ANALYTICAL CHEMISTRY (CHM421)

LABORATORY REPORT

EXPERIMENT 5:

DISTILLATION AND HARDNESS OF WATER

GROUP: AS2464D

NAME:

LECTURER:

DR. MUHD FIRDAUS BIN KASIM

DATE OF EXPERIMENT:

29/04/2020

DATE OF SUBMISSION:

06/05/2020

Distillation and Hardness of Water (Exp. 5)

Abstract:

The distillation is the every purifying method for liquids, in this experiment the boiling range for
the jotted temperature sample was recorded while handling the distillation, the resulted data is
about 97.5 ° C. The EDTA solution was undergo standardization process, where the samples
were titrated with it against white background, till the red solution change to sky blue solution
and the final reading at burette was taken. In addition, the total process for part B was repeated
with other two types of samples. The concentration average of the EDTA solution was recorded
0.004934 M The same method was applied in part C, the burettes again filled with EDTA
solution and the sample was titrated, at initial red wine colour detected till change to sky blue
solution. Hardness (soft) have for samples distilled home tap water (3.9179 ppm), 0.1 M NaCl
(16.8268 ppm), home tap water (32.5926 ppm) and lab tap water and lab distilled water (37.5257
ppm) while hardness (medium) recorded with deionized water (114.6145 ppm)

Keyword: distillation, titration, standardization, hardness, samples

Introduction

The most commonly used method of separation is distillation, the main function of dilution is to
purify and to separate the component in the mixtures refereeing on the differences in the
situation required, as the liquid can be heated with range boiling point from the initial and final
reading. Boiling might happen during substances vapor pressure is same as confining pressure.
Regular boiling point happen when the ambient pressure is equal to the underlying pressure.

While, hard water is produced in the water samples by the presence of ions such as calcium and
magnesium. Calcium (Ca+2) and magnesium (Mg+2) ions are the main causes of hardness but
other metals may also lead to hardness. Therefore, hardness in the sample is an indicator of such
ions. In this analysis, the acumulate calcium and magnesium content in water was calculated by
titrating with a regular ethylenediamine-tetraactic acid (EDTA) solution and due to the low
concentration value of these ions, hardness is usually written in ppm units, rather than molarity
or known as complexometric titration.

Objective:

1. To purify water sample by distillation

2. To standardize EDTA solution
3. To analyze hardness of water samples by titration with EDTA

Methodology

A. Distillation of the home tap water.

A normal distillation was illustrated as figure 7 shown in the laboratory manual, by
referring the figure of the distillation equipment shown, a 150 mL of round bottom flask
was applied for the distilling flask process and 250 mL of conical flask was employed as
the collector to assemble the distillate. For this experiment, the clamp was ensured to
fastener the apparatus fittingly at the suitable place to avoid adulterations. Then, the
distilling flask was filled up at two third with tap water from house and a couple of
boiling chips was put into the flask to avoid bumping. The cap then was set on, and the
water flow upward and the mercury bulb of the thermometer were also checked in the,
condenser. The thermometer should be lowered than the junction of the condenser with
the distillation column while meticulously the Bunsen burner was switch on and the
heating process of the distillation flask was started. As the boiling occurs, the
condensation will lead and the water collection was begun, as the distillation occurred,
the titration equipment was established to standardize the EDTA and be caution not to
stumble the distillation configuration. The first 20 drops, or the next drop the distilled
water was dispensed as they might hold volatile impurities or also from the glassware.
The temperature then was recorded at the first data of 1 mL of the distillate and the
distillation process was continued and ensures to not let dried out. As the collection has
sufficient for the experiment, the flame was turned off before the flask is totally dried off.
The temperature at the distillation over, the data was jotted.

