1、Designation: D 6143 05Standard Test Method forIron Content of Bisphenol A (4,4* - Isopropylidenediphenol)1This standard is issued under the fixed designation D 6143; 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 covers the procedure to determine theiron content of bisphenol A (4,48-isopropylidenediphenol).1.2 This
3、test 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
4、expected (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 E 29.1.
5、4 The 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-
6、priate safety and health practices and determine the applica-bility of regulatory limits prior to use. For a specific hazardstatement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 4297 Practice for Sampling and Handling Bisphenol A(4,48 - Isopropyl
7、idenediphenol)D 6809 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 SpecificationsE 691 Practice for Conducting an Interlaboratory Study toDetermine Precisio
8、n of a Test Method2.2 Other Documents:OSHA Regulations 29CFR paragraphs 1910.1000 and1910.1200.33. Summary of Test Method3.1 Bisphenol A is dissolved in methanol, then treated withhydroxylamine hydrochloride to convert any ferric iron presentto ferrous iron. The ferrous iron is then complexed withFe
9、rroZine to form a purple/maroon chromophore that isquantified by visible spectrophotometry at 560 nm.4. Significance and Use4.1 Iron may increase the color of bisphenol A and affectother properties of end-use products.4.2 High purity bisphenol A typically has less than 1 mg/kgof iron.5. Interference
10、s5.1 No direct interferences have been observed in the use ofthis method.6. Apparatus6.1 Visible Spectrophotometer, capable of measuring absor-bance at 560 nm.6.2 Analytical Balance, capable of weighing 100 g to thenearest 0.01 g.6.3 Glassware, 100 mL and 1 L volumetric flasks, 500 mLgraduated cylin
11、ders, 10 mL volumetric pipettes, 1 cm squarequartz cuvettes.6.4 All Glassware used in this test method should bededicated and thoroughly cleaned prior to use.7. Reagents and Materials7.1 Methanol, ACS reagent grade, $ 99.8 % purity.7.2 Sodium Acetate, pH 5.5.7.2.1 This solution may be prepared by di
12、ssolving 272.0 g6 0.1g of reagent grade sodium acetate in 1000 mL distilledwater and adjusting to pH 5.5 with concentrated hydrochloricacid.7.3 Distilled Water, conforming to Type IV of SpecificationD 1193.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and
13、Related Chemicals and is the direct responsibility ofD16.02 on Oxygenated Aromatics.Current edition approved July 1, 2005. Published July 2005. Originally approvedin 1997. Last previous edition approved in 1997 as D 6143 97.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcont
14、act 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, Washington, DC 20401.
15、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.7.4 Standard Iron Solution, Titrisol, 100 mg/L (ca. 98mg/kg) iron chloride in 15 % hydrochloric acid or equivalent.7.5
16、Sodium Hydroxide, 0.5 normal, ACS reagent grade.7.6 Hydroxylamine Hydrochloride, 99.999 % min.7.7 Hydroxylamine Hydrochloride SolutionMake up a10 % by weight aqueous solution.7.8 Ferrozine Iron Reagent, 3(2Pyridyl)-5,6diphenyl-1,2,4triazine-p,p-disulfonic acid, or equivalent.7.9 Ferrozine Solution:7
17、.9.1 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.8. Hazards8.1 Consult current OSHA regulations, local regulations,and suppliers Material Safety Data Sheets for all materialsused in this test method.9. Sampling and Hand
18、ling9.1 Sample bisphenol A (BPA) in accordance with PracticeD 4297.10. Calibration10.1 Weigh into separate 100 mL volumetric flasks, to thenearest 0.01 g, the following amounts of the standard ironsolution in 7.4: 0.2, 0.5, 1.0, 2.0, 4.0, 8.0, and 10.0. Dilute tovolume with distilled water, stopper,
19、 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.10.2 Prepare and analyze two 10.0 6 0.1 g aliquots of eachof the above calibration standard solutions and two blanks inaccordance with the instructions given in Section 1
20、1.10.3 Calibrate the instrument in accordance with manufac-turers instructions.10.4 If manual calibration is required, calculate the averageof the replicate measurements of each of the calibration andblank solutions.10.5 Plot the nominal concentrations versus the averageabsorbance measurement for ea
21、ch of the calibration standards.10.6 Using linear regression, determine the slope and inter-cept of the calibration curve according to Eq 1:C 5 mA 1 b (1)where:C = concentration of iron in the solution in mg/kg,m = slope of the calibration curve, mg/kg per absorbencyunits,A = absorbance of the solut
