Acid Number in Lubricating and Motor Oil: Reliable Determination According To ASTM D664 and IP 177

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TITRATION APPLICATION NOTE T-096

Acid number in lubricating and


motor oil
Reliable determination according to ASTM D664 and IP 177
Fresh as well as used petroleum products may equivalence point. A flexible sleeve diaphragm
contain acidic components as additives or facilitates its cleaning especially after use in heavily
degradation products. The acid number (AN) is a contaminated samples, such as in used engine oils.
measure for the relative amount of acids present Using the correct electrode greatly increases the
expressed as mg KOH per g sample. Moreover, AN is precision and reliability of the results.
used as a quality parameter of lubricating oils both
This Application Note describes the potentiometric
for assessing the quality of new formulations and as
determination of the acid number according to
an indicator for the degradation of such
ASTM D664 and IP 177 using the pH electrode
formulations during service.
Solvotrode easyClean.
The use of a pH electrode suitable for non-aqueous
titrations ensures the reliable determination of the

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SAMPLE AND SAMPLE PREPARATION RESULTS

This application is demonstrated on lubricating oil For the tested samples, well-defined titration curves
and fresh motor oil. are obtained with acceptable results and low
standard deviations. Results are summarized in Table
Care should be taken to use a representative, well-
1. An example titration curve is displayed in Figure 2.
homogenized sample portion. Otherwise, no sample
preparation is necessary.
Table 1. Results for the acid number determination according to
ASTM D664 on a fully automated OMNIS system.
EXPERIMENTAL
AN in mg lubricating oil motor oil
The analysis is carried out on an automated system
KOH/g sample (n = 3) (n = 28)
consisting of an OMNIS Sample Robot S and an
OMNIS Advanced Titrator equipped with a Mean 1.088 1.9171
Solvotrode easyClean.
SD(abs) 0.005 0.034
Before the samples are measured, a blank
determination is performed using the same amount SD(rel) 0.47 1.78
of solvent as for the sample titration.

The sample is dissolved in the solvent mixture


consisting of toluene, isopropanol (IPA), and CO2-
free water. Then the sample is titrated with
standardized potassium hydroxide in isopropanol
until after the equivalence point is reached.

After each sample determination, the electrode


needs to be rinsed with solvent solution, then IPA,
followed by a rehydration of the glass membrane in
deionized water. Afterwards, the electrode is briefly
dipped in IPA to remove any adhering water. Figure 2. Example titration curve of the acid number
determination of motor oil.

SUMMARY

Fully automated determination of the acid number


of petroleum products according to ASTM D664 and
IP 177 can be achieved using a Metrohm OMNIS
system. Using an OMNIS Sample Robot allows the
fully automated titration of up to four samples in
parallel. The OMNIS platform offers the opportunity
to customize your system according to your need
and expand it for other required titration
Titration Application Note T-096, Version 3 – 2020-07

applications.

Figure 1. Sample Robot and OMNIS Titrator Advanced equipped Analytes: Acid number, TAN
with a Solvotrode easyClean for the determination of the acid Matrix: Lubricants, coolants,
number of lubricating and motor oil.
cutting fluids; Mineral oils;
AW TI CH1-1238-122016

Fuels – fossil
Method: Titration
Industry: Petrochemicals & biofuels
Standards: ASTM D664; IP 177

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