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: D4739 − 23

Standard Test Method for

Base Number Determination by Potentiometric Hydrochloric
Acid Titration1
This standard is issued under the fixed designation D4739; 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.

INTRODUCTION

Currently, there are two ASTM test methods under the jurisdiction of Committee D02 used for
determining base number by potentiometric titration: Test Method D2896 and Test Method D4739.
They are both used throughout the petroleum industry. Test Method D2896 is for new oils and is used
in setting specifications since it is more accurate than Test Method D4739. Test Method D4739 shall
be used exclusively for the purpose of tracking base number loss as an oil proceeds in service. In many
cases, the test methods will provide different results. Some comparisons are given in the Scope and
the Significance and Use sections of this test method to distinguish between the two standards and to
provide guidance to users.

1. Scope* values obtained by this test method only; base numbers

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1.1 This test method covers a procedure for the determina-
tion of basic constituents in petroleum products and new and
obtained by this test method are not intended to be equal to
values by other test methods. Although the analysis is made
under closely specified conditions, this test method is not
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used lubricants. This test method resolves these constituents
into groups having weak-base and strong-base ionization
properties, provided the dissociation constants of the more
intended to, and does not, result in reported basic properties
that can be used under all service conditions to predict

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strongly basic compounds are at least 1000 times than that of
the next weaker groups. This test method covers base numbers
performance of an oil; for example, no overall relationship is
known between bearing corrosion or the control of corrosive
up to 250. wear in the engine and base number.
1.2 In new and used lubricants, the constituents ASTM that can D4739-23
be 1.4 This test method was developed as an alternative for the
former base number portion of Test Method D664 (last
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considered to have basic properties are primarily organic and
published in Test Method D664 – 81).
inorganic bases, including amino compounds. This test method
uses hydrochloric acid as the titrant, whereas Test Method 1.4.1 Colorimetric test methods for base number are Test
D2896 uses perchloric acid as the titrant. This test method may Method D974, IP 139, and 5102.1 on acid and base number by
or may not titrate these weak bases and, if so, it will titrate extraction (color-indicator titration) of Federal Test Method
them to a lesser degree of completion; some additives such as Standard No. 791b. Test results by these methods may or may
inhibitors or detergents may show basic characteristics. not be numerically equivalent to this test method.
1.3 When testing used engine lubricants, it should be 1.5 The values stated in SI units are to be regarded as
recognized that certain weak bases are the result of the service standard. No other units of measurement are included in this
rather than having been built into the oil. This test method can standard.
be used to indicate relative changes that occur in oil during use 1.6 This standard does not purport to address all of the
under oxidizing or other service conditions regardless of the safety concerns, if any, associated with its use. It is the
color or other properties of the resulting oil. The values responsibility of the user of this standard to establish appro-
obtained, however, are intended to be compared with the other priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
1
This test method is under the jurisdiction of ASTM Committee D02 on dance with internationally recognized principles on standard-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of ization established in the Decision on Principles for the
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
Development of International Standards, Guides and Recom-
Current edition approved July 1, 2023. Published August 2023. Originally
approved in 1987. Last previous edition approved in 2017 as D4739 – 17. DOI: mendations issued by the World Trade Organization Technical
10.1520/D4739-23. Barriers to Trade (TBT) Committee.

