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: D664 − 18´2 British Standard 4457

Designation 177/96

Standard Test Method for

Acid Number of Petroleum Products by Potentiometric
Titration1
This standard is issued under the fixed designation D664; 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.

ε1 NOTE—Subsection 13.3.1 and a statement in the Summary of Changes were corrected editorially in December 2018.
ε2 NOTE—Subsections 16.1.1.1 and 16.1.2.1 were corrected editorially in January 2019.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* NOTE 2—The acid number obtained by this standard may or may not be
numerically the same as that obtained in accordance with Test Methods
1.1 This test method covers procedures for the determina- D974 and D3339. There has not been any attempt to correlate this method
tion of acidic constituents in petroleum products, lubricants, with other non-titration methods.
biodiesel, and blends of biodiesel. NOTE 3—A few laboratories have made the observation that there is a
1.1.1 Test Method A—For petroleum products and lubricants difference in Test Method D664 results when aqueous versus nonaqueous
buffers are used.
soluble or nearly soluble in mixtures of toluene and propan-2-
ol. It is applicable for the determination of acids whose 1.3 The values stated in SI units are to be regarded as
dissociation constants in water are larger than 10–9; extremely standard. No other units of measurement are included in this
weak acids whose dissociation constants are smaller than 10–9 standard.
do not interfere. Salts react if their hydrolysis constants are 1.4 This standard does not purport to address all of the
larger than 10–9. The range of acid numbers included in the safety concerns, if any, associated with its use. It is the
precision statement is 0.1 mg ⁄g KOH to 150 mg ⁄g KOH. responsibility of the user of this standard to establish appro-
1.1.2 Test Method B—Developed specifically for biodiesel priate safety, health, and environmental practices and deter-
and biodiesel blends with low acidity and slightly different mine the applicability of regulatory limitations prior to use.
solubility. This test method requires the use of an automatic 1.5 This international standard was developed in accor-
titrator with automatic endpoint-seeking capability. dance with internationally recognized principles on standard-
NOTE 1—In new and used oils, the constituents that may be considered ization established in the Decision on Principles for the
to have acidic characteristics include organic and inorganic acids, esters, Development of International Standards, Guides and Recom-
phenolic compounds, lactones, resins, salts of heavy metals, salts of
ammonia and other weak bases, acid salts of polybasic acids, and addition mendations issued by the World Trade Organization Technical
agents such as inhibitors and detergents. Barriers to Trade (TBT) Committee.
1.2 The test method may be used to indicate relative 2. Referenced Documents
changes that occur in oil during use under oxidizing conditions
regardless of the color or other properties of the resulting oil. 2.1 ASTM Standards:2
Although the titration is made under definite equilibrium D974 Test Method for Acid and Base Number by Color-
conditions, the test method is not intended to measure an Indicator Titration
absolute acidic property that can be used to predict perfor- D1193 Specification for Reagent Water
mance of oil under service conditions. No general relationship D3339 Test Method for Acid Number of Petroleum Products
between bearing corrosion and acid number is known. by Semi-Micro Color Indicator Titration
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1
This test method is under the jurisdiction of ASTM Committee D02 on D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Petroleum Products
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
Current edition approved Nov. 1, 2018. Published November 2018. Originally
approved in 1942. Last previous edition approved in 2017 as D664 – 17a. DOI:
2
10.1520/D0664-18E02. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method was adopted as a joint ASTM-IP standard in 1964. ASTM Test contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Method D4739 has been developed as an alternative to the base number portion of Standards volume information, refer to the standard’s Document Summary page on
D664. the ASTM website.

