Experiment No.

3 Application of Tritrimetric Analysis

Experiment No. 3
Application of Titrimetric Analysis

Objectives

1. To prepare standard solutions for various type of titration.

2. To determine the amount of unknown from a sample using various titrimetric analysis

Reagents

Conc HCl EDTA

NaOH pellets Magnesium chloride hexahydrate
Distilled water (previously boiled and cooled) EBT indicator
Phenolphthalein indicator Unknown sample
KHP (primary grade) Water sample
CaCO3 (primary grade)
Methyl orange indicator

Apparatus

25-mL volumetric pipette Suction bulb

250-mL Erlenmeyer flask Watch glass
Analytical balance Burette
Hotplate Burette clamp

Procedure

Water Hardness Analysis by Complexometric Titration

1. Preparation and Standardization of EDTA (~0.005M)

a. Dissolve about 1.0 g of Na2H2Y2 H2O (372.24 g/mole) in 450 mL of distilled
water, 0.5 g of NaOH and 0.05g of MgCl2 6H2O. Dilute to 500 mL and mix well.
b. Transfer the solution to a labeled plastic storage bottle.
c. Weigh accurately 0.20 g to 0.25 g dried CaCO3 primary standard into a 200-
mL beaker.
d. Carefully add 5 mL of concentrated HCl solution to the sample. After dissolution
is complete and effervescence has ceased, add about 50 mL of distilled water,
rinsing down the sides of the beaker in the process.
e. Boil for 5 minutes to remove carbon dioxide and then cool.
f. Transfer the cooled solution and rinsing to a 500-mL volumetric flask and dilute
to mark with distilled water.
g. Pipet a 25.00-mL aliquot of this standard calcium solution into each of three
250-mL Erlenmeyer flasks, add 10.00 mL of ammonia buffer solution, and 2 to
3 drops of EBT indicator, and titrate until the first appearance of a clear blue
color. Ordinarily, the initial wine-red color slowly turns to purple and then

Page 1 of 2 Experiment 3 CM124-1L

 sharply to blue. All buret readings should agree to within 0.05 mL. If they do
not, repeat until you have three that do.
h. Calculate the molarity of your EDTA for each of the three titrations and calculate
the mean and the uncertainty based on 95% confidence level. Record in your
notebook.

2. Determination of water hardness

a. Acidify 100.0-mL aliquots of the sample water with a few drops of HCl, and boil
gently for a few minutes to eliminate CO2. Cool, add 3 to 4 drops of methyl red,
and neutralize with 0.1 M NaOH.
b. Pipet a 25.00-mL aliquot of this sample into each of three 250-mL Erlenmeyer
flasks, add 10.00 mL of ammonia buffer solution, and 3 to 4 drops of EBT
indicator, and titrate with the standardized EDTA solution until the first
appearance of a clear blue color. Ordinarily, the initial wine-red color slowly
turns to purple and then sharply to blue.
c. Calculate the water hardness as ppm CaCO3 for each of the three titrations and
calculate the mean and the uncertainty based on 95% confidence level. Record
in your notebook.

Page 2 of 2 Experiment 3 CM124-1L