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: D3242 − 11 (Reapproved 2017)

Designation: 354/98

Standard Test Method for

Acidity in Aviation Turbine Fuel1
This standard is issued under the fixed designation D3242; 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.

1. Scope sample, required to titrate a sample in a specified solvent to a

1.1 This test method covers the determination of the acidity specified endpoint using a specified detection system.
in aviation turbine fuel in the range from 0.000 mg ⁄g to 3.1.1.1 Discussion—in this test method, the solvent is a
0.100 mg ⁄g KOH. toluene-water-isopropanol mixture and the end point is deter-
mined when a green/green brown color is obtained using the
1.2 The values stated in SI units are to be regarded as specified p-naphtholbenzein indicator solution.
standard. No other units of measurement are included in this
standard. 4. Summary of Test Method
1.3 This standard does not purport to address all of the 4.1 The sample is dissolved in a mixture of toluene and
safety concerns, if any, associated with its use. It is the isopropyl alcohol containing a small amount of water. The
responsibility of the user of this standard to establish appro- resulting single phase solution is blanketed by a stream of
priate safety and health practices and determine the applica- nitrogen bubbling through it and is titrated with standard
bility of regulatory limitations prior to use. alcoholic potassium hydroxide to the end point indicated by the
1.4 This international standard was developed in accor- color change (orange in acid and green in base) of the added
dance with internationally recognized principles on standard- p-naphtholbenzein solution.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 5. Significance and Use
mendations issued by the World Trade Organization Technical 5.1 Some acids can be present in aviation turbine fuels due
Barriers to Trade (TBT) Committee. either to the acid treatment during the refining process or to
naturally occurring organic acids. Significant acid contamina-
2. Referenced Documents tion is not likely to be present because of the many check tests
2.1 ASTM Standards:2 made during the various stages of refining. However, trace
D664 Test Method for Acid Number of Petroleum Products amounts of acid can be present and are undesirable because of
by Potentiometric Titration the consequent tendencies of the fuel to corrode metals that it
D1193 Specification for Reagent Water contacts or to impair the water separation characteristics of the
aviation turbine fuel.
3. Terminology
5.2 This test method is designed to measure the levels of
3.1 Definitions: acidity that can be present in aviation turbine fuel and is not
3.1.1 acid number, n—the quantity of a specified base, suitable for determining significant acid contamination.
expressed in milligrams of potassium hydroxide per gram of
6. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D02 on
6.1 Buret—A 25 mL buret graduated in 0.1 mL
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of subdivisions, or a 10 mL buret graduated in 0.05 mL subdivi-
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. sions.
Current edition approved May 1, 2017. Published June 2017. Originally
approved in 1973. Last previous edition approved in 2011 as D3242 – 11. DOI: NOTE 1—An automated buret capable of delivering titrant amounts in
10.1520/D3242-11R17. 0.05 mL or smaller increments can be used, but the stated precision data
This test method has been approved by the sponsoring committees and accepted were obtained using manual burets only.
by the cooperating societies in accordance with established procedures.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 7. Reagents and Materials
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 7.1 Purity of Reagents—Reagent grade chemicals shall be
the ASTM website. used in all tests. Unless otherwise indicated, it is intended that

