The idiometric test to differentiate Pure & Hybrid polyurea.This will help to eliminate poor quality polyurea at the material stage itself.

1. Thermo. Titr. Application Note No. H-059
Title: Determination of Amines by Non-Aqueous
Titration
Scope: Determination of amines in non-aqueous media.
Principle: Dissolution of the amine in glacial acetic acid, and titration
with standard 0.1mol/L perchloric acid using
hydroxyacetone (acetol) as a thermometric endpoint
indicator.
Reagents: Titrant: 0.1mol/L perchloric acid in glacial acetic acid (BDH
Cat. No.190934T .
Endpoint indicator: Hydroxyacetone (acetol) - Aldrich Cat.
No. 138185-100G
Solvent: Glacial acetic acid - Ajax Univar
Test substance: Piperidine (hexahydropyridine) - Fluka
Cat. No. 80640, stated ≥99.0% (GC)
Method: Basic Experimental Parameters:
Titrant delivery rate (mL/min.) 2
No. of exothermic endpoints 1
Data smoothing factor (DSF) 60
Stirring speed (802 stirrer) 8
A test solution of ~0.1mol/L was prepared by accurately
weighing ~1.7g piperidine in a 200mL volumetric flask, and
making to volume with glacial acetic acid. For highest
precision, aliquots between 1 – 5mL were dispensed with
a 10mL Dosino burette into a vessel containing 30mL
glacial acetic acid. A 1mL dose of acetol was added to the
vessel immediately prior to the commencement of the
titration.
Example: Purity of piperidine
100.3 ± 0.12% (n=7) – the substance is also reported to
contain ~0.3% pyridine, which may be anticipated to
enhance the result
1

2. Calculations:
((Titre, mL − blank, mL ) × HClO4 mol / L × 85.15)
C5H11N % =
(aliquot, g)
Thermometric Titration Plot:
Legend:
Red = solution
temperature curve
Black =second derivative
curve (for endpoints)
Titration of piperidine
Determination of blank:
Blank determination - amines by non-aqueous titration
5.5
5.0
4.5
mL 0.1 mol/L HClO4
4.0 y = 1.01013x + 0.03400
R2 = 1.00000
3.5
3.0
2.5
2.0
1.5
1.0
1.0 2.0 3.0 4.0 5.0
mL piperidine solution
2