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Wash
14、ington, DC 20401, http:/www.access.gpo.gov.*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 States17.4 All Glassware used in this test method should bededicated and thoroughly c
15、leaned prior to use.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specification of the Committeeon Analytical Reagents of the American Chemical Society,where such spec
16、ifications are available.4Other 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.8.2 Methanol, ACS reagent grade, 99.8 % purity.8.3 Sodium Acetate, pH 5.5.8.3.1 This solution may be
17、 prepared by dissolving 272.0 g6 0.1g of reagent grade sodium acetate in 1000 mL distilledwater and adjusting to pH 5.5 with concentrated hydrochloricacid.8.4 Purity of Water, Unless otherwise indicated, referencesto water shall be understood to mean any reagent conformingto Type IV of Specification
18、 D1193.8.5 Standard Iron Solution, Titrisol, 100 mg/L (ca. 98mg/kg) iron chloride in 15 % hydrochloric acid or equivalent.8.6 Sodium Hydroxide, 0.5 normal, ACS reagent grade.8.7 Hydroxylamine Hydrochloride, 99.999 % min.8.8 Hydroxylamine Hydrochloride SolutionMake up a10 % by weight aqueous solution
19、.8.9 Ferrozine Iron Reagent, 3(2Pyridyl)-5,6diphenyl-1,2,4triazine-p,p-disulfonic acid, or equivalent.8.10 Ferrozine Solution:8.10.1 Ina1Lvolumetric flask, dissolve 1.00 6 0.01 g offerrozine iron reagent in 20 mL of 0.5 N NaOH and dilute to1 L with methanol.9. Hazards9.1 Consult current OSHA regulat
20、ions, local regulations,and suppliers Material Safety Data Sheets for all materialsused in this test method.10. Sampling and Handling10.1 Sample bisphenolA(BPA) in accordance with PracticeD4297.11. Calibration11.1 Weigh into separate 100 mL volumetric flasks, to thenearest 0.01 g, the following amou
21、nts of the standard ironsolution in 8.5: 0.2, 0.5, 1.0, 2.0, 4.0, 8.0, and 10.0. Dilute tovolume with distilled water, stopper, and shake to mix. Thiswill give solutions with nominal concentrations of 0.2, 0.5, 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 a
22、liquots of eachof the above calibration standard solutions and two blanks inaccordance with the instructions given in Section 12.11.3 Calibrate the instrument in accordance with manufac-turers instructions.11.4 If manual calibration is required, calculate the averageof the replicate measurements of
23、each of the calibration andblank solutions.11.5 Plot the nominal concentrations versus the averageabsorbance measurement for each of the calibration standards.11.6 Using linear regression, determine the slope and inter-cept of the calibration curve according to Eq 1:C 5 mA1b (1)where:C = concentrati
24、on of iron in the solution in mg/kgm = slope of the calibration curve, mg/kg per absorbencyunitsA = absorbance 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 thenearest 0.1 g into a 100mL volumetric
25、 flask.12.2 Label a second, clean, empty, 100 mL volumetric flaskas a blank.12.3 Add 40 mL of methanol to each 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 ofthe flasks.12.6 Gently swirl then allow to stand for appro
26、ximately 10min.12.7 Add 2 mL of the 10 % aqueous hydroxylamine hydro-chloride solution.12.8 Gently swirl then allow to stand for approximately 10min.12.9 Add 4 mL of ferrozine solution to each of the flasks.12.10 Dilute the contents of each flask to the mark withmethanol, cap and shake the flasks to
27、 thoroughly mix thecontents.12.11 Set a timer for 10 min to allow the color complex tobecome stable.NOTE 1The color is somewhat unstable and care should be taken toadhere to this development time as closely as possible.12.12 Transfer a portion of each of the above solutions to a1 cm quartz cuvette a
28、nd read the absorbance using thespectrophotometer set to 560 nm.4Reagent 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,
29、 BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D6143 132NOTE 2It is crucial, especially for low levels of iron, that the windowsof the cuvette be absolutely clean. Carefully wiping the windows with ap
30、aper towel wetted with water followed by one wetted with methanol andthen drying with a clean paper towel after the sample has been added tothe cuvette is strongly recommended.13. Calculation and Report13.1 If manual calculations are required, calculate the con-centration of iron in each of the samp
31、les as follows:C15 mAS2 AB!1b (2)where:C1= concentration of iron in the sample in mg/kg,m = slope of the calibration curve from Section 11, mg/kgper absorbency units,AS= absorbance of the sample solution in absorbency units,AB= absorbance of the blank solution in absorbency units,b = intercept of th
32、e calibration curve from Section 11,inmg/kg.13.2 Report iron in the bisphenolAto the nearest 0.1 mg/kg.14. Precision and Bias514.1 The criteria in Table 1 should be used to judge theacceptability at the 95 % probability level of the resultsobtained by this test method (95 % confidence level). Thecri
33、teria were derived from an interlaboratory study of fivesamples in triplicate between three laboratories. Practice E691was followed for the design and analysis of the data; the detailsare given in ASTM Research Report RR:D16-1034.14.2 RepeatabilityResults in the same laboratory shouldnot be consider
34、ed suspect unless they differ by more than theamounts listed in Table 1. Results differing by less than “r”have a 95 % probability of being correct.14.3 ReproducibilityResults submitted by two laborato-ries should not be considered suspect unless they differ bymore than the amounts listed in Table 1
35、. Results differing byless than “R” have a 95 % probability of being correct14.4 BiasSince there is no accepted reference materialsuitable for determining the bias in this test method formeasuring these impurities, bias has not been determined.15. Quality Guidelines15.1 Laboratories shall have a qua
36、lity control system inplace.15.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical quality control practices.15.1.2 A quality control sample is a stable material isolatedfrom the production process and
37、 representative of the samplebeing analyzed.15.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.15.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines describ
38、ed in GuideD6809 or similar statistical quality control practices.16. Keywords16.1 bisphenol A; ironSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue (D614309)that may impact the use of this standard. (Approved June 1, 2013.)(1) Bro
39、ught all Sections up-to-date with current D16 EditorialGuidelines.(2) Section 3 added and all subsequent sections re-numbered.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1034.TABLE 1 Summary of Precision DataPrecision, c
40、haracterized by repeatability, Sr, r,and reproducibility, SR, R for analysis of Fe in BPASample #mg/kgAverageSr 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 133ASTM International takes no position respec
41、ting 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 entirely their own responsibility.This sta
42、ndard 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 should be addressed to ASTM Internati
43、onal 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 Standards, at the address shown below
44、.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/).D6143 134
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