Standard Test Methods for Iron in Rosin Tall Oil Fatty Acids and Other Related Products (Withdrawn 2002)

SCOPE
1.1 These test methods cover colorimetric procedures for the determination of iron in rosin tall oil fatty acids and other related products. Both spectrophotometric and visual methods are covered.  
1.2 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.

General Information

Status
Withdrawn
Publication Date
31-Dec-1996
Withdrawal Date
09-May-2002
Current Stage
Ref Project

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ASTM D1064-97 - Standard Test Methods for Iron in Rosin Tall Oil Fatty Acids and Other Related Products (Withdrawn 2002)
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1064 – 97
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods for
Iron in Rosin Tall Oil Fatty Acids and Other Related
Products
This standard is issued under the fixed designation D 1064; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope tee on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
1.1 These test methods cover colorimetric procedures for
used, provided it is first ascertained that the reagent is of
the determination of iron in rosin tall oil fatty acids and other
sufficiently high purity to permit its use without lessening the
related products. Both spectrophotometric and visual methods
accuracy of the determination.
are covered.
3.2 Unless otherwise indicated, references to water shall be
1.2 This standard does not purport to address all of the
understood to mean deionized or distilled water.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
SPECTROPHOTOMETRIC METHOD
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
4.1 Ferrous iron, in a dilute hydrochloric acid solution,
2. Significance and Use
forms a red-colored complex with 1,10-phenanthroline. The
2.1 Iron is a possible contaminant in naval stores products,
intensity of the color is measured at approximately 505 nm by
being introduced into these products during their production
means of a spectrophotometer.
from various raw material sources. Gum rosin in particular is
prone to iron contamination as the equipment used for its
5. Apparatus
collection and processing is often made from iron containing
5.1 Photometer—Any spectrophotometer or filter photom-
metals.
eter that will measure accurately the transmittance of the
2.2 Iron is a troublesome contaminant in rosin and fatty
solutions in the range from 500 to 520 nm.
acids, as even trace quantities will catalyze the oxidation and a 3
5.2 Dishes, high-silica glass, silica, or porcelain, 50 and
subsequent darkening of these products.
100-mL capacity.
2.3 The test methods described in this standard were devel-
NOTE 1—Platinum or platinum-rhodium dishes are not recommended
oped many years ago and to a large extent have been replaced
as they sometimes cause a color interference with the phenanthroline
by modern instrumental methods such as atomic absorbance
reagent.
and inductively coupled plasma spectroscopies. The test meth-
5.3 Watch Glasses, to cover the dishes described in 5.2.
ods described in this standard are subject to interferences from
5.4 Pipets—One 100-mL, two 10-mL, three 5-mL, and two
other species in the sample being tested. However, the test
2-mL pipets.
methods described here are acceptable if approximate or trend
5.5 Measuring Pipet, Mohr-type, 10-mL.
values are required and if appropriate analytical instrumenta-
5.6 Volumetric Flasks, 1-L and 50-mL capacities.
tion is not available.
5.7 Absorption Cells, having a capacity of at least 25 mL.
3. Reagents
3.1 Purity of Reagents—Reagent grade chemicals shall be
Reagent Chemicals, American Chemical Society Specifications, American
used in all tests. Unless otherwise indicated, it is intended that
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
all reagents shall conform to the specifications of the Commit-
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopoeial Convention, Inc. (USPC), Rockville,
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint MD.
and Related Coatings, Materials, and Applications and are the direct responsibility The sole source of supply of the high-silica glass known to the committee at
of Subcommittee D01.34 on Naval Stores. this time is Vycor. If you are aware of alternative suppliers, please provide this
Current edition approved June 10, 1997. Published September 1997. Originally information to ASTM Headquarters. Your comments will receive careful consider-
published as D 1064 – 49. Last previous edition D 1064 – 93. ation at a meeting of the responsible technical committee, which you may attend.
D 1064
Smaller cells may be used when the color is developed in a 2). When the iron content is too high to be read from the
flask or beaker. calibration curve, take a smaller aliquot and dilute to 10 mL
with water. Add 2 mL of hydroxylamine hydrochloride or
6. Reagents
hydroquinone solution, 5 mL of 1,10-phenanthroline solution,
6.1 Hydrochloric Acid (1 + 19)—Dilute 1 volume of A.C.S. and 5 mL of sodium acetate solution, using volumetric pipets.
grade HCl (sp gr 1.18) with 19 volumes of water.
Mix thoroughly after each addition.
6.2 Iron Solution, Standard (1 mL 5 0.1 mg Fe)—Dissolve
NOTE 2—When 25-mL absorption cells are not available for the
0.1000 g of pure iron wire (99.85 % iron) in 10 mL of H SO
2 4
spectrophotometer, develop color as described in 7.4, but in a flask,
(1 + 9) and 3 mL of HNO (sp gr 1.42). Dilute with water to 1
3 beaker, or large test tube, and transfer an aliquot of the solution to a
L in a volumetric flask.
suitable absorption cell.
6.3 Iron Solution, Standard (1 mL 5 0.01 mg Fe)—Pipet
8.5 Blank—Run a blank along with the sample to be sure
100 mL of standard iron solution (1 mL 5 0.1 mg Fe) into a
none of the reagents have become contaminated (Note 3) and
1-L volumetric flask and dilute to the mark with HCl (1 + 19).
for a reference solution against which the transmittance of the
6.4 Hydroxylamine Hydrochloride Solution—Dissolve 10 g
sample is measured. Measure the transmittance of the blank
of (c.p.) hydroxylamine hydrochloride in 190 mL of water.
with the spectrophotometer adjusted to read 100 % transmit-
This reagent is stable at room temperature.
tance, or zero percent absorbance at a wavelength of 505 nm
6.5 Hydroquinone Solution—Dissolve 2.5 g of hydro-
when the absorption cel
...

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