Designation: D 565 – 99 An American National Standard

Standard Test Method for

Carbonizable Substances in White Mineral Oil1
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.

1. Scope (H2SO4) under prescribed conditions and the resulting color is

1.1 This test method covers white mineral oil (Mineral Oil compared with a reference standard to determine whether it
USP and Light Mineral Oil NF) to determine whether it passes or fails the test.
conforms to the standard of quality required for
pharmaceutical use as defined by the United States 4. Significance and Use
Pharmacopeia and the National Formulary, or the Food and 4.1 This test method is a means for ascertaining whether
Drug Administration. pharmaceutical mineral oil conforms to the standards of the
1.2 The values stated in SI units are to be regarded as the United States Pharmacopeia, the National Formulary, and the
standard. Food and Drug Administration.
1.2.1 The dimensions for the color comparator (see 5.3 and
Fig. 1) are excepted for that part of the apparatus. 5. Apparatus
1.3 This standard does not purport to address all of the 5.1 Test Tube, as shown in Fig. 1, of heat-resistant glass
safety concerns, if any, associated with its use. It is the fitted with a well-ground glass stopper, the stopper and the
responsibility of the user of this standard to establish appro- tube bearing identical and indestructible numbers. The tube
priate safety and health practices and determine the applica- shall be 140 6 2 mm in length and between 14.5 and 15.0
bility of regulatory limitations prior to use. For specific hazard mm in outside diameter, and shall be calibrated at the 5 6 0.2
statements, see Notes 1-5. mL and 10 6 0.2 mL liquid levels. The capacity of the tube
with stopper inserted shall be between 13.6 and 15.6 mL. A
2. Referenced Documents rolled edge can be provided for suspending the tube on the
2.1 ASTM Standards: cover of the water bath.
D 1193 Specification for Reagent Water2 5.2 Water Bath, suitable for immersing the test tube
D 4057 Practice for Manual Sampling of Petroleum and above the 10 mL line equipped to maintain a temperature
Petroleum Products3 of 100 6 0.5°C. The bath shall be provided with a cover of
D 4177 Pratice for Automatic Sampling of Petroleum and any suitable material with holes approximately 16 mm in
Petroleum Products3 diameter through which the test tubes can be suspended.
2.2 Offıcial Compendia:4 5.3 Color Comparator, of a suitable type for observing the
United States Pharmacopeia—Current Edition color of the acid layer in comparison with the reference
Monograph on Mineral Oil standard color solution. The size and shape of the comparator
National Formulary—Current Edition are optional, but the size and shape of the apertures shall
Monograph on Light Mineral Oil conform to the dimensions prescribed in Fig. 1.

2.3 Government Document:5 6. Reagents

21CFR 172.878 Food and Drug Administration Title 6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
3. Summary of Test Method all reagents shall conform to the specifications of the Commit-
3.1 The mineral oil is treated with concentrated sulfuric acid tee on Analytical Reagents of the American Chemical Society,
where such specifications are available.6 Other grades may be
used, provided it is first ascertained that the reagent is of
1
This test method is under the jurisdiction of ASTM Committee D-2 on sufficiently high purity to permit its use without lessening the
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.06on Analysis of Lubricants. accuracy of the determination.
Current edition approved Nov. 10, 1999. Published January 2000. Originally
published as D 565 – 40. Last previous edition D 565 – 88. 6
Reagent Chemicals, American Chemical Society Specifications, American
2
Annual Book of ASTM Standards, Vol 11.01. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
Annual Book of ASTM Standards, Vol 05.02. listed by the American Chemical Society, see Analar Standards for Laboratory
4
Available from U.S. Pharmacopeial Convention, 12601 Twinbrook Parkway, Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Rockville, MD 20852. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
5
Available from Standardization Documents Order Desk, Bldg. 4 Section D, MD.
700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

