ASTM D565-99(2019)

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.  
FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Dec-2018
• 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(2013) - Standard Test Method for Carbonizable Substances in White Mineral Oil
• Effective Date: 01-Jan-2019
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM D565-99(2019), Standard Test Method for Carbonizable Substances in White Mineral Oil, establishes a definitive protocol for determining the presence of carbonizable substances in pharmaceutical-grade white mineral oil. This test method is essential for verifying compliance with the quality standards specified by the United States Pharmacopeia (USP), the National Formulary (NF), and the U.S. Food and Drug Administration (FDA).

White mineral oil is widely used in pharmaceutical, food, and cosmetic products, making strict quality assurance vital for end-user safety. This standard provides a systematic approach for assessing mineral oil, ensuring it meets stringent requirements for use in critical applications.

Key Topics

• Scope: Covers procedures to determine whether white mineral oil (Mineral Oil USP, Light Mineral Oil NF) contains impurities detectable as carbonizable substances.
• Significance: Ensures that mineral oil meets USP, NF, and FDA standards, crucial for pharmaceutical quality and consumer safety.
• Referenced Units: Results and apparatus dimensions are specified using SI units; selected components include both SI and inch-pound units.
• Method Summary:
  • The mineral oil sample is treated with concentrated sulfuric acid.
  • The sample is subjected to a heating and shaking protocol.
  • A color comparison is made between the acid layer in the test sample and a reference standard using a color comparator.
  • The test is passed if the oil shows no color change, and the acid layer is not darker than the reference standard.
• Safety Notice: The standard highlights user responsibility for safety, health, and environmental measures when applying this test, as well as regulatory compliance.

Applications

ASTM D565 is widely applicable to industries where the quality of white mineral oil must be assured, especially for:

• Pharmaceutical Manufacturing: Ensures oils conform to USP and NF specifications for medicinal and personal care products.
• Food Industry: Supports compliance with FDA requirements for white mineral oil used in food processing and handling.
• Cosmetics Production: Validates the suitability of white mineral oil in creams, ointments, and other topical products.
• Regulatory Testing: Used by laboratories and regulatory agencies for routine quality assurance and batch release of white mineral oil.
• Supplier and Procurement Quality Control: Helps manufacturers, suppliers, and buyers confirm product suitability before use or distribution.

Adhering to this test method helps maintain product integrity, reduce risk, and ensure regulatory acceptance in global markets.

Related Standards

For comprehensive quality control and regulatory compliance, the following standards and references are frequently used alongside ASTM D565:

• ASTM D1193 - Specification for Reagent Water, which covers the requirements for water purity in test methods.
• United States Pharmacopeia (USP) - Current monographs on Mineral Oil and Light Mineral Oil.
• National Formulary (NF) - Compendia standards for pharmaceutical ingredients.
• 21 CFR 172.878 - FDA regulations for white mineral oil used in food.
• ASTM D02 Standards - Additional standards for petroleum products, fuels, and lubricants.

Conclusion

ASTM D565-99(2019) is a critical standard for verifying the absence of carbonizable substances in pharmaceutical white mineral oil. Its robust protocol supports industries in achieving compliance with USP, NF, and FDA standards, thereby protecting consumer safety and ensuring product quality for sensitive applications. Manufacturers, laboratories, and regulatory agencies rely on this standard as part of their quality assurance programs for white mineral oil.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D565 − 99 (Reapproved 2019)
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 Monograph on Light Mineral Oil
1.1 This test method covers white mineral oil (Mineral Oil
2.3 Government Document:
USP and Light Mineral Oil NF) to determine whether it
conformstothestandardofqualityrequiredforpharmaceutical 21CFR 172.878 Food and Drug Administration Title
use as defined by the United States Pharmacopeia and the
National Formulary, or the Food and Drug Administration. 3. Summary of Test Method
3.1 Themineraloilistreatedwithconcentratedsulfuricacid
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this (H SO ) under prescribed conditions and the resulting color is
2 4
compared with a reference standard to determine whether it
standard.
1.2.1 Exception—Dimension requirements for the color passes or fails the test.
comparator in Fig. 1 are in SI and inch-pound units.
4. Significance and Use
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 This test method is a means for ascertaining whether
responsibility of the user of this standard to establish appro- pharmaceutical mineral oil conforms to the standards of the
priate safety, health, and environmental practices and deter- United States Pharmacopeia, the National Formulary, and the
mine the applicability of regulatory limitations prior to use. Food and Drug Administration.
For specific hazard statements, see Section 6.
1.4 This international standard was developed in accor- 5. Apparatus
dance with internationally recognized principles on standard-
5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
ization established in the Decision on Principles for the
fittedwithawell-groundglassstopper,thestopperandthetube
Development of International Standards, Guides and Recom-
bearing identical and indestructible numbers. The tube shall be
mendations issued by the World Trade Organization Technical
140 mm 6 2 mm in length and between 14.5 mm and
Barriers to Trade (TBT) Committee.
15.0 mm in outside diameter, and shall be calibrated at the
5mL 6 0.2 mL and 10 mL 6 0.2 mL liquid levels. The
2. Referenced Documents
capacity of the tube with stopper inserted shall be between
2.1 ASTM Standards:
13.6 mL and 15.6 mL. A rolled edge can be provided for
D1193 Specification for Reagent Water
suspending the tube on the cover of the water bath.
2.2 Offıcial Compendia:
5.2 Water Bath, suitable for immersing the test tube above
United States Pharmacopeia—Current Edition
the10 mLlineequippedtomaintainatemperatureof100 °C 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
which the test tubes can be suspended.
This test method is under the jurisdiction of ASTM Committee D02 on
5.3 Color Comparator, of a suitable type for observing the
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
color of the acid layer in comparison with the reference
Current edition approved Jan. 1, 2019. Published January 2019. Originally
standard color solution. The size and shape of the comparator
approved in 1940. Last previous edition approved in 2013 as D565 – 99 (2013).
are optional, but the size and shape of the apertures shall
DOI: 10.1520/D0565-99R19.
conform to the dimensions prescribed in Fig. 1.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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
D565 − 99 (2019)
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 g 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 mLiodine flask, add 40 mLof water. Prepare a 6 M acetic
HCl with 1170 mL of water. Slowly add the acid to the water.
acid (CH COOH) (Warning—Corrosive. Combustible. Vapor
Dissolve 65 g 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
water. Add 4 mL of 6 M CH COO
...