Experiment 5 (CHM421)

EXPERIMENT 5: DISTILLATION AND HARDNESS OF WATER
OBJECTIVES:
1) To purify water sample by distillation
2) To standardize EDTA solution
3) To analyze hardness of water samples by titration with EDTA solution
INTRODUCTION
This lab is concerned with hardness, which is the amount of divalent metallic cations in the
water. The primary causes of hardness are calcium (Ca +2) and magnesium (Mg+2) ions, but
other metals such as strontium, ferrous iron, manganous, aluminium, and ferric iron can also
contribute to hardness. Of these, ferric iron and aluminium ions tend to have little effect on
hardness in natural waters since they are not very soluble in water at natural pH levels. Since
the hardness in water primarily originates from contact with the soil and with rock
formations, hard waters tend to originate in areas where topsoil is thick and limestone
formations are present. Soft waters (those containing relatively little hardness) originate in
areas where the topsoil is thin and limestone formations are sparse or absent. In order for
hardness to enter water from the rocks and soil, the water must be somewhat acidic.
Rainwater usually has a neutral pH and is incapable of dissolving most solids in rocks and
soil, but carbon dioxide is released into the water by bacterial action as the water percolates
down through the soil. This carbon dioxide forms carbonic acid and makes the water acidic
and thus able to dissolve basic materials, such as limestone. Since limestone is primarily
composed of calcium carbonate, calcium is usually the largest cause of hardness in water.
But most limestone also has some impurities such as sulphates, chlorides, and silicates which
can also pass into solution as the carbonates dissolve away around them. It is easy to confuse
hardness with alkalinity because both are measured in ppm CaCO 3 and both often enter the
water from limestone. In fact, when limestone is the only cause of hardness and alkalinity in
water, the amount of alkalinity and hardness in the water should be about the same. To see
why, consider the following chemical equation:
CaCO3 Ca+2 + CO3-2

PROCEDURE
B) STANDARDISATION OF THE EDTA SOLUTION

1) A 50 ml burette was clean thoroughly and the insides was rinsed with distilled
water. Finally the burette was rinsed with the EDTA solution.
2) The EDTA solution was poured into the burette beyond the zero mark.
3) 25.0 ml aliquots of the prepared standard Ca2+¿ ¿ solution was pipetted and transferred to
a 250ml conical flask. The concentration of the CaCO3 was recorded.

4) 8ml of pH 10 ammonia-ammonium chloride buffer, 15ml of distilled water and 3 drops
of Eriochrome Black T indicator were added. Titrate the sample with EDTA solution
against a white tile background until the solution turns to sky blue. The volume of the
burette was recorded at the endpoint.
C) HARDNESS OF WATER
1) The burette was filled up with more EDTA solution.
2) A 25ml pipetted was rinsed with tap water and 25.0ml of lab tap water was pipetted into
a 250ml conical flask.

3) Similarly, 8ml of the ammonia-ammonium chloride and 3 drops of Eriochrome Black
were added into water sample in the flask. The initial burette reading was recorded to
nearest 0.01ml. The rate of the releasing the EDTA solution into the flask was slow
down when started to see the formation of blue colored solution.
4) The method was repeated for the rest of the samples; lab distilled water, home tap water,
distilled home tap water, deionized water, o.1M NaCl.

RESUTS AND CALCULATION
B. Standardization of the EDTA Solution

Concentration of standard Ca2+¿ ¿ solution = 0.007M
Volume of the standard Ca2+¿ ¿ solution = 0.025L
i. First Trial
0.007 mol Ca 2+¿

¿
2+¿ 1 mol EDTA
1 L Ca × ¿
2 +¿ 0.025 LCa2+ ¿
1 mol Ca × =0.0049 M ¿ ¿
0.0354 L EDTA
ii. Second Trial
0.007 mol Ca 2+¿

¿
2+¿ 1 mol EDTA
1 L Ca × ¿
2 +¿ 0.025 LCa2+ ¿
1 mol Ca × =0.0049 M ¿ ¿
0.0354 L EDTA
iii. Third Trial
0.007 mol Ca 2+¿