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
1
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.
 D3242 − 11 (2017)
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available.3 Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
NOTE 2—Commercially available reagents may be used in place of
laboratory preparations when they are certified in accordance with 7.1.
7.2 Purity of Water— References to water shall be under-
stood to mean distilled water as defined by Type III water of
Specification D1193.
7.3 p-Naphtholbenzein 4,5 Indicator Solution—The
p-naphtholbenzein must meet the specifications given in Annex
A1. Prepare a solution of p-naphtholbenzein in titration solvent
equal to 10 g ⁄L 6 0.01 g ⁄L.
7.4 Nitrogen, dry-type, carbon dioxide-free. (Warning—
FIG. 1 Titration Flask
Compressed gas under high pressure. Gas reduces oxygen
available for breathing.)
7.5 Potassium Hydroxide Solution, Standard Alcoholic
(0.01 N)—Add 0.6 g of solid KOH (Warning—Highly corro- the potassium hydroxide alcoholic solution to either of the
sive to all body tissue both in solid form and in solution.) to following end points: (1) when the titration is electrometric,
approximately 1 L of anhydrous isopropyl alcohol titrate to a well-defined inflection point at the voltage that
(Warning—Flammable. Vapor harmful. Keep away from heat, corresponds to the voltage of the basic buffer solution; (2)
sparks, and open flame.) (containing less than 0.9 % water) in when the titration is colorimetric, add 6 drops of phenolphtha-
a 2 L Erlenmeyer flask. Boil the mixture gently for 10 min to lein indicator solution and titrate to the appearance of a
15 min, stirring to prevent the solids from forming a cake on permanent pink color. Perform the blank titration on the water
the bottom. Add at least 0.2 g of barium hydroxide (Ba(OH)2) used to dissolve the potassium acid phthalate. Calculate the
(Warning—Poisonous if ingested. Strongly alkaline, causes normality using the equation:
severe irritation producing dermatitis.) and again boil gently
for 5 min to 10 min. Cool to room temperature, allow to stand Wp 1000
Normality 5 3 (1)
for several hours, and filter the supernatant liquid through a 204.23 V 2 V b
fine sintered-glass or porcelain filtering funnel; avoid unnec- where:
essary exposure to carbon dioxide (CO2) during filtration. Wp = weight of the potassium acid phthalate, g,
Store the solution in a chemically resistant dispensing bottle 204.23 = molecular weight of the potassium acid phthalate,
out of contact with cork, rubber, or saponifiable stopcock V = volume of titrant used to titrate the salt to the
lubricant and protected by a guard tube containing soda lime. specific end point, mL, and
NOTE 3—Because of the relative large coefficient of cubic expansion of Vb = volume of titrant used to titrate the blank, mL.
organic liquids, such as isopropyl alcohol, the standard alcoholic solutions 7.5.2 Phenolphthalein Indicator Solution—Dissolve 0.1 g
should be standardized at temperatures close to those employed in the
titration of samples. 6 0.01 g of pure solid phenolphthalein in 50 mL of water, free
of CO2, and 50 mL of ethanol.
7.5.1 Standardization of Potassium Hydroxide Solution—
Standardize frequently enough to detect changes of 0.0002N. 7.6 Titration Solvent—Add 500 mL of toluene (Warning—
One way to accomplish this is as follows. Weigh, to the nearest Flammable. Vapor harmful. Keep away from heat, sparks, and
0.1 mg, approximately 0.02 g of potassium acid phthalate, open flame.) and 5 mL of water to 495 mL of anhydrous
which has been dried for at least 1 h at 110 °C 6 1 °C and isopropyl alcohol.
dissolve in 40 mL 6 1 mL of water, free of CO2. Titrate with
8. Procedure
3
Reagent Chemicals, American Chemical Society Specifications, American
8.1 Introduce 100 g 6 5 g of the sample weighed to the
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not nearest 0.5 g, into a 500 mL wide-mouth Erlenmeyer flask.
listed by the American Chemical Society, see Annual Standards for Laboratory (One type of suitable modified flask is shown in Fig. 1.) Add
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia 100 mL of the titration solvent and 0.1 mL of the indicator
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. solution. Introduce nitrogen through a 6 mm to 8 mm outside
4
In a 2006 study, only Kodak, Baker (Mallinkrodt), Fluka, and Aldrich were diameter glass tube to a point within 5 mm of the flask bottom
found to meet the specifications in Annex A1. However, Kodak brand is no longer at a rate of 600 mL ⁄min to 800 mL ⁄min. Bubble the solution
available.
5
for 3 min 6 30 s with occasional mixing.
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1626. Contact ASTM Customer 8.1.1 The vapor from this treatment contains toluene and
Service at [email protected]. should be removed with adequate ventilation.

Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
2
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.
 D3242 − 11 (2017)
8.2 Continue the nitrogen addition and titrate without delay TABLE 1 PrecisionA
at a temperature below 30 °C. Add 0.01 N KOH solution in NOTE 1—All values are in acid number units.
increments and swirl to disperse. When the solution first turns Average Acid Number Repeatability Reproducibility
green, reduce the increment size to dropwise (manual buret) or 0.001 0.0004 0.0013
between 0.01 mL and 0.05 mL (automated buret). Continue 0.002 0.0006 0.0018
until a persistent green end point is reached and held for a 0.005 0.0009 0.0029
0.010 0.0013 0.0041
minimum of 15 s after the addition of the last increment. 0.020 0.0019 0.0057
0.050 0.0030 0.0091
NOTE 4—The temperature can be measured by any suitable temperature 0.100 0.0042 0.0128
measuring device. A
These precision data were derived as follows:
8.3 Blank—Perform a blank titration on 100 mL of the Repeatability 50.0132 œa
titration solvent and 0.1 mL of the indicator solution, introduc- Reproducibility 50.0406 œ a
ing the nitrogen in the same manner and titrating to the same where: a = acid number

end point as above.

