TEST METHOD OF HYDRAZINE

(B) TITRIMETRIC
1.

SCOPE
This method covers the estimation of hydrazine of high concentrations.

2.

APPLICATION
Boiler water during wet preservation and hydrazine solution as purchased.

3.

PRINCIPLE
Hydrazine reacts with potassium iodate in strong acid medium as follows:
IO-3 + N2H4 + 2H+ + Cl- ICl + N2 + 3H2O

A known volume of hydrazine solution containing few ml of immiscible solvents like

chloroform or carbon tetra chloride is titrated with standard potassium iodate. The end
point is the disappearance of violet colour from the solvent.
4.

REAGENTS
(i)

(ii)

Potassium Iodate Solution 0.1M (0.4 N)

Weigh accurately 21.4 gm of pot. iodate, previously dried at 120 oC for 1
hour into a clean 1000 ml standard measuring flask. Dissolve and make up
to the mark with deionised water.
Potassium Iodate Solution (0.02 N)
Pipette out 25 ml of the above solution into a 500 ml standard measuring
flask and make up to the mark with deionised water.

(iii) Hydrochloric Acid A.R.(conc.)

(iv) Solvents CCl4 or CHCl3
5.

APPARATUS
Burette, Pipette, 250 ml reagent bottle or a narrow neck conical flask, etc.
6.

PROCEDURE

6.1 For Hydrazine Solution as Purchased

i)

Weigh out accurately about 5.0 gms of N2H4 solution into a 500 ml standard
measuring flask, make up to the mark and mix well.

Created by
KR.VEERAPPAN,LPS,SHARJAH,u.a.e./Asst.Manager,
TCPLKR.VEERAPPAN,LPS,SHARJAH,u.a.e./Asst.Manager,
TCPL

ii)

Pipette out 20 ml of sample into a 250 ml reagent bottle or conical flask.

iii) Add 30 ml of conc. HCl.

iv) Add 5 ml of CCl4 or CHCl3.
v)

Titrate against 0.4 N pot. iodate with gentle shaking until the organic layer is just
decolourised. Note down the titre value.

6.1.1 CALCULATIONS
% by wt. of N2H4 as N2H4 = V1 N1 x 8.011 x 100
V2 x W x 2
W = wt. of N2H4 solution taken, gram.
V1 = Titre value, ml.
V2 = Vol. of the N2H4 solution taken, ml.
N1 = Normality of KIO3.
The above eqn. can be written as:
V1 x 0.4 x 8.011 x 100 = V1 x 8.011
20 x 2 x W
W
6.2 For Boiler Wet Preservation Water
Follow steps ii to iv as in 6.1 and titrate against 0.02 N KIO 3 as described in
6.1(v).
6.2.1 CALCULATIONS
ppm N2H4 as N2H4 = V1 N1 x 8011
V2
V1 = Vol. of KIO3 , ml.
N1 = Normality of KIO3.
V2 = Vol. of boiler water taken , ml.
To report as N2H4.H2O multiply the N2H4 conc. by 1.56
REFERENCE
VOGELS Textbook of Quantitative Inorganic Analysis.
Note
The advantage of this method over the iodimetric method which is used at present, is
that the end point is sharp. Iodimetric method can still be used.

Created by
KR.VEERAPPAN,LPS,SHARJAH,u.a.e./Asst.Manager,
TCPLKR.VEERAPPAN,LPS,SHARJAH,u.a.e./Asst.Manager,
TCPL