CYCLE - I Experiment No: 1

ESTIMATION OF DIFFERENT TYPES OF ALKALINITY IN WASTE WATER

SAMPLE
Experiment No. : 1 Date: 18/07/2016

Principle:

Alkalinity in water is due to the presence of OH-, CO32- and HCO3- ions. The alkalinity of a
given sample of water can be obtained by neutralizing the above mentioned ions with standard
HCl. Titrating the given sample of water at a pH of 8.3 or till the pink color (which appears on
addition of Phenolphthalein indicator) disappears will indicate the complete neutralization of
OH- ions and half of CO32- ions. Titrating the same sample of water at a pH of 4.4 or till a sharp
color change from yellow to orange of methyl orange indicator will indicate the total alkalinity
i.e. the amount of OH-, CO32- and HCO3- present in the given sample

OH H H 2 O

CO32 H HCO3

HCO3 H [ H 2CO3 ] H 2O CO2

OH- and HCO3- ions cannot exist in water together because they combine instantaneously to form
CO32- ions.
OH HCO3 CO32 H 2O

NaOH NaHCO3 Na2CO3 H 2O

It is for this reason, the three ions OH-, CO32- and HCO3- cannot exist together.

Requirements
Reagents and solutions:
Standard solutions of sodium carbonate (0.1N), hydrochloric acid (0.1N), waste water
sample, methyl orange and phenolphthalein indicator solutions.
Apparatus: Burette, pipette, conical flask, standard flask and burette stand

Procedure
Titration I: Standardization of hydrochloric acid
Pipette out 20 mL of standard sodium carbonate solution (0.1 N) into a clean 250 mL conical
flask. Add 2 or 3 drops of methyl orange indicator to it. Titrate this mixture against hydrochloric
acid taken in the burette. The end point of the titration is indicated by the colour change from
yellow to orange. Repeat the titration for concordant titre values. From the titre value the
strength of hydrochloric acid is calculated.

Titration II: Estimation of Alkalinity

Transfer the given sample of water sample solution in a clean 100mL standard flask and make up
to the mark using distill water. Pipette out 20 mL of the given water sample into a clean 250 mL
conical flask. To this add 2 drops of phenolphthalein indicator and titrate the solution against
HCl taken in the burette. The end point is disappearance of pink colour. The corresponding
burette reading is noted and it is denoted as phenolphthalein end point [p].

To the same solution, add two drops of methyl orange indicator and continue the titration. The
end point is color change from pale yellow to orange. This end point indicates complete
neutralization of alkalinity present in water sample and is known as methyl orange end point [m].
Repeat the titration for concordant titre values.
 OBSERVATION AND CALCULATIONS
Titration I - Standardization of hydrochloric acid
Burette: HCl solution
Conical Flask: 20 mL of sodium carbonate + 2 drops of methyl orange
End point: Yellow to orange-red

S. No. Volume of Na2CO3 (mL) Burette reading (mL) Volume of HCl

(V1) Initial Final (V2, mL)
1 20 0 19.2 19.2
2 20 0 19.1 19.1
3 20 0 19.1 19.1
Concordant titre value 19.1

Volume of Standard sodium carbonate (V1) = 20 mL

Strength of Standard sodium carbonate (N1) = 0.1 N
Volume of HCl(V2) = 19.1 mL
Strength of HCl (N2) = ?
V1N1 = V2N2
V1N1
N2 = ---------------- = (20*0.1)/19.1 N
V2

The strength of HCl (N2) = 0.1047 N

Titration II: Estimation of Alkalinity

Concordant
Burette reading (mL)
Volume value (mL)
of Water Final
S. No.
Sample At At
Initial [p] [m]
(mL) phenolphthalein methyl orange
end point [p] end point [m]
1 20 0 9.1 12.5
2 20 0 8.8 12.1 8.8 12.1
3 20 0 8.9 12.2
4 20 0 8.8 12.1 8.8 12.1

Phenolphthalein alkalinity (mg/L) as CaCO3

 [P] mL of HCl X Normality of HCl X 50 X 1000
= -------------------------------------------------------------------
Volume of water sample taken

= (8.8*0.1047*50*100)/20

= 230.34 ppm [P]

Methyl orange alkalinity (mg/L) as CaCO3 (Total alkalinity)

[M] mL of HCl X Normality of HCl X 50 X 1000

= -----------------------------------------------------------------
Volume of water sample taken

= (12.1*0.1047*50*100)/20

= 316.72 ppm [M]

ALKALINITY TABLE:

Volume of p Alkalinity due to

and m (mL) OH- CO32- HCO3-
[p] = 0 0 0 [M]

[p] = [m] [M] 0 0

[p] = [m] 0 2[P] 0

[p] > [m] 2[P] - [M] 2[M] - 2[P] 0

[p] < [m] 0 2[P] [M] 2[P]

Result
The given water sample contains OH- and CO32- ions.

Amount of OH- alkalinity = 230.34 ppm [P] ppm

Amount of CO32- alkalinity = 316.72 [M] ppm

Total alkalinity or methyl orange alkalinity of the water sample

547.06 ppm

Evaluation of result

Sample Experimental Actual Value Percentage of Marks awarded

number value error