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Acid Number of Insulating Oil: Acid Base Titration (Non Aqueous) by Automatic Potentiometric Titrator

The document discusses measuring the acid number of insulating oil through potentiometric titration. The acid number indicates the amount of potassium hydroxide in mg needed to neutralize 1g of oil and must be maintained within specifications. The test procedure involves titrating an oil sample with potassium hydroxide ethanol solution while monitoring the potential, with toluene-ethanol as the solvent. The acid number is calculated based on the titration volume and other parameters. Automatic potentiometric titration systems can provide stable, reliable measurements of insulating oil acid number.

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38 views4 pages

Acid Number of Insulating Oil: Acid Base Titration (Non Aqueous) by Automatic Potentiometric Titrator

The document discusses measuring the acid number of insulating oil through potentiometric titration. The acid number indicates the amount of potassium hydroxide in mg needed to neutralize 1g of oil and must be maintained within specifications. The test procedure involves titrating an oil sample with potassium hydroxide ethanol solution while monitoring the potential, with toluene-ethanol as the solvent. The acid number is calculated based on the titration volume and other parameters. Automatic potentiometric titration systems can provide stable, reliable measurements of insulating oil acid number.

Uploaded by

benlahneche
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Petroleum Acid number of insulating oil

Acid⋅base titration (non aqueous) by


Automatic Potentiometric Titrator
JIS C 2101 BS 14 8
Standard JPI-5S-57-99
ASTM D 974

1.Abstract
To maintain the acid number within specified level is the key of quality control of
the insulating oil. Acid number is expressed by potassium hydroxide in mg required to
neutralize free fatty acid in 1g of oil.

Measurement of acid number of insulating oil is specified in JIS-C2101 Test Method


for Electrical Insulating Oil and JPI-5S-57-99 Neutralization Test Method for
Electrical Insulating Oil – Total Acid Number Indicator Photometric Titration.

The oil sample is titrated with 0.05mol/L potassium hydroxide ethanol as reagent
and with toluene ethanol (3+2 ) as solvent and with alkali blue 6B ethanol, and the
endpoint is detected on titration curve. The acid number is calculated from the
titration volume of reagent reaching the endpoint.

2.Reference
１） JIS-C2101-1999 Test Method for Electrical Insulating Oil
２） JPI-5S-57-99 Japan Petroleum Institute - Neutralization Test Method for
Electrical Insulating Oil – Total Acid Number Indicator Photometric Titration
３） ASTM D974-06 Standard Test Method for Acid and Base Number by
Color-Indicator Titration
４） BS148-1998 Specification for unused and reclaimed mineral insulating oils for
transformers and switchgear

3.Cautions in measurement
１） The indicator of alkali blue 6B is hard to dissolve in ethanol, and needs to be
stirred more than 2 hours before titration.
２） The indicator is liable to change, and recommended to use within 2 days after
prepared.
３） Be aware the accuracy of measurement depends on the correct amount of
indicator when added during the process of titration.

4.Post-measurement care
No special note

上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Http://www.shxf17.com


Tel： 021-66581985，63172460 Fax： 021-66581986 周峰 13916388882 [email protected]
TIA-07019 Ver.01 1/4
5.Test equipment
Main unit：Automatic potentiometric titrator （Photometric preamplifier: PTA－）
Detector ：Photometric electrode 12-001-100-48（λ＝650nm）

6.Reagent
Reagent ： 0.05mo1/L potassium hydroxide・ethanol solution ( f=0.6823 )
Solvent ： Toluene + ethanol (3+2) mixture
Indicator ： Alkali blue ６B ethanol solution

7.Test procedure
―Preparation―
1) Obtain the factor of reagent using amide sulfuric acid.
2) Dissolve 0.1～0.2g alkali blue 6B in 100mL ethanol, and filtrate as indicator.
3) Calibrate transmissivity with 100mL solvent added with 3mL indicator and 2mL
reagent as 100%T, and with 100mL solvent added with 3mL indicator as 0%T
respectively.

―Measurement―
1) Transfer 20g sample to a 200mL beaker, and weigh it on a balance.
2) Add 100mL solvent and 3mL indicator.
3) Titrate with 0.05mol/L potassium hydroxide ethanol.
4) Perform a blank test in advance to obtain blank level.

