ASTM D1065-96(2006)
(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 D 803 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 D 804 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.
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
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D1065 – 96 (Reapproved 2006)
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 3.2 Theamountofunsaponifiablematterintalloilandother
related products is important in characterizing such products as
1.1 This test method covers the determination of the per-
it indicates the level of nonacidic material, both free and
centage of material in Naval Stores products as defined in
combined, present in the test material. The unsaponifiable in
Terminology D804 including rosin, tall oil and related prod-
naval stores products is primarily composed of higher molecu-
ucts, other than insoluble dirt or similar visible foreign matter
lar weight alcohols, sterols, and hydrocarbons.
that does not yield a water-soluble soap when the sample is
saponified with potassium hydroxide.
4. Apparatus
1.2 The values stated in SI units are to be regarded as
4.1 Erlenmeyer or Other Flat-Bottom Flask, of 125-mL to
standard. No other units of measurement are included in this
250-mL capacity, with standard-taper 24/40 joint.
standard.
4.2 Erlenmeyer Flask, of 250-mL to 300-mL capacity, with
1.3 This standard does not purport to address all of the
wide mouth.
safety concerns, if any, associated with its use. It is the
4.3 Separatory Funnels, of 300-mL to 500-mL capacity,
responsibility of the user of this standard to establish appro-
with glass or polytetrafluoroethylene (PFTE) stoppers.
priate safety and health practices and determine the applica-
4.4 Graduated Cylinder, one of 10 to 25-mL and one of 50
bility of regulatory limitations prior to use.
to 100-mL capacity.
2. Referenced Documents 4.5 Beaker, of up to 250-mL capacity.
2.1 ASTM Standards:
5. Reagents
D509 Test Methods of Sampling and Grading Rosin
5.1 Purity of Reagents—Reagent grade chemicals shall be
D803 Test Methods for Testing Tall Oil
used in all tests. Unless otherwise indicated, it is intended that
D804 Terminology Relating to Naval Stores, Including Tall
all reagents shall conform to the specifications of the Commit-
Oil and Related Products
tee onAnalytical Reagents of theAmerican Chemical Society,
E177 Practice for Use of the Terms Precision and Bias in
where such specifications are available. Other grades may be
ASTM Test Methods
used, provided it is first ascertained that the reagent is of
E691 Practice for Conducting an Interlaboratory Study to
sufficiently high purity to permit use without lessening the
Determine the Precision of a Test Method
accuracy of the determination.
3. Significance and Use 5.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean distilled, or deionized
3.1 This test method is designed to broaden the scope of the
water.
previous edition of the test method by the inclusion of tall oil
and tall oil derived from products as test materials. Test
6. Preparation of Sample
Methods D803 currently includes a method for the determina-
6.1 Procurement and handling of samples will vary depend-
tion of unsaponifiable matter.
ing upon the physical state of the material. In all instances, the
sampling should conform to accepted sampling techniques
which ensure the sample is representative of the material being
This test method is under the jurisdiction of ASTM Committee D01 on Paint
sampled.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.34 on Naval Stores.
Current edition approved Nov. 1, 2006. Published November 2006. Originally
approved in 1949. Last previous edition approved in 2001 as D1065 – 96 (2001). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D1065-96R06. 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.
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D1065 – 96 (2006)
6.2 Uniform liquid material should be mixed well and an 8.2 To the aqueous soap layer in the second funnel, add 30
aliquot removed for analysis.Titer in fatty acid samples should mL ether and extract as before. Drain the aqueous soap layer
be resolubilized by gentle heating and agitation. Rosin crystal- into the original saponification flask. Add the ether layer from
lization in liquid samples, such as distilled tall oil (DTO), the second separatory funnel to the first separatory funnel,
should be resolubilized by heating to 160°C with periodic thereby combining the extracts. Pour the aqueous soap layer
agitation. Homogeneous representative samples are impera- from the original saponification flask into the second separa-
tive. tory funnel, add 30 mL ether and extract for the third time.
6.3 Solids that melt at relatively low temperature (that is, Drain the aqueous soap layer from the second separatory
tall oil pitch) should be warmed to liquification to facilitate funnel into the original saponification flask again, and add the
mixing and pouring. Homogeneous representative samples are ether layer to the first funnel as before, thereby combining it
imperative. with the two previous extracts. Now drain off, and add to the
6.4 Solids that melt at relatively high temperatures (that is, soapsolutionalreadyintheoriginalsaponificationflask,allbut
rosin) should be fractured and chipped if possible, (see Test a few drops of aqueous soap solution that has collected at the
Methods D509). The sample taken for analysis shall consist of bottom of the first separatory funnel below the combined ether
small pieces of rosin chipped from a freshly exposed part of a extract layers.Add 2 mLof water to the first separatory funnel
lump of lumps, and thereafter crushed to facilitate weighing and drain off all but a few drops, combining it in the
and solution. The sample shall be prepared the same day on saponification flask.
which the test is begun in order to avoid changes in properties 8.3 Again pour the combined aqueous soap layers from the
due to surface oxidation that is very pronounced on ground original saponification flask into the second separatory funnel,
rosin having a large surface area exposed to the air. add 30 mL ether, and extract for the fourth time. After
separation of the layers, discard the aqueous soap layer (lower
7. Reagents
layer) from the second separatory funnel and add the ether
7.1 Alkali (ti
...
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