¿
2+¿ 1 mol EDTA
1 L Ca × ¿
2 +¿ 0.025 LCa2+ ¿
1 mol Ca × =0.0049 M ¿ ¿
0.0354 L EDTA
iv. Fourth Trial
0.007 mol Ca2 +¿

¿
1 mol EDTA
1 L Ca2+¿ × ¿
2 +¿ 0.025 LCa2+¿
1 mol Ca × =0.0050 M ¿ ¿
0.0353 L EDTA
v. Average Concentration of EDTA
0.0049 M +0.0049 M +0.0049 M + 0.0050 M

X́ = =0.004925 M
4
C. Hardness of Water
Concentration of EDTA = 0.004925M
Concentration of water samples:

i. Lab tap water (l.t.w)
2+ ¿
Mg 0.0019 L EDTA
2+¿ ×
0.004925 mol EDTA 1 mol EDTA 0.025 L Ca 2+ ¿Mg
2+¿
¿
¿
M l .t . w = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.0003743 M
ii. Lab distilled water (l.d.w)

2+ ¿
Mg 0.0008 LEDTA
2+¿ ×
0.004925 mol EDTA 1 mol EDTA 0.025 LCa2+ ¿Mg ¿ ¿
¿ 2+¿
M l .d .w = ×1 mol Ca ¿
1 L EDTA
¿ 0.0001576 M
iii. Home tap water (h.t.w)

2+ ¿
Mg 0.0017 L EDTA
2+¿ ×
0.004925 mol EDTA 1 mol EDTA 0.025 L Ca2+ ¿Mg ¿ ¿
¿ 2+¿
M h .t . w = ×1 mol Ca ¿
1 L EDTA
¿ 0.0003349 M
iv. Deionized water (d.i)

2+ ¿
Mg 0.001 L EDTA
2 +¿ ×
0.004925 mol EDTA 1 mol EDTA 0.025 LCa 2+ ¿Mg
2 +¿
¿
¿
M d . i= × 1mol Ca ¿
¿
1 L EDTA
¿ 0.0001970 M
v. 0.1M NaCl
2+ ¿
Mg 0.0036 LEDTA
2+¿ ×
0.004925 mol EDTA 1 mol EDTA 0.025 LCa 2+ ¿Mg
2+¿
¿
¿
M NaCl = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.0007092 M
Hardness of water samples (ppm CaCO 3 ¿:
i. Lab tap water
Ca2+¿ 1 mol CaCO3

0.0003743 mol × ¿
1L 2+¿ 100.1 gCaCO 3 1000 mgCaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 g CaCO3
¿ 37.467 ppm
ii. Lab distilled water
Ca2+¿ 1 mol C aCO 3

0.0001576 mol × ¿
1L 2+ ¿ 100.1 g CaCO3 1000 mgCaCO3
1 mol Ca × × ¿
1mol CaCO 3 1 g CaCO3
¿ 15.776 ppm
iii. Home tap water
Ca2 +¿ 1 mol CaCO3

0.0003349 mol × ¿
1L 2+¿ 100.1 g CaCO 3 1000 mgCaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 gCaCO 3
¿ 33.523 ppm
iv. Deionized water
C a2 +¿ 1 mol CaCO3
0.0001970 mol × ¿
1L 2+¿ 100.1 g CaCO3 1000mg CaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 g CaCO 3
¿ 19.720 ppm
v. 0.1M NaCl
Ca2 +¿ 1 mol CaCO3

