Designation: D565 − 99 (Reapproved 2013)
Standard Test Method for
Carbonizable Substances in White Mineral Oil1
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:4
1.1 This test method covers white mineral oil (Mineral Oil 21CFR 172.878 Food and Drug Administration Title
USP and Light Mineral Oil NF) to determine whether it
conforms to the standard of quality required for pharmaceutical 3. Summary of Test Method
use as defined by the United States Pharmacopeia and the 3.1 The mineral oil is treated with concentrated sulfuric acid
National Formulary, or the Food and Drug Administration. (H2SO4) under prescribed conditions and the resulting color is
1.2 The values stated in SI units are to be regarded as compared with a reference standard to determine whether it
standard. No other units of measurement are included in this passes or fails the test.
standard.
1.2.1 Exception—Dimension requirements for the color 4. Significance and Use
comparator in Fig. 1 are in SI and inch-pound units. 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 Section 6. 5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
fitted with a well-ground glass stopper, the stopper and the tube
2. Referenced Documents bearing identical and indestructible numbers. The tube shall be
140 6 2 mm in length and between 14.5 and 15.0 mm in
2.1 ASTM Standards:2
outside diameter, and shall be calibrated at the 5 6 0.2 mL and
D1193 Specification for Reagent Water
10 6 0.2 mL liquid levels. The capacity of the tube with
2.2 Offıcial Compendia:3 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
which the test tubes can be suspended.
1
This test method is under the jurisdiction of ASTM Committee D02 on
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. color of the acid layer in comparison with the reference
Current edition approved Oct. 1, 2013. Published October 2013. Originally standard color solution. The size and shape of the comparator
approved in 1940. Last previous edition approved in 2009 as D565 – 99 (2009)ε1.
DOI: 10.1520/D0565-99R13.
are optional, but the size and shape of the apertures shall
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or conform to the dimensions prescribed in Fig. 1.
contact ASTM Customer Service at service@astm.org. 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
1
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
6.1 Purity of Reagents—Reagent grade chemicals shall be thiosulfate (Na2S2O3) solution, using starch solution as an
used in all tests. Unless otherwise indicated, it is intended that indicator. Each millilitre of Na2S2O3 solution is equivalent to
all reagents shall conform to the specifications of the Commit- 0.0238 g of CoCl2·6H2O. Adjust the final volume of CoCl2
tee on Analytical Reagents of the American Chemical Society, solution by the addition of HCl solution so that 1 mL contains
where such specifications are available.5 Other grades may be 59.5 mg of CoCl2·6H2O.
used, provided it is first ascertained that the reagent is of
NOTE 1—This freshly prepared H2SO4 solution will be hot. Allow to
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- (CuSO4·5H2O) in enough HCl solution to make 1000 mL of
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 (CH3COOH) (Warning—Corrosive. Combustible. Vapor
Dissolve 65 6 1 g of cobaltous chloride hexahydrate irritating.) solution by mixing 353 mL of concentrated
(CoCl2·6H2O) in the HCl solution to make 1000 mL of CH3COOH 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 mL of 6M CH3COOH, 3 g of Kl and 5 mL of HCl
mL iodine flask. Prepare a solution of sodium hydroxide
to the flask. Titrate the liberated iodine with 0.100 M Na2S2O3
(NaOH) ( Warning—Corrosive. Can cause severe burns or
solution, using starch solution as an indicator. Each millilitre of
blindness. Evolution of heat produces a violent reaction or
Na2S2O3 solution is equivalent to 0.0250 g of CuSO4·5H2O.
eruption upon too rapid a mixture with water.) by mixing 5 g
of NaOH with 20 mL of water. Add 15 mL of this NaOH Adjust the final volume of the CuSO4 solution by the addition
solution to the iodine flask. Add 5 mL of hydrogen peroxide of diluted HCl solution so that 1 mL contains 62.4 mg
(H2O2) (3 % v/v). Boil for 10 6 1 min, cool, and add 2 g of CuSO4·5H2O.
