Designation: D6304 − 16´1

Standard Test Method for

Determination of Water in Petroleum Products, Lubricating
Oils, and Additives by Coulometric Karl Fischer Titration1
This standard is issued under the fixed designation D6304; 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.

ε1 NOTE—Reference to a Summary of Changes was removed editorially in September 2016.

1. Scope D1298 Test Method for Density, Relative Density, or API

1.1 This test method covers the direct determination of Gravity of Crude Petroleum and Liquid Petroleum Prod-
water in the range of 10 mg ⁄kg to 25 000 mg ⁄kg entrained ucts by Hydrometer Method
water in petroleum products and hydrocarbons using auto- D4052 Test Method for Density, Relative Density, and API
mated instrumentation. This test method also covers the Gravity of Liquids by Digital Density Meter
indirect analysis of water thermally removed from samples and D4057 Practice for Manual Sampling of Petroleum and
swept with dry inert gas into the Karl Fischer titration cell. Petroleum Products
Mercaptan, sulfide (S− or H2S), sulfur, and other compounds D4177 Practice for Automatic Sampling of Petroleum and
are known to interfere with this test method (see Section 5). Petroleum Products
D5854 Practice for Mixing and Handling of Liquid Samples
1.2 This test method is intended for use with commercially of Petroleum and Petroleum Products
available coulometric Karl Fischer reagents and for the deter- E203 Test Method for Water Using Volumetric Karl Fischer
mination of water in additives, lube oils, base oils, automatic Titration
transmission fluids, hydrocarbon solvents, and other petroleum
products. By proper choice of the sample size, this test method 3. Summary of Test Method
may be used for the determination of water from mg/kg to 3.1 An aliquot is injected into the titration vessel of a
percent level concentrations. coulometric Karl Fischer apparatus in which iodine for the Karl
1.3 The values stated in SI units are to be regarded as Fisher reaction is generated coulometrically at the anode.
standard. No other units of measurement are included in this When all of the water has been titrated, excess iodine is
standard. detected by an electrometric end point detector and the titration
1.4 This standard does not purport to address all of the is terminated. Based on the stoichiometry of the reaction, 1 mol
safety concerns, if any, associated with its use. It is the of iodine reacts with 1 mol of water; thus, the quantity of water
responsibility of the user of this standard to establish appro- is proportional to the total integrated current according to
priate safety and health practices and determine the applica- Faraday’s Law.
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bility of regulatory limitations prior to use. 3.2 The sample injection can be done either by mass or
volume.
2. Referenced Documents 3.3 The viscous samples can be analyzed by using a water
2.1 ASTM Standards:2 vaporizer accessory that heats the sample in the evaporation
D1193 Specification for Reagent Water chamber, and the vaporized water is carried into the Karl
Fischer titration cell by a dry inert carrier gas.

1
4. Significance and Use
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of 4.1 A knowledge of the water content of lubricating oils,
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. additives, and similar products is important in the
Current edition approved July 1, 2016. Published July 2016. Originally approved
in 1998. Last previous edition approved in 2007 as D6304 – 07, which was
manufacturing, purchase, sale, or transfer of such petroleum
withdrawn in April 2016 and reinstated in July 2016. DOI: 10.1520/D6304-16. products to help in predicting their quality and performance
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or characteristics.
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 4.2 For lubricating oils, the presence of moisture could lead
the ASTM website. to premature corrosion and wear, an increase in the debris load

