ASTM D8266-19

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.
Designation: D8266 − 19
Standard Test Method for
Analysis of Bisphenol A (4,4'-Isopropylidenediphenol) by
High Performance Liquid Chromatography
This standard is issued under the fixed designation D8266; 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 -Isopropylidinediphenol)
D6809 Guide for Quality Control and Quality Assurance
1.1 This test method covers the determination of trace
Procedures for Aromatic Hydrocarbons and Related Ma-
impurities in bisphenol A (4,4'-Isopropylidenediphenol) by
terials
reverse-phase gradient high performance liquid chromatogra-
E29 Practice for Using Significant Digits in Test Data to
phy (HPLC). It is generally meant for the analysis of bisphenol
Determine Conformance with Specifications
A of 99.5 % or greater.
E691 Practice for Conducting an Interlaboratory Study to
1.2 This method is applicable to bisphenol A samples
Determine the Precision of a Test Method
containing impurity concentration between 2 and 400 mg/kg.
2.2 Other document:
Users of this method believe it is linear over a wider range.
OSHA Regulations 29 CFR paragraphs 1910.1000 and
1.3 In determining the conformance of the test results using
1910.1200
thismethodtoapplicablespecification,resultsshallberounded
off in accordance with the rounding-off method of Practice
3. Summary of Test Method
E29.
3.1 A known amount of an internal standard is added to a
1.4 The values stated in SI units are to be regarded as
sample of bisphenol A. The prepared sample is mixed and
standard. No other units of measurement are included in this
analyzed by a reverse-phase gradient liquid chromatography
standard.
(HPLC)equippedwithanultravioletdetector.Thepeakareaof
1.5 This standard does not purport to address all of the
each impurity and the internal standard is measured. The
safety concerns, if any, associated with its use. It is the
amountofeachimpurityiscalculatedfromtheratioofthepeak
responsibility of the user of this standard to establish appro-
area of the internal standard versus the peak area of the
priate safety, health, and environmental practices and deter-
impurity.
mine the applicability of regulatory limitations prior to use.
For a specific hazard statement, see Section 8.
4. Significance and Use
1.6 This international standard was developed in accor-
4.1 Bisphenol A is used for production of polycarbonate or
dance with internationally recognized principles on standard-
epoxy resin. The presence of impurities in bisphenol A is
ization established in the Decision on Principles for the
undesirable because they may slow down the polymerization
Development of International Standards, Guides and Recom-
and be impurities in the final product.
mendations issued by the World Trade Organization Technical
4.2 Determination of the trace impurities, such as isomer of
Barriers to Trade (TBT) Committee.
bisphenol A and the unreacted raw material, is often required.
2. Referenced Documents
This test method is suitable for setting specifications and for
using as an internal quality control where these products are
2.1 ASTM Standards:
produced or used.
D4297 PracticeforSamplingandHandlingBisphenolA(4,4'
4.3 Purity is commonly reported by subtracting the deter-
mined expected impurities and water from 100 %. However, a
This test method is under the jurisdiction of ASTM Committee D16 on
HPLC analysis cannot determine absolute purity if unknown
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
components are contained within the material being examined.
bility of Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved June 1, 2019. Published November 2019. DOI:
10.1520/D8266-19.
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 Available from U.S. Government Printing Office, Superintendent of
Standards volume information, refer to the standard’s Document Summary page on Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
the ASTM website. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8266 − 19
5. Interferences Society, where such specifications are available. Other grades
may be used, provided it is first ascertained that the reagent is
5.1 The internal standard chosen must be sufficiently re-
of sufficiently high purity to permit its use without lessening
solved from any impurity and the bisphenol A peak.
the performance or accuracy of the determination. Reagent
5.2 Anysolventusedmustalsobesufficientlyresolvedfrom
chemicals shall be used for all tests.
any impurity, the internal standard, and the bisphenol A peak. NOTE 1—Calibration and detection limits of this test method can be
biased by the purity of the reagents.
6. Apparatus
7.2 Bisphenol A Standard for Calibration—A certified bis-
phenolAcalibration standard should be 99.9 % purity or high,
6.1 High Performance Liquid Chromatograph (HPLC)—
and must also be sufficiently resolved from any impurity in the
Any HPLC capable of pumping the mobile phase at flow rates
samples.
between 0.1 and 2.0 mL/min. The system should have suffi-
cient sensitivity to obtain a minimum peak height response for 7.3 Purity of Water—HPLC grade.
a 2 mg/kg impurity twice the height of the signal background
7.4 Methanol—HPLC grade.
noise.
7.5 Acetonitrile—HPLC grade.
6.2 Sample Injection System—Capable of injecting 20 µLof
7.6 Pure Compounds for Calibration—Shall include phenol
testing solution with a repeatability of no more than 1 %.
(CAS No. 108-95-2), indane bisphenol (CAS No. 10527-11-4),
6.3 Detector—Variable wavelength ultraviolet photometric
2,4-isopropylidenebisphenol(CASNo.837-08-1,theisomerof
detector (VWD), multi-wavelength detector, or photometric bisphenol A), and chromanone component (I) (CAS No.
diode array detector (PDA)—capable of operating at 280 nm.
472-41-3, 4- (2,2,4-trimethylbenzopyran-4-yl) phenol). The
purity of all reagents should be 95.0 % or greater. The
6.4 Column Oven—Any suitable HPLC column oven (block
concentration and identification of impurities must be known
heating or air circulating) capable of maintaining a constant
so that the composition of the standard can be adjusted for the
temperature within the range of 20 to 70.
presence of the impurities.
6.5 Chromatography Data System.
7.7 Internal Standard—o-cresol is one possible internal
6.6 HPLC Columns: standard. However, other compounds may be found acceptable
provided they meet the criteria as defined in Section 5 and 7.6.
6.6.1 A stainless steel HPLC column packed with an octa-
decylsilane (C18) chemically bonded silica stationary phase is
7.8 Internal Standard Solution—30 mg/kg. Weigh 0.03 g
suitable. See Table 1 for recommended operating conditions.
o-cresol in 7.7 and 50 g acetonitrile, to the nearest 0.0001 g,
6.6.2 A C18 column with different dimensions (inner
into a 100-mL Erlenmeyer flask, cap the flask and mix well.
diameter, length, particle size, etc.) that provides adequate
Weigh2gofthe above solution and 40 g acetonitrile, to the
resolution to impurities in a bisphenol A sample can also be
nearest0.0001g,intoa100-mLErlenmeyerflask,captheflask
used.
and mix well. Calculate the mass fraction of o-cresol in the
internal standard solution.
6.7 Analytical Balance—Readable to 60.0001 g.
7.9 Mobile Phase:
6.8 Sample Filter—A disposable syringe filter made of
7.9.1 Solution A is acetonitrile:methanol = 9:1 (volume
cellulose acetate, with a pore size between 0.22 and 0.45 µm,
ratio), Solution B is water.
and is chemically inert to aqueous solutions, is recommended
7.9.2 Gradient—The starting composition of the mobile
for the removal of particulate matter from the sample solution.
phase is Solution A:Solution B = 30:70 (volume ratio),
followed by a gradual increase in the concentration of Solution
7. Reagents and Materials
A, and the composition of mobile ph
...