Method ID: HI3606EN

Acid number according to ASTM D664

(Fixed end-point pH titration)

This is a method for the determination of the acidic

components of petroleum products. The titration is run Sample Analysis:
in non-aqueous media using 0.1 M KOH in 2-propanol
as titrant. The result is expressed as mg of KOH
necessary to titrate 1g of product. 1.Take oil Sample weight in 100mL beaker as given in
Reference: ASTM D664 table with respect to acid number
2.Add 60mL Solvent mixture in 100mL oil sample
Electrode: beaker .
3.Place the Beaker Assembly under stirrer assembly.
• HI 1049B Combination pH electrode 4.Start the titration
• HI 7662-T temperature probe 5.Once the titration completed Direct reading of Acid
Number mg/g KOH
Chemicals: 6..Record the reading
7.Remove pH electrode from sample from the sample
1.Toluene and rinse it with tiotration solventand then with distilled
2.Propanol water.
3.Distilled Water
4.KOH AR Grade
5.KHP(Potassium Hydrogen phthalate(AR) Grade Acid number Sample Accuracy of
weight (g) Weighing (g)
: 0.05 – 1.0 20.0  2.0 0.10
Preparation of Solvent Mixture: 1.0 – 5.0 5.0  0.5 0.02
5 – 20 1.0  0.1 0.005
Solvent mixture: Mix 500mL toluene, 495mL 2- 20 – 100 0.25  0.02 0.001
propanol, and 5mL of de-ionized water. 100 - 260 0.1  0.01 0.0005

Titrant: 0.1N KOH in 2-Propanol

Procedure:

Calibration of pH Electrode :
Calibrate pH electrode HI1049B in pH4, pH7 & pH10
Successively.

Standardinzation of 0.1N KOH in 2-Proanol:

1.Create method for standardization of 0.1N KOH

1.Prime/Fill the burette with 0.1N KOH give min.3
rinsing.
2.Accurately weigh 0.700gm Potassium Hydrogen
phthalate in 100mL weaker add 60mL water.
3.Keep the beaker under stirrer assembly and start the
titration.
4.Once the Titration Completd the Normality value of
KOH to be enter in TAN Method .

Blank Titration:

2.Take 60mL of Solvent mixture in 100mL beaker

3.Create method for TAN number.
4.Place the the beaker under stirrer assembly and start
the titration.
5.When the titration ends record the value of titrant
dispensed in L(Litre)
6.Add the Blank L value in blank Value in method
options of TAN Number.

Titrator Application Methods: Petroleum Methods - r. 1.0

 Method ID: HI3606EN

Acid number according to ASTM D664

(Fixed end-point pH titration)

Method Parameters: Results:

Name: Acid number EndPoint Titration Report
Method Revision: 1.0 Method Name: Acid number EndPoint
Titration Type: Standard Titration Time & Date: 12:24 August 31, 2009
Pump Configuration: Titration ID: Ti_00035
Titrant pump: Pump 1
Dosing Type: Dynamic Titration Results
Min Vol: 0.010 mL Method Name: Acid number EndPoint
Max Vol: 0.100 mL Time & Date: 12:24 August 31, 2009
delta E: 4.500 mV Analyte Size: 0.924 g
End Point Mode: Fixed 11.000 pH End Point Volume: 0.613 mL
Recognition Options: pH Fixed End Point: 11.000
Threshold: 300 mV/mL Results: 3.11325 mg/g
Range: NO Initial & Final pH: 5.629 to 11.710
Filtered Derivatives: NO Titration Duration: 7:08 [mm:ss]
Pre-Titration Volume: 0.000 mL Titration went to Completion
Pre-Titration Stir Time: 30 Sec Operator Name:
Measurement Mode: Signal Stability Analyst Signature: _____________________
delta E: 0.5 mV
delta t: 10.0 Sec
Min wait: 3 Sec
Max wait: 10 Sec
Electrode Type: pH
Blank Option: V - Blank
Blank Value: 1.0000E-4 L
Calculations: Sample Calc. by Weight
Dilution Option: Disabled
Titrant Name: KOH
Titrant Conc.: 0.1000 M (mol/L)
Analyte Size: 0.924 g
Analyte Entry: Manual
Maximum Titrant Volume: 7.000 mL
Stirring Speed: 1400 rpm
Potential Range: -2000.0 to 2000.0 mV
Volume/Flow Rate: 10 mL / 20.0 mL / min
Signal Averaging: 1 Reading
Final Result Format: X.XX

Calculations:
Calculations: Sample Calc. by Weight
Titrant units: M (mol/L)
Titrant Conc.: 0.1000 M (mol/L)
Titrant volume dosed: V (L)
Blank volume: 1.000E-4L
Analyte Size: 0.924 g
Sample/Titrant: 1.000 mol/mol
Mw of sample: 56.110 g/mol
mg/g = [(V-1.0E-4)*0.1*1*56.11*1000mg/g]/[g]

Titrator Application Methods: Petroleum Methods - r. 1.0