LUBRIZOL TEST PROCEDURE

TP-AATM-109-01
Edition: August 12, 2006
Previous Edition: May 1, 2000

Acid Value
DEFINITION

REAGENTS

Acid Value is expressed as milligrams of potassium

hydroxide required to neutralize the free acids in
one gram of the material.
Acidity (as defined in USP) is expressed as the
number of milliliters of 0.1N alkali required to
neutralize the free acids in 10 grams of the
substance.
NOTE: Use part I for all samples plus in-process
samples that also require Hydroxyl Value. For inprocess samples not needing Hydroxyl Value, use
Part II which provides a fast estimation of the Acid
Value.

1.

EQUIPMENT REQUIRED

3.

1.
2.
3.
4.
5.
6.

Erlenmeyer flasks - 125 ml.

Dispensing devices capable of dispensing 25
ml ( 1%) or 50 ml ( 1%).
Analytical balance capable of weighing to the
nearest 0.1mg.
Hot plate, Magnetic stirrer, stirring bars.
Dispensing device capable of dispensing 1 ml.
Burette, in compliance with one of the
following:
10 ml graduated in 0.05 ml divisions with
a tolerance of 0.04ml
25 ml graduated in 0.10 ml divisions with
a tolerance of 0.05ml
50 ml graduated in 0.10 ml divisions with
a tolerance of 0.07ml

2.

4.
5.

Neutralized ethanol or IPA (see below*) - to 1

liter of Reagent Ethanol or LC Grade IPA
add 1 ml 1% Phenolphthalein Indicator.
Titrate with 0.1N Methanolic Potassium
Hydroxide to a faint pink color.
0.1N Methanolic Potassium Hydroxide commercially available.
NOTE: The normality of this base is
accurate to 3 significant figures while we only
report to 2 significant figures. The base is
used up to about 1 month. Past standardizations have shown that the titer does not
change significantly.
0.5N
Methanolic
KOH
solution
commercially available (can be standardized
by method AATM 1002).
1% Phenolphthalein in I.P.A. - commercially
available.
Anhydrous Ether - reagent grade*.

PROCEDURE - Part I
1.

Accurately weigh the specified amount of

sample into a tared 125 ml Erlenmeyer flask
and record weight to the nearest 0.1 mg.
Determine sample size as follows:
Anticipated
Acid Value

Sample Size

Less than 1.0

1 - 25
25 - 50
50 - 150
Greater than 150

4 (0.1)g
2 (0.1)g
1 (0.1)g
3 (0.1)g
2.5 (0.1)g

Normality KOH
0.1N
0.1N
0.1N
0.5N
0.5N

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Lubrizol Test Procedure TP-AATM-109-01

Acid Value
Page 2 of 2

2.

Using a dispensing device, add 50 ml

neutralized IPA and a stirring bar and mix to
dissipate, warming on a heat source if
necessary. Allow sample to cool.
*For products insoluble in IPA after warming,
substitute the following:
Add 25 ml
neutralized ethanol.
Warm, stirring to
dissolve. Cool and add 25 ml anhydrous
ether.
Prepare a reagent blank containing 50 ml
neutralized IPA, or 25 ml each neutralized
ethanol and ether if used. NOTE: When
using 0.5N KOH no blank is needed.
Using a dispensing device, add approximately
1 ml phenolphthalein.
Fill burette and titrate using Potassium
Hydroxide solution to a faint pink color which
remains for 30 seconds or more.
Read the burette as accurately as possible to
two decimal places.

3.

4.
5.

6.

PROCEDURE - Part II
1.
2.

3.
4.

5.

Weigh 2.8 g of filtered (if necessary) sample

into a tared 125 ml Erlenmeyer flask.
Using a dispensing device, add 50 ml
neutralized IPA and a stirring bar and mix to
dissipate, warming on a heat source if
necessary. Allow sample to cool.
For products insoluble in IPA after
warming, substitute the following: Add
25 ml neutralized ethanol. Warm, stirring
to dissolve. Cool and add 25 ml
anhydrous ether.
Using a dispensing device, add approximately 1 ml phenolphthalein.
Fill burette and titrate using Potassium
Hydroxide solution to a faint pink color
which remains for 30 seconds or more.
Read the burette as accurately as possible
to 2 decimal places.

CALCULATIONS for Part I

CALCULATIONS for Part II

Acid Value = (ml sample - ml blank) x N KOH x 56.1

g sample

Acid Value = ml for sample x 2

Using 0.5N KOH:

ml sample x N KOH x 56.1
g sample

PRECISION:
In those cases where the ml of 0.1N KOH used is
less than 1.
Combining two sets of data, we obtain:

Average of 13 determinations = 0.46

Standard Deviation = 0.0375
95% Confidence Limit = 0.46 0.02

In those cases where the ml of KOH used is

greater than 1.
Example using a Wool Grease:

Average of 12 determinations = 7.72

Standard Deviation = 0.110
95% Confidence Limit 7.722 0.070