ASTM D1065-96(2001)
(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
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 This standard does not purport to address all of the safety problems, 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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Designation: D 1065 – 96 (Reapproved 2001)
Standard Test Method for
Unsaponifiable Matter in Naval Stores, Including Rosin, Tall
Oil, and Related Products
This standard is issued under the fixed designation D 1065; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Apparatus
4.1 Erlenmeyer or Other Flat-Bottom Flask, of 125-mL to
1.1 This test method covers the determination of the per-
centage of material in Naval Stores products as defined in 250-mL capacity, with standard-taper 24/40 joint.
Terminology D 804 including rosin, tall oil and related prod- 4.2 Erlenmeyer Flask, of 250-mL to 300-mL capacity, with
ucts, other than insoluble dirt or similar visible foreign matter wide mouth.
that does not yield a water-soluble soap when the sample is 4.3 Separatory Funnels, of 300-mL to 500-mL capacity,
saponified with potassium hydroxide. with glass or polytetrafluoroethylene (PFTE) stoppers.
1.2 This standard does not purport to address all of the 4.4 Graduated Cylinder, one of 10 to 25-mL and one of 50
safety concerns, if any, associated with its use. It is the to 100-mL capacity.
responsibility of the user of this standard to establish appro- 4.5 Beaker, of up to 250-mL capacity.
priate safety and health practices and determine the applica-
5. Reagents
bility of regulatory limitations prior to use.
5.1 Purity of Reagents—Reagent grade chemicals shall be
2. Referenced Documents
used in all tests. Unless otherwise indicated, it is intended that
2.1 ASTM Standards: all reagents shall conform to the specifications of the Commit-
D 509 Test Methods of Sampling and Grading Rosin tee onAnalytical Reagents of theAmerican Chemical Society,
2 4
D 803 Test Methods forTesting Tall Oil where such specifications are available. Other grades may be
D 804 TerminologyRelatingtoNavalStores,IncludingTall used, provided it is first ascertained that the reagent is of
Oil and Related Products sufficiently high purity to permit use without lessening the
E 177 Practice for Use of the Terms Precision and Bias in accuracy of the determination.
ASTM Test Methods 5.2 Purity of Water—Unless otherwise indicated, references
E 691 Practice for Conducting an Interlaboratory Study to to water shall be understood to mean distilled, or deionized
Determine the Precision of a Test Method water.
3. Significance and Use 6. Preparation of Sample
3.1 This test method is designed to broaden the scope of the 6.1 Procurement and handling of samples will vary depend-
previous edition of the test method by the inclusion of tall oil ing upon the physical state of the material. In all instances, the
and tall oil derived from products as test materials. Test sampling should conform to accepted sampling techniques
Methods D 803 currently includes a method for the determi- which ensure the sample is representative of the material being
nation of unsaponifiable matter. sampled.
3.2 Theamountofunsaponifiablematterintalloilandother 6.2 Uniform liquid material should be mixed well and an
related products is important in characterizing such products as aliquot removed for analysis.Titer in fatty acid samples should
it indicates the level of nonacidic material, both free and be resolubilized by gentle heating and agitation. Rosin crystal-
combined, present in the test material. The unsaponifiable in lization in liquid samples, such as distilled tall oil (DTO),
naval stores products is primarily composed of higher molecu- should be resolubilized by heating to 160°C with periodic
lar weight alcohols, sterols, and hydrocarbons. agitation. Homogeneous representative samples are impera-
tive.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.34 on Naval Stores. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Dec. 10, 1996. Published February 1997. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1065 – 49 T. Last previous edition D 1065 – 92. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.03. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 14.02. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 1065
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 D 509).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 (titrant), Standard Alcoholic Solution (0.1 N)—
layer to the combined ether extracts in the first separatory
Dissolve 6.6 g KOH or 5.2 g NaOH, preferably in pellet form,
funnel. Carefully drain off any remaining aqueous soap layer
in 1 L of methanol (99.5 %) or ethanol (95 %) denatured by
that may have collected above the stopcock under the ether
Formula No. 3A or No. 30 of the U.S. Bureau of Internal
extracts in the first separatory funnel.Add 2 mLof water, swirl
Revenue. Standardize this so
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