*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

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 D4739 − 23
2. Referenced Documents titration curve according to the criteria given in Section 12 and
2.1 ASTM Standards: 2 used to calculate a base number.
D664 Test Method for Acid Number of Petroleum Products 5. Significance and Use
by Potentiometric Titration
D974 Test Method for Acid and Base Number by Color- 5.1 New and used petroleum products can contain basic
Indicator Titration constituents that are present as additives. The relative amount
D1193 Specification for Reagent Water of these materials can be determined by titration with acids.
D2896 Test Method for Base Number of Petroleum Products The base number is a measure of the amount of basic
by Potentiometric Perchloric Acid Titration substances in the oil always under the conditions of the test. It
D4057 Practice for Manual Sampling of Petroleum and is sometimes used as a measure of lubricant degradation in
Petroleum Products service. However, any condemning limit shall be empirically
D4175 Terminology Relating to Petroleum Products, Liquid established.
Fuels, and Lubricants 5.2 As stated in 1.2, this test method uses a weaker acid to
D4177 Practice for Automatic Sampling of Petroleum and titrate the base than Test Method D2896, and the titration
Petroleum Products solvents are also different. Test Method D2896 uses a stronger
2.2 IP Standard:3 acid and a more polar solvent system than Test Method D4739.
IP 139 Petroleum products and lubricants—Determination As a result, Test Method D2896 will titrate salts of weak acids
of acid and base number—Colour-indicator titration (soaps), basic salts of polyacidic bases, and weak alkaline salts
method of some metals. They do not protect the oil from acidic
2.3 U.S. Federal Test Method:4 components due to the degradation of the oil. This test method
Federal Test Method Standard No. 791b Lubricants Liquid may produce a falsely exaggerated base number. Test Method
Fuels and Related Products; Methods of Testing D4739 will probably not titrate these weak bases but, if so, will
titrate them to a lesser degree of completion. It measures only
3. Terminology the basic components of the additive package that neutralizes

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3.1 Definitions: acids. On the other hand, if the additive package contains weak
3.1.1 For definitions of terms used in this test method, refer basic components that do not play a role in neutralizing the
to Terminology D4175. acidic components of the degrading oil, then the Test Method
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3.2 Definitions of Terms Specific to This Standard:
3.2.1 base number, n—the quantity of a specified acid,
D4739 result may be falsely understated.
5.3 Particular care is required in the interpretation of the
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expressed in terms of the equivalent number of milligrams of
potassium hydroxide per gram of sample, required to titrate a
base number of new and used lubricants.
5.3.1 When the base number of the new oil is required as an
sample in a specified solvent to a specified endpoint using a expression of its manufactured quality, Test Method D2896 is
specified detection system. preferred, since it is known to titrate weak bases that this test
3.2.1.1 Discussion—In this test method, the ASTM sample D4739-23
is method may or may not titrate reliably.
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titrated to a meter reading corresponding to aqueous acidic 5.3.2 When the base number of in-service or at-term oil is
buffer solution or appropriate inflection point. required, this test method is preferred because in many cases,
3.2.2 strong base number, n—the quantity of acid, expressed especially for internal combustion engine oils, weakly basic
in terms of the equivalent number of milligrams of potassium degradation products are possible. Test Method D2896 will
hydroxide per gram of sample, that is required to titrate a titrate these, thus giving a false value of essential basicity. This
sample dissolved in the specified solvent from the initial meter test method may or may not titrate these weak acids.
reading to a meter reading corresponding to a basic buffer 5.3.3 When the loss of base number value, as the oils
solution. proceed in service, is the consideration, this test method is to be
preferred and all values including the unused oil shall be
4. Summary of Test Method determined by this test method. Base numbers obtained by this
4.1 The sample is dissolved in a mixture of toluene, test method shall not be related to base numbers obtained by
propan-2-ol (isopropyl alcohol), chloroform, and a small another test method such as Test Method D2896.
amount of water and titrated potentiometrically with alcoholic 5.3.4 In ASTM Interlaboratory Crosscheck Programs for
hydrochloric acid solution. The test results of this procedure both new and used lubricants, historically Test Method D2896
are obtained by titration mode of fixed increment and fixed gives a higher value for base number.
time additions of the titrant. An endpoint is selected from a
6. Apparatus
2
6.1 Potentiometric Titration, automatic or manual, with
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM capability of adding fixed increments of titrant at fixed time
Standards volume information, refer to the standard’s Document Summary page on intervals (see Annex A1).
the ASTM website.
3
6.1.1 The titrimeter must automatically (or manually) con-
Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
trol the rate of addition of titrant as follows: Delivery of titrant
U.K., http://www.energyinst.org.
4
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, will be incremental; after delivery of precisely a 0.100 mL
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098. increment (see 6.1.2), the delivery is stopped and a fixed time