*A Summary of Changes section appears at the end of this standard

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

1
 D664 − 18´2
E177 Practice for Use of the Terms Precision and Bias in ness of oil or biodiesel and blends under service conditions. No
ASTM Test Methods general correlation is known between acid number and the
corrosive tendency of biodiesel and blends or oils toward
3. Terminology metals.
3.1 Definitions:
3.1.1 acid number, n—the quantity of a specified base, 6. Apparatus
expressed in milligrams of potassium hydroxide per gram of 6.1 Manual Titration Apparatus:
sample, required to titrate a sample in a specified solvent to a 6.1.1 Meter, a voltmeter or a potentiometer that will operate
specified endpoint using a specified detection system. with an accuracy of 60.005 V and a sensitivity of 60.002 V
3.1.1.1 Discussion—This test method expresses the quantity over a range of at least 60.5 V when the meter is used with the
of base as milligrams of potassium hydroxide per gram of electrodes specified in 6.1.2 and 6.1.3 and when the resistance
sample, that is required to titrate a sample in a mixture of between the electrodes falls within the range from 0.2 MΩ to
toluene and propan-2-ol to which a small amount of water has 20 MΩ. The meter shall be protected from stray electrostatic
been added from its initial meter reading in millivolts to a fields so that no permanent change in the meter readings over
meter reading in millivolts corresponding to an aqueous basic the entire operating range is produced by touching, with a
buffer solution or a well-defined inflection point as specified in grounded lead, any part of the exposed surface of the glass
the test method. electrode, the glass electrode lead, the titration stand, or the
3.1.1.2 Discussion—This test method provides additional meter.
information. The quantity of base, expressed as milligrams of
potassium hydroxide per gram of sample, required to titrate a NOTE 4—A suitable apparatus could consist of a continuous-reading
electronic voltmeter designed to operate on an input of less than 5 × 10−12
sample in the solvent from its initial meter reading in millivolts A, when an electrode system having 1000 MΩ resistance is connected
to a meter reading in millivolts corresponding to a freshly across the meter terminals and provided with a metal shield connected to
prepared aqueous acidic buffer solution or a well-defined the ground, as well as a satisfactory terminal to connect the shielded
inflection point as specified in the test method shall be reported connection wire from the glass electrode to the meter without interference
as the strong acid number. from any external electrostatic field.
3.1.1.3 Discussion—The causes and effects of the so-called 6.1.2 Sensing Electrode, standard pH, suitable for nonaque-
strong acids and the causes and effects of the other acids can be ous titrations.
very significantly different. Therefore, the user of this test 6.1.3 Reference Electrode, silver/silver chloride (Ag/AgCl)
method shall differentiate and report the two, when they are reference electrode, filled with 1M to 3M LiCl in ethanol.
found. 6.1.3.1 Combination Electrodes—Sensing electrodes may
have the Ag/AgCl reference electrode built into the same
4. Summary of Test Method electrode body, which offers the convenience of working with
4.1 The sample is dissolved in a titration solvent and titrated and maintaining only one electrode. The combination electrode
potentiometrically with alcoholic potassium hydroxide using a shall have a sleeve junction on the reference compartment and
glass indicating electrode and a reference electrode or a shall use an inert ethanol electrolyte, for example, 1M–3M
combination electrode. The meter readings are plotted manu- LiCl in ethanol. These combination electrodes shall have the
ally or automatically against the respective volumes of titrating same response or better response than a dual electrode system.
solution and the end points are taken only at well-defined They shall have removable sleeves for easy rinsing and
inflections in the resulting curve. When no definite inflections addition of electrolyte.
are obtained and for used oils, end points are taken at meter NOTE 5—A third electrode, such as a platinum electrode, may be used
readings corresponding to those found for aqueous acidic and to increase the electrode stability in certain systems.
basic buffer solutions.
6.1.4 Variable-Speed Mechanical Stirrer, a suitable type,
5. Significance and Use equipped with a propeller-type stirring paddle. The rate of
stirring shall be sufficient to produce vigorous agitation without
5.1 New and used petroleum products, biodiesel, and blends spattering and without stirring air into the solution. A propeller
of biodiesel may contain acidic constituents that are present as with blades 6 mm in radius and set at a pitch of 30° to 45° is
additives or as degradation products formed during service, satisfactory. A magnetic stirrer is also satisfactory.
such as oxidation products. The relative amount of these 6.1.4.1 If an electrical stirring apparatus is used, it shall be
materials can be determined by titrating with bases. The acid electrically correct and grounded so that connecting or discon-
number is a measure of this amount of acidic substance in the necting the power to the motor will not produce a permanent
oil, always under the conditions of the test. The acid number is change in the meter reading during the course of the titration.
used as a guide in the quality control of lubricating oil 6.1.5 Burette, 10 mL capacity, graduated in 0.05 mL divi-
formulations. It is also sometimes used as a measure of sions and calibrated with an accuracy of 60.02 mL. The
lubricant degradation in service. Any condemning limits must burette shall have a tip that extends 100 mm to 130 mm beyond
be empirically established. the stopcock and shall be able to deliver titrant directly into the
5.2 Since a variety of oxidation products contribute to the titration vessel without exposure to the surrounding air or
acid number and the organic acids vary widely in corrosion vapors. The burette for KOH shall have a guard tube containing
properties, the test method cannot be used to predict corrosive- soda lime or other CO2-absorbing substance.

2
 D664 − 18´2
6.1.6 Titration Beaker, 250 mL, 125 mL, or suitable 7.7 Potassium Hydroxide. (Warning—Causes severe
capacity, made of borosilicate glass or other suitable material. burns.)
6.1.7 Titration Stand, suitable for supporting the electrodes,
7.8 Propan-2-ol, Anhydrous, (less than 0.1 % H2O).
stirrer, and burette.
(Warning—Flammable.) If adequately dry reagent cannot be
NOTE 6—An arrangement that allows the removal of the beaker without procured, it can be dried by distillation through a multiple plate
disturbing the electrodes and stirrer is desirable. column, discarding the first 5 % of material distilling overhead
6.2 Automatic Titration Apparatus: and using the 95 % remaining. Drying can also be accom-
6.2.1 Automatic titration systems shall be able to carry out plished using molecular sieves such as Linde Type 4A, by
the necessary analyses as prescribed in the method. As a passing the solvent upward through a molecular sieve column
minimum, the automatic titration system shall meet the perfor- using one part of molecular sieve per ten parts of solvent.
mance and specification requirements listed in 6.1 as war- NOTE 7—It has been reported that, if not originally inhibited against it,
ranted. propan-2-ol can contain peroxides. When this occurs, an explosion is
possible when the storage of the vessel or other equipment such as a
6.2.2 A dynamic mode of titrant addition shall be used. dispensing bottle, is near empty and approaching dryness.
During the titration, the speed and volume of the addition shall
vary depending on the rate of change of the system. The 7.9 Commercial Aqueous pH 4, pH 7, and pH 10 Buffer
recommended maximum volume increment is 0.5 mL and the Solutions—These solutions shall be replaced at regular inter-
recommended minimum volume increment is 0.05 mL. vals consistent with their stability or when contamination is
6.2.3 Graduated Cylinder—50 mL, or dispensing device suspected. Information relating to their stability should be
capable of delivering 50 mL 6 0.5 mL. obtained from the manufacturer.
6.2.4 Pipette—2.0 mL, Class A.
6.2.5 Titration Beaker—250 mL, 125 mL, or suitable 8. Electrode System
capacity, made of borosilicate glass or other suitable material. 8.1 Preparation of Electrodes—When a Ag/AgCl reference
electrode is used for the titration and it contains an electrolyte
7. Reagents which is not 1M–3M LiCl in ethanol, replace the electrolyte.
7.1 Purity of Reagents—Reagent-grade chemicals shall be Drain the electrolyte from the electrode, wash away all the salt
used in all tests. Unless otherwise indicated, it is intended that (if present) with water and then rinse with ethanol. Rinse
all reagents shall conform to the specifications of the commit- several times with the LiCl electrolyte solution. Finally, replace
tee on Analytical Reagents of the American Chemical Society, the sleeve and fill the electrode with the LiCl electrolyte to the
where such specifications are available.3 Other grades may be filling hole. When refitting the sleeve, ensure that there will be
used, provided it is first ascertained that the reagent is of a free flow of electrolyte into the system. A combination
sufficiently high purity to permit its use without lessening the electrode shall be prepared in the same manner. The electrolyte
accuracy of the determination. in a combination electrode can be removed with the aid of a
7.1.1 Commercially available solutions may be used in vacuum suction.
place of laboratory preparations, provided the solutions have 8.2 Testing of Electrodes—Test the meter-electrode combi-
been certified as being equivalent. nation when first put into use, or when new electrodes are
7.1.2 Alternate volumes of the solutions may be prepared, installed, and retest at intervals thereafter. Rinse the electrodes
provided the final solution concentration is equivalent. with solvent then with water, and dip them into a pH 4 aqueous
7.2 Purity of Water—Unless otherwise indicated, reference buffer solution. Read the mV value after stirring 1 min.
to water shall be understood to mean reagent water that meets Remove the electrodes and rinse with water. Dip the electrodes
the requirements of either Type I, II, or III of Specification into a pH 7 aqueous buffer. Read the mV value after stirring
D1193. 1 min. Calculate the mV difference. A good electrode system
7.3 Primary Standard—Where specified, these samples, or will have a difference of at least 162 mV (20 °C to 25 °C). If
samples of commercially available primary standards, are to be the difference is less than 162 mV, lift the sleeve of the
used in standardizing the volumetric solutions. electrode and ensure electrolyte flow. Repeat the measure-
ments. If the difference is still less than 162 mV, clean or
7.4 Ethanol. (Warning—Flammable and toxic, especially replace the electrode(s).
when denatured.)
8.2.1 When the sensing electrode and the reference elec-
7.5 Lithium Chloride, LiCl. trode are separate, one pair of electrodes shall be considered as
7.6 Lithium Chloride Electrolyte, Prepare a 1M–3M solu- one unit. If one or the other is changed, it shall be considered
tion of lithium chloride (LiCl) in ethanol. as different pair and shall be retested.
8.3 Maintenance and Storage of Electrodes—Cleaning the
electrodes thoroughly, keeping the ground-glass joint free of
3
Reagent Chemicals, American Chemical Society Specifications, American foreign materials, and regular testing of the electrodes are very
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not important in obtaining repeatable potentials, since contamina-
listed by the American Chemical Society, see Annual Standards for Laboratory
tion may introduce uncertain erratic and unnoticeable liquid
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, contact potentials. While this is of secondary importance when
MD. end points are chosen from inflection points in the titration