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 D6304 − 16´1
resulting in diminished lubrication and premature plugging of TABLE 1 Test Sample Size Based on Expected Water Content
filters, an impedance in the effect of additives, and undesirable Expected Water Sample Size µg Water
support of deleterious bacterial growth. Concentration g or mL Titrated
10 mg ⁄kg to 100 mg/kg or µg/mL 3.0 30 to 300
10 mg ⁄kg to 500 mg/kg or µg/mL 2.0 200 to 1000
5. Interferences 0.02 % to 0.1 % 1.0 200 to 1000
5.1 A number of substances and classes of compounds 0.1 % to 0.5 % 0.5 500 to 2500
0.5 % to 2.5 % 0.25 1250 to 6250
associated with condensation or oxidation-reduction reactions
interferes in the determination of water by Karl Fischer
titration. In petroleum products, the most common interfer-
ences are mercaptans and sulfides. At levels of less than
500 mg ⁄kg as sulfur, the interference from these compounds is 7. Reagents and Materials
insignificant for water concentrations greater than 0.02 % by 7.1 Purity of Reagents—Reagent grade chemicals shall be
mass. For more information on substances that interfere in the used in all tests. Unless otherwise indicated, all reagents shall
determination of water by the Karl Fischer titration method, conform to the specifications of the Committee on Analytical
see Test Method E203. Some interferences, such as ketones, Reagents of the American Chemical Society3, where such
may be overcome if the appropriate reagents are used. specifications are available. Use other grades, provided the
5.2 The significance of the mercaptan and sulfide interfer- reagent is of sufficiently high purity to permit its use without
ence on the Karl Fischer titration for water in the 10 mg ⁄kg to lessening the accuracy of the determination.
200 mg ⁄kg range has not been determined experimentally. At 7.2 Purity of Water—Unless otherwise indicated, references
these low water concentrations, however, the interference may to water shall be understood to mean reagent water as defined
be expected to be significant for mercaptan and sulfide con- by Type II of Specification D1193.
centrations of greater than 500 mg ⁄kg as sulfur.
7.3 Xylene, Reagent Grade, less than 100 mg ⁄kg to
5.3 Helpful hints in obtaining reliable results are given in 200 mg ⁄kg water, dried over a molecular sieve (Warning—
Appendix X1. Flammable. Vapor harmful).
6. Apparatus 7.4 Karl Fischer Reagent, standard commercially available
reagents for coulometric Karl Fischer titrations.
6.1 Coulometric Karl Fischer Apparatus (using electromet-
7.4.1 Anode Solution—Mix six parts of commercial Karl
ric end point)—A number of automatic coulometric Karl
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Fischer anode solution with four parts of reagent grade xylene

Fischer titration assemblies consisting of titration cell, plati-
on a volume basis. Newly made Karl Fischer anode solution
num electrodes, magnetic stirrer, and a control unit are avail-
shall be used. Other proportions of anode solution and xylene
able on the market. Instructions for operation of these devices
may be used and determined for a particular reagent, apparatus,
are provided by the manufacturers and are not described
and sample tested. Some samples may not require any xylene,
herein.
whereas others will require the solvent effect of the xylene
6.1.1 Water Vaporizer Accessory—A number of automatic
(Warning—Flammable, toxic if inhaled, swallowed, or ab-
water vaporizer accessories are available on the market.
sorbed through skin).
Instructions for the operation of these devices are provided by
the manufacturers and are not described herein. NOTE 1—Toluene may be used in place of xylene. However, the
precision data in Section 17 were obtained using xylene.
6.2 Syringes—Samples are most easily added to the titration
vessel by means of accurate glass or disposable plastic syringes 7.4.2 Cathode Solution—Use standard commercially avail-
with luer fittings and hypodermic needles of suitable length to able cathode Karl Fischer solution. Newly made solution shall
dip below the surface of the anode solution in the cell when be used (Warning—Flammable, may be fatal if inhaled,
inserted through the inlet port septum. The bores of the needles swallowed, or absorbed through skin. Possible cancer hazard.).
used shall be kept as small as possible, but large enough to 7.4.3 If the sample to be analyzed contains ketone, use
avoid problems arising from back pressure or blocking while commercially available reagents that have been specially
sampling. Suggested syringe sizes are as follows: modified for use with ketones.
6.2.1 Ten microlitres, with a needle long enough to dip NOTE 2—Some laboratories add the ketone suppressing reagent as part
below the surface of the anode solution in the cell when of their standard analytical procedure since often the laboratory does not
inserted through the inlet port septum and graduated for know whether the sample contains ketone.
readings to the nearest 0.1 µL or better. This syringe can be 7.5 Hexane, Reagent Grade, less than 100 mg ⁄kg to
used to accurately inject a small quantity of water to check 200 mg ⁄kg water (Warning—Flammable. Vapor harmful).
reagent performance as described in Section 10. Dried over molecular sieve.
6.2.2 As identified in Table 1, syringes of the following
capacities: 250 µL accurate to the nearest 10 µL; 500 µL
accurate to the nearest 10 µL; 1 mL accurate to the nearest 3
Reagent Chemicals, American Chemical Society Specifications, American
0.01 mL; 2 mL accurate to the nearest 0.01 mL; and 3 mL Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
accurate to the nearest 0.01 mL. A quality gas-tight glass Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
syringe with a TFE-fluorocarbon plunger and luer fitting is and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
recommended. MD.

