Determination of Total Acid Number (TAN) According To ASTM 664

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SI Analytics-Application report

Titration

Determination of Total acid number


(TAN) according to ASTM 664

Description
Determination of acidic compounds in petroleum products and lubricants by potentiometric titration.
The total acid number TAN is the quantity of base, expressed in milligrams of potassium hydroxide, which is
required to neutralize all acidic constituents in 1 g of sample. The titration is done in a mixture of toluene,
Isopropyl alcohol and water with KOH in Isopropyl alcohol. The use of Tetrabutylammonium hydroxide as
titrant is also possible.
The result is calculated as mg (KOH) / g.

Instruments
Titrator TL 7000 or higher
Electrode N 6480 eth
Cable L1A
Stirrer Magnetic stirrer TM 235 or similar
Lab accessory glass beaker 150 ml
Watch glass
Magnetic stirrer bar 30 mm

Reagents
1 KOH 0,1 mol/l in Isopropylalcohol
2 Toluene
3 Isopropyl alcohol
4 Distilled water
All reagents should be of analytical grade or better.

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Titration procedure
Reagents
KOH in Isopropyl alcohol 0.1 mol/l
It is recommended to use a ready 0.1 mol/l solution.
The solution must be protected against CO2 with a CO2 absorbent like soda lime.
The titer determination is done as described in the application note “Titer KOH”.

Solvent mixture
500 ml Toluene, 495 ml Isopropyl alcohol and 5 ml water are mixed in a bottle.

Cleaning of the electrode


For cleaning and conditioning of the electrode 3 steps are necessary:
First the electrode is rinsed with the solvent mixture to remove residues of the sample.
Then it is conditioned in water.
After the conditioning step the electrode is rinsed with solvent mixture to remove the water.
The electrode is stored in a solution of 1.5 mol/l LiCl in Ethanol (or, if another electrolyte is used, in this
electrolyte solution).

Blank value
For blank titration 125 ml solvent are placed in a 250 ml beaker and titrated with 0.1 mol/l KOH. The Blank
should be below 0.3 ml.

Sample preparation
The sample is weighed into a 250 ml beaker, dissolved in 125 ml of the solvent and titrated with 0.1 mol/l
KOH. The sample weight should be calculated and selected that the titration amount is not more than 4-5
ml because of the long titration time.
The required amount of sample can be estimated according to this rule of thumb:
20
𝑊(𝑔) =
𝑒𝑥𝑝𝑒𝑐𝑡𝑒𝑑 𝑇𝐴𝑁

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Titration parameter
Blank titration

Default method Blank TAN-TBN


Method type Automatic titration
Modus linear
Measured value mV
Measuring speed / drift User defined Fixed delax time 12 s
Initial waiting time 10 s
Linear Steps 0.01 ml
Damping strong Titration direction decrease
Pretitration off Delay time 0s
End value off
EQ On (1) Slope value 60
Max. titration volume 10 ml
Dosing speed 100% Filling speed 30 s

Calculation:
𝑚𝑙 = 𝐸𝑄1

The result is saved in a global memory, e.g. M01. We recommend to use statistics = 3.

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Sample titration

Default method TAN ASTM 664


Method type Automatic titration
Modus linear
Measured value mV
Measuring speed / drift User defined Minimum holding time 7s
Maximum holding time 20 s
Measuring time 4s
Drift 10 mV/min
Initial waiting time 10 s
Linear Steps 0.05 ml
Damping strong Titration direction decrease
Pretitration off Delay time 0s
End value off
EQ On (1) Slope value 120
Max. titration volume 6 ml
Dosing speed 100% Filling speed 30 s

For samples with very low TAN values the linear steps can be reduced to 0.02 or 0.01 ml.

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Calculation:

(𝐸𝑄1 − 𝐵) ∗ 𝑇 ∗ 𝑀 ∗ 𝐹1
𝑇𝐴𝑁 [𝑚𝑔(𝐾𝑂𝐻)/𝑔] =
𝑊 ∗ 𝐹2

B M01 Blank value, saved in global Memory M01


EQ1 Consumption of titrant at first Equivalence point
T WA concentration of the titrant
M 56,11 Molecular mass
W man Weight of the sample in g
F1 1 Conversion factor
F2 1 Conversion factor

Any questions? Please contact the application team:

Xylem Analytics Germany Sales GmbH & Co. KG, SI Analytics


Hattenbergstraße 10
D-55122 Mainz, Germany
Telefon: + 49 6131 66 5126
Fax: + 49 6131 66 5101
E-Mail: titration@si-analytics.com

Xylem Analytics Germany Sales GmbH & Co. KG · Hattenbergstr. 10 · D-55122 Mainz ·
Germany Telefon: +49 6131.66. 5111 · E-Mail: Info.si-analytics@Xyleminc.com · www.si-
analytics.com

Alle Namen sind eingetragene Handelsnamen oder Warenzeichen der Xylem Inc. oder eines seiner
Tochterunternehmen. Technische Änderungen vorbehalten.
© 2018 Xylem Analytics Germany Sales GmbH & Co. KG.

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