ASTM D565-99(2013)

Standard Test Method for Carbonizable Substances in White Mineral Oil

SIGNIFICANCE AND USE
4.1 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2013
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.06 - Analysis of Liquid Fuels and Lubricants

Relations

• Replaces: ASTM D565-99(2009)e1 - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 01-Oct-2013
• Replaced By: ASTM D565-99(2019) - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 01-Jan-2019

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D565 − 99 (Reapproved 2013)
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 U.S. 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
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
1.3 This standard does not purport to address all of the
United States Pharmacopeia, the National Formulary, and the
safety concerns, if any, associated with its use. It is the
Food and Drug Administration.
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
statements, see Section 6.
fittedwithawell-groundglassstopper,thestopperandthetube
bearing identical and indestructible numbers. The tube shall be
2. Referenced Documents
140 6 2 mm in length and between 14.5 and 15.0 mm in
2.1 ASTM Standards:
outside diameter, and shall be calibrated at the 5 6 0.2 mLand
D1193 Specification for Reagent Water
10 6 0.2 mL liquid levels. The capacity of the tube with
2.2 Offıcial Compendia:
stopper inserted shall be between 13.6 and 15.6 mL. A rolled
United States Pharmacopeia—Current Edition
edge can be provided for suspending the tube on the cover of
Monograph on Mineral Oil
the water bath.
National Formulary—Current Edition
5.2 Water Bath, suitable for immersing the test tube above
Monograph on Light Mineral Oil
the 10 mL line equipped to maintain a temperature of 100 6
0.5°C. The bath shall be provided with a cover of any suitable
material with holes approximately 16 mm in diameter through
This test method is under the jurisdiction of ASTM Committee D02 on
which the test tubes can be suspended.
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
5.3 Color Comparator, of a suitable type for observing the
Subcommittee D02.06 on Analysis of Lubricants.
Current edition approved Oct. 1, 2013. Published October 2013. Originally
color of the acid layer in comparison with the reference
ε1
approved in 1940. Last previous edition approved in 2009 as D565 – 99 (2009) .
standard color solution. The size and shape of the comparator
DOI: 10.1520/D0565-99R13.
2 are optional, but the size and shape of the apertures shall
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM conform to the dimensions prescribed in Fig. 1.
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
D565 − 99 (2013)
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum
6. Reagents dissolved, titrate the liberated iodine with 0.100 M sodium
thiosulfate (Na S O ) solution, using starch solution as an
2 2 3
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.
where such specifications are available. Other grades may be 2 2
used, provided it is first ascertained that the reagent is of
NOTE 1—This freshly prepared H SO solution will be hot. Allow to
2 4
sufficiently high purity to permit its use without lessening the
cool before continuing.
accuracy of the determination.
6.4 Cupric Sulfate Solution (0.25 M)—Prepare a solution of
6.2 Purity of Water—Unless otherwise indicated, references
HCl (Warning—see 6.3) by mixing 30 mL of concentrated
to water shall be understood to mean distilled water or water of
HCl with 1170 mL of water. Slowly add the acid to the water.
equal purity conforming to Type III of Specification D1193.
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, transfer 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
2 2
CH COOH with 1000 mL of water. Slowly add the acid to the
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.Eachm
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