Austin Community College Chemistry

Saul Sanchez Experiment 8

Title: Determination of Hardness of Water

Goal: To determine the [Ca2+] in a water sample. The units of [Ca2+] are ppm = parts per million,
where: 1 ppm = 1 g CaC03/1 million g H20 or 1 mg CaC03/1 L H20

We will standardize a solution of EDTA (ethylenediaminetetraacetic acid) by titration against a standard

solution made from CaCO3 to determine the hardness of an unknown water sample.
Since both are colorless, we will use Calmagite as an indicator, MgLn - with Mg2+ ion. The titration’s end-
point is determined by a sky blue color in the solution.
It contains six donor atoms (underlined) that form a complex ion with Ca 2+. One Ca reacts with one
EDTA.

Procedure:

1) Get a 50 ml buret, a 250 ml flask, and 25 and 50 ml pipets from the stock room.
2) Put 0.5 g of CaCO3 in a 50 ml beaker and weigh the beaker and contents.
3) Use a spatula to transfer about 0.4 g of the carbonate to a 250 ml beaker and weigh.. Determine the
sample mass by difference.
4) Add 25 ml of distilled water to the 250 ml beaker and slowly drop 40 drops of 6 M HCL.
5) Cover the beaker with the beaker with a watch glass and allow the reaction to produce until it
dissolves completely.
6) Rinse the walls of the beaker with distilled water from your wash bottle and heat the solution until it
starts boiling.
7) Add 50 ml of distilled water to the beaker and transfer the solution, using a stirring rod as a pathway,
to the volumetric flask. Rinse the beaker with small portions of distilled water and transfer each
portion to the flask.
8) Fill the volumetric flask to the horizontal mark with distilled water, adding at least few ml of a drop
at a time with your wash bottle.
9) Stopper the flask and mix the solution by inverting the flask at least a dozen times, and shaking at
intervals for more than 5 min.
10) Clean your buret and draw about 200 ml of EDTA solution from the carboy into a dry 250 ml
Erlenmeyer flask. Rinse the buret with a few ml of the solution 3 times. Drain through the stopcock
and fill the buret with the EDTA solution.
11) Prepare reference solution by adding 50 ml of DI-water and 5 ml of pH 10 buffer to a 125 ml
Erlenmeyer flask. Add 8 drops of Calmagite indicator. The solution should turn sky blue.
12) Pipet a 25 ml aliquot of Ca2+ solution into a clean 125 ml Erlenmeyer flask. Add 5 ml of the pH 10
buffer and 8 drops of Calmagite indicator, which will cause the solution to turn red. Read the level in
the buret and add EDTA to the solution.
13) The End-point occurs where the last tinge of red disappears and the solution takes a color like that in
the reference. The reaction is slow so take your time.
14) Record the buret level at end-point Keep tour titrated solution as a reference for your next titration.
15) Refill your buret and titrate two more 25 ml aliquots of the calcium containing solution, using 5 ml og
pH 10 buffer and 8 drops of indicator.
16) Your instructor will furnish you a sample of water for hardness analysis. Pipet 50 ml of water sample
for each titration. Add 8 drops of indicator and 5 ml of pH 10 buffer before titrating.
17) Carry out as many titrations as necessary to obtain two volumes of EDTA that agree within about 3
percent. It takes at least 20 ml of EDTA to reach the end-point.