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 D4739 − 23
period of 90 s is allowed to pass before another 0.100 mL 7.4 Buffer, Aqueous Basic—Commercial pH 10 buffer solu-
increment of titrant is delivered. This procedure is repeated tion with a tolerance of 60.02 pH units at 25 °C. This solution
until the titration is completed. shall be replaced at regular intervals consistent with its stability
6.1.2 The precision of addition of the 0.100 mL increments or when contamination is suspected. Information related to the
of titrant must be 60.001 mL for automatic titrators. For stability should be obtained from the manufacturer.
manual buret, it should be 60.005 mL. A higher incremental 7.5 Chloroform—Reagent grade. (Warning—Toxic and
precision is required for an automatic buret, because the total suspected carcinogen.)
volume to the end point is summed from the individual
increments; it is read from a scale with a manual buret. 7.6 Hydrochloric Acid Solution, Standard Alcoholic
(0.1 M)—Mix 9 mL of reagent grade hydrochloric acid (HCl,
6.2 Sensing Electrode, standard pH with glass membrane,
sp gr 1.19) (Warning—Toxic and corrosive), with 1 L of
suitable for non-aqueous titrations.
anhydrous isopropyl alcohol. Standardize frequently enough to
6.3 Reference Electrode, Silver/Silver Chloride (Ag/AgCl) detect normality changes of 0.0005 by potentiometric titration
reference electrode with sleeve junction, filled with 1 M to 3 M of approximately 8 mL (accurately measured) of the 0.1 M
LiCl in ethanol. alcoholic KOH solution diluted with 125 mL CO2-free water.
6.3.1 Combination Electrode—Sensing electrodes may have
7.7 Ethanol—reagent grade. (Warning—Flammable and
the Ag/AgCl reference electrode built into the same electrode
toxic, especially when denatured.)
body, which offers the convenience of working with and
maintaining only one electrode. The combination electrode 7.8 Lithium Chloride Electrolyte—Prepare a solution of 1 M
shall have a sleeve junction type of reference and shall use an to 3 M LiCl in ethanol.
inert ethanol electrolyte, for example, 1 M to 3 M LiCl in
7.9 Potassium Hydroxide—(Warning—Causes severe
ethanol. In the reference compartment, the sensing electrode
burns.)
part shall use a glass membrane designed for non-aqueous
titrations. These combination electrodes shall have the same 7.10 Potassium Hydroxide Solution, Standard Alcoholic
response or better response than a dual electrode system. They (0.1 M)—Add 6 g of reagent grade potassium hydroxide
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shall have removable sleeves for easy rinsing and addition of
electrolyte. (Warning—When a movable sleeve is part of the
(KOH) (Warning—Toxic and corrosive), to approximately 1 L
of anhydrous isopropyl alcohol. Boil gently for 10 min to effect