22、ion in absorbency units, andb = intercept of the calibration curve in mg/kg.11. Procedure11.1 Weigh 10.0 g of the BPA sample to be analyzed to thenearest 0.1 g into a 100mL volumetric flask.11.2 Label a second, clean, empty, 100 mL volumetric flaskas a blank.11.3 Add 40 mL of methanol to each of the
23、 above flasks.11.4 Gently swirl until all of the sample is dissolved.11.5 Add 30 mL of the sodium acetate solution to each ofthe flasks.11.6 Gently swirl then allow to stand for approximately 10min.11.7 Add 2 mL of the 10 % aqueous hydroxylamine hydro-chloride solution.11.8 Gently swirl then allow t
24、o stand for approximately 10min.11.9 Add 4 mL of ferrozine solution to each of the flasks.11.10 Dilute the contents of each flask to the mark withmethanol, cap and shake the flasks to thoroughly mix thecontents.11.11 Set a timer for 10 min to allow the color complex tobecome stable.NOTE 1The color i
25、s somewhat unstable and care should be taken toadhere to this development time as closely as possible.11.12 Transfer a portion of each of the above solutions to a1 cm quartz cuvette and read the absorbance using thespectrophotometer set to 560 nm.NOTE 2It is crucial, especially for low levels of iro
26、n, that thewindows of the cuvette be absolutely clean. Carefully wiping the windowswith a paper towel wetted with water followed by one wetted withmethanol and then drying with a clean paper towel after the sample hasbeen added to the cuvette is strongly recommended.12. Calculation and Report12.1 If
27、 manual calculations are required, calculate the con-centration of iron in each of the samples as follows:C15 mAS2 AB! 1 b (2)where:C1= concentration of iron in the sample in mg/kg,m = slope of the calibration curve from Section 10, mg/kgper absorbency units,AS= absorbance of the sample solution in
28、absorbencyunits,AB= absorbance of the blank solution in absorbency units,andb = intercept of the calibration curve from Section 10,inmg/kg.12.2 Report iron in the bisphenolAto the nearest 0.1 mg/kg.13. Precision and Bias413.1 The criteria in Table 1 should be used to judge theacceptability at the 95
29、 % probability level of the resultsobtained by this test method. The criteria were derived from aninterlaboratory study of five samples in triplicate between three4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D161034.TABLE 1 S
30、ummary of Precision DataPrecision, characterized 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 2.55D6143052laborato
31、ries. The results were derived using the protocol setforth in Practice E 691.13.2 RepeatabilityResults in the same laboratory shouldnot be considered suspect unless they differ by more than theamounts listed in Table 1.13.3 ReproducibilityResults submitted by two laborato-ries should not be consider
32、ed suspect unless they differ bymore than the amounts listed in Table 1.13.4 BiasSince there is no accepted reference materialsuitable for determining the bias in this test method formeasuring these impurities, bias has not been determined.14. Quality Guidelines14.1 Refer to Guide D 6809 for suggest
33、ed QA/QC activitiesthat can be used as a part of this method. It is recommendedthat the operator of this method select and perform relevantQA/QC activities like the ones in Guide D 6809 to help ensurethe quality of data generated by this method.15. Keywords15.1 bisphenol A; ironSUMMARY OF CHANGESCom
34、mittee D16 has identified the location of selected changes to this standard since the last issue(D 6143 97) that may impact the use of this standard. Entire document was reviewed and updated based oncurrent D16 editorial guidelines with regards to Section and Subsection titles, order, and numbering.
35、(1) Section 1: Revised scope to match ILS data reported andchanged the wording in 1.3.(2) Section 2: Added reference to Guide D 6809.(3) Section 3: Slight changes to wording(4) Section 5: Old method had a number of potential interfer-ences listed, these were removed.(5) Sections 6 and 7: Extensively
36、 modified to bring up to dateand make consistent with greatly improved method.(6) Sections 10-12: Completely re-done to reflect modern andgreatly improved methodology.(7) Section 13: Modified based on ILS data and modified to fitcurrent editorial guidelines.(8) Section 14: Added, used to be Keywords
37、.(9) Section 15: Used to be Section 14.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
38、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 invited either for revision of
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40、ke 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).D6143053
