Designation: D 1240 02

Standard Test Methods for

Rosin Acids Content of Naval Stores, Including Rosin, Tall

Oil, and Related Products1
This standard is issued under the fixed designation D 1240; 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.

rosin acids content of naval stores products into a single

method.
4.1.1 For materials containing less than 15 % rosin, the
modified Glidden procedure has gained acceptance over the
Herrlinger-Compeau. For materials containing more than 15 %
rosin the modified Wolfe Method is preferred. The modified
Wolfe and modified Glidden procedures differ only in their
details. They have been combined here into a single procedure.
This procedure can be run using either a potentiometer or an
internal indicator to determine the end point of the titration.
Use of a potentiometer is preferred and is the referee method.
Use of an internal indicator is the principal alternative method.
They will be referred to as the Potentiometric Method and the
Internal Indicator Method to distinguish them from the
Herrlinger-Compeau and Linder-Persson methods.
4.1.2 The Herrlinger-Compeau Method is limited in application to materials containing less than 15 % rosin. It is little
used in the industry today. Much early work is based on this
test method so it is included here to provide a historical basis
for the overall test method.
4.1.3 The Linder-Persson Method is also little used in the
industry today. It is applicable for measuring the rosin acids
content of naval stores products containing greater than 60 %
rosin. Like the Herrlinger-Compeau, it is included here to
provide a historical basis for the test method. In those instances
where they are used, the Herrlinger-Compeau and LinderPersson methods are often in conjunction to cover the whole
range of rosin content.

1. Scope
1.1 These test methods cover the determination of rosin
acids in tall oil, tall oil fatty acid, tall oil rosin, and other naval
stores products.
1.2 These test methods may not be applicable to adducts or
derivatives of rosin, fatty acid, or other naval stores products.
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.
2. Referenced Documents
2.1 ASTM Standards:
D 1585 Test Methods for Fatty Acids Content of Naval
Stores, Including Rosin, Tall Oil, and Related Products2
E 70 Test Method for pH of Aqueous Solutions with the
Glass Electrode3
E 177 Practice for the Use of the Terms Precision and Bias
in ASTM Test Methods4
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method4
3. Summary of Test Method
3.1 The rosin acids content is determined by one of three
procedures; by selective esterification of fatty acids to form
methyl esters followed by titration of the unreacted rosin acids,
by selective esterification of fatty acids to form butyl esters
followed by titration of the unreacted rosin acids, or by
selective esterification of fatty acids to form methyl esters
followed by extraction of the sulfuric acid catalyst and titration
of the unreacted rosin acids.

5. Reagents
5.1 Purity of ReagentsReagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society
where such specifications are available.5 Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the

4. Significance and Use

4.1 This is revision of the method for measuring rosin acids
content combines the three major ways of determining the
1
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.34 on Naval Stores.
Current edition approved May 10, 2002. Published July 2002. Originally
published as D 1240 52 T. Last previous edition D 1240 96.
2
Annual Book of ASTM Standards, Vol 06.03.
3
Annual Book of ASTM Standards, Vol 15.05.
4
Annual Book of ASTM Standards, Vol 14.02.

5
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

D 1240
(C6H4COOKCOOH) in 60 mL of water followed by 40 mL of
methanol; 2.553 g of potassium acid phthalate will be neutralized by 25.00 mL of 0.5 N KOH solution. Protect the
standardized solution against evaporation and absorption of
carbon dioxide (CO2) from the air. Restandardize the solution
frequently, either potentiometrically or colorimetrically, using
phenolphthalein as the indicator.
10.1.1 For fatty acids containing low concentrations of rosin
acids, 0.1 N alcoholic potassium hydroxide may give superior
results.
10.2 Ethanol (95 %)Denatured alcohol conforming to
Formula No. 3A or No. 30 of the U.S. Bureau of Internal
Revenue, neutralized by the addition of KOH.
10.3 Methanol (99.5 %).
10.4 Methyl Sulfuric Acid SolutionSlowly pour 100 g of
concentrated sulfuric acid (H2SO4 sp gr 1.82 to 1.84), while
stirring constantly, into 400 g of methanol. Extreme caution
should be taken while preparing the methyl sulfuric acid.
Adding sulfuric acid too rapidly may cause the methanol to
flash out of its container. Store the methyl sulfuric acid in a
glass-stoppered bottle.
10.5 Toluene.

accuracy of the determination.