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electrode system, ensure that the sleeve is unimpaired before solution. Allow the solution to stand for 2 days, and then filter
every titration.) the supernatant liquid through a fine sintered-glass funnel.
Store the solution in a chemically resistant bottle. Dispense in
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6.4 Stirrer, Buret, Stand, Titration Vessel, as specified in
Annex A1, are required. a manner such that the solution is protected from atmospheric
carbon dioxide (CO2) by means of a guard tube containing
soda lime or soda non-fibrous silicate absorbent, and such that
7. Reagents
it does not come into contact with cork, rubber, or saponifiable
7.1 Purity of Reagents—Reagent-grade chemicals ASTM
shall D4739-23
be stopcock grease. Standardize frequently enough to detect
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used in all tests. Unless otherwise indicated, it is intended that normality changes of 0.0005 by potentiometric titration of
all reagents shall conform to the specifications of the Commit- weighed quantities of potassium acid phthalate dissolved in
tee on Analytical Reagents of the American Chemical Society, CO2-free water.
where such specifications are available.5 Other grades may be
used, provided it is first ascertained that the reagent is of 7.11 Propan-2-ol (Isopropyl Alcohol)—Anhydrous, (less
sufficiently high purity to permit its use without lessening the than 0.1 % H2O). (Warning—Flammable.) If dry reagent
accuracy of the determination. cannot be procured, dry it by distillation through a multiple
plate column, discarding the first 5 % of material distilling over
7.2 Purity of Water—Unless otherwise indicated, references and using the 95 % remaining. Also, drying can be accom-
to water shall be understood to mean reagent water that meets plished using molecular sieves by passing the solvent upward
the requirement of either Type I, II, or III of Specification through a molecular sieve column using one part of molecular
D1193. sieve per ten parts of solvent. (Warning—It has been reported
7.3 Buffer, Aqueous Acid—Commercial pH 3 buffer solution that, if not inhibited against it, propan-2-ol can contain
with a tolerance of 60.02 pH units at 25 °C. This solution shall peroxides. When this occurs, an explosive mixture is possible
be replaced at regular intervals consistent with its stability or when the storage vessel or other equipment such as a dispens-
when contamination is suspected. Information related to the ing bottle, are near empty and approaching dryness.
stability should be obtained from the manufacturer. 7.12 Commercially available solutions may be used in place
of laboratory preparations provided the solutions have been
certified as equivalent.
5
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
7.13 Alternate volumes of solutions may be prepared pro-
DC. For suggestions on the testing of reagents not listed by the American Chemical vided the final solution concentration is equivalent.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- 7.14 Toluene—Reagent grade. (Warning—Extremely flam-
copeial Convention, Inc. (USPC), Rockville, MD. mable.)

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 D4739 − 23
7.15 Titration Solvent—In a brown reagent bottle, add 9. Standardization of Apparatus
30 mL of water to 1 L of isopropyl alcohol, and mix thor- 9.1 Determination of Meter Readings for the Aqueous
oughly. Add 1 L each of toluene and chloroform, and mix Buffer Solution—Ensure comparable selection of end points
thoroughly. when definite inflection points are not obtained in the titration
curve. Determine daily, for each electrode pair, the meter
8. Preparation of Electrode System readings obtained with the aqueous acidic buffer solution to be
8.1 Maintenance and Storage of Electrodes—Cleaning the used for the determination of base numbers and with the
electrode thoroughly, keeping the ground-glass joint free of aqueous basic buffer solution to be used for the determination
foreign materials, and regular testing of the electrodes are very of strong base numbers.
important in obtaining repeatable potentials, since the contami- 9.2 Prepare the electrodes as described in 8.2, immerse them
nation may introduce uncertain erratic and unnoticeable liquid in the appropriate aqueous buffer solution, and stir for at least
contact potentials. While this is of secondary importance when 2 min, maintaining the temperature of the buffer solution at a
end points are chosen from inflection points in the titration temperature within 2 °C of that at which the titrations are to be
curve, it may be very serious when end points are chosen at made. Read the cell voltage. The reading so obtained in the
experimentally determined cell potentials as outlined in the acidic buffer solution is taken as the end point for the base
procedure. number if an inflection is not observed as specified in 12.1, and
8.1.1 Clean the pH indicating electrode or the pH indicating the reading obtained in the basic buffer solution is taken as the
part of the combination electrode at frequent intervals based on end point for the strong base number.
use and type of samples being analyzed by immersing in
10. Preparation of Sample
non-chromium containing, strongly oxidizing cleaning solu-
tion. The electrode shall be cleaned periodically when in use or 10.1 When applicable, refer to Practice D4057 (Manual
when a new electrode is installed. Drain the LiCl electrolyte Sampling) or Practice D4177 (Automatic Sampling) for proper
from the electrode at least once each week, and refill with fresh sampling techniques.
LiCl electrolyte as far as the filling hole. Ensure that there are 10.1.1 When sampling used lubricants, the specimen shall

