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.
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
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
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%