5.2 Unless otherwise indicated, references to water shall be
understood to mean deionized or distilled water.
6. Preparation of Sample
6.1 Homogeneous liquid materials may be used without
further preparation.
6.2 Nonhomogeneous liquid materials should be heated
until they are homogeneous, then a portion taken for analysis.
6.3 Solid samples are subject to surface oxidation which
may affect the results. Prepare the sample for analysis by
chipping small pieces from a freshly exposed surface of a lump
or lumps and crush to a coarse powder to facilitate weighing
and solution. Prepare fresh on the same day, prior to weighing,
in order to avoid changes due to surface oxidation of crushed
rosin on exposure to the air.
ROSIN ACIDS CONTENT BY THE
POTENTIOMETRIC METHOD
(Referee Method)
7. Scope
7.1 This test method covers the determination of rosin acids
content of tall oil rosin, tall oil fatty acid, and other naval stores
products, where the most reproducible results are desired. By
using the potentiometric inflection end points, the error due to
colorimetric end points is avoided.

11. Procedure
11.1 Weigh the sample to the nearest 0.001 g in a 250-mL
flask. Choose the amount of sample so that the second titration
will consume between 10 and 30 mL of KOH solution. For
rosin acids, this will be about 5 g of material. For fatty acids
containing less than 15 % rosin, this will be about 40 g of
material. For fatty acids containing less than 3 % rosin acids
titrating with 0.1 N KOH may give superior results. Table 1
gives suggested amounts of material to use.
11.2 Dissolve the sample in 100 mL of methanol in a
250-mL flask. If the sample has a high rosin content it may be
helpful first to dissolve it in 25 mL of toluene before adding the
methanol. For material believed to contain less than 15 % fatty
acid, that is, high in rosin, add 5 mL of methyl sulfuric acid,
connect the flask assembly, and reflux the solution for 2 min.
(Solid samples must be in solution before beginning reflux.)
For materials believed to contain concentrations of fatty acid
higher than 15 %, that is, low in rosin, use 10 mL of methyl
sulfuric and reflux for 20 min. Measure reflux time from the
moment the first drop of solvent returns to the flask from the
condenser. Cool and transfer to a 400-mL beaker, using a total
of 100 mL of methanol (Note 1) in three successive rinsings.

8. Summary of Test Method

8.1 A sample is refluxed with methyl sulfuric acid to esterify
the fatty acids. The rosin acids and sulfuric acid are then
titrated potentiometrically, and the rosin acids content calculated from the difference between the two inflection points
obtained.
9. Apparatus
9.1 pH MeterAn indicating potentiometer having a limit
of error not greater than 60.1 pH over a range from pH 1 to pH
13, using an alkali-resistant glass electrode and a saturated
calomel half-cell. The pH meter shall conform to the requirements of Test Method E 70. Alternatively, an automatic potentiometric titrator may be used.
9.2 Stirrer,
magnetic,
equipped
with
poly(tetrafluoroethylene)-coated stir bar.
9.3 Buret, 50-mL capacity, with 0.1-mL divisions. The
so-called automatic buret is preferable as its use minimizes
errors due to evaporation. The automatic buret should be
guarded with soda-lime tubes against the absorption of CO2
from the air.
9.4 Erlenmeyer Flask, 250-mL or larger of a chemically
resistant glass with a standard-taper 24/40 joint.
9.5 Condenser, water-cooled, equipped with a joint fitting
the flask described in accordance with 9.4.

NOTE 1Ethanol is preferable when an automatic titrator is used.