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no air bubbles in the electrode liquid. If air bubbles are
observed, hold the electrode in a vertical position and gently
be representative of the system sampled and shall be free of
contamination from external sources.
10.1.2 Agitate used oil samples thoroughly to ensure that
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tap it to release the bubbles. Maintain the electrolyte level in
the electrode above that of the liquid in the titration beaker at any sediment present is homogeneously suspended before
all times. analysis, as the sediment can be acidic or basic or have

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8.1.2 When not in use, immerse the lower halves of the
electrodes in either water (sensing) or the LiCl in isopropyl
adsorbed acidic or basic material from the sample. When
necessary, samples are warmed to aid mixing.
alcohol electrolyte (reference). Do not allow them to remain NOTE 1—As used oils can change appreciably in storage, samples
ASTM
immersed in titration solvent for any appreciable period D4739-23
of time 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.
between titrations. While the electrodes are not extremely
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fragile, handle them carefully at all times. 11. Procedure for Base Number and Strong Base
8.1.3 Electrode Life—Typically, electrode usage is limited Number
to 3 to 6 months, depending upon usage. Electrodes have a 11.1 Calculate the quantity of sample required for its
limited shelf life and shall be tested before use (8.3). expected base number as follows:
8.2 Preparation of Electrodes: A 5 7/E (1)
8.2.1 When Ag/AgCl reference electrode is used for the where:
titration and it contains an electrolyte that is not 1 M to 3 M
A = approximate mass of sample, g and
LiCl in ethanol, replace the electrolyte. Drain the electrolyte
E = expected base number.
from the electrode, wash away all the salt (if present) with
water and then rinse with ethanol. Rinse several times with the 11.1.1 Take a maximum of 5 g and a minimum of 0.1 g for
LiCl electrolyte solution. Finally, replace the sleeve and fill the analysis. The precision of weighing is as follows:
electrode with the LiCl electrolyte to the filling hole. When Size of Sample, g Precision of Weighing, g
refitting the sleeve, ensure that there will be a free flow of 1–5 0.005
0.1–1 0.002
electrolyte into the system. A combination electrode shall be
prepared in the same manner. The electrolyte in a combination 11.2 Into a suitable titration vessel, introduce a weighed
electrode can be removed with the aid of a vacuum suction. quantity of sample as prescribed in 11.1.1, and add 75 mL of
titration solvent. If 75 mL of solvent is not sufficient to
8.2.2 Prior to each titration, soak the prepared electrodes in
properly cover the electrodes, add just enough additional
water, pH 4.5 – 5.5 acidified with HCL, for at least 5 min.
solvent to do so. Ensure the electrodes are properly immersed.
Rinse the electrode with propan-2-ol immediately before use,
Prepare the electrodes as directed in 8.2. Place the beaker or
and then with the titration solvent.
titration vessel on the titration stand, and adjust its position so
8.3 Testing of Electrodes—See Appendix X2 for the proce- that the electrodes are about half immersed. Start the stirrer,
dure to check electrode performance. and stir throughout the determination at a rate sufficient to

