Part -1: - Caustic solution analysis: (For the solution formed in reactor)
1) Weight about 2.0 to 3.0 grams of test sample into a 250 ml conical flask, containing 50 ml of
Distilled water.
2) Note down the weight of sample taken (W).
3) Add 100 ml of Distilled water and swirl the conical flask to dissolve the contents.
4) Add 3-4 drops of Phenolphthalein indicator solution.
5) Note down the initial burette reading (A).
6) Titrate the contents of the flask with 1.0 N of Hydrochloric Acid solution until the colour of
the solution changes from pink to colour-less which indicates the end point.
7) Note down the final burette reading (B).
8) The difference between (A) and (B) gives the volume, mark it as TV.
% Caustic in sample = TV × N × 40 × 100W × 1000
Where,
TV = Titer value of 1.0 N Hydrochloric Acid.
N = Normality of 1.0 N Hydrochloric Acid Solution.
W = Weight of sample taken in grams.
Part -2: - 30% SMO (Sodium Methoxide) solution Analysis:
A) Moisture Content:
1) Fill the titration vessel with 30 to 40 ml of methanol and add 5 to 10 ml of glacial acetic
acid.
2) Switch on the instrument and press the start button to neutralize the methanol and glacial
acetic acid medium using Karl Fischer reagent.
3) Again, press start button, when the sound of buzzer is heard.
4) Add about 2 to 3 grams of sample and transfer it into titration vessel.
5) Note down the titer value (TV), when the beep sound is heard.
6) Calculate the moisture content of the test sample by the following formula.
Moisture Content (%w/v) = (T.V. × KFR × 100) / (W × 1000)
Where,
T.V. = Titer value of KF solution.
KFR = Karl Fischer Reagent Factor.
W = Weight of sample taken in grams.
B) %Free Alkali as NaOH:
C) Determination of Sodium Carbonate Contents :
1) Weight about 2.0 to 3.0 grams of test sample into a 250 ml conical flask, containing 50 ml
of Distilled water.
2) Note down the weight of sample taken (W).
3) Add 100 ml of Distilled water and swirl the conical flask to dissolve the contents.
4) Add 2-3 drops of Methyl Orange indicator solution.
5) Note down the initial burette reading (R1).
6) Titrate the contents of the flask with 0.2 N of Hydrochloric Acid solution until the colour of
the solution changes from yellow to orange which indicates the end point.
7) Note down the final burette reading (R2).
8) The difference between (R1) and (R2) gives the volume, mark it as T2.
% Sodium Carbonate = (T2 × N × 53.06 × 100) / (W ×1000)
Where,
T1 = Titer value of 0.02 N Hydrochloric Acid.
N = Normality of 0.02 N Hydrochloric Acid Solution.
W = Weight of sample taken in grams.
D) Determination of Assay as Sodium methoxide:
1) Weight about 2.0 to 3.0 grams of test sample into a 250 ml conical flask, containing 50 ml
of Distilled water.
2) Note down the weight of sample taken (W).
3) Add 100 ml of Distilled water and swirl the conical flask to dissolve the contents.
4) Add 3-4 drops of Phenolphthalein indicator solution.
5) Note down the initial burette reading (I).
6) Titrate the contents of the flask with 1.0 N of Hydrochloric Acid solution until the colour of
the solution changes from pink to colour less which indicates the end point.
7) Note down the final burette reading (F).
8) The difference between (F) and (I) gives the volume, mark it as T1.
% Total Alkali as methoxide = (T1 × N × 54.04 × 100) / (W × 1000)
Where,
T1 = Titer value of 1.0 N Hydrochloric Acid.
N = Normality of 1.0 N Hydrochloric Acid Solution.
W = Weight of sample taken in grams.
% Sodium Methoxide = % Total Alkali as methoxide - % Free Alkali as NaOH - % Sodium Carbonate