3
 D664 − 18´2
curve, it may be quite serious when end points are chosen at 10.1.2 Agitate used oil samples thoroughly to ensure that
arbitrarily fixed cell potentials. any sediment present is homogeneously suspended before
analysis as the sediment can be acidic or basic or have
NOTE 8—See Appendix X1 for a possible procedure to check the
electrode performance. adsorbed acidic or basic material from the sample. When
necessary, samples are warmed to aid mixing.
8.3.1 Clean the glass electrode at frequent intervals based on
use and type of samples being analyzed (not less than once NOTE 10—As used oil can change appreciably in storage, samples
every week during continual use) by immersing in non- should be tested as soon as possible after removal from the lubricating
system and the dates of sampling and testing, if known, should be noted.
chromium containing, strongly oxidizing cleaning solution.
The reference electrode shall be cleaned periodically when in Test Method A
use or when a new electrode is installed. Drain the reference
electrode at least once each week and refill with the fresh LiCl 11. Reagents
electrolyte as far as the filling hole. Ensure that there are no air 11.1 See Section 7.
bubbles in the electrode liquid. If air bubbles are observed,
11.2 Hydrochloric Acid (HCl)—Relative density 1.19.
hold the electrode in a vertical position and gently tap it to
(Warning—Corrosive, causes burns.)
release the bubbles. Maintain the electrolyte level in the
reference electrode above that of the liquid in the titration 11.3 Toluene. (Warning—Flammable.)
beaker or vessel at all times. 11.4 Hydrochloric Acid Solution, Standard Alcoholic, (0.1
8.3.2 Prior to each titration, soak the prepared electrodes in mol/L). (Warning—See 11.2 and 7.8.) Mix 9 mL of hydro-
water (pH 4.5 to 5.5) for at least 5 min. Rinse the electrodes chloric (HCl, relative density 1.19) acid with 1 L of anhydrous
with propan-2-ol immediately before use, and then with the propan-2-ol. Standardize frequently enough to detect concen-
titration solvent. tration changes of 0.0005 by potentiometric titration of ap-
8.3.3 When not in use, immerse the lower half of the proximately 8 mL (accurately measured) of the 0.1-mol/L
reference electrode in LiCl electrolyte. When the glass elec- alcoholic KOH solution diluted with 125 mL of CO2-free
trode is used, store it in water that has been acidified with HCl water.
to a pH of 4.5 to 5.5. Do not allow electrodes to remain
immersed in titration solvent for any appreciable period of time 11.5 Potassium Hydroxide Solution, Standard Alcoholic,
between titrations. While the electrodes are not extremely (0.1 mol//L). (Warning—See 7.7 and 7.8.) Add 6 g of
fragile, handle them carefully at all times. potassium hydroxide (KOH) to approximately 1 L of propan-
8.3.3.1 Electrode Life—Typically, electrode usage is limited 2-ol. Boil gently for 10 min to effect solution. Allow the
to 3 to 6 months, depending upon usage. Electrodes have a solution to stand for two days and then filter the supernatant
limited shelf life and shall be tested before use (see 8.2). liquid through a fine sintered-glass funnel. Store the solution in
a chemically resistant bottle. Dispense in a manner such that
9. Standardization of Apparatus the solution is protected from atmospheric carbon dioxide
(CO2) by means of a guard tube containing soda lime or soda
9.1 Determination of Meter Readings for the Aqueous
non-fibrous silicate absorbents and such that it does not come
Buffer Solutions—To ensure comparable selection of end points
into contact with cork, rubber, or saponifiable stopcock grease.
when definite inflection points are not obtained in the titration
Standardize frequently enough to detect concentration changes
curve, determine daily, for each electrode pair, the meter
of 0.0005 by potentiometric titration of weighed quantities of
readings obtained with aqueous acidic and basic buffer solu-
potassium acid phthalate dissolved in CO2-free water.
tions.
11.6 Titration Solvent—Add 5 mL 6 0.2 mL of water to
NOTE 9—The response of different glass electrodes to hydrogen ion
activity is not the same. Therefore, it is necessary to establish regularly for
495 mL 6 5 mL of anhydrous propan-2-ol and mix well. Add
each electrode system the meter readings corresponding to the buffer 500 mL 6 5 mL of toluene. (Warning—Flammable.) The
solutions arbitrarily selected to represent acidic or basic end points. titration solvent should be made up in large quantities, and its
9.2 Immerse the electrodes in the pH 4 and the pH 10 blank value determined daily by titration prior to use.
aqueous buffers and stir each of them for approximately 5 min, 11.7 Chloroform. (Warning—Flammable. Hazardous mate-
maintaining the temperature of the buffer solution at a tem- rial.)
perature within 2 °C of that at which the titrations are to be
made. Read the cell voltage for each of them. The readings so 12. Procedure for Acid Number and Strong Acid
obtained are taken as the end points in titration curves having Number
no inflection points. 12.1 Into a 250 mL beaker or a suitable titration vessel,
introduce a weighed quantity of sample as recommended in
10. Preparation of Sample Table 1(a) (see Note 11) and add 125 mL of titration solvent
10.1 When applicable, refer to Practice D4057 (manual (see Note 12). Alternatively, into a 125 mL beaker or a suitable
sampling) or Practice D4177 (automatic sampling) for proper titration vessel, introduce a weighed quantity of sample as
sampling techniques. recommended in Table 1(b) and add 60 mL of titration solvent.
10.1.1 When sampling used lubricants, the specimen shall Prepare the electrodes as directed in 8.1. Place the beaker or
be representative of the system sampled and shall be free of titration vessel on the titration stand and adjust its position so
contamination from external sources. that the electrodes are about half immersed. Start the stirrer,

