ASTM D464-05(2010)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D464 −05(Reapproved2010)
Standard Test Methods for
Saponification Number of Naval Store Products Including
Tall Oil and Other Related Products
This standard is issued under the fixed designation D464; 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 Tall Oil and Related Products
E70 Test Method for pH of Aqueous Solutions With the
1.1 These test methods cover the determination of the
Glass Electrode
saponification number of tall oil and products obtained by the
fractionation of tall oil such as rosin, fatty acids and distilled
3. Significance and Use
talloilasdefinedinTerminologyD804.Thesetestmethodsare
3.1 These test methods are designed to broaden the scope of
also applicable to gum and wood rosin. Two test methods are
theearliereditionsofthetestmethodbytheinclusionoftalloil
covered as follows:
and tall oil derived products as test materials and is referenced
1.1.1 Test method using a potentiometric method, and
in Test Methods D803.
1.1.2 Test method using an internal indicator method.
3.2 The saponification number is an important property of
1.2 The potentiometric method is suitable for use with both
talloilandtheproductsobtainedbythefractionationoftalloil.
light- and dark-colored test samples. It should be considered
It is the test method widely used to determine the total acid
the referee method. The internal indicator method is suitable
content, both free and combined, of these products.
for use only with light- and medium-colored test samples. It
should be considered the alternate method.
3.3 The potentiometric test method should be used when the
most reproducible results are required.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Preparation of Sample
standard.
4.1 If the sample for analysis is rosin, it shall consist of
1.4 This standard does not purport to address all of the
small pieces of rosin chipped from a freshly exposed part of a
safety concerns, if any, associated with its use. It is the
lump or lumps, and thereafter crushed to facilitate weighing
responsibility of the user of this standard to establish appro-
and dissolution. Prepare the sample the same day on which the
priate safety and health practices and determine the applica-
test is begun in order to avoid changes in properties due to
bility of regulatory limitations prior to use.
surface oxidation. Changes are very pronounced on ground
rosin that has a large surface area exposed to air. Existing rosin
2. Referenced Documents
dust and powdered rosin must not be used.
2.1 ASTM Standards:
4.2 If the sample is a nonhomogeneous liquid, heat the
D803 Test Methods for Testing Tall Oil
entire sample in a closed container fitted with a capillary vent
D804 Terminology Relating to Pine Chemicals, Including
or the equivalent. Some kind of agitation, even if done
occasionally by hand, saves much time. Heat by immersion in
open steam or hot water bath to avoid overheating. When
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct dealing with crystallized rosin, a higher temperature of ap-
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
proximately 160°C may be needed. Remove samples for
Resins.
testing only when the entire sample is homogeneous and has
Current edition approved June 1, 2010. Published June 2010. Originally
been well stirred.
approved in 1937. Last previous edition approved in 2005 as D464 – 05. DOI:
10.1520/D0464-05R10.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5. Purity of Reagents and Water
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.1 Unless otherwise indicated, it is intended that all re-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. agents shall conform to the specifications established by the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D464−05(2010)
Committee on Analytical Reagents of the American Chemical ment and techniques as used in the actual saponification
Society, wheresuchspecificationsareavailable.Referencesto number determination.
water shall be understood to mean distilled or deionized water.
7.5 Acid, Standard (0.5 N)—Standardize a 0.5 N solution of
HCl to 60.001 N by any accepted procedure.
POTENTIOMETRIC TEST METHOD (Referee Method)
7.6 Borax Buffer, Standard Solution (0.01 M, pH 9.18 at
25°C)—Dissolve 3.81 6 0.01 g of disodium tetraborate
6. Apparatus
(Na B 07·10 H O) in water and dilute to 1 L in a volumetric
2 4 2
flask. Use the special grade of borax prepared specifically for
6.1 Erlenmeyer Flask, 250-mL, of chemically resistant
use as a pH standard.As an alternative, commercially available
glass with standard-taper glass joint.
buffer with a pH between 9 and 11 may be used.
6.2 Hot Plates.
6.3 Water-Cooled Reflux Condenser, with standard-taper
8. Procedure
joint to fit the Erlenmeyer flask.
8.1 Transfer 2.95 to 3.05 g of the sample, weighed to the
6.4 Buret, with 0.1 mL divisions.
nearest 0.001 g, to the Erlenmeyer flask. If necessary, 10 mLof
isopropyl alcohol-toluene solution (1:1) can be added to the
6.5 Stirrer, variable-speed, with a polytetrafluoroethylene
flask to predissolve the sample. Using a constant delivery pipet
(PTFE) coated magnetic stir bar.
or volumetric pipet add 50.0 mL of the alkali solution. Add
6.6 Delivery or Volumetric Pipet, 50-mL constant.
several PTFE boiling stones or glass beads and connect the
6.7 PTFE Boiling Stones, or glass beads.
flask to the condenser.
6.8 Beaker, 400-mL tall-form.
8.2 Place the flask on a hot plate and maintain the solution
at reflux for 1 h.At the end of the reflux time, while the sample
6.9 Glass Electrode pH Meter, conforming to the require-
is still warm, transfer the contents of the Erlenmeyer flask into
ments of Test Method E70. Use either standard or alkali-
a 400-mL tall-form beaker rinsing with 100 mL of isopropyl
resistant electrodes for this test. Alternatively, an automatic
alcohol in three washings. Place samples on a heated surface
potentiometric titrator may be used.
until they can be titrated. In order to avoid highly variable
results, make sure that the temperature of the samples is
7. Reagents
approximately 60 to 70°C when titrated.
7.1 Ethyl Alcohol (95 %) denatured by Formula No. 3A or
8.3 Titratewith0.5Nacid,recordingtheburetandpHmeter
No. 30 of the U.S. Bureau of Internal Revenue.
readings. Sufficient acid may be added initially to bring the pH
7.2 Isopropyl Alcohol, Reagent grade.
of the solution to about 12. Allow sufficient time for the
7.3 Toluene, Reagent grade.
electrode system to reach equilibrium. Add acid in 1.0-mL
portions until the change in pH per addition exceeds 0.3 pH
7.4 Alkali Solution, Standard Alcoholic (0.5 N)—Dissolve
units. Reduce the additions of acid to 0.1 mL or smaller until
33 g of potassium hydroxide (KOH), preferably in pellet form,
the end point has been passed, as indicated by a significant
in ethyl alco
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