9. Quality Control Checks N = normality of the KOH solution, and
W = sample used, g.
9.1 Confirm the performance of the equipment or the
procedure each day it is in use, by analyzing a quality control 11. Report
(QC) sample. It is advisable to analyze additional QC samples 11.1 Report the result to the nearest 0.001 mg KOH ⁄g as
as appropriate, such as at the end of a batch of samples or after Acid Number (Test Method D3242) = (Result).
a fixed number of samples to ensure the quality of the results.
Analysis of result(s) from these QC samples can be carried out 12. Precision and Bias7
using control chart techniques.6 When the QC sample result 12.1 Precision—The precision of this test method as deter-
causes the laboratory to be in an out-of-control situation, such mined by statistical examination of interlaboratory results is as
as exceeding the laboratory’s control limits, instrument recali- follows:
bration may be required. An ample supply of QC sample 12.1.1 Repeatability—The difference between two test
material shall be available for the intended period of use, and results, obtained by the same operator with the same apparatus
shall be homogeneous and stable under the anticipated storage under constant operating conditions on identical test material,
conditions. If possible, the QC sample shall be representative would in the long run, in the normal and correct operation of
of samples typically analyzed and the average value and the test method, exceed the following values only in one case
control limits of the QC sample shall be determined prior to in twenty (see Table 1).
monitoring the measurement process. The QC sample preci- 12.1.2 Reproducibility—The difference between two single
sion shall be checked against the ASTM method precision to and independent results obtained by different operators work-
ensure data quality. ing in different laboratories on identical test material would, in
NOTE 5—Because the acid number can vary while the QC sample is in
the long run, in the normal and correct operation of the test
storage, when an out-of-control situation arises, the stability of the QC method, exceed the following values only in one case in twenty
sample can be a source of the error. (see Table 1).
10. Calculations NOTE 6—The precision statements were based on the use of manual
burets only. The user is cautioned that the precision statements may or
10.1 Calculate the acid number as follows: may not be applicable to titrations performed with the use of automated
burets, since no interlaboratory study has been conducted to date to
Acid number, mg of KOH/g 5 @ ~ A 2 B ! N 3 56.1# /W (2) statistically evaluate results determined by both techniques.
where: 12.2 Bias—The procedure in this test method has no bias
A = KOH solution required for titration of the sample (8.2), because the value of the acid can be defined only in terms of
mL, the test method.
B = KOH solution required for titration of the blank (8.3),
13. Keywords
mL,
13.1 acidity; aviation turbine fuel

6 7
MNL 7, Manual on Presentation of Data Control Chart Analysis, Section 3: Supporting data have been filed at ASTM International Headquarters and may
Control Charts for Individuals, 6th ed., ASTM International, W. Conshohocken, be obtained by requesting Research Report RR:D02-1010. Contact ASTM Customer
1990. Service at [email protected].

Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
3
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.
 D3242 − 11 (2017)
ANNEXES

(Mandatory Information)

A1. SPECIFICATIONS FOR p-NAPHTHOLBENZEIN

A1.1 Conformity Requirements A1.1.5 pH Range:

A1.1.5.1 Indicator turns to the first clear green at a relative
A1.1.1 Appearance—Red amorphous powder.
pH of 11 6 0.5 when tested by the method for pHr range of
A1.1.2 Chlorides—Less than 0.5 %. p-naphtholbenzein indicator as described in Annex A2.
A1.1.5.2 Requires not more than 0.5 mL of 0.01 N KOH
A1.1.3 Solubility—Ten grams shall dissolve completely in
solution above that for the blank to bring the indicator solution
1 L of titration solvent.
to the first clear green.
A1.1.4 Minimum Absorbance—Exactly 0.1000 g of the A1.1.5.3 Requires not more than 1.0 mL of 0.01 N KOH
sample is dissolve in 250 mL of methanol. (Warning— solution above that for the blank to bring the indicator solution
Flammable.) Five millilitres of this solution is made up to to a blue color.
100 mL with pH 12 buffer. This final dilution should have a A1.1.5.4 Initial pHr of the indicator solution is at least as
minimum absorbance of 1.20 when read at the 650 nm peak high as that of the blank.
using a Beckman DU or alternative type spectrophotometer, A1.1.5.5 Buffer is made by mixing 50 mL of 0.05 M dibasic
1 cm cells, and water as the blank. sodium phosphate with 26.9 mL 0.1 M sodium hydroxide.