4
 D664 − 18´2
TABLE 1 Recommended Size of Test Portion
(a) 125 mL Solvent (b) 60 mL Solvent
Mass of Test Portion, Accuracy of Weighing, Mass of Test Portion, Accuracy of Weighing,
Acid Number Acid Number
g g g g
0.05 to <1.0 20.0 ± 2.0 0.10 0.05 to <1.0 10.0 ± 1.0 0.10
1.0 to <5.0 5.0 ± 0.5 0.02 1.0 to <5.0 2.5 ± 0.25 0.02
5 to <20 1.0 ± 0.1 0.005 5 to <20 0.5 ± 0.05 0.005
20 to <100 0.25 ± 0.02 0.001 20 to <100 0.25 ± 0.02 0.001
100 to <260 0.1 ± 0.01 0.0005 100 to <260 0.1 ± 0.01 0.0005

and stir throughout the determination at a rate sufficient to presence of such acids. Record the volume of KOH added to
produce vigorous agitation without spattering and without reach the mV of the pH 4 aqueous buffer. This value is used to
stirring air into the solution. calculate the strong acid number. Proceed with the automatic
NOTE 11—If it suspected that the recommended sample size will foul titration and record potentiometric curves or derivative curves
the electrodes, a smaller sample size can be taken. Results using smaller as the case may be.
sample size may not be equivalent to results obtained with the recom-
mended sample size. The precision statement does not include results 12.4.3 Titrate with the 0.1 mol ⁄L alcoholic KOH solution.
when using a smaller sample size. The apparatus shall be adjusted or programmed such that,
NOTE 12—A titration solvent that contains chloroform (Warning— when an inflection point, suitable for use in the calculation is
May be fatal if swallowed. Harmful if inhaled. May produce toxic vapors approached, the rate of addition of titrant and volume of titrant
if burned) can be used in place of toluene to completely dissolve certain added are based on the change in slope of the titration curve.
heavy residues of asphaltic materials. Results using chloroform may not
be equivalent to results obtained using toluene. The precision statement The titrant shall be added in increments of a suitable size to
does not include results when using chloroform. achieve a potential difference of 5 mV to 15 mV per increment.
12.2 Select the right burette, fill with the 0.1 mol ⁄L alco- Increment volume shall vary between 0.05 mL and 0.5 mL.
holic KOH solution, and place the burette in position on the The next increment shall be added if the signal does not change
titration assembly, ensuring that the tip is immersed about more than 10 mV in 10 s. The maximum waiting time in
25 mm in titration vessel liquid. Record the initial burette and between increments shall not exceed 60 s.
meter (cell potential) readings. 12.4.4 The titration can be terminated when the signal
reaches the pH 10 buffer potential past 200 mV. An equiva-
12.3 Manual Titration Method: lence point is recognizable if the first derivative of the titration
12.3.1 Add suitable small portions of 0.1 mol ⁄L alcoholic curve produces a maximum, which is significantly higher than
KOH solution and wait until a constant potential has been the noise produced by electrostatic effects. See also 13.1.1.
established, record the burette and meter readings. 12.4.5 The goal of cleaning is to rinse the residue from the
12.3.2 At the start of the titration and in any subsequent previous sample and to rehydrate the electrode. On completion
regions (inflections) where 0.1 mL of the 0.1 mol ⁄L KOH of the titration, rinse the electrodes and burette tip with titration
solution consistently produces a total change of more than solvent. If clean, then rinse with 2-propanol and then with
30 mV in the cell potential, add 0.05 mL portions. water. Immerse the electrodes in pH 4.5–5.5 water for at least
12.3.3 In the intermediate regions (plateau) where 0.1 mL of 3 min to 5 min to rehydrate the aqueous gel layer of the glass
0.1 mol ⁄L alcoholic KOH changes the cell potential less than electrode. Rinse with 2-propanol prior to beginning the next
30 mV, add larger portions sufficient to produce a total poten- sample to remove the water. If sample residue remains after the
tial change approximately equal to, but not greater than 30 mV. rinse with titration solvent, another solvent such as toluene,
12.3.4 Titrate in this manner until the potential changes less xylene, heptane, or chloroform may be used for rinse. The rinse
than 5 mV ⁄0.1 mL of KOH and the cell potential indicates that may be more effective if a beaker of solvent is used with strong
the solution is more basic than the aqueous basic buffer. stirring. Using automated equipment, cleaning may be done by
12.3.5 Remove the titration solution, rinse the electrodes rinsing with titration solvent, soaking with stirring in a solvent
and burette tip with the titration solvent, then with propan-2-ol such as toluene, xylene, heptane, or chloroform for 45 s,
and finally with reagent grade water. Immerse the electrodes in soaking briefly in 2-propanol to removed the solvent, then
water for at least 5 min before starting another titration to soaking in pH 4.5–5.5 water 3 min to 5 min to rehydrate. Dip
restore the aqueous gel layer of the glass electrode. After 5 min in 2-propanol briefly to remove water before beginning the
in the water, rinse the electrodes with propan-2-ol then the next sample. The same solvent cleaning beaker, 2-propanol
titration solvent before proceeding to the next titration. If the beaker and water beaker may be used for a short series of
electrodes are found to be dirty and contaminated, proceed as samples. They should be changed at reasonable intervals,
in 8.1. Store electrodes according to 8.3.3. before contamination builds up. The user shall ensure that the
12.4 Automatic Titration Method: electrode is adequately cleaned and hydrated. If electrodes are
12.4.1 Adjust the apparatus in accordance with the manu- found dirty and contaminated, proceed as in 8.1. Store elec-
facturer’s instructions to provide a dynamic mode of titrant trodes according to 8.3.3.
addition.
NOTE 13—When acid numbers about or below 0.1 are expected, better
12.4.2 Verify that the instrument will determine the amount precision can be obtained by modifying the method in one or more ways,
of strong acid when the initial mV of the test sample, relative such as by substituting a 0.01 M or 0.05 M alcoholic KOH solution;
to the mV reading of the aqueous acidic buffer, indicates the increasing the sample size above 20 g; or switching from a manual