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 D6304 − 16´1
7.6 White Mineral Oil—Also called paraffin oil or mineral intervals are initially with fresh reagent and then after every ten
oil. Reagent grade. determinations (see 11.3).
7.7 Molecular Sieve 5Å—8 to 12 mesh.
11. Procedure A (by Mass)
8. Sampling 11.1 Add newly made solvents to the anode and cathode
8.1 Sampling is defined as all the steps required to obtain an compartments of the titration vessel and bring the solvent to
aliquot representative of the contents of any pipe, tank, or other end-point conditions as described in Section 9.
system and to place the sample into a container for analysis by 11.2 Add the petroleum product test specimen to the titra-
a laboratory or test facility. tion vessel using the following method:
8.2 Laboratory Sample—The sample of petroleum product 11.2.1 Starting with a clean, dry syringe of suitable capacity
presented to the laboratory or test facility for analysis by this (see Table 1 and Note 5), withdraw and discard to waste at least
test method. Only representative samples obtained as specified three portions of the sample. Immediately withdraw a further
in Practices D4057 and D4177 and handled and mixed in portion of sample, clean the needle with a paper tissue, and
accordance with Practice D5854 shall be used to obtain the weigh the syringe and contents to the nearest 0.1 mg. Insert the
laboratory sample. needle through the inlet port septum, start the titration, and
with the tip of the needle just below the liquid surface, inject
NOTE 3—Examples of laboratory samples include bottles from a the test specimen. Withdraw the syringe, wipe clean with a
manual sampling, receptacles from automatic samplers, and storage
containers holding a product from a previous analysis.
paper tissue, and reweigh the syringe to the nearest 0.1 mg.

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After the end point is reached, record the micrograms of water
8.3 Test Specimen—The aliquot obtained from the labora- titrated.
tory sample for analysis by this test method. Once drawn, use
the entire portion of the test specimen in the analysis. NOTE 5—If the concentration of water in the sample is completely
unknown, it is advisable to start with a small trial portion of sample to
8.4 Select the test specimen size as indicated in Table 1 avoid excessive titration time and depletion of the reagents. Further
based on the expected water concentration. adjustment of the aliquot size may then be made as necessary.
11.2.2 When the background current or titration rate returns
9. Preparation of Apparatus to a stable reading at the end of the titration as discussed in 9.5,
9.1 Follow the manufacturer’s directions for preparation additional specimens may be added as per 11.2.1.
and operation of the titration apparatus. 11.3 Replace the solutions when one of the following occurs
9.2 Seal all joints and connections to the vessel to prevent and then repeat the preparation of the apparatus as in Section
atmospheric moisture from entering the apparatus. 9.
9.3 Add the Karl Fischer anode solution to the anode (outer) 11.3.1 Persistently high and unstable background current.
compartment. Add the solution to the level recommended by 11.3.2 Phase separation in the anode compartment or oil
the manufacturer. coating the electrodes.
11.3.3 The total oil content added to the titration vessel
9.4 Add the Karl Fischer cathode solution to the cathode exceeds one quarter of the volume of solution in the anode
(inner) compartment. Add the solution to a level 2 mm to 3 mm compartment.
below the level of the solution in the anode compartment. 11.3.4 The solutions in the titration vessel are greater than
9.5 Turn on the apparatus and start the magnetic stirrer for one week old.
a smooth stirring action. Allow the residual moisture in the 11.3.5 The instrument displays error messages that directly
titration vessel to be titrated until the end point is reached. Do or indirectly suggest replacement of the electrolytes—see
not proceed beyond this stage until the background current (or instrument operating manual.
background titration rate) is constant and less than the maxi- 11.3.6 The result of a 10 µL injection of water is outside
mum recommended by the manufacturer of the instrument. 10 000 µg 6 200 µg.
NOTE 4—High background current for a prolonged period may be due 11.4 Thoroughly clean the anode and cathode compartment
to moisture on the inside walls of the titration vessel. Gentle shaking of the with xylene if the vessel becomes contaminated with product.
vessel (or more rigorous stirring action) will wash the inside with Never use acetone or similar ketones. Clogging of the frit
electrolyte. Keep the titrator on to allow stabilization to a low background
current.
separating the vessel compartments will cause instrument
malfunction.
10. Calibration and Standardization 11.5 For products too viscous to draw into a syringe, add the
10.1 In principle, standardization is not necessary since the sample to a clean, dry bottle and weigh the bottle and product.
water titrated is a direct function of the coulombs of electricity Quickly transfer the required amount of sample to the titration
consumed. However, reagent performance deteriorates with vessel by suitable means, such as with a dropper. Reweigh the
use and shall be regularly monitored by accurately injecting a bottle. Titrate the sample as in 11.2.
known quantity of water (see 7.2) that is representative of the
typical range of water concentrations being determined in 12. Procedure B (by Volume)
samples. As an example, one may accurately inject 10 000 µg 12.1 Follow steps 11.2.1 through 11.5 from Procedure A,
or 10 µL of water to check reagent performance. Suggested taking sample by volume instead of mass.

