ASTM D612-88(2004)
(Test Method)Standard Test Method for Carbonizable Substances in Paraffin Wax
Standard Test Method for Carbonizable Substances in Paraffin Wax
SIGNIFICANCE AND USE
This test method is a means for ascertaining whether pharmaceutical paraffin wax conforms to the standards for quality prescribed by the U.S. National Formulary.
SCOPE
1.1 This test method covers determination of carbonizable substances in paraffin wax. The test method is applicable to paraffin wax for pharmaceutical use, as defined by the U.S. National Formulary, with a melting point as determined in accordance with Test Method D 87, between 117 and 149°F (47 and 65°C).
1.2 The values stated in inch-pound units are to be regarded as the 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. Specific warning statements are given in Annex A1.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D612–88 (Reapproved 2004)
Standard Test Method for
Carbonizable Substances in Paraffin Wax
This standard is issued under the fixed designation D 612; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 5. Apparatus
1.1 This test method covers determination of carbonizable 5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
substances in paraffin wax. The test method is applicable to fittedwithawell-groundglassstopper,thestopperandthetube
paraffin wax for pharmaceutical use, as defined by the U.S. bearing identical and indestructible numbers. The tube shall be
National Formulary, with a melting point as determined in 140 6 2 mm in length and between 14.5 and 15.0 mm in
accordance with Test Method D 87, between 117 and 149°F outside diameter, and shall be calibrated at the 5 6 0.2-mLand
(47 and 65°C). 10 6 0.2-mL liquid levels. The capacity of the tube with
1.2 The values stated in inch-pound units are to be regarded stopper inserted shall be between 13.6 and 15.6 mL. A rolled
as the standard. edge may be provided for suspending the tube on the cover of
1.3 This standard does not purport to address all of the the water bath.
safety concerns, if any, associated with its use. It is the 5.2 Water Bath, suitable for immersing the test tube above
responsibility of the user of this standard to establish appro- the 10-mL line and equipped to maintain a temperature of 158
priate safety and health practices and determine the applica- 6 1.0°F (70 6 0.5°C).The bath shall be provided with a cover
bility of regulatory limitations prior to use. Specific warning of any suitable material, with holes approximately 16 mm in
statements are given in Annex A1. diameter through which the test tubes may be suspended.
5.3 Color Comparator, of a suitable type for observing the
2. Referenced Documents
color of the acid layer in comparison with the reference
2.1 ASTM Standards: standard color solution. The size and shape of the comparator
D 87 Test Method for Melting Point of Petroleum Wax
are optional, but the size and shape of the apertures shall
(Cooling Curve)
conform to the dimensions prescribed in Fig. 1.
D 1193 Specification for Reagent Water
6. Reagents
3. Summary of Test Method
6.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 Five millilitres of melted wax are treated with 5 mL of used in all tests. Unless otherwise indicated, it is intended that
concentrated, nitrogen-free sulfuric acid at 158°F (70°C). The
all reagents shall conform to the specifications of the Commit-
color of the acid layer is compared with that of a colorimetric tee onAnalytical Reagents of theAmerican Chemical Society,
reference standard. If the color is not darker than the standard,
where such specifications are available. Other grades may be
the wax is reported as passing the test. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
4. Significance and Use
accuracy of the determination.
4.1 This test method is a means for ascertaining whether
6.2 Purity of Water—Unless otherwise indicated, references
pharmaceutical paraffin wax conforms to the standards for
to water shall be understood to mean distilled water, such as
quality prescribed by the U.S. National Formulary.
reagent water corresponding to Specification D 1193, Type III,
or water of equal purity.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.10 on Properties of Petroleum Wax. Borosilicate glass has been found satisfactory for this purpose.
Current edition approved May 1, 2004. Published June 2004. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1941. Last previous edition approved in 1999 as D 612–88 (1999). 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 Annual 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.
D612–88 (2004)
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum
6.3 Cobaltous Chloride Solution (0.5 N)—Dissolve about final volume of CuSO solution by the addition of diluted HCl
65 g of cobaltous chloride (CoCl ·6H O) in enough diluted (1 + 39) so that 1 mL contains 62.4 mg of CuSO ·5H O.
2 2 4 2
hydrochloricacid(HCl,1 + 39)(Warning—Hydrochloricacid 6.6 Ferric Chloride Solution (0.5N)—Dissolve about 55 g
(concentrated) causes burns, vapor extremely irritating. See of ferric chloride (FeCl ·6H O) in enough diluted HCl
3 2
A1.2) to make 1000 mL of solution. Transfer exactly 5 mL of (Warning—Hydrochloric acid (concentrated) causes burns,
this solution to a flask; add 15 mL of sodium hydroxide vapor extremely irritating. See A1.2) (1 + 39) to make 1000
(NaOH, 1 + 5) (Warning—Sodium hydroxide, corrosive, can mL of solution. Transfer exactly 10 mL of the solution to a
cause severe burns or blindness. Evolution of heat produces a flask, add 5 mLof HCl (sp gr 1.19), 25 mLof water, and about
violent reaction or eruption upon too rapid a mixture with 3 g of KI. Stopper and allow the mixture to stand for 5 min.
water. See A1.4), and 5 mL of hydrogen peroxide. Boil for 10 Dilutethemixturewith50mLofwater,andtitratetheliberated
min, cool, and add2gof potassium iodide (KI) and 20 mL of iodine with 0.1 N Na S O solution, using starch solution as an
2 2 3
sulfuric acid (H SO , 1+4) (Warning—Sulfuric acid (con- indicator. Each millilitre of 0.1 N Na S O solution is equiva-
2 4 2 2 3
centrated) causes burns, vapor irritating, strong oxidizer. See lentto0.02703gofFeCl ·6H O.Adjustthefinalvolumeofthe
3 2
A1.3). When the precipitate has dissolved, titrate the liberated FeCl solution by the addition of diluted HCl (1 + 39) so that
iodine with 0.1 N sodium thiosulfate (Na S O ) solution using 1 mL contains 45.0 mg of FeCl ·6H O.
2 2 3 3 2
starchsolutionasanindicator.Eachmillilitreof0.1 NNa S O 6.7 Sulfuric Acid (94.7 6 0.2 %)—The sulfuric acid
2 2 3
solution consumed is equivalent to 0.023799 g of CoCl ·6H O. (H SO)(Warning—Sulfuric acid (concentrated) causes
2 2 2 4
Adjust the final volume of CoCl solution by the addition of burns, vapor irritating, strong oxidizer. See A1.3) shall be
diluted HCl (1 + 39) so that 1 mL contains 59.5 mg of nitrogen-free when analyzed in accordance with the following
CoCl ·6H O. procedure: Dilute a small amount of the acid with an equal
2 2
volume of water and superimpose 10 mL of the cooled liquid
6.4 Colorimetric Reference Standard Solution—Prepare a
upon diphenylamine solution (1 g of diphenylamine in 100 mL
referencestandardpaleambersolutionforcolorcomparisonby
of concentrated H SO ). A blue color should not appear at the
mixing together 1.5 parts of CoCl solution, 3.0 parts of FeCl
2 3 2 4
zone of contact within 1 h. This test det
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