Chemline India Determination of Acidity / Acid value by

Limited titration method.

Page 1 of 7 REV: 1.0 DT: 01/03/2013 REF. NO. RM/STP-

004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

Part-A :- Determination of Acidity / Acid value by titration method - General

Part-B :- For Nitrocellulose

Part-C :- For Hexane

Part-D :- For Maize Starch

Part-E :- For Rosins

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PART-'A'

Title : Determination of Acidity / Acid value by titration method.

Principle : Acid value : A number or value which indicates the amount of

acid present in a substance. It is expressed by the number of
miligrams
of KOH required to neutralize the free acid in one gram of
sample.

Summary : Known amount of sample is dissolved in specified neutral

solvent such
as water or IPA and treated against std. NaOH of specified
strength
using specified indicator such as Bromo Thymol blue or
Phenolphthalein.

Scope : Acid value is required to be determined for following classes of

products. Monomers, Plasticizers, Emulsifiers, Solvents,
Chloroparaffin or any other item for which the test is referred
in specs.

Procedure :
Apparatus : Conical flask (250 ml), Burette (50 ml), Weighing balance (1
mg).
Chemline India Determination of Acidity / Acid value by
Limited titration method.

Page 2 of 7 REV: 1.0 DT: 01/03/2013 REF. NO. RM/STP-

004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

Reagents : Neutral distilled water or neutral IPA, NaOH soln. (0.02N &
0.1N),
Bromothymol blue or Phenolphthalein indicator.

Details : 1) Take 25 g of sample or as required, in a prewashed (with

neutral solvent)
and dry 250 ml conical flask.

2) Add 25 ml of neutral water for all samples excluding MOM

or
MIOM. Use 50 ml of IPA for MOM or MIOM. Neutral water
is
prepared freshly by neutralising distilled water with 0.02N
NaOH
using Bromothymol indicator.

3) Add 2 to 4 drops of Bromothymol blue indicator.

4) Titrate against 0.02N NaOH solution with end point from

yellow
to blue.

5) Note the burette reading and calculate as follows.

6) Calculation :
Acidity in ppm = V x N x E x 1000
W

Acid Value = V x N x E
W
Where,
V = ml of NaOH solution required.
N = Normality of NaOH solution.
E = Eq.Wt. of KOH = Mol.Wt./1 = 56.1
W= Weight of sample.
Reference :- CIL Internal method

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Chemline India Determination of Acidity / Acid value by
Limited titration method.

Page 3 of 7 REV: 1.0 DT: 01/03/2013 REF. NO. RM/STP-

004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

PART 'B' ---- For Nitrocellulose

1) Weigh 2 g of dried Nitrocellulose in a clean,dry 250ml stoppered

conical
flask.
2)Add 90 ml of acetone,stopper the flask & shake well till
nitrocellulose dissolves.

3) Add 10ml of distilled water , shake the flask to dissolve any

precipitated
Nitrocellulose.
4) Add 0.5ml mixed indicator(Neutral Red & Bromocresol green)
and the
solution is titrated with 0.01N NaOH until green colour appears.
5) A blank titration is carried out using 90 ml of Acetone,10ml of
Distilled water &
0.5ml of the indicator.
6) Calculation
( A- B ) x 0.49 x C
Acidity as % H2SO4 = ------------------------
W
Where
A = ml of 0.01 N NaOH for
Sample
B = ml of 0.01 N NaOH for
Blank
C = Normality of 0.01 N NaOH
W = Weight of Sample .

Reference :- CIL Internal method

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PART -'C'-- FOR HEXANE

Subject: Test Method for determination of Acid value of Hexane by titration

method.
Chemline India Determination of Acidity / Acid value by
Limited titration method.

Page 4 of 7 REV: 1.0 DT: 01/03/2013 REF. NO. RM/STP-

004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

Scope : This method is applicable for determination of acid value in Hexane or

any other item
for which the test is referred in specs.

Apparatus : Clean and dry Erlenmeyer Conical flask (250 ml & 500 ml), Burette
(50 ml),
Weighing Balance (1 mg).

Reagents: IPA (AR grade), 0.01N alcoholic KOH soln (Note : Normality of
alcoholic KOH
shall be verified just before use), Phenolphthalein indicator.