11.3 Turn the pH meter on and allow a few minutes for it to

come to equilibrium. Balance the meter using a standard buffer
solution as described in Test Method E 70; then rinse the
electrodes thoroughly with water and then with alcohol.
TABLE 1 Sample Size and Titrant

10. Reagents
10.1 Alcoholic Alkali, Standard Solution (0.5 N)Dissolve
33 g of potassium hydroxide (KOH), preferably in pellet form,
in methanol (CH3OH) and dilute to 1 L with methanol.
Standardize to 60.001 N with potassium acid phthalate

Material
Rosin
Fatty acid, <15 % rosin
Fatty acid, <3 % rosin

Sample Size,
g

Reflux Time,
min

KOH
Normality,
N

5
40
40

2
20
20

0.5
0.5
0.1

D 1240
16. Reagents
16.1 Alcoholic Alkali, Standard SolutionSee 10.1.
16.2 MethanolSee 10.3
16.3 Methyl Sulfuric Acid SolutionSee 10.4.
16.4 Thymol Blue Indicator Solution (1 g/L)Dissolve 1 g
of thymol blue in 1000 mL of methanol.
16.5 Toluene.

11.4 Immerse the electrode in the sample solution. Start the

stirrer and adjust its speed for vigorous stirring without
splattering.
11.5 Titrate the sample solution with 0.5 N KOH to a fixed
pH of 4.0, the first end point. If it appears that the buret does
not contain sufficient KOH to continue the titration to the
second end point, refill the buret at this point. Continue the
titration to the fixed pH of 10.8, the second point. Record the
amount of KOH required for the titration between the first and
second end point. If an automatic titrator is used, the end points
shall be taken at the inflection points or at the fixed pH of 4.0
and 10.8.

17. Procedure
17.1 Weigh the sample to the nearest 0.001 g in a 250-mL
flask. Choose the amount of sample so that the titration will
consume between 10 and 30 mL of 0.5 N KOH. For rosin acids,
this will be about 5 g of material. For fatty acids containing less
than 15 % rosin, this will be about 40 g of material. For fatty
acids containing less than 3 % rosin acids, titrating with 0.1 N
KOH may give superior results. Table 1 gives suggested
amounts of material to use.
17.2 Dissolve the sample in 100 mL of methanol in a
250-mL flask. If the sample has a high-rosin content it may be
helpful first to dissolve it in 25 mL of toluene before adding the
methanol. For material believed to contain less than 15 % fatty
acid, add 5 mL of methyl sulfuric acid, connect the flask
assembly, and reflux the solution for 2 min. (Solid samples
must be in solution before beginning reflux.) For materials
believed to contain concentrations of fatty acid higher than
15 %, use 10 mL of methyl sulfuric and reflux for 20 min.
Measure reflux time from the moment the first drop of solvent
returns to the flask from the condenser. Cool, add 1 mL of
thymol blue indicator.
17.3 Titrate with the KOH solution to the first end point,
about pH 4.0, when the solution changes color from red to
yellow. Record the reading or refill the buret. Continue the
titration to the second end point, about pH 10.8, when the
solution changes color from yellow to blue. Record to the
nearest 0.1 mL the millilitres of KOH solution required for
titration between the two end points.

12. Calculation
12.1 Calculate the percentage of rosin acids as follows:
12.1.1 For materials containing less than 15 % rosin:
Rosin acids, % 5 @~AN/B! 3 30.24# 2 1.1

(1)

where:
A
= KOH solution required for titration between the
first and second end points, mL,
N
= normality of the KOH solution,
B
= sample used, g, and
30.24 = (mol weight of abietic acid 3 100)/1000
12.1.2 For materials containing greater than 15 % rosin:
Rosin acids, % 5 ~AN/B! 3 30.24

(2)

where:
A
= KOH solution required for titration between the
first and second end points, mL,
N
= normality of the KOH solution,
B
= sample used, g, and
30.24 = (mol wt of abietic acid 3 100)/1000
12.2 Report the percentage of rosin acids calculated by
either 12.1.1 or 12.1.2 to the first decimal place.
ROSIN ACIDS CONTENT BY THE INTERNAL
INDICATOR METHOD
(Alternative Method)

NOTE 2These end points approximate the inflection points under the
nonaqueous conditions employed.

