ASTM D565-99

Standard Test Method for Carbonizable Substances in White Mineral Oil

SCOPE
1.1 This test method is applicable to 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 the inch-pound units are to be regarded as the standard. The values in parentheses are for information only.
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 Notes 1 through 5.

General Information

• Status: Historical
• Publication Date: 09-Nov-1999
• 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

• Replaced By: ASTM D565-99(2005) - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 01-May-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D565–99
Standard Test Method for
Carbonizable Substances in White Mineral Oil
This standard is issued under the fixed designation D 565; 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 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 the
passes or fails the test.
standard.
1.2.1 The dimensions for the color comparator (see 5.3 and
4. Significance and Use
Fig. 1) are excepted for that part of the apparatus.
4.1 This test method is a means for ascertaining whether
1.3 This standard does not purport to address all of the
pharmaceutical mineral oil conforms to the standards of the
safety concerns, if any, associated with its use. It is the
United States Pharmacopeia, the National Formulary, and the
responsibility of the user of this standard to establish appro-
Food and Drug Administration.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
5. Apparatus
statements, see Notes 1-5.
5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
fittedwithawell-groundglassstopper,thestopperandthetube
2. Referenced Documents
bearing identical and indestructible numbers. The tube shall be
2.1 ASTM Standards:
2 140 6 2 mm in length and between 14.5 and 15.0 mm in
D 1193 Specification for Reagent Water
outside diameter, and shall be calibrated at the 5 6 0.2 mLand
D 4057 Practice for Manual Sampling of Petroleum and
10 6 0.2 mL liquid levels. The capacity of the tube with
Petroleum Products
stopper inserted shall be between 13.6 and 15.6 mL. A rolled
D 4177 Pratice for Automatic Sampling of Petroleum and
edge can be provided for suspending the tube on the cover of
Petroleum Products
4 the water bath.
2.2 Offıcial Compendia:
5.2 Water Bath, suitable for immersing the test tube above
United States Pharmacopeia—Current Edition
the 10 mL line equipped to maintain a temperature of 100 6
Monograph on Mineral Oil
0.5°C. The bath shall be provided with a cover of any suitable
National Formulary—Current Edition
material with holes approximately 16 mm in diameter through
Monograph on Light Mineral Oil
which the test tubes can be suspended.
5.3 Color Comparator, of a suitable type for observing the
color of the acid layer in comparison with the reference
This test method is under the jurisdiction of ASTM Committee D02 on standard color solution. The size and shape of the comparator
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
are optional, but the size and shape of the apertures shall
D02.06 on Analysis of Lubricants.
conform to the dimensions prescribed in Fig. 1.
Current edition approved Nov. 10, 1999. Published January 2000. Originally
published as D 565 – 40. Last previous edition D 565 – 88.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.02.
4 5
Available from U.S. Pharmacopeial Convention, 12601 Twinbrook Parkway, AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Rockville, MD 20852. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D565–99
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum
6. Reagents thiosulfate (Na S O ) solution, using starch solution as an
2 2 3
indicator. Each millilitre of Na S O solution is equivalent to
2 2 3
6.1 Purity of Reagents—Reagent grade chemicals shall be
0.0238 g of CoCl ·6H O. Adjust the final volume of CoCl
used in all tests. Unless otherwise indicated, it is intended that 2 2 2
solution by the addition of HCl solution so that 1 mL contains
all reagents shall conform to the specifications of the Commit-
59.5 mg of CoCl ·6H O.
tee onAnalytical Reagents of theAmerican Chemical Society, 2 2
where such specifications are available. Other grades may be
NOTE 1—This freshly prepared H SO solution will be hot. Allow to
2 4
used, provided it is first ascertained that the reagent is of
cool before continuing.
sufficiently high purity to permit its use without lessening the
6.4 Cupric Sulfate Solution (0.25 M)—Prepare a solution of
accuracy of the determination.
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 D 1193. Dissolve 65 6 1 g of cupric sulfate pentahydrate
6.3 Cobaltous Chloride Solution (0.25 M)—Prepare a solu- (CuSO ·5H O) in enough HCl solution to make 1000 mL of
4 2
tion of hydrochloric acid (HCl) (Warning—Causes burns. solution. Using a pipet, transfet 10 mL of the solution to a
Vapor extremely irritating.) by mixing 30 mL of concentrated 250-mL iodine flask, add 40 mL of water. Prepare a 6M acetic
HCl with 1170 mL of water. Slowly add the acid to the water.
acid (CH COOH) (Warning— Corrosive. Combustible.Vapor
Dissolve 65 6 1 g of cobaltous chloride hexahydrate
irritating.) solution by mixing 353 mL of concentrated
(CoCl ·6H O) in the HCl solution to make 1000 mL of
CH COOH with 1000 mL of water. Slowly add the acid to the
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
...