ASTM D565-99(2009)e1

Standard Test Method for Carbonizable Substances in White Mineral Oil

SIGNIFICANCE AND USE
This test method is a means for ascertaining whether pharmaceutical mineral oil conforms to the standards of the United States Pharmacopeia, the National Formulary, and the Food and Drug Administration.
SCOPE
1.1 This test method covers white mineral oil (Mineral Oil USP and Light Mineral Oil NF) to determine whether it conforms to the standard of quality required for pharmaceutical use as defined by the United States Pharmacopeia and the National Formulary, or the Food and Drug Administration.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exception—Dimension requirements for the color comparator in Fig. 1 are in SI and inch-pound units.
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. For specific hazard statements, see Section 6.
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum

General Information

• Status: Historical
• Publication Date: 14-Apr-2009
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.06 - Analysis of Liquid Fuels and Lubricants

Relations

• Replaces: ASTM D565-99(2005) - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 15-Apr-2009
• Replaced By: ASTM D565-99(2013) - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 01-Oct-2013

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation: D565 − 99(Reapproved 2009)
Standard Test Method for
Carbonizable Substances in White Mineral Oil
This standard is issued under the fixed designation D565; 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.
This standard has been approved for use by agencies of the Department of Defense.
´ NOTE—Updated 1.2.1 and deleted information inch-pound units to make solely SI standard editorially in July 2009.
1. Scope 2.3 Government Document:
21CFR 172.878 Food and Drug Administration Title
1.1 This test method covers white mineral oil (Mineral Oil
USP and Light Mineral Oil NF) to determine whether it
3. Summary of Test Method
conformstothestandardofqualityrequiredforpharmaceutical
3.1 Themineraloilistreatedwithconcentratedsulfuricacid
use as defined by the United States Pharmacopeia and the
(H SO ) under prescribed conditions and the resulting color is
2 4
National Formulary, or the Food and Drug Administration.
compared with a reference standard to determine whether it
1.2 The values stated in SI units are to be regarded as
passes or fails the test.
standard. No other units of measurement are included in this
standard. 4. Significance and Use
1.2.1 Exception—Dimension requirements for the color
4.1 This test method is a means for ascertaining whether
comparator in Fig. 1 are in SI and inch-pound units.
pharmaceutical mineral oil conforms to the standards of the
United States Pharmacopeia, the National Formulary, and the
1.3 This standard does not purport to address all of the
Food and Drug Administration.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 6. fittedwithawell-groundglassstopper,thestopperandthetube
bearing identical and indestructible numbers. The tube shall be
140 6 2 mm in length and between 14.5 and 15.0 mm in
2. Referenced Documents
outside diameter, and shall be calibrated at the 5 6 0.2 mLand
2.1 ASTM Standards:
10 6 0.2 mL liquid levels. The capacity of the tube with
D1193 Specification for Reagent Water
stopper inserted shall be between 13.6 and 15.6 mL. A rolled
2.2 Offıcial Compendia:
edge can be provided for suspending the tube on the cover of
United States Pharmacopeia—Current Edition
the water bath.
Monograph on Mineral Oil
5.2 Water Bath, suitable for immersing the test tube above
National Formulary—Current Edition
the 10 mL line equipped to maintain a temperature of 100 6
Monograph on Light Mineral Oil
0.5°C. The bath shall be provided with a cover of any suitable
material with holes approximately 16 mm in diameter through
which the test tubes can be suspended.
5.3 Color Comparator, of a suitable type for observing the
This test method is under the jurisdiction of ASTM Committee D02 on
color of the acid layer in comparison with the reference
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
standard color solution. The size and shape of the comparator
D02.06 on Analysis of Lubricants.
Current edition approved April 15, 2009. Published July 2009. Originally
are optional, but the size and shape of the apertures shall
approved in 1940. Last previous edition approved in 2005 as D565–99(2005). DOI:
conform to the dimensions prescribed in Fig. 1.
10.1520/D0565-99R09E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6. Reagents
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
Available from U.S. Pharmacopeial Convention, 12601 Twinbrook Parkway, Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Rockville, MD 20852. Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D565 − 99 (2009)
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum
6.1 Purity of Reagents—Reagent grade chemicals shall be indicator. Each millilitre of Na S O solution is equivalent to
2 2 3
used in all tests. Unless otherwise indicated, it is intended that
0.0238 g of CoCl ·6H O. Adjust the final volume of CoCl
2 2 2
all reagents shall conform to the specifications of the Commit-
solution by the addition of HCl solution so that 1 mL contains
tee onAnalytical Reagents of theAmerican Chemical Society,
59.5 mg of CoCl ·6H O.
2 2
where such specifications are available. Other grades may be
NOTE 1—This freshly prepared H SO solution will be hot. Allow to
used, provided it is first ascertained that the reagent is of 2 4
cool before continuing.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
6.4 Cupric Sulfate Solution (0.25 M)—Prepare a solution of
HCl (Warning—see 6.3) by mixing 30 mL of concentrated
6.2 Purity of Water—Unless otherwise indicated, references
HCl with 1170 mL of water. Slowly add the acid to the water.
to water shall be understood to mean distilled water or water of
equal purity conforming to Type III of Specification D1193. Dissolve 65 6 1 g of cupric sulfate pentahydrate
(CuSO ·5H O) in enough HCl solution to make 1000 mL of
4 2
6.3 Cobaltous Chloride Solution (0.25 M)—Prepare a solu-
solution. Using a pipet, transfer 10 mL of the solution to a
tion of hydrochloric acid (HCl) (Warning—Causes burns.
250-mL iodine flask, add 40 mL of water. Prepare a 6M acetic
Vapor extremely irritating.) by mixing 30 mL of concentrated
acid (CH COOH) (Warning—Corrosive. Combustible. Vapor
HCl with 1170 mL of water. Slowly add the acid to the water. 3
irritating.) solution by mixing 353 mL of concentrated
Dissolve 65 6 1 g of cobaltous chloride hexahydrate
CH COOH with 1000 mL of water. Slowly add the acid to the
(CoCl ·6H O) in the HCl solution to make 1000 mL of
2 2
solution. Using a pipet, transfer 5 mL of this solution to a 250 water.Add 4 mLof 6M CH COOH,3gofKland5mLofHCl
mL iodine flask. Prepare a solution of sodium hydroxide
to the flask. Titrate the liberated iodine with 0.100 M Na S O
2 2 3
(NaOH) (Warning—Corrosive. Can cause severe burns or
solution,usingstarchsolutionasanindicator.Eachmillilitreof
blindness. Evolution of heat p
...