13. Scope
13.1 This test method covers the determination of rosin
acids content of tall oil rosin, tall oil fatty acid, and other naval
stores products, using an internal indicator for the determination of the end point. It gives good results when routinely
applied by a skilled analyst. However, where the most reproducible results by different analysts and laboratories are desired, the referee method (Sections 6 to 11) should be used.

18. Calculation
18.1 Calculate the percentage of rosin acids as described in
12.1.
18.2 Report the percentage of rosin acids to the first decimal
place.
19. Precision and Bias
19.1 Interlaboratory Test ProgramAn interlaboratory
study of the rosin acid content of three substances, tall oil fatty
acids, distilled tall oil, and rosin, was run in 1994. Each of 14
laboratories tested each of the three materials. The design of
the experiment, similar to that of Practice E 691 and a
within-between analysis of the data are given in ASTM
Research Report.6
19.2 Test ResultThe precision information given below
for the rosin acid content of naval stores products is for the

14. Summary of Test Method

14.1 A sample is refluxed with methyl sulfuric acid to
esterify the fatty acids. The rosin acids and sulfuric acid are
then titrated in the presence of thymol blue indicator. The rosin
acids content is then calculated from the difference between the
two color end points obtained.
15. Apparatus
15.1 The apparatus for the esterification and titration of the
sample shall consist of the flask, condenser, and buret described in Section 9.

6
Supporting data are available from ASTM International Headquarters. Request
RR: D01 - 1087.

D 1240
23.6 Potassium Hydroxide Standard Alcoholic Solution (0.2 or 0.5 N)Dissolve 13.3 g of KOH (preferably in
pellet form) for a 0.2-N solution or 33.3 g for a 0.5-N solution
(see 24.3) in methanol (99.5 %) and dilute to 1 L with
methanol. Standardize to 60.001 N. The standardized solution
should be protected against evaporation and the absorption of
CO2 from the air, and should be restandardized frequently.
23.7 Sodium Sulfate SolutionDissolve 100 g Na2SO4 in
water and dilute to 1 L. The resulting solution should have a pH
of 7.2 60.4 (Note 2).

comparison of two test results, each of which is the average of

three test determinations as follows:
19.2.1 Repeatability Limit, 95 % (within laboratory) = 0.6 %.
19.2.2 Reproducibility Limit, 95 % (between laboratories) = 1.4 %.
19.3 These terms (repeatability limit and reproducibility
limit) are used as specified in Practice E 177. The respective
standard deviations among test results, related to the above
numbers by the factor of 2.8, are as follows:
19.3.1 Repeatability standard deviation = 0.2 %.
19.3.2 Reproducibility standard deviation = 0.5 %.
19.4 BiasThese test methods have no bias because rosin
acid content is defined only in terms of these test methods.

NOTE 3A suitable pH adjustment may be made by adding dilute (5 %)

NaOH solution to a faint pink-red phenolphthalein color, then adding
dilute sulfuric acid (5 %) solution until the color is discharged.