5
 D664 − 18´2

Key:
Curve A—Blank on 125 mL of titration solvent.
Curve B—10.00 g of used crankcase oil plus 125 mL of titration solvent. Since no sharp inflections are apparent, the end points are chosen at the meter readings obtained
with the two aqueous buffer solutions.
Curve C—10.00 g of oil containing a weak acid plus 125 mL of titration solvent. The end point is chosen as the point at which the curve is most nearly vertical.
Curve D—10.00 g of oil containing weak and strong acids plus 125 mL of titration solvent. The end points are chosen as the points at which the curve is most nearly vertical.
FIG. 1 Illustrative Titration Curves

operated burette (that is, graduated in 0.05 mL divisions) to an automated 13. Calculation
burette that can dispense smaller increments of the KOH solution, if
samples are being analyzed by manual titration. 13.1 Manual Titration—Plot the volumes of the 0.1 mol ⁄L
alcoholic KOH solution added against the corresponding meter
12.5 Blanks: readings (see Fig. 1). Mark as an end point only a well-defined
12.5.1 For each set of samples and for every new batch of inflection point (see Note 14) that is closest to the cell voltage
titration solvent, perform a blank titration of 125 mL or 60 mL corresponding to that obtained with the aqueous acidic or basic
depending on the volume of the solvent that will be used for buffer. If inflections are ill defined or no inflection appears (see
sample analysis. For manual titration, add 0.1 mol ⁄L alcoholic Fig. 1, Curve B), mark the end point at the meter reading
KOH solution in 0.01 mL to 0.05 mL increments, waiting corresponding to that obtained with the appropriate aqueous
between each addition until a constant cell potential is reached. buffer.
Record the meter and readings when the former becomes NOTE 14—One inflection point is generally recognizable by inspection
constant after each increment. For automatic titration, use the whenever several successive 0.05 mL increments each produce a cell
same mode of titration as for the determination of the acidic potential change greater than 15 mV at least 30 % greater than those
produced by previous or subsequent increments of the same size.
property of the sample but use smaller increments of titrant Generally, definite inflection points may be discerned only in regions
addition, 0.01 mL to 0.05 mL. Recheck the blank periodically where increments of the same size are used.
based on the sample load. 13.1.1 Some additive chemistry may produce an inflection
12.5.2 When strong acids are present and a strong acid point beyond the buffer endpoint. For additives, take the last
number is to be determined, perform a blank titration of inflection point for calculation. If using an automatic titrator, a
125 mL or 60 mL depending on the volume of the titration change in the instrument parameters may be required to detect
solvent that will be used for sample analysis. Add 0.1 mol ⁄L this type of endpoint.
alcoholic HCl solution in 0.01 mL to 0.05 mL increments in a 13.1.2 For all acid titrations on used oils, mark as an end
manner comparable to that specified in 12.5.1. point the point on the curve that corresponds to the meter

