ASTM D6143-97

Standard Test Method for Iron Content of Bisphenol A (4,4&#180 - Isopropylidenediphenol)

SCOPE
1.1 This test method describes the procedure to determine the iron content of bisphenol A (4,4' -isopropylidenediphenol).
1.2 This test method has a lower detection limit of 0.1 mg/kg, and an upper limit of 20 mg/kg of iron in bisphenol A. If the iron content is higher, it will be necessary to dilute the sample.
1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding off method of Practice E 29.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8.

General Information

• Status: Historical
• Publication Date: 09-Jun-1997
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Replaced By: ASTM D6143-05 - Standard Test Method for Iron Content of Bisphenol A (4,4´ - Isopropylidenediphenol)
• Effective Date: 01-Jul-2005
• Referred By: ASTM E1615-22 - Standard Test Method for Determination of Trace Quantities of Iron by Visible Spectrophotometry
• Effective Date: 10-Jun-1997

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 6143 – 97
Standard Test Method for
Iron Content of Bisphenol A (4,4* - Isopropylidenediphenol)
This standard is issued under the fixed designation D 6143; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope ferrous iron. The ferrous iron is then complexed with Fer-
roZine to form a red/pink chromophore that is quantified by
1.1 This test method describes the procedure to determine
visible spectrophotometry at 560 nm.
the iron content of bisphenol A (4,48-isopropylidenediphenol).
1.2 This test method has a lower detection limit of 0.1
4. Significance and Use
mg/kg, and an upper limit of 20 mg/kg of iron in bisphenolA.
4.1 Iron may increase the color of bisphenol A and affect
If the iron content is higher, it will be necessary to dilute the
other properties of end-use products.
sample.
4.2 High purity bisphenolAtypically has less than 2 mg/kg
1.3 The following applies to all specified limits in this test
of iron.
method: for purposes of determining conformance with this
test method, an observed value or a calculated value shall be
5. Interferences
rounded off “to the nearest unit” in the last right-hand digit
5.1 Acetone and ethanol cause slow color development and
used in expressing the specification limit, in accordance with
should not be used as solvents for this test method.
the rounding off method of Practice E 29.
1.4 This standard does not purport to address all of the
6. Apparatus
safety concerns, if any, associated with its use. It is the
6.1 Vis. Spectrophotometer.
responsibility of the user of this standard to establish appro-
6.2 Glass cell,10cm.
priate safety and health practices and determine the applica-
6.3 Volumetric Flasks, 100 mL and 1000 mL.
bility of regulatory limits prior to use. For a specific hazard
statement, see Section 8. NOTE 1—All glassware used in this test method should be dedicated
and thoroughly cleaned prior to use, by rinsing with concentrated
2. Referenced Documents
hydrochloric acid solution followed by ferrozine solution, prepared as a
blank in Section 7.
2.1 ASTM Standards:
D 1193 Specification for Reagent Water 6.4 pH Meter.
D 4297 Practice for Sampling and Handling Bisphenol A
3 7. Reagents and Materials
(4,48 - Isopropylidenediphenol)
E 29 Practice for Using Significant Digits in Test Data to 7.1 Hydrochloric Acid, concentrated, American Chemical
Society (ACS) reagent grade.
Determine Conformance with Specifications
E 691 Practice for Conducting an Interlaboratory Study to 7.2 Methanol, ACS reagent grade. Do not use methanol
stored in steel containers.
Determine Precision of a Test Method
2.2 Other Documents: 7.3 Sodium Acetate,2 M solution, ACS reagent grade.
7.3.1 This solution may be prepared by dissolving 272.0 g
OSHA Regulations 29CFR paragraphs 1910.1000 and
1910.1200. 6 0.1g of ACS reagent grade sodium acetate trihydrate or
164.0 60.1gofACSreagentgradesodiumacetatein1000mL
3. Summary of Test Method
distilled water.
3.1 Bisphenol A is dissolved in methanol, then acidified 7.3.2 The sodium acetate trihydrate or sodium acetate may
with hydrochloric acid to convert any ferric iron present to contain iron and should be purified as follows: To a separatory
funnel, add 10 mL of bathophenanthroline solution (prepared
by dissolving 0.25 g bathophenanthroline in 250 mL metha-
This test method is under the jurisdiction of ASTM Committee D16 on
nol), and 100 mL of 2 M solution of sodium acetate, and mix
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
D16.02 on Oxygenated Aromatics. well. Add 15 mL of chloroform and shake the solution for 30
Current edition approved June 10, 1997. Published August 1997.
s.Allowthelayerstoseparate.Drawoffanddiscardthebottom
Annual Book of ASTM Standards, Vol 11.01.
red layer. Repeat the extraction with 15-mL portions of
Annual Book of ASTM Standards, Vol 06.04
chloroform until the bottom layer is colorless.
Annual Book of ASTM Standards, Vol 14.02.
Available from the Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6143
7.4 Distilled Water, conforming to Type IV of Specification
5.00 0.5
10.00 1.0
D 1193.
7.5 Standard Iron Solution, 1000 mg/L.
9.4 Zero the vis-spectrophotometer at 560 nm with the
7.5.1 The iron solution is prepared by digesting 1.00 g of
blank.
ACS reagent grade iron with 4 mL of concentrated ACS
9.5 Measure the absorbance at 560 nm of the three prepared
reagent grade hydrochloric acid in a 100-mL beaker until a
calibration solutions.
clear solution is obtained. This solution is quantitatively
9.6 Plot a standard curve of absorbance versus iron concen-
transferred into a 1000-mL volumetric flask, with careful
tration. The range covered is 0.1 to 1.0 mg/kg.
rinsing, containing about 500 mL of distilled water. The flask
9.7 Calculate an absorbance factor ( F) as the inverse of the
is then diluted to the mark with distilled water.
slope of a line drawn through data plotted in 9.6 as follows:
7.6 Sodium Hydroxide, 0.5 normal, ACS Reagent grade.
F 5 @1/ ~ d~Ab! / d~mg/L!# (1)
7.7 Ferrozine, 0.1 % in methanol.
7.8 Bathophenanthroline, 0.1 % in
...