23.8 Sulfuric Acid (sp gr 1.84).

ROSIN ACIDS BY THE HERRLINGER-COMPEAU

METHOD

24. Procedure
24.1 Dissolve 40 60.1 g of the sample in 100 ml of
methanol in a 250-mL flat-bottomed flask. Swirl the flask to
dissolve the oil and add a clean boiling chip. Add slowly t mL
of H2SO4, while swirling the flask vigorously. Connect the
flask to the condenser, apply heat, and reflux the contents for
10 min. Cool the flask to room temperature with cold water.
24.2 Add 250 mL of the Na2SO4 solution to a 500-mL
separatory funnel. Pour the contents of the flask into the funnel
and complete the quantitative transfer of the flask contents with
100 mL of ether. Thoroughly shake the mixture in the funnel.
Allow to settle, draw off the salt layer, and discard. Wash the
contents of the funnel twice again with 250-mL portions of
Na2SO4 solution. The last washing should not react pink to
methyl orange indicator.
24.3 After removing the last wash, drain the contents of the
separatory funnel into a 500-mL Erlenmeyer flask. Rinse the
funnel with 20 mL of ether and add the rinsings to the flask.
Add 20 mL of ethyl alcohol and 1 mL of the phenolphthalein
indicator solution. Titrate to the appearance of the pink-red
color using 0.2-N alcoholic KOH solution if the rosin acids is
less than 5 % or 0.5 N if more than 5 %.

20. Scope
20.1 The Herrlinger-Compeau Method given here has been
largely superseded by the methods described in Sections 1
through 18.
20.2 This test method covers the determination of rosin
acids in fatty acids when the rosin acids content does not
exceed 15 %.
21. Summary of Test Method
21.1 The rosin acids are determined by titration, after
esterification of the fatty acids with methanol in the presence of
sulfuric acid as a catalyst, followed by separation of the acids.
This test method requires use of an experimentally determined
correction factor dependent upon the amount of rosin acids
present.7
22. Apparatus
22.1 Flask, 250-mL flat-bottom, of chemically resistant
glass with a standard-taper 24/40 neck.
22.2 Condenser, water-cooled, with a joint fitting the flask
described in 22.1
22.3 Separatory Funnel, 500-mL, pear-shaped, fitted with a
glass stopper.
22.4 Buret, 50-mL capacity, with 0.1-mL divisions.

25. Calculation
25.1 Calculate the percentage of rosin acids as follows:
Rosin acids, % 5 ~1.031 3 AN 3 30.2!/S 2 0.74

23. Reagents
23.1 AlcoholNeutral methanol, neutral isopropanol (91 to
99 %), neutral 95 % ethanol, or neutral denatured alcohol
conforming to formula No. 30 or No. 3A of the U.S. Bureau of
Internal Revenue.
23.2 Ethyl Ether.
23.3 Methanol (99.5 %).
23.4 Methyl Orange Indicator SolutionDissolve 0.1 g of
methyl orange in 100 mL of water.
23.5 Phenolphthalein Indicator SolutionDissolve 1 g of
phenolphthalein in 100 mL of methanol.

where:
A
=
N
=
S
=
0.74 =

(3)

KOH solution used for titration of the sample, mL,

normality of KOH solution,
sample used, g, and
correlation factor6 for a rosin acids content not over
15 %.

ROSIN ACIDS BY THE LINDER-PERSSON METHOD8

26. Scope
26.1 This test method covers the determination of rosin
acids content of rosin, unmodified by such materials as maleic

7
For information on the development of this test method and the establishment
of the correction factor, see Herrlinger, R., and Compeau, G. M., The Determination of Rosin in Fatty Acids. Journal of the American Oil Chemists Society,
August 1952, pp. 342344.

8
Linder, A., and Persson, V., Determination of Rosin Acids in Mixtures with
Fatty Acids, Journal of the American Oil Chemists Society, Vol XXXIV, No. 1,
1957, pp. 1227.

D 1240
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,
where such specifications are available.5 Other grades may be
used, provided it is first determined that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the test.
29.2 Cyclohexane.
29.3 n-Butyl Alcohol.
29.4 Butyl Alcohol-Sulfuric Acid Esterification Reagent
Add 500 mL of n-butyl alcohol, 500 mL of cyclohexane, and
3.3 mL (6 g) of sulfuric acid (H2SO4) in a 2 L round-bottom
flask with ground glass joint, connect to a moisture trap and
condenser, and reflux on a hot plate for 30 min to distill out the
water and form butyl-sulfuric acid. Cool and store in a
glass-stoppered bottle.
29.5 0.25 N Potassium Hydroxide, Methanolic Standard
SolutionDissolve 16.5 g of potassium hydroxide pellets in 1
L of methanol. Standardize against potassium acid phthalate
primary standard.
29.6 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid
(H2SO4).
29.7 Thymol Blue Indicator Solution (10 g /L)Mix 1 g of
thymol blue indicator with 100 mL of ethyl alcohol.

