ASTM D1065-96(2010)
(Test Method)Standard Test Method for Unsaponifiable Matter in Naval Stores, Including Rosin, Tall Oil, and Related Products
Standard Test Method for Unsaponifiable Matter in Naval Stores, Including Rosin, Tall Oil, and Related Products
SIGNIFICANCE AND USE
This test method is designed to broaden the scope of the previous edition of the test method by the inclusion of tall oil and tall oil derived from products as test materials. Test Methods D803 currently includes a method for the determination of unsaponifiable matter.
The amount of unsaponifiable matter in tall oil and other related products is important in characterizing such products as it indicates the level of nonacidic material, both free and combined, present in the test material. The unsaponifiable in naval stores products is primarily composed of higher molecular weight alcohols, sterols, and hydrocarbons.
SCOPE
1.1 This test method covers the determination of the percentage of material in Naval Stores products as defined in Terminology D804 including rosin, tall oil and related products, other than insoluble dirt or similar visible foreign matter that does not yield a water-soluble soap when the sample is saponified with potassium hydroxide.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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)
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Designation:D1065 −96(Reapproved2010)
Standard Test Method for
Unsaponifiable Matter in Naval Stores, Including Rosin, Tall
Oil, and Related Products
This standard is issued under the fixed designation D1065; 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 Methods D803 currently includes a method for the determina-
tion of unsaponifiable matter.
1.1 This test method covers the determination of the per-
centage of material in Naval Stores products as defined in
3.2 Theamountofunsaponifiablematterintalloilandother
Terminology D804 including rosin, tall oil and related
related products is important in characterizing such products as
products, other than insoluble dirt or similar visible foreign
it indicates the level of nonacidic material, both free and
matter that does not yield a water-soluble soap when the
combined, present in the test material. The unsaponifiable in
sample is saponified with potassium hydroxide.
naval stores products is primarily composed of higher molecu-
lar weight alcohols, sterols, and hydrocarbons.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Apparatus
standard.
4.1 Erlenmeyer or Other Flat-Bottom Flask, of 125-mL to
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 250-mL capacity, with standard-taper 24/40 joint.
responsibility of the user of this standard to establish appro-
4.2 Erlenmeyer Flask, of 250-mL to 300-mL capacity, with
priate safety and health practices and determine the applica-
wide mouth.
bility of regulatory limitations prior to use.
4.3 Separatory Funnels, of 300-mL to 500-mL capacity,
with glass or polytetrafluoroethylene (PFTE) stoppers.
2. Referenced Documents
2.1 ASTM Standards: 4.4 Graduated Cylinder, one of 10 to 25-mL and one of 50
D509 Test Methods of Sampling and Grading Rosin to 100-mL capacity.
D803 Test Methods for Testing Tall Oil
4.5 Beaker, of up to 250-mL capacity.
D804 Terminology Relating to Pine Chemicals, Including
Tall Oil and Related Products
5. Reagents
E177 Practice for Use of the Terms Precision and Bias in
5.1 Purity of Reagents—Reagent grade chemicals shall be
ASTM Test Methods
used in all tests. Unless otherwise indicated, it is intended that
E691 Practice for Conducting an Interlaboratory Study to
all reagents shall conform to the specifications of the Commit-
Determine the Precision of a Test Method
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
3. Significance and Use
used, provided it is first ascertained that the reagent is of
3.1 This test method is designed to broaden the scope of the
sufficiently high purity to permit use without lessening the
previous edition of the test method by the inclusion of tall oil
accuracy of the determination.
and tall oil derived from products as test materials. Test
5.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean distilled, or deionized
water.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
Current edition approved June 1, 2010. Published June 2010. Originally
approved in 1949. Last previous edition approved in 2006 as D1065 – 96 (2006). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D1065-96R10. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1065−96(2010)
6. Preparation of Sample mL water, transfer to a separatory funnel, and rinse the flask
with an additional 20 mL of water that is added to the
6.1 Procurement and handling of samples will vary depend-
separatory funnel. Rinse the flask with 40 mL of ethyl ether,
ing upon the physical state of the material. In all instances, the
adding the ether rinse to the separatory funnel. Stopper and
sampling should conform to accepted sampling techniques
shake the separatory funnel, then allow to stand until the ether
which ensure the sample is representative of the material being
layer separates from the water/soap layer. Drain the aqueous
sampled.
soap layer (lower layer) into a second separatory funnel,
6.2 Uniform liquid material should be mixed well and an
allowing a few drops of the aqueous layer to remain above the
aliquot removed for analysis.Titer in fatty acid samples should
stopcock to prevent loss of ether extract by creepage through
be resolubilized by gentle heating and agitation. Rosin crystal-
the stopcock joint.
lization in liquid samples, such as distilled tall oil (DTO),
8.2 To the aqueous soap layer in the second funnel, add 30
should be resolubilized by heating to 160°C with periodic
mL ether and extract as before. Drain the aqueous soap layer
agitation. Homogeneous representative samples are impera-
into the original saponification flask. Add the ether layer from
tive.
the second separatory funnel to the first separatory funnel,
6.3 Solids that melt at relatively low temperature (that is,
thereby combining the extracts. Pour the aqueous soap layer
tall oil pitch) should be warmed to liquification to facilitate
from the original saponification flask into the second separa-
mixing and pouring. Homogeneous representative samples are
tory funnel, add 30 mL ether and extract for the third time.
imperative.
Drain the aqueous soap layer from the second separatory
6.4 Solids that melt at relatively high temperatures (that is,
funnel into the original saponification flask again, and add the
rosin) should be fractured and chipped if possible, (see Test
ether layer to the first funnel as before, thereby combining it
Methods D509). The sample taken for analysis shall consist of
with the two previous extracts. Now drain off, and add to the
small pieces of rosin chipped from a freshly exposed part of a
soapsolutionalreadyintheoriginalsaponificationflask,allbut
lump of lumps, and thereafter crushed to facilitate weighing
a few drops of aqueous soap solution that has collected at the
and solution. The sample shall be prepared the same day on
bottom of the first separatory funnel below the combined ether
which the test is begun in order to avoid changes in properties
ext
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