0.0007092 mol × ¿
1L 2+¿ 100.1 g CaCO3 1000 mg CaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 g CaCO3
¿ 70.991 ppm
DISCUSSION
In this experiment, the total amount of calcium and magnesium in water is determined
by titrating with a standard solution of ethylenediamine-tetraacetic acid (EDTA). This
method of titration is known as Complexometric Titration. The amount of calcium and
magnesium present in water can be used to determine the hardness of the water. Hardness is
more commonly expressed in units of ppm rather than molarity because of the low
concentration value of these ions. The EDTA solution was first standardized against a known
concentration of calcium carbonate which was 0.007M. The average concentration of EDTA
solution calculated after 4 trials was found to be 0.004925M. This 0.004925M EDTA
solution was used to determine the concentration and hardness of water samples. The highest
concentration of hardness was NaCl which is 70.991ppm. It was found that lab tap water has
a high amount of calcium and magnesium ions and therefore had a higher hardness
concentration compared to other water samples but lower than NaCl which is 37.467ppm.
The lowest concentration of hardness among the water samples was lab distilled water which
has a hardness of 15.776ppm. It can be concluded that through distillation that most of the
calcium and magnesium ions are removed from the water. Some errors might have occurred
in this experiment such as other contaminants in the water sample provided that would give
inaccurate readings due to unknown variables that cannot be avoided such as other metal
ions. Besides that, since each water sample was titrated once, it could not be determined if the
reading was precise.
CONCLUSION
The EDTA solution was standardized against 0.007M of calcium carbonate and the
average concentration obtain is 0.004925M.
The hardness of each water sample was determined by titration against EDTA
solution. The water samples are lab tap water, lab distilled water, home tap water, Deionized
water, and 0.1M NaCl and the hardness of each water sample is 37.467ppm, 15.776ppm,
33.523ppm, 19.720ppm and 70.991ppm respectively.
QUESTIONS
1) Why should the water in the condenser flow uphill during distillation?
The flowing of cool water should be uphill to prevent the condenser from becoming
too hot on it inner surface. If the condenser became too hot, the distillate will escape
as a vapor from the system.
2) Compare the hardness between i) lab tap water and distilled water ii) home tap water
and home distilled water. Did the distillation have a significant effect on the water
hardness? Explain your answer.
Lab tap water is more hardness than lab distilled water. Home tape water is more
hardness than home distilled tap water. Distillations have significant effect on the
water hardness. Distillation process will remove the impurities in the water, so
distilled water and home distilled tap water is clean because it does not contain
impurities.
3) Water with hardness in the range 0-60ppm is termed soft, 60-120ppm medium hard,
120-180ppm hard and above 180ppm very hard. Classify the water samples that you
analyzed in this experiment.
Hardness (soft):
-lab tap water
-lab distilled water
-home tap water
-Deionized water
Hardness (medium):
-0.1M NaCl
4) Do you think there should be a correlation between conductance and hardness

results? Explain your answer.
Conductivity will have a large concentration to the water hardness because
concentration of calcium is easier to measure than the calcium ion concentration. The
conductivity contribution due to the sodium can be subtracted from the total observed
electrolyte conductivity
5) Suggest any ways you can think of to improve any part(s) of this experiment.
For part C of the experiment, at least 3 readings should have been taken to obtain a more
precise reading for the hardness of water samples.
REFERENCES
1) Taylor, F. Sherwood (1945). "The Evolution of the Still". Annals of Science 5 (3):
186.
2) Aristotle. “Meteorology – Book II" (PDF). The University of Adelaide. Retrieved 2010-
06-14.

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EXPERIMENT 5: DISTILLATION AND HARDNESS OF WATER

CaCO3 Ca+2 + CO3-2

B) STANDARDISATION OF THE EDTA SOLUTION

a 250ml conical flask. The concentration of the CaCO3 was recorded.

a 250ml conical flask.

distilled home tap water, deionized water, o.1M NaCl.

B. Standardization of the EDTA Solution

0.007 mol Ca 2+¿

0.007 mol Ca 2+¿

0.007 mol Ca 2+¿

0.007 mol Ca2 +¿

0.0049 M +0.0049 M +0.0049 M + 0.0050 M

Concentration of water samples:

ii. Lab distilled water (l.d.w)

iii. Home tap water (h.t.w)

iv. Deionized water (d.i)

i. Lab tap water

Ca2+¿ 1 mol CaCO3

Ca2+¿ 1 mol C aCO 3

Ca2 +¿ 1 mol CaCO3

Ca2 +¿ 1 mol CaCO3

4) Do you think there should be a correlation between conductance and hardness

precise reading for the hardness of water samples.

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