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
Urea properties:
CO(NH2)2
60.06 g/mol
factor : 2
Precipitation Method is Also called?
Argentometric titration
Volumetric methods based on
reactions that yield ionic
compounds of limited
solubility
Argentometric titration
primary analyte use to find Argentometric titration is ???
Chlorine/ Halides
Common titrant use in Argentometric titration?
Silver Nitrate