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 D6304 − 16´1
NOTE 6—A volume aliquot of the product is titrated to an electrometric use and shall be homogeneous and stable under the anticipated
end point using a coulometric Karl Fischer apparatus. The steps described storage conditions. Prior to monitoring the measurement
in Procedure A are followed except as noted. The volume injection method
is applicable only when the vapor pressure and viscosity of the sample
process, the user of the method needs to determine the average
permit an accurate determination of the volume of the sample. value and control limits of the QC sample. The QC sample
NOTE 7—The referee procedure for determination of water in liquid precision shall be checked against the ASTM method precision
petroleum products by coulometric Karl Fischer titration is Procedure A, to ensure data quality.
which uses a mass measurement of the product test specimen.
NOTE 8—The presence of gas bubbles in the syringe can be a source of 15. Calculation
uncertainly. The tendency of product to form gas bubbles is a function of
product type and corresponding vapor pressure. Viscous products can 15.1 Calculate the water concentration in mg/kg or µL/mL
prove to be difficult to measure volumetrically with a precision syringe. of the sample as follows:
NOTE 9—Helpful hints in obtaining reliable results are given in W1
Appendix X1. water, mg/kg or µg/g 5 or (1)
W2
13. Procedure C (Water Evaporator Accessory)
V1
13.1 If using the water evaporator accessory for samples water, µL/mL 5
V2
difficult to analyze by Procedure A or B due to sample
viscosity, matrix interference, or extremely small concentra- where:
tions of water (for example, <100 mg ⁄kg), add 10 mL of white W1 = mass of water titrated, mg or µg (as appropriate),
oil to the evaporator accessory. Bubble dry nitrogen gas at W2 = mass of sample used, kg or g (as appropriate),
about 300 mL ⁄min through the oil. Heat the oil to the tempera- V1 = volume of water titrated, µL, and
ture suggested by the instrument manufacturer for a particular V2 = volume of sample used, mL.
product type. 15.2 Calculate the water concentration, in mass or volume
13.2 Dissolve 5 g 6 0.01 g of accurately weighed viscous %, of the sample as follows:
sample in a 10 mL volumetric flask. Make up to volume with W1
water, mass % 5 or (2)
dried hexane. Shake the sample until it is completely dissolved 10 000 3 W 2
in the solvent.
V1
NOTE 10—All parts of the glass assembly must be thoroughly dry volume % 5
10 3 V 2
before use. The smallest amount of contamination by moisture will cause
erroneous results. Perform several preliminary runs with known content where W1, W2, V1, and V2 are same as in 15.1.
standards to determine that the system is operating correctly. Water-in-
alcohol standards must be capped with rubber septa rather than rubber 15.3 Use the following equations for calculating the water
stoppers. content of the sample in units of volume % from mass %, or of
13.3 Inject 1 mL of dissolved sample into the evaporator mass % from volume %.
assembly. Start the operating sequence. Follow steps 11.1
through 11.5 in Procedure A. After the end point is reached, water, volume % 5 water, mass % 3 F density of sample at t
density of water at tG (3)
record the micrograms of water titrated from the digital readout
on the instrument. water, mass % 5 water, volume %/ Fdensity of sample at t
density of water at t G (4)

14. Quality Control Checks where:

14.1 Confirm the performance of the instrument or the t = test temperature.
procedure each day it is in use by analyzing a QC sample that 15.3.1 Density may be measured using approved test meth-
is representative of samples typically analyzed. Quality control ods such as Test Method D1298 and Test Method D4052. If the
frequency should be increased if a large number of samples are density is measured in units of g/mL and the density of water
routinely analyzed. If the analysis is shown to be in statistical at test temperature is assumed to be 1 g/mL, Eq 5 and Eq 6
control, QC frequency may be reduced. Analysis of result(s) simplify to:
from these QC samples may be performed using control chart
water, volume % 5 water, mass % 3 density of sample at t ~ g/mL!
techniques4 or other statistical techniques. If the QC sample
result determined causes the laboratory to be in an out-of- (5)
control situation, such as exceeding the laboratory’s control water, mass % 5 water, volume %/density of sample at t ~ g/mL! (6)
limits, investigate and take corrective action to bring the test
16. Report
back into control before proceeding. An ample supply of QC
sample material shall be available for the intended period of 16.1 Report the water concentration to the nearest whole
(mg/kg), nearest 0.01 % by mass, nearest whole µL/mL, or
nearest 0.01 % by volume.
4
ASTM MNL7, Manual on Presentation of Data Control Chart Analysis, 6th
Edition, Section 3: Control Charts for Individuals, ASTM International, W. 16.2 Report the water concentration as obtained by Test
Conshohocken, PA. Method D6304, Procedure A, Procedure B, or Procedure C.