Procedure :-
A) Neutralization of IPA:
1) Take 100 ml of IPA in a clean and dry 500 ml conical flask.
2) Add 0.5 ml of Phenolphthalein indicator.
3) Titrate carefully with 0.01 N alcoholic KOH (drop wise near the end point),
till
colour changes from colourless to pink. (colour should remain for about 30
secs)

B) Acid value titration:

1) Weigh 250 ml conical flask with stopper (W-1 grams).
2) Take 25 ml of Hexane, stopper it and weigh (W-2 grams).
3) Add quickly, 75 ml of neutralized IPA and mix well. (Phenolphthalein
indicator is already
present in neutralized IPA)
4) Titrate carefully with 0.01 N alcoholic KOH (drop wise near the end point),
till colour changes from colourless to pink. (colour should remain for about
30secs)
5) Note the burette reading and calculate as follows.
6) Calculation:
Acid value = V X N X E
(W2-W1)

Where,
Chemline India Determination of Acidity / Acid value by
Limited titration method.

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004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

V = ml of KOH solution required.

N = Exact Normality of KOH solution.
E = Equivalent. Wt of KOH = Mol. Wt/1 = 56.10.
W1 = Weight of empty conical flask with stopper.
W2 = Weight of conical flask with sample.

Reference :- CIL Internal method

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PART -'D' - FOR MAIZE STARCH

Title : Determination of free acidity by titration method.

Principle : Free acidity: It is the value which indicates the amount of free
acid
present in a substance. It is expressed by the ml of 0.1 N NaOH
required
to neutralize the free acid in 10 grams of sample

Summary : Known amount of sample is throughly mixed with distilled

water and titrated
against std. NaOH of specified strength, using Phenolphthalein
indicator.

Scope : This method is applicable to maize starch or any other item for
which the test is referred in specs.

Procedure :
Apparatus : Conical flask (250 ml), Burette (50 ml), Weighing balance (1
mg).

Reagents : Neutralised Distilled water, NaOH soln. (0.1N), Phenolphthalein

indicator.
Chemline India Determination of Acidity / Acid value by
Limited titration method.

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004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

Details : 1) Take approx 10 g of sample (W g) in a dry 250 ml conical

flask.

2) Add 25 ml of freshly distilled & neutralised water and mix

thoroughly.

3) Add 2 to 4 drops of Phenolphthalein indicator.

4) Titrate against 0.1N NaOH solution with end point from

colourless to
light pink.

5) Note the burette reading (V ml) and calculate as follows.

6) Calculation :
Free acidity as 0.1 N NaOH = V X N X 100

Where,
V = ml of NaOH solution required.
N = Exact Normality of 0.1 N NaOH solution.
W = Weight of sample.
Reference :- CIL Internal method
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PART - E -- FOR ROSINS

Subject: Test Method for determination of Acid value of Rosins

Scope : This method is applicable for determination of acid value Rosins

Apparatus : Conical flask (250 ml & 500 ml), Burette (50 ml),
Weighing Balance (1 mg), Measuring cylinder 50 ml,

Reagents: IPA (AR grade), Tolune ( AR grade ), 0.01 N NaOH, 0.1 N alcoholic
Chemline India Determination of Acidity / Acid value by
Limited titration method.

Page 7 of 7 REV: 1.0 DT: 01/03/2013 REF. NO. RM/STP-

004
PREPARED BY : CHECKED BY: APPROVED BY :
MR. RAJESH GUPTA MR.SANJAY JHA MR.SS TUSHAR
Assistant Manager, Quality Manager,R&D AGM Operation

KOH soln
Phenolphthalein indicator,

Procedure :-
A) Neutralization of IPA + Tolune mixure
1) Make Tolune and IPA 1 : 3 mixture ( about 100 ml ) in 500 ml conical flask.
2) Add 0.5 ml of Phenolphthalein indicator.
3) Add 2-3 drops of 0.1 N alcoholic NaOH Solution
4)It gives pink colour.(This process is called previously neutralize)
5)Weigh accurately about 4gm of sample and transferred it in a 250 ml conical
flask(Neutralize solvent mixture)
6)Warm the solution and dissolve it completely.
7)When the solution cooled titrate . Titrate carefully with 0.1 N alcoholic KOH
( drop wise near the end point ),
till colour changes from colourless to pink. (colour should remain for about
30secs)

8) Note the burette reading and calculate as follows.

6) Calculation:
Acid value ( mgKOH / g ) = V X N X E
Weight of sample

Where,
V=ml of 0.1 N Alcoholic KOH solution required.
N=Exact Normality of 0.1 N Alcoholic KOH solution.
E= Equivalent Wt.of KOH = Mol.wt/l = 56.10
W= Weight of sample
Reference:-CIL Internal method