potassium iodide (KI). Prepare a solution of H2SO4 6.5 Ferric Chloride Solution (0.166 M)—Prepare a solution
(Warning—Causes burns. Vapor extremely irritating. Strong of HCl (Warning—see 6.3) by mixing 30 mL of concentrated
oxidizer.) by mixing 6 mL of H2SO4 with 18 mL of water. HCl with 1170 mL of water. Dissolve 55 6 1 g of ferric
Slowly add the acid to the water (see Note 1). Add 20 mL of chloride hexahydrate (FeCl3·6H2O) in enough HCl to make
this H2SO4 solution to the flask.) When the precipitate has 1000 mL of solution. Using a pipet, transfer 10 mL of this
solution into a 250-mL iodine flask, add 15 mL water, 3 g KI
5
Reagent Chemicals, American Chemical Society Specifications, American and 5 mL HCl, and allow the mixture to stand for 15 6 1 min.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not Dilute with 100 mL of water and titrate the liberated iodine
listed by the American Chemical Society, see Annual Standards for Laboratory with 0.100 M Na2S2O3 solution, using starch solution as an
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, indicator. Each millilitre of Na2S2O3 solution is equivalent to
MD. 0.0270 g of FeCl3·6H2O. Adjust the final volume of FeCl3
2
D565 − 99 (2013)
solution by the addition of the HCl solution so that 1 mL shakes over an amplitude of about 127 mm, shaking the test
contains 45.0 mg of FeCl3·6H2O. tube quickly and at a rate corresponding to 5 shakes/s. (A
6.6 The solutions prepared in 6.3 – 6.5 may be prepared in shaking machine may be employed provided the results that
different quantities, provided the ratios of components are can be obtained agree with those obtained by the prescribed
equivalent. manual agitation.) Repeat every 30 s. Do not keep the test tube
out of the bath longer than 3 s for each shaking period.
6.7 Colorimetric Reference Standard Solution—Prepare a
reference standard pale amber solution for color comparison by 7.4 At the end of 10 min from the time the test tube was first
mixing together 1.5 parts of CoCl2 solution, 3.0 parts of the placed in the bath, remove the test tube and allow to stand in
FeCl3 solution, and 0.5 parts of the CuSO4 solution. Measure the room for not less than 10 min nor more than 30 min.
5 mL of this mixture into a test tube as specified in 5.1. This Observe and record any discoloration of the oil layer. Place the
pale amber reference standard shall then be overlaid with 5 mL test tube in the color comparator, and compare the acid layer
of white mineral oil. with 5 mL of the standard colorimetric solution and 5 mL of
white mineral oil in a test tube that has been shaken vigorously
6.8 Sulfuric Acid (94.7 6 0.2 %)—The H2SO4 shall be for 10 s and allowed to stand just long enough for the contents
nitrogen-free when analyzed in accordance with the following to separate into two layers.
procedure: Dilute a small amount of the acid with an equal
volume of water and superimpose 10 mL of the cooled liquid 8. Interpretation of Results
upon diphenylamine solution (1 g of diphenylamine in 100 mL 8.1 White mineral oil shall be reported as passing the test
of concentrated H2SO4). A blue color should not appear at the only when the oil layer shows no change in color (see Note 2)
zone of contact within 1 h. This test detects as little as and when the acid layer is not darker than the reference
0.0002 % nitric acid (HNO3). standard colorimetric solution.
7. Procedure NOTE 2—A bluish haze or a slight pink or yellow color in the oil layer
should not be interpreted as a change in color.
7.1 Clean a test tube with a chromic acid (H2 CrO4) cleaning
solution (Warning—Causes severe burns. A recognized car- 8.2 If the oil layer is discolored or if the acid layer is darker
cinogen. Strong oxidizer.), or use a nonchromium containing, than the reference standard colorimetric solution, white min-
strongly oxidizing cleaning solution. eral oil shall be reported as not passing the test.
7.2 Fill the test tube to the 5 mL mark with H2SO4 (94.7 6 9. Precision and Bias
0.2 %). Then add the oil to be tested to the 10-mL mark, insert 9.1 No statement is made about either the precision or bias
the stopper loosely, and place the test tube in position in the of this test method since the result merely states whether there
water bath at 100 6 0.5°C. is conformance to the criteria for success specified in the
7.3 After the test tube has been in the water bath for 30 s, procedure.
loosen the stopper sufficiently to release any pressure and
reinsert, remove the test tube from the bath quickly, hold with 10. Keywords
a finger over the stopper, and give three vigorous, vertical 10.1 carbonizable substances; mineral oil
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