ASTM D6143-23

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6143 − 18 D6143 − 23
Standard Test Method for
Iron Content of Bisphenol A (4,4' - Isopropylidenediphenol)
This standard is issued under the fixed designation D6143; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the procedure to determine determination of the iron content of bisphenol A (4,4'-
isopropylidenediphenol).
1.2 This test method has a lower detection limit of 0.10.1 mg mg/kg, ⁄kg, and an upper limit of 1010 mg mg/kg ⁄kg of iron in
bisphenol A. If the iron (Fe) content is higher, it may be necessary to dilute the sample. A longer path length cell can also be used
for better accuracy at lower Fe levels, as well as calibration within the range expected (for example, 00 mg ⁄kg to 1 mg/kg versus
00 mg ⁄kg to 10 mg/kg for samples expected to be in the 00 mg ⁄kg to 1 mg/kg range.
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off
in accordance with the rounding-off method of Practice 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 responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability 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 standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4297 Practice for Sampling and Handling Bisphenol A(4,4' -Isopropylidinediphenol)
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1615 Test Method for Determination of Trace Quantities of Iron by Visible Spectrophotometry
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of D16.02
on Oxygenated Aromatics.
Current edition approved June 1, 2018April 1, 2023. Published June 2018June 2023. Originally approved in 1997. Last previous edition approved in 20132018 as
D6143 – 13.D6143 – 18. DOI: 10.1520/D6143-18.10.1520/D6143-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D6143 − 23
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200 paragraphs 1910.1000 and 1910.1200Air contaminates –
table of exposure limits and hazard communication
3. Terminology
3.1 See Terminology D4790 for definitions of terms used in this standard.
4. Summary of Test Method
4.1 Bisphenol A is dissolved in methanol, then treated with hydroxylamine hydrochloride to convert any ferric iron present to
ferrous iron. The ferrous iron is then complexed with an iron reagent to form a purple/maroon chromophore that is quantified by
visible spectrophotometry at 560 nm.
5. Significance and Use
5.1 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. Interferences
6.1 No direct interferences have been observed in the use of this method.
7. Apparatus
7.1 Visible Spectrophotometer, 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 quartz
cuvettes.
7.4 All Glassware All Glassware used in this test method should be dedicated and thoroughly cleaned prior to use.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specification of the Committee on Analytical Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy 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 prepared by dissolving 272.0 g 6 0.1g0.1 g of reagent grade sodium acetate in 1000 mL distilled water
and adjusting to pH 5.5 with concentrated hydrochloric acid. Alternate volumes of solutions may be prepared so long as the
preparation meets the concentration specified.
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.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American chemicalChemical Society, see Analar
Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc.
(USPC), Rockville, MD.
D6143 − 23
8.4 Purity of Water, Unless otherwise indicated, references to water shall be understood to mean any reagent conforming to Type
IV I or II of Specification D1193.
8.5 Standard Iron Solution, 100 mg/L (ca. 98 mg/kg) iron chloride in 15 % hydrochloric acid or equivalent. Alternate volumes of
solutions may be 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 Solution—Make up a 10 % by weight aqueous solution.
8.9 Iron Reagent, 3–(2–Pyridyl)-5,6–diphenyl-1,2,4–triazine-p,p’-disulfonic acid, acid (CAS [69898-45-9]), or equivalent.
8.10 Iron Reagent Solution:
8.10.1 In a 1 L volumetric flask, dissolve 1.001.00 g 6 0.01 g of iron reagent in 20 mL of 0.5 N NaOH and dilute to 1 L with
methanol. Alternate volumes of solutions may be prepared so long as the preparation meets the concentration specified.
9. Hazards
9.1 Consult current OSHA regulations, local regulations, and supplier’s Safety Data Sheets for all materials used in this test
method.
10. Sampling and Handling
10.1 Sample bisphenol A (BPA) in accordance with Practice D4297.
11. Calibration
11.1 Weigh into separate 100 mL volumetric flasks, to the nearest 0.01 g, the following amounts of the standard iron solution in
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 solutions
with nominal concentrations of 0.2,0.2 mg 0.5,⁄kg, 0.5 mg 1.0,⁄kg, 1.0 mg 2.0,⁄kg, 2.0 mg 4.0,⁄kg, 4.0 mg 8.0,⁄kg, 8.0 mg ⁄kg, and
10 mg/kg, respectively.
11.2 Prepare and analyze two 10.0 6 0.1 g 10.0
...