or fumaric acid, or phenols. Rosin acids determined by this

method include free rosin.
27. Summary of Test Method
27.1 The rosin acids are determined by a selective esterification of fatty acids with n-butyl alcohol using sulfuric acid as
a catalyst. The rosin acids content is then found by titration.
27.2 The method is applicable for measuring the rosin acids
content of naval stores products containing greater than 60 %
rosin.
28. Apparatus
28.1 Condenser, water-cooled, equipped with a 24/40
standard-taper joint.
28.2 Buret, as in 9.3.
28.3 Erlenmeyer Flask, 250mL of a chemically resistant
glass with a standard-taper 24/40 joint.
28.4 Moisture Collection Trap, constructed according to
details shown in Fig. 1. Alternatively, a commercial DeanStark trap with a minimal collection volume, preferably 5 mL,
can be used. Wrap with insulation.
28.5 Pipet, 50 mL capacity
28.6 Stirrer, magnetic, equipped with a stir bar coated with
poly(tetrafluorethylene).
29. Reagents and Materials
29.1 Purity of ReagentsReagent grade chemicals shall be

30. Procedure
30.1 Transfer 1 to 1.2 g of sample, weighed to the nearest
0.0001 g to a 250mL Erlenmeyer flask.
30.2 Pipet exactly 50 mL of the butyl sulfuric acid esterification reagent into the flask.
30.3 Connect the flask to the moisture collection trap,
having filled the collection arm with butanol. Connect the trap
to a condenser and place the flask on a hot plate. Heat to
boiling and reflux for 20 min, measuring from the time the first
drop of condensate falls from the condenser. At the end of
heating, allow the flask to cool somewhat, then remove and
cool to room temperature.
30.4 Add 0.5 ml of thymol blue indicator solution and titrate
with the alcoholic KOH solution to the second end point,
yellow to blue, at about pH 10.8.
30.5 Make a blank titration on 50 mL of the esterification
solution, after refluxing it in the same manner.
31. Calculation
31.1 Calculate the percent rosin acids in the sample using
the following equation.
Rosin acids, % 5 ~A2B! 3 N 3 30.244 3 1.0184/S 2 0.30

(4)

where:
A
= alcoholic KOH solution required for titration of
the sample, mL,
B
= alcoholic KOH solution required for titration of
the blank, mL,
N
= normality of the KOH solution used,
S
= weight of the sample, g,
30.244 = molecular weight of abietic acid multiplied by
100 and divided by 1000,

FIG. 1 Mositure Collection Trap

D 1240
should agree within 0.81 %. Such values are suitable for
averaging.
32.1.1 The between-laboratory standard deviation was
found to be 0.43 %, absolute. Single determinations from two
laboratories should agree within 1.2 %.
32.2 BiasNo bias can be determined since no standard
naval stores products are available.

1.0184 = factor to correct for the slight esterification of

rosin acids, and
0.30
= factor to correct for unesterified fatty acids.
31.2 Report the results to one decimal place.
32. Linder-Persson Method Precision and Bias
32.1 PrecisionThe following information was developed
by the laboratories of a single company. As such, it does not
meet the requirements normally expected for a precision
statement. However, the information should be useful for
comparative purposes. The within-laboratory standard deviation of this method was found to be 0.29 %, at the 83.6 % rosin
acid level. Duplicate determination from a single laboratory

33. Keywords
33.1 fatty acids; Glidden method; Herrlinger-Compeau
method; rosin; tall oil; tall oil fatty acid; tall oil rosin; Wolfe
Method

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