Non – Aqueous Titration & KJELDAHL Method Flashcards
3 reason why Non – Aqueous Titration use
- Most organic acids and bases are insoluble in water
❖ Most organic acids and bases are weak acids and bases
❖ Moisture must be avoided or at least limited to 0.05%
Non – Aqueous Titration: Acid titrant
Perchloric acid in glacial acetic acid or dioxane
Non – Aqueous Titration: Base titrant
Sodium methoxide,
Lithium methoxide in
ethylenediamine, n-butylamine, morpholine
Non – Aqueous Titration: Indicators
ACIDIMETRY - Weak bases
common: Crystal violet
malachite green,
quinaldine red,
methylrosaniline
Non – Aqueous Titration: Indicators
ACIDIMETRY - (relatively stronger base)
Methyl orange, methyl red, Thymol blue
Non – Aqueous Titration: Indicators
ALKALIMETRY - (weak acids)
Azoviolet
Non – Aqueous Titration: Indicators
ALKALIMETRY - (strong acids)
Thymol blue
Non – Aqueous Titration: Indicators
ALKALIMETRY - (most preferred)
potentiometric methods
A method designed to determine and quantify ammonia in
ammonium sulfate obtained by decomposing organic
substance with sulfuric acid
Nitrogen determination
KJELDAHL Method
Standardization in Non-aqueous titration: __________ + Perchloric acid —->__________+_______
1: Potassium Hydrogen Phthalate
2: Phthalic acid
3: Potassium Chlorate
KJELDAHL Method: standard sol- H2SO4
Sx + H2SO4 (CUSO4, Se) —> (NH4)SO4 + H2O
formation of Ammonium Sulfate
What step is this ?
Step 1: Digestion
KJELDAHL Method: standard sol- NaOH
(NH4)SO4 + NaOH—> NH3 + Na2SO4 + H2O
formation of Ammonia
What step is this?
Step 2: Neutralization
KJELDAHL Method: standard sol- H3BO3 (boric acid)
NH3 + H3BO3—–> (NH4)2B4O7+H2O
formation of Diammonium Tetraborate
What step is this?
Step 3: Distillation
KJELDAHL Method: standard sol- HCl
(NH4)2B4O7+HCl —-> (NH4)Cl + H3BO3
formation of Ammonium chloride
What step is this?
Step 4: Titration
if N is as NO3, _______ is add
salicylic acid
- USP Methods
- Method I for ________
- Method II for _______
macroanalysis (1)
semimicroanalysis (2)
Kjeldahl set-up
heater
Digestion flask (step 1)
Trap [digestion of sample nitrogen converted to ammonia]
Condenser [Distillation of ammonia into a trapping solution]
trapping flask [quantification of the ammonia by titration w/ a standard solution]
% sample = (ml x N) acid - (ml x N) base x meq sample
—————————————— x 100
wt of sample
formula for – Acidimetric assay, Nitrogen determination
Nitrogen determination use in ?
Protein in food, fertilizer, blood, assays of Heparin,
insulin, urea, povidone