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 D4739 − 23
produce vigorous agitation without spattering and without
stirring air into the solution.
11.3 Select and fill a suitable buret with the 0.1 M alcoholic
HCl solution, and place the buret in position on the titration
assembly, taking care that the tip is immersed about 25 mm in
the liquid in titration vessel. Record the initial buret and meter
(cell potential) readings.
11.4 Titration—The reaction of the hydrochloric acid with
the basic components is very slow with most titrations for base
number. As a result, these titrations are not at equilibrium.
Because of this, the titration conditions are tightly specified
and must be strictly adhered to in order to achieve the precision
as stated.
NOTE 2—When best precision of titration is desired, if the titrant tip has
been sitting for more than 30 min without being used, it is best to purge (A) Titration curve has no inflections. Take end point at the
the tips by dispensing a few millilitres of titrant before beginning a
titration.
buffer potential.
NOTE 3—See Appendix X1 for techniques for reducing the titration (B) Titration curve has well-defined inflection within pre-
time of a sample. Pre-dosing techniques have been found to provide scribed window. Take well-defined inflection as the end point.
satisfactory results, although the precision using these techniques has not (C) Titration curve has inflection prior to buffer potential
been determined. but not in prescribed window. Take end point at buffer
11.4.1 Whether the titration is carried out manually or potential.
automatically, the following procedure of fixed increment, fixed FIG. 1 Example Titration Curves to Illustrate Selection of End
time addition of titrant shall be followed. Add 0.1 M HCl in Points
increments of 0.100 mL throughout the titration with a 90 s
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pause between each incremental addition. Take millivolt read-
ings at the end of each 90 s interval.

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11.4.1.1 The meter readings of potential difference are whenever at least five successive cell potential changes, ∆, caused by the
addition of the corresponding five increments of titrant, exhibit a maxi-
plotted manually or automatically against the respective vol- mum illustrated as follows:
umes of titrant, and the end point is taken as described in 12.1.
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11.4.2 On completion of the titration, remove the titration
vessel and rinse the electrodes and buret tip with the titration
Titrant, mL
1.8
1.9
∆, mV
8.3
10.7
2.0 11.3
solvent, then with water, then again with titration solvent. 2.1 10.0
(Soak electrodes in distilled water for at least 5 ASTM D4739-23
min before 2.2 7.9
using for another titration.) Store the sensing electrode in
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The ∆ at the maximum should be at least 5 mV, and the difference in ∆
deionized or distilled water and the reference electrode in a between the maximum and both the first and last ∆ should be at least
saturated solution of LiCl in isopropyl alcohol when not in use 2 mV.
(see 8.1). 12.2 Calculate the base number and strong base number as
11.4.3 Blanks—For each set of samples, make a blank follows:
titration of the same volume of titration solvent used for the
sample. For the base number blank, add 0.1 M alcoholic HCl Base number, mg KOH⁄g 5 @ ~ A 2 B ! × M × 56.1# /W (2)
solution in 0.01 mL increments, waiting 12 s between each Strong base number, mg KOH/g 5 @ ~ CM1Dm! × 56.1# /W (3)
addition, until a potential which is 100 mV past the buffer
where:
potential (see 11.4) is reached. For the strong base number
blank, add KOH titrant under the same conditions until the A = alcoholic HCl solution, mL, used to titrate the sample to
potential corresponding to the basic buffer solution is reached. the end point (aqueous acidic pH 3 buffer or
inflection—see 7.3 and 12.1),
12. Calculation B = alcoholic HCl, mL, used to titrate the solvent blank to
the same potential at which the sample end point
12.1 If an inflection (see Note 4) occurs in the potential occurs,
region between the pH 3 buffer potential (see 11.4) and a point M = molarity of the alcoholic HCl solution,
100 mV past this potential, mark this inflection as the end W = sample, g,
point. If more than one inflection points are observed, use the C = alcoholic HCl solution, mL, used to titrate the sample to
last well-defined inflection point. If no well-defined inflection an end point that occurs at a meter reading correspond-
occurs in the above mentioned potential region, mark as the ing to the aqueous basic pH 10 buffer (see 7.4 and
end point the point on the curve that corresponds to the acidic 12.1),
aqueous pH 3 buffer potential. See Fig. 1 for examples of end D = alcoholic KOH solution, mL, used to titrate the solvent
points. blank to the potential corresponding to C, and
NOTE 4—An inflection point is generally recognizable by inspection
m = molarity of the alcoholic KOH solution.