A2. TEST METHOD FOR DETERMINING pHr RANGE OF p-NAPHTHOLBENZEIN INDICATOR

A2.1. Scope that all reagents shall conform to the specifications of the
A2.1.1 This test method is intended for determining the Committee on Analytical Reagents of the American Chemical
acceptability of p-naphtholbenzein indicator for use in Test Society, where such specifications are available.3 Other grades
Method D3242 with regard to color change over a pHr range. may be used, provided it is first ascertained that the reagent is
of sufficiently high purity to permit its use without lessening
A2.2. Terminology the accuracy of the determination.
A2.2.1 Definitions of Terms Specific to This Standard: A2.5.2 Purity of Water—References to water shall be un-
A2.2.1.1 pHr—an arbitrary term which expresses the rela- derstood to mean distilled water.
tive hydrogen ion activity in the toluene-isopropyl alcohol A2.5.3 Acidic Buffer Solution (pHr = 4.0):
medium in a manner similar to that in which the term pH
A2.5.3.1 2,4,6 Trimethyl Pyridine (γ Collidine)—
expresses the actual hydrogen ion activity in aqueous solutions.
((CH3)3C5H2N)—(mol weight 121.18). (Warning—2,4,6-
For the purpose of this test method, the pHr acidity scale is
trimethyl pyridine (γ collidine) is hazardous if swallowed,
defined by two standard buffer solutions which have been
breathed, or spilled on skin or eyes.) (Warning—Wear chemi-
designated pHr 4 and pHr 11. The exact relation between pHr
cal safety goggles, neoprene or rubber gloves and an apron.
and the true pH of a toluene-isopropyl alcohol solution is not
Use only in a well-ventilated hood, or wear an approved
known and cannot be readily determined.
respirator for organic vapor or a supplied-air respirator. Do not
A2.3. Summary of Test Method take internally.) Conform to the following requirements:
Boiling range 168 °C to 170 °C
A2.3.1 A prescribed amount of indicator is titrated electro- Refractive index, nD20 1.4982 ± 0.0005
metrically through the various color changes with alcoholic Color colorless
potassium hydroxide and results plotted against meter readings A2.5.3.2 Store the reagent over activated alumina, and keep
converted to pHr units. it in a brown glass bottle.
A2.5.3.3 Buffer Stock Solution A—(Warning—Flammable.)
A2.4. Apparatus
(Warning—2,4,6-trimethyl pyridine (γ collidine) is hazardous
A2.4.1 Meter, Reference and Glass Electrodes or Combina- if swallowed, breathed, or spilled on skin or eyes.)
tion Electrode, Stirrer, Beaker, and Stand, as specified in Test (Warning—Wear chemical safety goggles, neoprene or rubber
Method D664 – IP 177. gloves and an apron. Use only in a well-ventilated hood, or
wear an approved respirator for organic vapor or a supplied-air
A2.5. Reagents respirator. Do not take internally.) Accurately weigh 24.2 g 6
A2.5.1 Purity of Reagents—Reagent grade chemicals shall 0.1 g of 2,4,6-trimethyl pyridine (γ -collidine), and transfer to
be used in all tests. Unless otherwise indicated, it is intended a 1 L volumetric flask containing 100 mL of propan-2-ol.

Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
4
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.
 D3242 − 11 (2017)
Using a 1 L graduated cylinder, add to the flask, while A2.5.9 Titration Solvent—Add 500 mL of toluene and 5 mL
continuously stirring its contents, 150/C 6 5 mL of 0.2 mol ⁄L of water to 495 mL of anhydrous isopropyl alcohol. The
alcoholic HCl solution (C being the exact molarity concentra- titration solvent should be made up in large quantities.
tion of the HCl solution found by standardization). Dilute to
the 1000 mL mark with propan-2-ol, and mix thoroughly. Use A2.6 Preparation of Electrode System
within two weeks. A2.6.1 Maintenance of Electrodes —Clean the glass elec-
A2.5.3.4 Buffer, Nonaqueous Acidic—Add 10 mL of buffer trode (Note A2.1) at frequent intervals (not less than once
stock Solution A to 100 mL of titration solvent. Use within 1 h. every week during continual use) by immersing in cold
A2.5.4 Alkaline Buffer Solution (pHr = 11.0): chromium-free cleaning solution or in other equipment clean-
A2.5.4.1 m-Nitrophenol (NO 2 C 6 H 4 OH) (mol weight ing solutions. (Warning—Causes severe burns. Strong oxi-
139.11). (Warning—m-Nitrophenol can be hazardous if dizer. Contact with materials may cause fire. Hygroscopic.)
swallowed, breathed, or spilled on skin or eyes. Wear Drain the electrode at least once each week, and refill with
chemical-safety goggles, neoprene or rubber gloves, and an fresh KCl electrolyte as far as the filling hole. Ascertain that
apron. Use only in a well-ventilated hood, or wear an approved crystallized KCl is present. Maintain the electrolyte level in the
respirator for organic vapor or a supplied-air respirator. Do not reference electrode above that of the liquid in the titration
take internally.) Conform to the following requirements: beaker or vessel at all times. When not in use, immerse the
lower halves of the electrodes in water. Do not allow them to
Melting point 96 °C to 97 °C
Color pale yellow remain immersed in titration solvent for any appreciable period
A2.5.4.2 Store the reagent in a brown glass bottle. of time between titrations. While the electrodes are not
A2.5.4.3 Buffer Stock Solution B—(Warning— extremely fragile, handle them carefully at all times.
Flammable.) (Warning—m-Nitrophenol can be hazardous if NOTE A2.1—Cleaning the electrodes8 thoroughly, keeping the ground-
swallowed, breathed, or spilled on skin or eyes. Wear glass joint free of foreign materials, and regular testing of the electrodes
chemical-safety goggles, neoprene or rubber gloves, and an are very important in obtaining repeatable potentials, since contamination
may introduce uncertain erratic and unnoticeable liquid contact potentials.
apron. Use only in a well-ventilated hood, or wear an approved While this is of secondary importance when end points are chosen from
respirator for organic vapor or a supplied-air respirator. Do not inflection points in the titration curve, it may be quite serious when end
take internally.) Accurately weigh 27.8 g 6 0.1 g of points are chosen at arbitrarily fixed cell potentials.
m-nitrophenol and transfer to a 1 L volumetric flask containing A2.6.2 Preparation of Electrodes—Before and after using,
100 mL of propan-2-ol. Using a 250 mL graduated cylinder, wipe the glass electrode thoroughly with a clean cloth, or a soft
add to the flask while continuously stirring its contents, 50/C2 absorbent tissue, and rinse with water. Wipe the reference
6 1 mL of 0.2 mol ⁄L alcoholic KOH solution (C2 being the electrode with a cloth or tissue, carefully remove the ground-
exact molarity concentration of the KOH solution found by glass sleeve, and thoroughly wipe both ground surfaces.
standardization). Dilute to the 1000 mL mark with propan-2-ol, Replace the sleeve loosely, and allow a few drops of electrolyte
and mix thoroughly. Use within two weeks. to drain through to flush the ground-glass joint. (Warning—
A2.5.4.4 Buffer Nonaqueous Basic—Add 10 mL of buffer Causes severe burns.) Wet the ground surfaces thoroughly with
stock Solution B to 100 mL of titration solvent. Use within 1 h. electrolyte, set the sleeve firmly in place, and rinse the
A2.5.5 Hydrochloric Acid, Standard Alcoholic Solution (0.2 electrode with water. Prior to each titration, soak the prepared
N)—Prepare and standardize in accordance with Test Method electrodes in water for at least 5 min immediately before use,
D664 – IP 177. and touch the tips of the electrodes with a dry cloth or tissue to
A2.5.6 p-Naphtholbenzein Indicator Solution—Prepare as remove the excess of water.
described in 7.3. A2.6.3 Testing of Electrodes—Test the meter-electrode
A2.5.7 Potassium Chloride Electrolyte—Prepare a saturated combination when first put into use, or when new electrodes
solution of potassium chloride (KCl) in water. are installed, and retest at intervals thereafter by dipping the
electrodes into a well-stirred mixture of 100 mL of the titration
A2.5.8 Potassium Hydroxide, Standard Alcoholic Solu- solvent and 1.0 mL to 1.5 mL of 0.1 mol ⁄L alcoholic KOH
tion—(0.2 N). (Warning—Flammable.) (Warning—Causes solution. For the meter-electrode combination to be suitable for
severe burns.). Add 12 g to 13 g of potassium hydroxide use, the potential between the electrodes should change by
(KOH) to approximately 1 L of anhydrous propan-2-ol. Boil more than 480 mV from the potential between the same
gently for 10 min to effect solution. Allow the solution to stand electrodes when dipped in the nonaqueous acidic buffer solu-
for two days, and then filter the supernatant liquid through a tion (Note A2.2).
fine sintered glass funnel. Store the solution in a chemically
resistant bottle. Dispense in a manner such that the solution is NOTE A2.2—Considerably more sensitive electrodes are now available
that will show a potential change of at least 590 mV under these
protected from atmospheric carbon dioxide (CO2) by means of conditions, and their use is recommended. When combination electrodes
a guard tube containing soda lime or soda non-fibrous silicate are used, test as in 8.3.
absorbants and such that it does not come into contact with
cork, rubber, or saponifiable stopcock grease. Standardize 8
For a detailed discussion of the need for care in preparation of the electrodes,
frequently enough to detect concentration changes of 0.0005 see Lykken, L., Porter, P., Ruliffson, H. D., and Tuemmler, F. D., “Potentiometric-
by potentiometric titration of weighed quantities of potassium Determination of Acidity in Highly Colored Oils,” Industrial and Engineering
acid phthalate dissolved in CO2-free water. Chemistry, Analytical Edition, IENAA, Vol 16, 1944, pp. 219–234.

Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
5
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.
 D3242 − 11 (2017)
A2.7 Standardization of Apparatus
A2.7.1 Prior to each test or series of tests, set the meter to
read on the pH scale, insert the electrodes into a beaker
containing the acidic nonaqueous buffer solution at a tempera-
ture of 25 °C 6 2 °C and stir the solution vigorously. When the
pH meter reading becomes constant adjust the asymmetry
potential dial of the instrument so that the meter reads 4.0.
A2.7.2 Remove the acidic buffer, clean the electrodes, and
immerse them in water for several minutes. Dry the electrodes
and insert them in a beaker containing alkaline nonaqueous
buffer solution at 25 °C 6 2 °C. When the pH meter reading
has become steady, record the exact value. If the reading is
within 0.2 pH units of 11.0, the initial acidity, pHr, of unknown
solutions may be read directly from the dial of the meter. If the
reading is not within 0.2 units of 11.0 prepare a correction
graph as shown in Fig. A2.1. Use this graph to convert pH FIG. A2.1 Calibration Curve for Conversion of pH Meter Read-
meter readings to initial acidity, pHr. ings to pHr

A2.8. Procedure
A2.8.1 Titrate 100 mL of titration solvent with 0.01 N KOH Amber to olive green
solution until the meter indicates a pHr between 13 and 14. Olive green to clear green
Clear green to bluish green
A2.8.2 Add 0.5 mL of indicator solution to a fresh portion Bluish green to blue
of titration solvent and after cleaning the electrodes titrate with A2.8.4 Plot the blank titration on the same paper used for
0.01 N KOH solution until the meter indicates a pHr between the indicator.
13 and 14.
A2.8.3 During the titration, plot the volume of titrant A2.9. Calculation
against the pHr or meter reading and note on the curve the A2.9.1 Subtract the volume of titrant used in the blank
various color changes at the corresponding pHr values. titration from that used for the indicator solution titration at the
NOTE A2.3—The following color changes, in order, are intended as a same pHr corresponding to the definite color changes between
guide: 10 to 12 pHr.

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/

Copyright by ASTM Int'l (all rights reserved); Mon Oct 9 21:34:49 EDT 2017
6
Downloaded/printed by
Fadhlan Asyraf (PT. Pertamina Persero) pursuant to License Agreement. No further reproductions authorized.