ASTM D464-15(2020)
(Test Method)Standard Test Methods for Saponification Number of Pine Chemical Products Including Tall Oil and Other Related Products
Standard Test Methods for Saponification Number of Pine Chemical Products Including Tall Oil and Other Related Products
SIGNIFICANCE AND USE
3.1 These test methods are designed to broaden the scope of the earlier editions of the test method by the inclusion of tall oil and tall oil derived products as test materials and is referenced in Test Methods D803.
3.2 The saponification number is an important property of tall oil and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the total acid content, both free and combined, of these products.
3.3 The potentiometric test method should be used when the most reproducible results are required.
SCOPE
1.1 These test methods cover the determination of the saponification number of tall oil and products obtained by the fractionation of tall oil such as rosin, fatty acids and distilled tall oil as defined in Terminology D804. These test methods are also applicable to gum and wood rosin. Two test methods are covered as follows:
1.1.1 Test method using a potentiometric method, and
1.1.2 Test method using an internal indicator method.
1.2 The potentiometric method is suitable for use with both light- and dark-colored test samples. It should be considered the referee method. The internal indicator method is suitable for use only with light- and medium-colored test samples. It should be considered the alternate method.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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.
General Information
Relations
Standards Content (Sample)
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: D464 −15 (Reapproved 2020)
Standard Test Methods for
Saponification Number of Pine Chemical 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 D804 Terminology Relating to Pine Chemicals, Including
Tall Oil and Related Products
1.1 These test methods cover the determination of the
E70 Test Method for pH of Aqueous Solutions With the
saponification number of tall oil and products obtained by the
Glass Electrode
fractionation of tall oil such as rosin, fatty acids and distilled
talloilasdefinedinTerminologyD804.Thesetestmethodsare
3. Significance and Use
also applicable to gum and wood rosin. Two test methods are
covered as follows:
3.1 These test methods are designed to broaden the scope of
1.1.1 Test method using a potentiometric method, and
theearliereditionsofthetestmethodbytheinclusionoftalloil
1.1.2 Test method using an internal indicator method.
and tall oil derived products as test materials and is referenced
in Test Methods D803.
1.2 The potentiometric method is suitable for use with both
light- and dark-colored test samples. It should be considered
3.2 The saponification number is an important property of
the referee method. The internal indicator method is suitable
talloilandtheproductsobtainedbythefractionationoftalloil.
for use only with light- and medium-colored test samples. It
It is the test method widely used to determine the total acid
should be considered the alternate method.
content, both free and combined, of these products.
1.3 The values stated in SI units are to be regarded as
3.3 The potentiometric test method should be used when the
standard. No other units of measurement are included in this
most reproducible results are required.
standard.
1.4 This standard does not purport to address all of the
4. Preparation of Sample
safety concerns, if any, associated with its use. It is the
4.1 If the sample for analysis is rosin, it shall consist of
responsibility of the user of this standard to establish appro-
small pieces of rosin chipped from a freshly exposed part of a
priate safety, health, and environmental practices and deter-
lump or lumps, and thereafter crushed to facilitate weighing
mine the applicability of regulatory limitations prior to use.
and dissolution. Prepare the sample the same day on which the
1.5 This international standard was developed in accor-
test is begun in order to avoid changes in properties due to
dance with internationally recognized principles on standard-
surface oxidation. Changes are very pronounced on ground
ization established in the Decision on Principles for the
rosin that has a large surface area exposed to air. Existing rosin
Development of International Standards, Guides and Recom-
dust and powdered rosin must not be used.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4.2 If the sample is a nonhomogeneous liquid, heat the
entire sample in a closed container fitted with a capillary vent
2. Referenced Documents
or the equivalent. Some kind of agitation, even if done
2.1 ASTM Standards:
occasionally by hand, saves much time. Heat by immersion in
D803 Test Methods for Testing Tall Oil
open steam or hot water bath to avoid overheating. When
dealing with crystallized rosin, a higher temperature of ap-
These test methods are under the jurisdiction of ASTM Committee D01 on
proximately 160°C may be needed. Remove samples for
Paint and Related Coatings, Materials, and Applications and are the direct
testing only when the entire sample is homogeneous and has
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
Resins. been well stirred.
Current edition approved June 1, 2020. Published June 2020. Originally
approved in 1937. Last previous edition approved in 2015 as D464 – 15. DOI:
5. Purity of Reagents and Water
10.1520/D0464-15R20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1 Unless otherwise indicated, it is intended that all re-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
agents shall conform to the specifications established by the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Committee on Analytical Reagents of the American Chemical
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D464 − 15 (2020)
Society, wheresuchspecificationsareavailable.Referencesto 7.5 Acid, Standard (0.5 N)—Standardize a 0.5 N solution of
water shall be understood to mean distilled or deionized water. HCl to 60.001 N by any accepted procedure.
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
POTENTIOMETRIC TEST METHOD (Referee Method)
(Na B 07·10 H O) in water and dilute to 1 L in a volumetric
2 4 2
6. Apparatus flask. Use the special grade of borax prepared specifically for
use as a pH standard.As an alternative, commercially available
6.1 Erlenmeyer Flask, 250-mL, of chemically resistant
4 buffer with a pH between 9 and 11 may be used.
glass with standard-taper glass joint.
8. Procedure
6.2 Hot Plates.
8.1 Transfer 2.95 to 3.05 g of the sample, weighed to the
6.3 Water-Cooled Reflux Condenser, with standard-taper
joint to fit the Erlenmeyer flask. nearest 0.001 g, to the Erlenmeyer flask. If necessary, 10 mLof
isopropyl alcohol-toluene solution (1:1) can be added to the
6.4 Buret, with 0.1 mL divisions.
flask to pre-dissolve the sample. Using a constant delivery
6.5 Stirrer, variable-speed, with a polytetrafluoroethylene
pipet or volumetric pipet add 50.0 mL of the alkali solution.
(PTFE) coated magnetic stir bar.
Add several PTFE boiling stones or glass beads and connect
the flask to the condenser.
6.6 Delivery or Volumetric Pipet, 50-mL constant.
8.2 Place the flask on a hot plate and maintain the solution
6.7 PTFE Boiling Stones, or glass beads.
at reflux for 1 h.At the end of the reflux time, while the sample
6.8 Beaker, 400-mL tall-form.
is still warm, transfer the contents of the Erlenmeyer flask into
6.9 Glass Electrode pH Meter, conforming to the require-
a 400-mL tall-form beaker rinsing with 100 mL of isopropyl
ments of Test Method E70. Use either standard or alkali-
alcohol in three washings. Place samples on a heated surface
resistant electrodes for this test. Alternatively, an automatic
until they can be titrated. In order to avoid highly variable
potentiometric titrator may be used.
results, make sure that the temperature of the samples is
approximately 60 to 70°C when titrated.
7. Reagents
8.3 Titratewith0.5Nacid,recordingtheburetandpHmeter
7.1 Ethyl Alcohol—(95 %) denatured by Formula No. 3Aor
readings. Sufficient acid may be added initially to bring the pH
No. 30 of the U.S. Bureau of Internal Revenue.
of the solution to about 12. Allow sufficient time for the
7.2 Isopropyl Alcohol, 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
7.3 Toluene, Reagent grade.
units. Reduce the additions of acid to 0.1 mL or smaller until
7.4 Alkali Solution, Standard Alcoholic (0.5 N)—Dissolve
the end point has been passed, as indicated
...
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