ASTM D465-05(2010)
(Test Method)Standard Test Methods for Acid Number of Naval Stores Products Including Tall Oil and Other Related Products
Standard Test Methods for Acid Number of Naval Stores Products Including Tall Oil and Other Related Products
SIGNIFICANCE AND USE
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 will be referenced in Test Methods D803.
The acid number is an important property of naval stores products, tall oil, and the products obtained by the fractionation of tall oil. It is the test method widely used to determine the total free acid content of these products.
The potentiometric test method should be used when the most reproducible results are required.
SCOPE
1.1 These test methods are intended for determining the acid number of naval store products as defined in Terminology D804 including tall oil products, wood and gum rosin, and other related materials. These test methods may not be applicable to all modified rosin products. Two test methods are covered, as follows:
1.1.1 Potentiometric method (referee), and
1.1.2 Internal indicator method (alternate).
1.2 The potentiometric method is suitable for use with both light- and dark-colored products. It should be considered the referee method. The internal indicator method is suitable for use only with light- and medium-colored products with a Gardner color of less than 12. 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D465 − 05 (Reapproved2010)
Standard Test Methods for
Acid Number of Naval Stores Products Including Tall Oil
and Other Related Products
This standard is issued under the fixed designation D465; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope E70 Test Method for pH of Aqueous Solutions With the
Glass Electrode
1.1 Thesetestmethodsareintendedfordeterminingtheacid
E177 Practice for Use of the Terms Precision and Bias in
number of naval store products as defined in Terminology
ASTM Test Methods
D804 including tall oil products, wood and gum rosin, and
E691 Practice for Conducting an Interlaboratory Study to
other related materials. These test methods may not be appli-
Determine the Precision of a Test Method
cable to all modified rosin products. Two test methods are
covered, as follows:
3. Significance and Use
1.1.1 Potentiometric method (referee), and
3.1 These test methods are designed to broaden the scope of
1.1.2 Internal indicator method (alternate).
theearliereditionsofthetestmethodbytheinclusionoftalloil
1.2 The potentiometric method is suitable for use with both
and tall oil derived products as test materials and will be
light- and dark-colored products. It should be considered the
referenced in Test Methods D803.
referee method. The internal indicator method is suitable for
3.2 Theacidnumberisanimportantpropertyofnavalstores
use only with light- and medium-colored products with a
products,talloil,andtheproductsobtainedbythefractionation
Gardner color of less than 12. It should be considered the
of tall oil. It is the test method widely used to determine the
alternate method.
total free acid content of these products.
1.3 The values stated in SI units are to be regarded as
3.3 Thepotentiometrictestmethodshouldbeusedwhenthe
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 and health practices and determine the applica-
lump or lumps, and thereafter crushed to facilitate weighing
bility of regulatory limitations prior to use.
and dissolution. Prepare the sample the same day on which the
test is begun, in order to avoid changes in properties due to
2. Referenced Documents
surface oxidation. This is very pronounced on ground rosin
2.1 ASTM Standards:
having a large surface area exposed to the air. Existing rosin
D803 Test Methods for Testing Tall Oil
dust and powdered rosin must not be used.
D804 Terminology Relating to Pine Chemicals, Including
4.2 If the sample is a nonhomogenous liquid, heat the entire
Tall Oil and Related Products
sample in a closed container fitted with a capillary vent or the
equivalent. Some kind of agitation, even if done occasionally
byhand,savesmuchtime.Heatbyimmersioninopensteamor
These test methods are under the jurisdiction of ASTM Committee D01 on
hot water bath to avoid overheating. When dealing with
Paint and Related Coatings, Materials, and Applications and are the direct
crystallized rosin a temperature of approximately 160°C may
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
Resins. be needed. Sampling should take place only when the entire
Current edition approved June 1, 2010. Published June 2010. Originally
sample is homogeneous and has been well stirred.
approved in 1937. Last previous edition approved in 2005 as D465 – 05. DOI:
10.1520/D0465-05R10. 4.3 For other products no special preparation is necessary
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
except storage in a closed container prior to testing.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D465 − 05 (2010)
4.4 Guideline for sample size, solvent, and titrant: the same equipment and techniques as used in the actual acid
number determination.
Sample Size, Solvent I, Solvent II, Titrant,
Sample g mL mL KOH
7.2 Alkali, Standard Solution (0.1 N)—Dissolve 6.6 g of
Fatty acids 4.0 ± 0.05 Isopropyl None 0.5N potassium hydroxide (KOH) (pellets or sticks) in methyl
A
DTO alcohol, or
alcohol conforming to 7.4, and dilute to 1 L with the same
Rosin soap
methanol
solvent.Standardizeto 60.001Nbydissolvingpotassiumacid
phthalate (KHP) in 60 mLof water followed by the addition of
FA esters 20 ± 0.1 Isopropyl None 0.1N
40 mL of isopropyl alcohol once the KHP has dissolved;
alcohol, or
0.5106 g of KHPwill be neutralized by 25.0 mLof 0.1 N KOH
methanol
solution. Protect the standardized solution against evaporation
and absorption of carbon dioxide (CO ) from the air. The
Rosin 4.0 ± 0.05 Toluene 25 Isopropyl 0.5N
A
solution should be standardized frequently, either potentio-
CTO alcohol 75
Pitch
metrically or colorimetrically using either phenolphthalein or
thymol blue as the indicator. The standardization should use
Rosin esters 10 ± 0.1 Toluene 25 Isopropyl 0.1N
the same equipment and techniques as used in the actual acid
10±0.1g alcohol 75
number determination.
A
DTO represents distilled tall oil, while CTO represents crude tall oil.
7.3 Isopropyl Alcohol, as in 5.1.
5. Purity of Reagents and Water
7.4 Methyl Alcohol, as in 5.1.
5.1 Unless otherwise indicated, it is intended that all re-
7.5 Toluene, as in 5.1.
agents shall conform to the specifications established by the
7.6 Borax Buffer, Standard Solution (0.01 M, pH 9.18 at
Committee on Analytical Reagents of the American Chemical
25°C)—Dissolve 3.81 6 0.01 g of disodium tetraborate
Society, where such specifications are available. References to
(Na B O 10H O) in water and dilute to 1 L in a volumetric
2 4 7 2
watershallbeunderstoodtomeandistilledordeionizedwater.
flask. Use the special grade of borax prepared specifically for
use as a pH standard. As an alternative, a commercially
POTENTIOMETRIC METHOD (REFEREE METHOD)
available buffer with a pH between 9 and 11 may be used
6. Apparatus instead of self-prepared standard.
6.1 Glass Electrode pH Meter, conforming to the require-
8. Standardization of Apparatus
ments of Test Method E70. Use either standard or alkali-
8.1 Adjust the pH meter with the standard buffer solution
resistant electrodes for this test. An automatic potentiometric
from 7.6, following essentially the same procedure as de-
titrator may be used in place of a pH meter.
scribed in Test Method E70.
6.2 Buret, 50 mL with 0.1 mL divisions.
6.3 Stirrer, variable-speed with polytetrafluoroethylene 9. Procedure
(PTFE) coated magnetic stir bar or other type mechanical
9.1 Transfer the prescribed amount of sample recommended
stirrer.
in 4.4, weighed to the nearest 0.001 g, to a 400-mL tall-form
6.4 Beaker, 400-mL tall-form.
beaker.Add the proper amount of solvent I (see 4.4) and swirl
to dissolve. Heat gently if necessary to di
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