8.Formula
Acid number ( mgKOH / g ) = ( EPl － BLl ) × TF × Cl × K1 / S
EPl ： Titration volume ( mL )
BLl ： Blank level ( 0.2999mL )
TF ： Reagent factor ( 0.6823 )
Cl ： Concentration conversion coefficient ( 56.l g/mL )
(equivalent to potassium hydroxide in 1mo1/L potassium hydroxide ethanol)
Kl ： Unit conversion coefficient ( 0.05 )
S ： Sample size ( g )

上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Http://www.shxf17.com


Tel： 021-66581985，63172460 Fax： 021-66581986 周峰 13916388882 [email protected]
TIA-07019 Ver.01 2/4
9.Example of measurement
－Ambient condition－
Room temperature：20.0 Humidity： 30 ％ Weather： Fair

The following parameters and titration curve were obtained by AT-610 titration system:
-Titration parameter- -Titration curve-
Model : AT-610
Method No. : 01
Titr.mode : Intermit
Titr.form : EP Stop

[Titration parameter] [Calculation parameter]

Burette No. : 1 Calc. Type : Sample


Max volume : 1.50 mL CO1 : On
Channel,Unit Unit : mgKOH/g
Ctrl. : Ch3,%T Formula :
Ref. : Off (EP1-BL1)*TF*K1*C1/S
pH polarity : EP position : EP1
Standard Decimal : 3 ***
Direction : Auto Fraction : Half adjust R e s u l t ***
Wait time : 0s Evaluation : Off Method No./Name :
Dose mode : None 01/MORITA
Active constant
C1 : 56.1 Sample No. : 01-01
[Control parameter] K1 : 0.05
Date : 2007/03/20 16:02
Number of EP : 1 Temp.comp. : off
End sense : Auto Titr.Reagent Name :
Gain : 1 0.05M KOH in EtOH
Data sampling : Set
Data sampling : Set Titr.time : 00:06:09
Data samp.pot. : 4.0 mV
Data samp.vol. : 0.05 mL Size : 20.0070 g
Ctl.speed mode : Set
Cut-off time : 10 s End point-1
Unit volume : 0.025mL Volume : 0.3287 mL
Disp speed : 1 s/mL Potential : -2.9 %T
Other control : Std.
Stir. Speed :3 Conc-1 : 0.003 mgKOH/g

Meaning of printout data:


≪Titration parameter≫
Burette No.: the burette used in titration / Max Volume: of titration
Channel,Unit: the detector used in potential detection and the unit of potential selected
pH polarity: direction of pH potential / Direction.: of titration / Wait Time: before titration starts
Dose mode: for fixed dose
≪Control parameter≫
Number of EP: number of endpoints detected / End sense: direction of EP sense / Gain: of detection signal
Data sampling: conditions / Ctl.speed mode: control speed mode
Other control: other controls / Stir. Speed: of stirrer during titration
≪Calculation parameter≫
Calc.Type: calculation type / CO1: concentration formula 1 /Unit: unit of calculation results
EP1: titration volume to reach EP1 / BL1: blank level / TF: factor of reagent
C1(mg/mL): concentration conversion coefficient / K1: unit conversion coefficient
S: sample size / EP position: for calculation / Decimal: number of digits after decimal point in calculation
Fraction: rounding fraction / Evaluuation: of calculation results

TIA-07019 Ver.01 3/4


－Measurement results－
Sample Titrated Acid number
n Statistics
(g) (mL) (mgKOH/g)
1 20.0070 0.3287 0.003 Mean 0.003 mg/g
2 20.0090 0.3228 0.002 SD 0.0006 mg/g
3 20.0096 0.3313 0.003 RSD 20.0 %
＊The above results were obtained from 3 tests of the same sample.
＊ Red underline shows the data from page 3/4.

10.Summary
Acid number is expressed by potassium hydroxide in mg required to neutralize free
fatty acid in 1g of oil. To maintain the acid number within specified level is the key of
quality control of the insulating oil.
The measurement results of the sample this time show a good repeatability.
The automatic potentiometric titration system provides stable and reliable
measurements. The acid number of insulating oil is measured by any of the models
shown below.

【AT-610】 【AT-510】 【AT-500N-1】

Awarded Product of Supreme • Compact and cost performance • Low cost and high performance
Technology from Kyoto City model • Easy view with back light LCD
• Easy key entry by touch panel of • PC card expands data memory for • GLP/GMP conformed model
large color LCD （8-inch wide） convenience and versatility.
• Simultaneous titration in parallel
• Both potentiometric and Karl
Fischer moisture titration
(coulometric・volumetric） can be
performed at a time.

上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Http://www.shxf17.com


Tel： 021-66581985，63172460 Fax： 021-66581986 周峰 13916388882 [email protected]
TIA-07019 Ver.01 4/4

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