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DETERMINATION OF NITROGEN

REAGENTS:
 Liquid Humic Acid
 0.1 N Sodium hydroxide
 0.2 N Hydrochloric acid
 Methyl red indicator

PROCEDURE:
Take 5ml liquid humic acid in to a conical flask, and add 100 ml of standard 0.1 N NaOH
solution. Place a small inverted funnel in the neck of the flask and boil the mixture. Bring a
conc. HCl dipped glass rod near the mouth of funnel. If no white fumes appear then the
reaction has completed. Now cool the solution & makeup to 100ml. Take 10 ml of this solution
and titrate against standard 0.2 N HCl using methyl red as an indicator. Take concordant
readings.

REAGENTS PREPARATION:
(Preparation of 0.1 N NaOH)

Amount = Normality x Eq.wt x Volume


1000
Amount = 0.1 x 40 x 100 = 0.4 g
1000

To make 0.1 N NaOH solution, dissolve 0.4 g NaOH into 100 ml of water.

(Preparation of 0.2 N HCl)

M2 = 10 x density x purity
Mol.wt
M2 = 10 x 1.19 x 37 = 12.063 M
36.5
M1V1 = M2V2
0.2 x 1000 = 12.063 x V2
V2 = 16.58 ml

To make 0.2 N HCl, 16.58 ml conc. HCl is added in to 1000 ml water.


OBSERVATION:
Thar sample treat with HNO3
S#No Sample Volume of consumed HCl(ml)
1 2% KOH 6.6
2 4% KOH 6.5
3 6% KOH 6.6
4 2% NaOH 5.7
5 4% NaOH 8.7
6 6% NaOH 7.3
7 2% (KOH+NaOH) 7.3
8 4% (KOH+NaOH) 6.2
9 6% (KOH+NaOH) 9.3

Lakhra sample treat with HNO3


S#No Sample Volume of consumed HCl(ml)
1 2% KOH 4.8
2 4% KOH 5.7
3 6% KOH 6.4
4 2% NaOH 5.4
5 4% NaOH 7.0
6 6% NaOH 8.2
7 2% (KOH+NaOH) 6.8
8 4% (KOH+NaOH) 6.3
9 6% (KOH+NaOH) 9.4

Thar sample treat with H2SO4


S#No Sample Volume of consumed HCl(ml)
1 2% KOH 4.8
2 4% KOH 7.3
3 6% KOH 7.0
4 2% NaOH 5.5
5 4% NaOH 7.2
6 6% NaOH 5.2
7 2% (KOH+NaOH) 5.0
8 4% (KOH+NaOH) 6.8
9 6% (KOH+NaOH) 8.2
lakhra sample treat with H2SO4
S#No Sample Volume of consumed HCl(ml)
1 2% KOH 5.1
2 4% KOH 6.5
3 6% KOH 4.5
4 2% NaOH 6.3
5 4% NaOH 6.9
6 6% NaOH 6.0
7 2% (KOH+NaOH) 6.4
8 4% (KOH+NaOH) 7.2
9 6% (KOH+NaOH) 6.2

CALCULATION
(Sample # 01 Thar coal treat with 2% KOH and HNO3)
1000 ml of 1N HCl consumed by = 17.032g NH3
1000 ml of 0.2 N HCl consumed by = 17.032 x 0.2
X ml of 0.2 N HCl consumed by = (17.032)(0.2)(X) g NH3
1000
(From Titration HCl consumed = 6.6 ml)
So,
6.6 ml of 0.2 N HCl consumed by = 17.032 x 0.2 x 6.6 g NH3
1000
3.6 ml of 0.2 N HCl consumed by = 0.0225 g NH3
17 g NH3 14 g N
0.0225 g NH3 14 x 0.0225
17
0.0225 g NH3 0.01844 g N
So,
5ml humic acid contains = 0.01844 g N

% Nitrogen

Mass of 5ml humic acid = volume of humic acid x density


Mass of 5ml humic acid = 5x1.0009
Mass of 5ml humic acid = 5.0045
%Nitrogen = Mass of nitrogen in given sample x 100
Mass of given sample
%N = 0.01844 x 100
5.0045
%N = 0.368% N

Result:

Thar sample treat with HNO3


S#No Sample % of Nitrogen in 5ml humic acid
1 2% KOH 0.368
2 4% KOH 0.349
3 6% KOH 0.358
4 2% NaOH 0.313
5 4% NaOH 0.747
6 6% NaOH 0.388
7 2% (KOH+NaOH) 0.397
8 4% (KOH+NaOH) 0.313
9 6% (KOH+NaOH) 0.507