6
 D664 − 18´2
reading for an aqueous basic buffer (pH 10) and the meter results of this investigation may, but not necessarily, result in
reading for the aqueous acid buffer (pH 4) when strong acids instrument recalibration.
are indicated. 14.4 The frequency of QC testing is dependent on the
NOTE 15—The cooperative work done on acid number determinations criticality of the quality being measured, the demonstrated
on fresh oils, additive concentrates, and used oils indicated well-defined stability of the testing process, and customer requirements.
inflection points for fresh oils and additive concentrates, and generally Generally, a QC sample should be analyzed each testing day.
ill-defined inflections, or no inflection points at all, for used oils.
The QC frequency should be increased if a large number of
13.2 Automatic Titration Method—Mark the end points on samples are routinely analyzed. However, when it is demon-
the curves obtained in 12.4, in the same way as for the manual strated that the testing is under statistical control, the QC
titration method. testing frequency may be reduced. The QC precision should be
13.3 Method of Calculation—The method of calculation in periodically checked against the precision listed in the Preci-
13.3.1 is applicable to both manual and automatic methods. sion and Bias section of this test method to ensure data quality.
13.3.1 Calculate the acid number and strong acid number as 14.5 It is recommended that, if possible, the type of QC
follows: sample that is regularly tested be representative of the samples
Acid number, mg KOH/g 5 ~ A 2 B ! 3 M 3 56.1/W (1) routinely analyzed. An ample supply of QC sample material
should be available for the intended period of use, and must be
Strong acid number, mg KOH/g 5 ~ CM1Dm! 3 56.1/W (2)
homogeneous and stable under the anticipated storage condi-
where: tions. Because the acid number can vary while the QC sample
A = volume of alcoholic KOH solution used to titrate is in storage, when an out-of-control situation arises, the
sample to end point that occurs at the meter reading of stability of the QC sample can be a source of the error.
the inflection point closest to the meter reading corre-
15. Report
sponding to the pH 10 aqueous buffer, or in case of
ill-defined or no inflection point, to the meter reading 15.1 Given there are two different ways to determine the
corresponding to the pH 10 aqueous buffer, mL. For endpoint, report the type of endpoint used: inflection point or
additives, A is the volume of alcoholic KOH at the last buffer endpoint. Report sample size used if it differs from the
inflection point, recommended sample size. Also, report if chloroform was used
B = volume corresponding to A for blank titration, mL, as solvent. Report the results as acid number or strong acid
M = concentration of alcoholic KOH solution, mol/L, number as follows:
m = concentration of alcoholic HCl solution, mol/L, Acid number ~ Test Method D664, Test Method A! 5 ~ result! (3)
W = sample, mass, g,
C = alcoholic KOH solution used to titrate the sample to Strong acid number ~ Test Method D664, Test Method A! 5 ~ result!
end point that occurs at a meter reading corresponding (4)
to the pH 4 aqueous buffer, mL, and 15.2 For used oil samples, report also the date of testing
D = alcoholic HCl solution used to titrate solvent blank to and, when available, the date the sample was taken.
end point corresponding to C, mL.
16. Precision and Bias56
14. Quality Control Checks 16.1 Acid Number:
14.1 Confirm the performance of the test procedure by 16.1.1 Repeatability Limit (r)—The difference between re-
analyzing a quality control (QC) sample that is, if possible, petitive results obtained by the same operator in a given
representative of the samples typically analyzed. laboratory applying the same test method with the same
NOTE 16—Because used oils, particularly used engine oils, are known apparatus under constant operating conditions on identical test
to change during storage, such samples may not be suitable for this material within short intervals of time would in the long run, in
purpose. the normal and correct operation of the test method, exceed the
14.2 Prior to monitoring the measurement process, the user following values only in one case in 20.
of the method needs to determine the average value and control 16.1.1.1 Repeatability can also be interpreted as maximum
limits of the QC sample.4 difference between two results, obtained under repeatability
14.3 Record the QC results and analyze by control charts or conditions, that is accepted as plausible due to random causes
other statistically equivalent technique to ascertain the statis- under normal and correct operation of the test method.
tical control status of the total testing process.4 Any out-of-
5
control data should trigger investigation for root cause(s). The Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1551. Contact ASTM Customer
Service at [email protected].
6
Supporting data have been filed at ASTM International Headquarters and may
4
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th be obtained by requesting Research Report RR:D02-1869. Contact ASTM Customer
edition, ASTM International, W. Conshohocken, PA. Service at [email protected].

7
 D664 − 18´2
TABLE 2 Precision for AN Using 60 mL and 125 mL of Solvent with Comparison Data
Volume of Solvent 60 mL 60 mL 125 mL 125 mL
r, Inflection r, Buffer EP (pH 10) r, Inflection r, Buffer EP (pH 10)
Calculation Formula 0.1938 · X0.8199 0.3456 · X0.9758 0.1275 · X1.0431 0.2028 · X1.0513
Precision @ 5 mg KOH/g 0.73 1.71 0.68 1.10
Precision @ 1 mg KOH/g 0.19 0.35 0.13 0.20

R, Inflection R, BEP (pH 10) R, Inflection R, BEP (pH 10)

Calculation Formula 0.4022 · X0.8199 0.5542 · X0.9758 0.2188 · X1.0431 0.3160 · X1.0513
Precision @ 5 mg KOH/g 1.50 2.67 1.17 1.72
Precision @ 1 mg KOH/g 0.40 0.55 0.22 0.32

Fresh and used oils 60 mL: two days and then filter the supernatant liquid through a fine
AN Inflection, mg KOH/g 2 Solvent 60 mL (5) sintered-glass funnel. Store the solution in a chemically resis-
tant bottle. Dispense in a manner such that the solution is
Repeatability 5 0.1938 · X 0.8199 protected from atmospheric carbon dioxide (CO2) by means of
AN Buffer EP ~pH 10!, mg KOH/g 2 Solvent 60 mL (6) a guard tube containing soda lime or soda non-fibrous silicate
absorbents and such that it does not come into contact with
Repeatability 5 0.3456 · X 0.9758 cork, rubber, or saponifiable stopcock grease. Standardize
frequently enough to detect concentration changes of
where:
0.0005 mol ⁄L by potentiometric titration of pipetted quantities
X = the average of the two test results. of potassium acid phthalate solution dissolved in CO2-free
16.1.2 Reproducibility (R)—The difference between two water.
single and independent results obtained by different operators 17.3 Potassium Acid Phthalate (KHC8H4O4), Primary
applying the same test method in different laboratories using Standard, Dried—Place 10 g to 20 g of primary standard
different apparatus on identical test material would, in the long potassium acid phthalate (KHC8H4O4) of 100-mesh fineness,
run, in the normal and correct operation of the test method, in a weighing bottle at 120 °C for 2 h. Stopper the container
exceed the following values only in one case in 20. and cool it in a dessicator.
16.1.2.1 Reproducibility can also be interpreted as maxi-
mum difference between two results, obtained under reproduc- 17.4 Potassium Acid Phthalate (KHP) Solution
ibility conditions, that is accepted as plausible due to random (0.01 mol ⁄L)—For a volumetric standard, weigh approxi-
causes under normal and correct operation of the test method. mately 1.0 g and record the weight to the nearest 60.0001 g of
Fresh and used oils 60 mL: dried potassium acid phthalate primary standard (KHC8H4O4)
and make up to the mark with DI Type II water in a 500 mL
AN Inflection, mg KOH/g 2 Solvent 60 mL (7) volumetric flask. Alternatively for a weight-based standard,
Reproducibility 5 0.4022 · X 0.8199 weigh the KHP and record the weight to the nearest 0.0001 g
and record the total amount of water and KHP to the nearest
AN Buffer EP ~pH 10!, mg KOH/g 2 Solvent 60 mL (8) 60.01 g and express the concentration as mg KHP/g of
Reproducibility 5 0.5542 · X 0.9758 solution. Mix thoroughly to dissolve the solution.