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 D 565

FIG. 1 Color Comparator for Carbonizable Substances in Liquid Petrolatum

6.2 Purity of Water—Unless otherwise indicated, acetic acid (CH3COOH) (Warning— Corrosive. Combustible.
references to water shall be understood to mean distilled water Vapor
or water of equal purity conforming to Type III of
Specification D 1193.
6.3 Cobaltous Chloride Solution (0.25 M)—Prepare a solu-
tion of hydrochloric acid (HCl) (Warning—Causes burns.
Vapor extremely irritating.) by mixing 30 mL of concentrated
HCl with 1170 mL of water. Slowly add the acid to the
water. Dissolve 65 6 1 g of cobaltous chloride hexahydrate
(CoCl2·6H2O) in the HCl solution to make 1000 mL of
solution. Using a pipet, transfer 5 mL of this solution to a
250 mL iodine flask. Prepare a solution of sodium
hydroxide (NaOH) (Warning—Corrosive. Can cause
severe burns or blindness. Evolution of heat produces a
violent reaction or 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 solution to the iodine flask. Add 5 mL
of hydrogen peroxide (H2O2) (3 % v/v). Boil for 10 6 1
min, cool, and add 2 g of potassium iodide (KI). Prepare a
solution of H2SO4 (Warning—Causes burns. Vapor
extremely irritating. Strong oxidizer.) by mixing 6 mL of
H2SO4 with 18 mL of water. Slowly add the acid to the
water (see Note 1). Add 20 mL of this H2SO4 solution to
the flask.) When the precipitate has dissolved, titrate the
liberated iodine with 0.100 M sodium thiosulfate (Na2S2O3)
solution, using starch solution as an indicator. Each
millilitre of Na2S2O3 solution is equivalent to 0.0238 g of
CoCl2·6H2O. Adjust the final volume of CoCl2 solution by
the addition of HCl solution so that 1 mL contains
59.5 mg of CoCl2·6H2O.
NOTE 1—This freshly prepared H2SO4 solution will be hot. Allow to
cool before continuing.
6.4 Cupric Sulfate Solution (0.25 M)—Prepare a solution of
HCl (Warning—see 6.3) by mixing 30 mL of concentrated
HCl with 1170 mL of water. Slowly add the acid to the
water. Dissolve 65 6 1 g of cupric sulfate pentahydrate
(CuSO4·5H2O) in enough HCl solution to make 1000 mL
of solution. Using a pipet, transfet 10 mL of the solution to
a 250-mL iodine flask, add 40 mL of water. Prepare a 6M
2
 D 565
irritating.) solution by mixing 353 mL of concentrated
CH3COOH with 1000 mL of water. Slowly add the acid to
the water. Add 4 mL of 6M CH 3 COOH,3g of Kl and5 mL
of HCl to the flask. Titrate the liberated iodine with 0.100 M
Na2S2O3 solution, using starch solution as an indicator. Each
millilitre of Na2S2O3 solution is equivalent to 0.0250 g of
CuSO4·5H2O. Adjust the final volume of the CuSO 4 solution
by the addition of diluted HCl solution so that 1 mL contains
62.4 mg CuSO4·5H2O.
6.5 Ferric Chloride Solution (0.166 M)—Prepare a
solution of HCl (Warning—see 6.3) by mixing 30 mL of
concentrated HCl with 1170 mL of water. Dissolve 55 6 1
g of ferric chloride hexahydrate (FeCl 3·6H2O) in enough
HCl to make 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 and 5 mL HCl, and allow the mixture to
stand for 15 6 1 min. Dilute with 100 mL of water and
titrate the liberated iodine with 0.100 M Na2S2O3 solution,
using starch solution as an indicator. Each millilitre of
Na2S2O3 solution is equivalent to 0.0270 g of FeCl3·6H2O.
Adjust the final volume of FeCl 3 solution by the addition
of the HCl solution so that 1 mL contains 45.0 mg of
FeCl3·6H2O.
6.6 The solutions prepared in 6.3-6.5 may be prepared in
different quantities, provided the ratios of components are
equivalent.
6.7 Colorimetric Reference Standard Solution—Prepare a
reference standard pale amber solution for color comparison
by mixing together 1.5 parts of CoCl 2 solution, 3.0 parts of
the FeCl3 solution and 0.5 parts of the CuSO 4 solution.
Measure 5 mL of this mixture into a test tube as specified in
5.1. This pale amber reference standard shall then be overlaid
with 5 mL of white mineral oil.
6.8 Sulfuric Acid (94.7 6 0.2 %)—The H2SO4 shall be
nitrogen-free when analyzed in accordance with the
following procedure: Dilute a small amount of the acid
with an equal volume of water and superimpose 10 mL of
the cooled liquid upon diphenylamine solution (1 g of
diphenylamine in 100 mL of concentrated H2SO4). A blue
color should not appear at the

3
 D 565
zone of contact within 1 h. This test detects as little as
0.0002 % nitric acid (HNO3). test tube in the color comparator, and compare the acid layer
with 5 mL of the standard colorimetric solution and 5 mL of
7. Procedure white mineral oil in a test tube that has been shaken
7.1 Clean a test tube with a chromic acid (H2CrO4) cleaning vigorously for 10 s and allowed to stand just long enough for
solution (Warning—Causes severe burns. A recognized car- the contents to separate into two layers.
cinogen. Strong oxidizer.), or use a nonchromium containing,
strongly oxidizing cleaning solution. 8. Interpretation of Results
7.2 Fill the test tube to the 5 mL mark with H2SO4 (94.7 8.1 White mineral oil shall be reported as passing the test
6 0.2 %). Then add the oil to be tested to the 10-mL mark, only when the oil layer shows no change in color (see Note 2)
insert the stopper loosely, and place the test tube in position and when the acid layer is not darker than the reference
in the water bath at 100 6 0.5°C. standard colorimetric solution.
7.3 After the test tube has been in the water bath for 30 s, NOTE 2—A bluish haze or a slight pink or yellow color in the oil layer
loosen the stopper sufficiently to release any pressure and should not be interpreted as a change in color.
reinsert, remove the test tube from the bath quickly, hold with
8.2 If the oil layer is discolored or if the acid layer is darker
a finger over the stopper, and give three vigorous, vertical
than the reference standard colorimetric solution, white min-
shakes over an amplitude of about 5 in. (127 mm), shaking the
eral oil shall be reported as not passing the test.
test tube quickly and at a rate corresponding to 5 shakes/s. (A
shaking machine may be employed provided the results that 9. Precision and Bias
can be obtained agree with those obtained by the prescribed
manual agitation.) Repeat every 30 s. Do not keep the test tube 9.1 No statement is made about either the precision or bias
out of the bath longer than 3 s for each shaking period. of this test method since the result merely states whether there
7.4 At the end of 10 min from the time the test tube was is conformance to the criteria for success specified in the
first placed in the bath, remove the test tube and allow to stand procedure.
in the room for not less than 10 min nor more than 30 min.
10. Keywords
Observe and record any discoloration of the oil layer. Place the
10.1 carbonizable substances; mineral oil

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