ASTM D612-88(1999)

Standard Test Method for Carbonizable Substances in Paraffin Wax

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 D87, 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 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. Specific precautionary statements are given in Notes 1 through 5 and Annex A1.

General Information

• Status: Historical
• Publication Date: 09-Apr-1999
• ICS: 75.140 - Waxes, bituminous materials and other petroleum products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.10.0A - Physical/Chemical Properties

Relations

• Replaced By: ASTM D612-88(2004) - Standard Test Method for Carbonizable Substances in Paraffin Wax
• Effective Date: 01-May-2004

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation: D 612 – 88 (Reapproved 1999)
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 fitted with a well-ground glass stopper, the stopper and the tube
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-mL and
(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 precau- of any suitable material, with holes approximately 16 mm in
tionary statements are given in Notes 1-5 and 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 on Analytical Reagents of the American 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.
1 4
This test method is under the jurisdiction of ASTM Committee D-2 on Borosilicate glass has been found satisfactory for this purpose.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Reagent Chemicals, American Chemical Society Specifications, American
D02.10 on Petroleum Wax. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Oct. 31, 1988. Published December 1988. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
e1
published as D 612 – 41. Last previous edition D 612 – 45 (1983) . Chemicals, BDH Ltd., Poole, Dorset, U. K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 05.01. and National Formulary, U. S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 612
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum
reagent water corresponding to Specification D 1193, Type III, solution is equivalent to 0.02497 g of CuSO ·5H O. Adjust the
4 2
or water of equal purity. final volume of CuSO solution by the addition of diluted HCl
6.3 Cobaltous Chloride Solution (0.5 N)—Dissolve about (1 + 39) so that 1 mL contains 62.4 mg of CuSO ·5H O.
4 2
65 g of cobaltous chloride (CoCl ·6H O) in enough diluted
2 2
NOTE 4—Warning: Acetic acid (glacial) is corrosive, combustible,
hydrochloric acid (HCl, 1 + 39) (Warning—See Note 1.) to
vapor irritating. See A1.5.
make 1000 mL of solution. Transfer exactly 5 mL of this
6.6 Ferric Chloride Solution (0.5N)—Dissolve about 55 g
solution to a flask; add 15 mL of sodium hydroxide (NaOH,
of ferric chloride (FeCl ·6H O) in enough diluted HCl
3 2
1+5) (Warning—See Note 2.), and 5 mL of hydrogen
(Warning—See Note 1.) (1 + 39) to make 1000 mL of
peroxide. Boil for 10 min, cool, and add2gof potassium
solution. Transfer exactly 10 mL of the solution to a flask, add
iodide (KI) and 20 mL of sulfuric acid (H SO , 1+4)
2 4
5 mL of HCl (sp gr 1.19), 25 mL of water, and about3gofKI.
(Warning—See Note 3.). When the precipitate has dissolved,
Stopper and allow the mixture to stand for 5 min. Dilute the
titrate the liberated iodine with 0.1 N sodium thiosulfate
mixture with 50 mL of water, and titrate the liberated iodine
(Na S O ) solution using starch solution as an indicator. Each
2 2 3
with 0.1 N Na S O solution, using starch solution as an
2 2 3
millilitre of 0.1 N Na S O solution consumed is equivalent to
2 2 3
indicator. Each millilitre of 0.1 N Na S O solution is equiva-
2 2 3
0.023799 g of CoCl ·6H O. Adjust the final volume of CoCl
2 2 2
lent to 0.02703 g of FeCl ·6H O. Adjust the final volume of the
3 2
solution by the addition of diluted HCl (1 + 39) so that 1 mL
FeCl solution by the addition of diluted HCl (1 + 39) so that
contains 59.5 mg of CoCl ·6H O.
2 2
1 mL contains 45.0 mg of FeCl ·6H O.
3 2
NOTE 1—Warning: Hydrochloric acid (concentrated) causes burns,
6.7 Sulfuric Acid (94.7 6 0.2 %)—The sulfuric acid
vapor extremely irritating. See A1.2.
(H SO )(Warning—See Note 3.) shall be nitrogen-free when
2 4
NOTE 2—Warning: Sodium hydroxide, corrosive, can cause severe
analyzed in accordance with the following procedure: Dilute a
burns or blindness. Evolution of heat produces a violent reaction or
small amount of the acid with an equal volume of water and
eruption upon too rapid a mixture with water. See A1.4.
superimpose 10 mL of the cooled liquid upon diphenylamine
NOTE 3—Warning: Sulfuric acid (concentrated) causes burns, vapor
irritating, strong oxidizer. See A1.3. solution (1 g of diphenylamine in 100 mL of concentrated
H SO ). A blue color should not appear at the zone of
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