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 D6304 − 16´1
17. Precision and Bias5 17.1.2 Reproducibility—The difference between 2 single
17.1 The precision of this test method as determined by the and independent results obtained by different operators work-
statistical examination of interlaboratory test results is as ing in different laboratories on identical test materials would, in
follows: the long run, exceed the following values in only 1 case in 20.
17.1.1 Repeatability—The difference between successive Volumetric Injection Mass Injection
Repeatability 0.08852 x 0.7 volume % 0.03813 x 0.6 mass %
results obtained by the same operator with the same apparatus Reproducibility 0.5248 x 0.7 volume % 0.4243 x 0.6 mass %
under constant operating conditions on identical test material where x is the mean of duplicate measurements.
would, in the long run, in the normal and correct operation of
the test method, exceed the following values only in 1 case in 17.2 Bias—This test method has no bias since the coulo-
20. metric determination can be defined only in terms of this test
method.

5
18. Keywords
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1436. 18.1 coulometric titration; Karl Fischer titration; water

APPENDIX
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(Nonmandatory Information)

X1. HELPFUL HINTS FOR COULOMETRIC KARL FISCHER WATER ANALYSIS

X1.1 Following precautions are suggested to obtain accu- or 10 µL of pure water. Suggested intervals are initially with
rate and precise results by this test method. Some of these fresh reagent, and then after every ten determinations.
suggestions are also described in the text of the test method, X1.1.8 Rinse the clean dry syringe at least three times with
but are compiled here for easy reference. the sample and discard the aliquots before taking an aliquot for
X1.1.1 A number of chemicals interfere in this titration: injecting into the titration vessel.
mercaptans, sulfides, amines, ketones, aldehydes, oxidizing X1.1.9 During the blank measurement instrument
and reducing agents, and so forth. Some of the interferences preparation, high background current for a prolonged period
can be eliminated by addition of suitable reagents, for example, may be due to moisture on the inside walls of the titration
addition of benzoic or succinic acid for aldehyde and ketone vessel. Wash the inside with the electrolyte by gently shaking
interference. the vessel or by more vigorously stirring.
X1.1.2 At low water concentrations (<0.02 % by mass), the X1.1.10 The frit separating the vessel compartments may
interference by mercaptan and sulfide (>500 mg ⁄kg as sulfur) get clogged with sample residues; Disassemble the apparatus in
may be significant (see Test Method E203). such cases and acid clean the frit.
X1.1.3 All equipment should be scrupulously clean of X1.1.11 Any time one of the following situations occurs,
moisture. Rinse all syringes, needles, and weighing bottles replace the anode and the cathode solutions and then repeat the
with anhydrous acetone after cleaning. Then dry in an oven at preparation of the apparatus as in Section 9.
100°C for at least an hour and store immediately in a X1.1.11.1 Persistently high and unstable background cur-
desiccator. rent.
X1.1.4 Fill the dry cooled sample bottle as rapidly as X1.1.11.2 Phase separation in the anode compartment or the
possible with the sample within 15 mm of the top and sample coating the electrodes.
immediately seal. X1.1.11.3 The total amount of sample added to the titration
vessel exceeds one fourth of the volume of solution in the
X1.1.5 After removing a sample aliquot from the bottle with anode compartment.
a dry hypodermic syringe, inject dry nitrogen into the sample X1.1.11.4 The solutions in the titration vessel are over one
bottle with the syringe to displace the removed sample void. week old.
X1.1.6 The presence of gas bubbles in the syringe may be a X1.1.11.5 The instrument displays error messages that sug-
source of uncertainty. Viscous samples may be difficult to gest replacement of the electrodes.
measure with a precision syringe. In such cases, taking the X1.1.11.6 The results of a 10 µL injection of water is
sample aliquot by mass is preferred to volume measurement. outside 10 000 µg 6 200 µg.
X1.1.7 Although standardization is not necessary in coulo- X1.1.12 If the titration vessel gets contaminated with the
metric titrations, reagent performance deteriorates with use and sample, thoroughly clean the anode and cathode compartments
must be regularly monitored by accurately injecting 10 000 µg with xylene. Never use acetone or similar ketones.

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