Lakhra sample treat with HNO3


S#No Sample % of Nitrogen in 5ml humic acid
1 2% KOH 0.269
2 4% KOH 0.316
3 6% KOH 0.349
4 2% NaOH 0.300
5 4% NaOH 0.383
6 6% NaOH 0.440
7 2% (KOH+NaOH) 0.371
8 4% (KOH+NaOH) 0.346
9 6% (KOH+NaOH) 0.519
Thar sample treat with H2SO4
S#No Sample % of Nitrogen in 5ml humic acid
1 2% KOH
2 4% KOH
3 6% KOH
4 2% NaOH
5 4% NaOH
6 6% NaOH
7 2% (KOH+NaOH)
8 4% (KOH+NaOH)
9 6% (KOH+NaOH)

Lakhra sample treat with H2SO4


S#No Sample % of Nitrogen in 5ml humic acid
1 2% KOH
2 4% KOH
3 6% KOH
4 2% NaOH
5 4% NaOH
6 6% NaOH
7 2% (KOH+NaOH)
8 4% (KOH+NaOH)
9 6% (KOH+NaOH)

Gravimetric analysis of humic acid


REAGENTS
 Liquid Humic Acid
 0.2 N Hydrochloric acid

PROCEDURE
Take 10ml humic acids in conical flask, an excess of 0.2 M HCl solution was added to precipitate.
The product was filtered after 24 hours and washed with distilled water. These products were
dried at 40 °C for 24 hours and then weighed, in order to calculate the extraction yield of humic
acids.
OBSERVATION:
Thar sample treat with HNO3
S#No Sample Weight of dried humic acid (gm)
1 2% KOH 0.5817
2 4% KOH 0.5742
3 6% KOH 1.3346
4 2% NaOH 0.5004
5 4% NaOH 0.2881
6 6% NaOH 0.2584
7 2% (KOH+NaOH) 0.5136
8 4% (KOH+NaOH) 0.9057
9 6% (KOH+NaOH) 0.6409

Lakhra sample treat with HNO3


S#No Sample Weight of dried humic acid (gm)
1 2% KOH 0.0483
2 4% KOH 0.1723
3 6% KOH 0.0408
4 2% NaOH 0.1045
5 4% NaOH 0.0412
6 6% NaOH 0.0691
7 2% (KOH+NaOH) 0.0660
8 4% (KOH+NaOH) 0.1650
9 6% (KOH+NaOH) 0.1354

Thar sample treat with H2SO4


S#No Sample Weight of dried humic acid
(gm)
1 2% KOH 0.3507
2 4% KOH 0.2333
3 6% KOH 0.4528
4 2% NaOH 0.2050
5 4% NaOH 0.1650
6 6% NaOH 0.3820
7 2% (KOH+NaOH) 0.2345
8 4% (KOH+NaOH) 0.2488
9 6% (KOH+NaOH) 0.2817

Lakhra sample treat with H2SO4


S#No Sample Weight of dried humic acid (gm)
1 2% KOH 0.0242
2 4% KOH 0.0740
3 6% KOH 0.0258
4 2% NaOH 0.0251
5 4% NaOH 0.0927
6 6% NaOH 0.0628
7 2% (KOH+NaOH) 0.0412
8 4% (KOH+NaOH) 0.0355
9 6% (KOH+NaOH) 0.0890

CALCULATION
(Sample # 01 Thar coal treat with 2% KOH and HNO 3)
Mass of 5ml humic acid = volume of humic acid x density
Mass of 5ml humic acid = 10x1.0009
Mass of 5ml humic acid = 10.009gm

%content of humic acid:


%content of humic acid = weight of dried hmic acid x 100
Taken weight of liquid humic acid
%content of humic acid = 0.5817 x 100
10.009
%content of humic acid = 5.811%

Result:
Thar sample treat with HNO3
S#No Sample %content of humic acid
1 2% KOH 5.811
2 4% KOH 5.476
3 6% KOH 12.94
4 2% NaOH 4.897
5 4% NaOH 4.408
6 6% NaOH 2.451
7 2% (KOH+NaOH) 4.995
8 4% (KOH+NaOH) 8.622
9 6% (KOH+NaOH) 6.252

Lakhra sample treat with HNO3


S#No Sample %content of humic acid
1 2% KOH 0.483
2 4% KOH 1.705
3 6% KOH 0.396
4 2% NaOH 1.035
5 4% NaOH 0.402
6 6% NaOH 0.661
7 2% (KOH+NaOH) 0.642
8 4% (KOH+NaOH) 1.615
9 6% (KOH+NaOH) 1.335

Thar sample treat with H2SO4


S#No Sample %content of humic acid
1 2% KOH
2 4% KOH
3 6% KOH
4 2% NaOH
5 4% NaOH
6 6% NaOH
7 2% (KOH+NaOH)
8 4% (KOH+NaOH)
9 6% (KOH+NaOH)

Lakhra sample treat with H2SO4


S#No Sample %content of humic acid
1 2% KOH
2 4% KOH
3 6% KOH
4 2% NaOH
5 4% NaOH
6 6% NaOH
7 2% (KOH+NaOH)
8 4% (KOH+NaOH)
9 6% (KOH+NaOH)