Tan Astm D 974 en

SI Analytics-Application report
Titration
Determination of Acid Number by Color-

Indicator Titration (ASTM D 974)
Description
The determination described in this report is based on the standard ASTM D 974.
Instruments
Titrator TL 7000 or higher
Interchangeable unit WA 10
Electrode OptiLine 6
Stirrer Magnetic stirrer TM 235
Lab accessory Glass beaker 150 ml
Magnetic stirring bars
Balance
Reagents
1 KOH in 2-propanol, 0.1 mol/L
2 Toluene
3 2-Propanol
4 Deionized water
5 p-Naphtholbenzein indicator solution
6 Potassium acid phthalate
8 Phenolphthalein indicator solution
All reagents should be of reagent grade or better.
TAN ASTM 974 -EN.docx 1/6

Standardization of Potassium Hydroxide Solution
The standardization can be carried out either potentiometric or colorimetric.
If a pH electrode is available. Please refer to the standard method Titer KOH and the application note “Titer
strong bases”.
The colorimetric indication is possible with phenolphthalein indicator solution. Weigh to the nearest 0.1 mg
approximately 0.1 g of potassium acid phthalate, which has been dried for at least 1 h at 110 °C and
dissolve in 80-100 mL of water, free of CO2. Add six drops of the phenolphthalein indicator solution and
titrate with linear titration steps to the inflection point. For highest accuracy repeat the titer determination
three times and calculate the mean value using the statistic function of the titrator
See the titration curve and method below.
Default method -
Method type Automatic Titration
Modus Linear
Measured value mV-E, 520 nm
Measuring speed / drift User defined Minimum holding time 05 s
Maximum holding time 15 s
Measuring time 3s
Drift 10 mV/min
Initial waiting time 10 s
Linear steps 0.05 ml
Damping None Titration direction decrease
Pretitration 6.00 ml Delay time 30 s
End value Off
EQ Off Slope value -
Max. titration volume 12 ml
Dosing speed 100% Filling speed 30 s

Calculation:
𝑊 ∗ 𝐹2
𝑇 [𝑚𝑚𝑚/𝑙] =
(𝐸𝐸 − 𝐵) ∗ 𝑀 ∗ 𝐹1
B 0 Blank value
W man Weight of the sample [g]
F2 1000 Conversion factor ml - l
EQ1 Consumption of titrant until first Equivalence point
M 204,22 Molecular mass
F1 1 Conversion factor
We recommend to store the exact concentration T into the exchangeable Unit (WA) automatically.
Titration solvent
Prepare by mixing toluene, water, and anhydrous isopropyl alcohol in the ratio 100/1/99.
Indicator solution
Prepare a solution of p-naphtholbenzein in titration solvent equal to 10 g/L.
Blank value determination
Perform a blank titration on 100 ml titration solvent and 0.5 mL of the p-Naphtholbenzein indicator solution.

Default method -
Modus Linear
Measuring time 4s
Drift 20 mV/min
Linear steps 0.02 ml
Pretitration off ml Delay time 0s
End value Off
Max. titration volume 0.3 ml
Calculation:
𝑅𝑅𝑅𝑅𝑅𝑅 𝑚𝑚 = 𝐸𝐸1
EQ1 Consumption of titrant at the first Equivalence point
The result is stored as global variable M01.
Sample titration
The sample is weight in into a 150 ml beaker. The amount of sample weight is adjusted to the expected
acid value.
Acid number (new Size of Sensitivity of

and Light oils) sample [g] Weighing [g]
0–3 20.0 +/- 2.0 0.05
Over 3 to 25 2.0 +/- 0.2 0.01
Over 25 to 250 0.2 +/- 0.02 0.001
Used or Dark-Colored Oils
0 to 25 2.0 +/- 0.2 0.01
Over 25 to 250 0.2 +/- 0.02 0.001
To the sample 100 ml of solvent and 0.5 ml of the indicator are added. Swirl until the sample is completely
dissolved. The color of the indicator must be yellow-orange. If the mixture assumes a green or green-black
color then the sample does not have any acid number and the base number can only be determined.
Immerse the OptiLine 6 and the titration tip (if not already happened) and start the titration method.

Default method -
Modus Linear
Measuring time 4s
Drift 20 mV/min
Linear steps 0.04 – 0.05 ml
Pretitration off ml Delay time 0s
End value Off
Max. titration volume 6 ml
Maybe use the manual stop!
Calculation:
(𝐸𝐸1 − 𝐵) ∗ 𝑇 ∗ 𝑀 ∗ 𝐹1
𝑅𝑅𝑅𝑅𝑅𝑅 [𝑚𝑚 𝐾𝐾𝐾/𝑔] =
𝑊 ∗ 𝐹2
B M01 Blank value

EQ1 Consumption of titrant at the first Equivalence point
T WA Actual Concentration of the titrant
M 56.1 Molecular weight
W man Sample weight in g
F1 0.1 Conversion factor 1
F2 1 Conversion factor 1

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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SI Analytics-Application report

Determination of Acid Number by Color-

TAN ASTM 974 -EN.docx 1/6

The standardization can be carried out either potentiometric or colorimetric.

See the titration curve and method below.

TAN ASTM 974 -EN.docx 2/6

Prepare a solution of p-naphtholbenzein in titration solvent equal to 10 g/L.

Blank value determination

TAN ASTM 974 -EN.docx 3/6

EQ1 Consumption of titrant at the first Equivalence point

The result is stored as global variable M01.

Acid number (new Size of Sensitivity of

TAN ASTM 974 -EN.docx 4/6

Maybe use the manual stop!

B M01 Blank value

TAN ASTM 974 -EN.docx 5/6

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

TAN ASTM 974 -EN.docx 6/6

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