1、Designation: D6143 09Standard 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 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 covers the procedure to determine theiron content of bisphenol A (4,48-isopropylidenediphenol).1.2 This tes
3、t 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 exp
4、ected (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 Th
5、e 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-pria
6、te 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:2D1193 Specification for Reagent WaterD4297 Practice for Sampling and Handling Bisphenol A(4,48 -Isopropylidinedi
7、phenol)D6809 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 Conducting an Interlaboratory Study toDetermine the Precision of
8、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 withFerroZ
9、ine 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. Interferences5.1
10、 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 cylinders
11、, 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 5.5.1This test method is under the jurisdiction o
12、f ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofD16.02 on Oxygenated Aromatics.Current edition approved Dec. 1, 2009. Published December 2009. Originallyapproved in 1997. Last previous edition approved in 2005 as D6143 05. DOI:10.1520/D6143-09.2F
13、or 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 Document Summary page onthe ASTM website.3Available from U.S. Government Printing Office Superintendent
14、of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.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.7.2.1 This solution
15、 may be 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.7.3 Distilled Water, conforming to Type IV of SpecificationD1193.7.4 Standard Iron Solution, Titrisol, 100 mg/L (ca. 98mg/kg) iron chlorid
16、e in 15 % hydrochloric acid or equivalent.7.5 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-disulfoni
17、c acid, or equivalent.7.9 Ferrozine Solution:7.9.1 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 material
18、sused in this test method.9. Sampling and Handling9.1 Sample bisphenol A (BPA) in accordance with PracticeD4297.10. 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. D
19、ilute 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.10.2 Prepare and analyze two 10.0 6 0.1 g aliquots of eachof the above calibration standard solutions and two blanks inaccord
20、ance with the instructions given in Section 11.10.3 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 ve
21、rsus the averageabsorbance measurement for each 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/kgm = slope of the calibration curve, mg/kg per
22、 absorbencyunitsA = absorbance of the solution in absorbency unitsb = intercept of the calibration curve in mg/kg11. 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
23、 Add 40 mL of methanol to each of the 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 so
24、lution.11.8 Gently swirl then allow to 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 comp
25、lex tobecome stable.NOTE 1The color is 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 cruc
26、ial, especially for low levels of iron, 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 recommen
27、ded.12. Calculation and Report12.1 If 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/kgm = slope of the calibration curve from Section 10, mg/kgper absorbency unitsAS= ab
28、sorbance of the sample solution in absorbencyunitsAB= absorbance of the blank solution in absorbency unitsb = intercept of the calibration curve from Section 10,inmg/kg12.2 Report iron in the bisphenolAto the nearest 0.1 mg/kg.TABLE 1 Summary of Precision DataPrecision, characterized by repeatabilit
29、y, 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 09213. Precision and Bias413.1 The criteria in Table 1 should be used to j
30、udge theacceptability at the 95 % probability level of the resultsobtained by this test method. The criteria were derived from aninterlaboratory study of five samples in triplicate between threelaboratories. The results were derived using the protocol setforth in Practice E691.13.2 RepeatabilityResu
31、lts 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 considered suspect unless they differ bymore than the amounts listed in Table 1.13.4 BiasSince there is no
32、accepted reference materialsuitable for determining the bias in this test method formeasuring these impurities, bias has not been determined.14. Quality Guidelines14.1 Labroatories shall have a quality control system inplace.14.1.1 Confirm the performance of the test instrument ortest method by anal
33、yzing a quality control sample followingthe guidelines of standard statistical quality control practices.14.1.2 A quality control sample is a stable material isolatedfrom the production process and representative of the samplebeing analyzed.14.1.3 When QA/QC protocols are already established inthe t
34、esting facility, these protocols are acceptable when theyconfirm the validity of test results.14.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines described in GuideD6809 or similar statistical quality control practices.15. Keywords15.1 bisphenol A; ironSUM
35、MARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue(D6143 05) that may impact the use of this standard. (Approved December 1, 2009.)(1) Brought Section 14 verbiage up-to-date.ASTM International takes no position respecting the validity o
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