where: 18. Procedure

X = the average of the two test results. 18.1 Standardization of the Titrant 0.01 M Alcoholic KOH:
16.2 Strong Acid Number: 18.1.1 Weigh 2 g of KHP solution into a 125 mL or suitable
16.2.1 Precision data have not been developed for strong size beaker and record the weight to the nearest 0.0001 g if
acid number because of its rare occurrence in sample analysis. using weight-based standard, or pipette 2 mL of KHP solution
16.3 Bias—The procedures in this test method have no bias into a vessel and add approximately 50 mL of CO2 free water.
because the acid values can be defined only in terms of the test Titrate the solution to determine the titer of 0.01M KOH. This
method. volume of KHP solution will use approximately 2 mL of the
0.01 M KOH.
Test Method B 18.1.2 Prepare two additional KHP solutions to standardize
the titrant as in 18.1.
17. Reagents 18.1.3 Use the three determinations to calculate the average
17.1 See Section 7. concentration (mol/L) of the KOH. The average of the titrant
17.2 Potassium Hydroxide Solution, Standard Alcoholic mol/L determinations should agree 60.0005 M.
(0.01 mol//L)—(Warning—See 7.7 and 7.8.) Add 0.56 g of 18.2 Determination of the Solvent Blank—Adjust the appa-
potassium hydroxide (KOH) to approximately 1 L of propan- ratus in accordance with the manufacturer’s instructions to
2-ol or weigh 1.122 g 6 0.02 g of 50 % KOH into 1 L of provide a dynamic mode of titration. Addition of titrant volume
propan-2-ol. Boil gently for 10 min to effect solution. Allow increments should not be greater than 0.2 mL. Measure pre-
the solution to stand protected from carbon dioxide (CO2) for cisely 50 mL of propan-2-ol using a graduated cylinder, pipet

8
 D664 − 18´2
or automated dispensing device capable of dispensing 50 mL
6 0.5 mL into a 125 mL or suitable size beaker. Stir the
solution and titrate. Record the volume (mL) of KOH to
60.01 mL used to titrate to the inflection point.
18.3 Analysis of the Sample:
18.3.1 Adjust the apparatus in accordance with the manu-
facturer’s instructions to provide a dynamic mode of titrant
addition.
18.3.2 Weigh 5 g of biodiesel into a 125 mL or suitable size
beaker on an analytical balance and record the weight to the
nearest 0.0001 g. Measure 50 mL 6 0.50 mL of IPA using a
pipet or automated dispensing device into a suitable beaker.
Prepare the electrodes as directed in 8.1. Place the beaker or
titration vessel on the titration stand and adjust its position so
that the electrodes are about half immersed. Start the stirrer,
and stir throughout the determination at a rate sufficient to
produce vigorous agitation without spattering and without
stirring air into the solution.
NOTE 17—It is important that the same volume of titration solvent
60.5 mL is used for the blank and samples or inconsistent results can
occur.
18.3.3 Select the right burette, fill with 0.01 mol ⁄L alcoholic
KOH solution, and place the burette in position on the titration
assembly, ensuring that the tip is immersed about 25 mm in
titration vessel liquid and titrate.
18.3.4 On completion of the titration, rinse the electrodes
and burette tip with propan-2-ol, followed by water. Immerse
the electrodes in water for at least 2 min before starting another
titration to restore the aqueous gel layer of the glass electrode. FIG. 2 Illustrative Titration Curve of Biodiesel Sample
Rinse the electrodes with propan-2-ol prior to running the next
sample. If electrodes are found dirty and contaminated, pro-
mg
ceed as in 8.1. Store electrodes according to 8.3.3. KHP solution concentration, (11)
g
18.3.5 Multiple titration inflection points are often found
during the analysis associated with organic acids which form ~ weight of KHP, g ! *1000
over time due to the oxidation of biodiesel over prolonged 5
204.23* ~ total weight of KHP solution, g !
storage periods. The volume of titrant for the last well-defined
mol
endpoint should be used to calculate the total acidity. KOH molarity, (12)
L
19. Calculation or Interpretation of Results
19.1 Calculation of KOH Solution Molarity, mol/L:
19.1.1 Calculation of KOH Molarity, mol/L by Volume of
mol/L of KHP Solution: 5
S mg
~ weight of KHP solution, g ! concentration of KHP solution, g D
volume of KOH, mL
mol NOTE 18—The average mol/L of three determinations should be used
KHP solution concentration, (9)
L for the determination of the acid number. The average should agree within
60.0005 M.
~ weight of KHP, g ! 19.2 Calculation of the Acid Number:
5
204.23* ~ total volume of KHP solution, L !
Acid number, mg KOH/g 5 ~ A 2 B ! 3 M 3 56.1/W (13)
mol
KOH molarity, (10) where:
L
A = Volume of alcoholic KOH solution used to titrate

5
S
~ 2.00 mL KHP solution! concentration of KHP solution, L
mol
D B
sample to last inflection end point, mL,
= volume corresponding to A for blank titration, mL,
volume of KOH, mL M = concentration of alcoholic KOH solution, mol/L, and
19.1.2 Calculation of KOH mol/L by Weight of mg/g of KHP W = sample, mass, g.
Solution:

9
 D664 − 18´2
20. Quality Control Checks TABLE 3 Acid Number of BiodieselA
Repeatability = 0.264E-01 · X0.4 mg/kg KOH
20.1 Confirm the performance of the test procedure by Reproducibility = 0.177 ·X0.4 mg/kg KOH
analyzing a quality control (QC) sample that is, representative A
The degree of freedom for R is less than 30 but greater than 15. Samples 4, 5,
of the samples typically analyzed, if possible. 6, 9 were excluded as these samples were below the Limit of Quantitation of the
test method.
NOTE 19—Because biodiesel is known to change during long-term
storage, such samples may not be suitable for this purpose. The analyst
may use the Potassium Acid Phthalate solution 0.01M as an acceptable
QC standard. When used as a QC standard, the KHP solution will provide
a good indicator when restandardization of the titrant (0.01M KOH in laboratories participated in this study, however the results from
IPA) is necessary. No data is available on the shelf life of the KHP one laboratory were excluded from the precision calculations
solution. Commercially prepared standard solutions may also be used.
due to a fairly consistent bias in their reported values. Each of
20.2 Prior to monitoring the measurement process, the user the laboratories was asked to report replicate test results for
of the method needs to determine the average value and control eleven different diesel and biodiesel blends and a blank. Every
limits of the QC sample.4 “test result” reported represents a single determination or
20.3 Record the QC results and analyze by control charts or measurement. D2PP was used for the analysis of the study
other statistically equivalent technique to ascertain the statis- data; the details are given in ASTM Research Report RR:D02-
tical control status of the total testing process.4 Any out-of- 1727.
control data should trigger investigation for root cause(s). The 22.1.1 Repeatability Limit (r)—Two test results obtained
results of this investigation may, but not necessarily, result in within one laboratory shall be judged not equivalent if they
instrument recalibration. differ by more than the “r” value for that material; “r” is the
20.4 The frequency of QC testing is dependent on the interval representing the critical difference between two test
criticality of the quality being measured, the demonstrated results for the same material, obtained by the same operator
stability of the testing process, and customer requirements. using the same equipment on the same day in the same
Generally, a QC sample should be analyzed each testing day. laboratory. Repeatability limits are listed in Table 3.
The QC frequency should be increased if a large number of 22.1.2 Reproducibility Limit (R)—Two test results shall be
samples are routinely analyzed. However, when it is demon- judged not equivalent if they differ by more than the “R” value
strated that the testing is under statistical control, the QC for that material; “R” is the interval representing the critical
testing frequency may be reduced. The QC precision should be difference between two test results for the same material,
periodically checked against the precision listed in the Preci- obtained by different operators using different equipment in
sion and Bias Section of this test method to ensure data quality. different laboratories. Reproducibility limits are listed in Table
3.
20.5 It is recommended that a QC standard be routinely 22.1.3 The above terms (repeatability limit and reproduc-
analyzed at a concentration level in the same range as the ibility limit) are used as specified in Practice E177.
samples analyzed. An ample supply of QC sample material 22.1.4 Any judgment in accordance with statements 22.1.1
should be available for the intended period of use, and must be and 22.1.2 would have an approximate 95 % probability of
homogeneous and stable under the anticipated storage condi- being correct.
tions.
22.2 The precision statement was determined through sta-
21. Report tistical examination of 138 results, from six laboratories, on a
21.1 Report acid number of biodiesel and blends to the 0.01 total of eleven different petroleum blends and a blank.
as mg KOH/g of sample (Test Method D664, Test Method B). 22.3 Bias—At the time of the study, there was no accepted
22. Precision and Bias 7 reference material suitable for determining the bias for this test
method, therefore no statement on bias is being made.
22.1 The precision of this test method is based on an
interlaboratory study of D664 conducted in 2009. Seven 23. Keywords
7
23.1 acid number; B5; B10; B20; B100; biodiesel; biodiesel
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1727. Contact ASTM Customer blend; lubricants; petroleum products; potentiometric; strong
Service at [email protected]. acid number; titration

10
 D664 − 18´2
APPENDIX

(Nonmandatory Information)

X1. CHECK FOR ELECTRODE PERFORMANCE

X1.1 The kinetic electrode test measures the kinetic re- X1.3.3 Remove the electrodes from the water, and place
sponse of the electrode. Electrodes can calibrate with accept- them in the pH 4 buffer. Start a stopwatch at about the moment
able slope and intercept values yet still not have a response when the buffer touches the electrode.
good enough for titration. The speed of response and subse-
quent stability is important for a titration electrode. A manual X1.3.4 After 30 s, note the potential. After an additional
check is described in this Appendix that can be carried out with 30 s, note the potential again. The difference between the two
a pH meter or titrator set to read millivolts continuously. potentials is termed the drift.
X1.3.5 Repeat the procedure for pH 7 buffer and pH 10
X1.2 The essence of this check is to challenge the electrode
buffer.
coming from rest in a water solution with buffers and measure
the potential after 30 s and 60 s. A fast electrode reaches a X1.4 Calculate the drift for each of the three buffers. The
stable point in less than 30 s and changes little from 30 s to electrode response may be judged as follows:
60 s. Use buffers pH 4, pH 7, and pH 10 for this check, as
drift < 1 excellent
needed. 1 < drift < 2 good
2 < drift < 3 acceptable
X1.3 Procedure 3 < drift < 4 questionable
4 < drift unacceptable
X1.3.1 Set the titrator or pH meter to read millivolts
continuously. Have provision for stirring the buffer solution at X1.5 The difference between the 60 s potentials for pH 4
the same speed used for the titrations. buffer and pH 7 buffer should be greater than 162 mV, or 54
X1.3.2 Allow the electrode to stabilize for 1 min in distilled mV/pH number. Electrodes with a slope less than 54 mV/pH
or equivalent deionized water. number are not reliable for titration.

SUMMARY OF CHANGES

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D664 – 17) that may impact the use of this standard. (Approved Nov. 1, 2018.)

(1) Changed pH 11 to pH 10 in selected locations throughout. (2) Revised Table 2.

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D664 – 17) that may impact the use of this standard. (Approved Dec. 15, 2017.)

(1) Section 10 was revised.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

11