B. Standardisation of the EDTA solution

 A 50 mL burette was washed rigorously and washed with distilled water for the inside
part. Then the stopcock was removed and the sample was removed entirely into a “waste”
beaker. Then the burette was washed carefully that there are no longer reagent spot left.
Next, the burette was washed with the EDTA solution and then discards the waste. After
ensure the burette valve was secured, the EDTA solution was transfer into burette beyond
the zero mark. The burette was fixed to burette stand, and ensures if there any bubble
detected in the tip of the burette, if there the bubble was discarded entirely by turn on the
stopcock at 360oC. At this moment, the pressure of the solution came from the burette
was hard enough to force the bubble out.as the removal of bubble was done, the initial
measurement was fixed at 0. Here, procrastinate to stick at the level 0 mL mark was not
suggested thus, the tip of the burette was wiped on the outside surface to discard any
adhering liquid. After that, 25 mL regular Ca2+ solution prepared aliquots was pipetted
and transferred into a 250 mL conical flask and the concentration of the CaCO 3 prepared
was jotted. Into the flask, with 8 mL of pH 10 ammonium-ammonium chloride buffer and
15 mL of distilled water and 3 drops of Eriochrome Black T indicator was added. The
sample was titrated against a white backdrop with the EDTA solution, before the red
solution changes to sky blue. The volume of burette was registered at the endpoint, and
then it repeats the entire cycle with two other samples.

C. Hardness of water
More EDTA solution was poured in to the burette. 25 mL of pipette was rinsed with tap
water and pipetted 25.0 mL of lab tap water into a 250 mL conical flask and the content
was transfer into the flask while the final drop was touched the wall of the flask. The
leftover liquid in the pipette will not blast into the flask as more than 25.0 mL was
supplied. 8 mL of the ammonia-ammonium chloride buffer were applied similarly as
above and three drops of the EBT indicator were applied to the flask sample, the initial
reading was jotted at the nearest 0.01 mL. The interior of a 25.0 mL distilled water
pipette is rinsed. Using rubber filler a bit of distilled water from the lab was collected.
The filler is withdrawn, inclined and the pipette rotated to clean the inside of the pipette
with the distilled water. The sample was properly titrated until the solution of red wine
transforms to sky blue. This process was repeated with two more samples, the titration.
 The whole procedure was replicated with 25.0 mL purified water from the laboratory,
25.0 mL deionized water, 25.0 mL home tap water, 25.0 mL diluted home tap water and
25.0 mL 0.1 M NaCl as samples.

Results

A. Distillation of home tap water

1. Temperature at the start of collecting the distillate = 96.0 °C

2. Temperature at the end of collecting the distillate = 99.0 °C

3. Experimental boiling range for collected sample = 97.5 °C

B. Standardisation of the EDTA solution

Concentration of standard Ca2+ solution = 0.007M

Volume of the standard Ca2+ solution = 25.0 ml

Rough 1 2
Final reading of EDTA solution 37.50 35.75 35.55

Initial reading of EDTA 0.10 0.15 0.20

solution
Volume of EDTA solution 37.40 35.60 35.35
(mL)

C. Hardness of Water
Concentration of EDTA = 0.004934 M

Water Lab tap Lab Home tap Distilled Deionized 0.1 M

sample water distilled water home tap water NaOH
water water
Final 2.00 4.00 1.85 0.30 9.90 10.85
reading of
standard
EDTA
Initial 0.10 2.10 0.20 0.10 4.10 10.00
reading of
standard
EDTA
Volume of 1.90 1.90 1.65 0.20 5.80 0.85
standard
EDTA
used (ml)
[Ca2+ + 0.0003749 0.0003749 0.0003256 0.00003947 0.001145 0.0001681
Mg2+]
(mol/L)
Hardness 37.5275 37.5275 32.5926 3.9179 114.6145 16.8268
(ppm)

*Hardness is usually expressed as ppm CaCO3

Calculation

Part B : Standardization of EDTA Solution

From stoichiometry, 1 mol EDTA = 1 mol Ca2+ and 1 mol Mg2+

1st titration: 2nd titration:

M a Va a
=
Mb V b b M a Va a
=
M a (35.60 mL) Mb V b b
1
=
(0.007 M)(25.0 mL) 1 M a (35.35 mL) 1
=
Ma (35.60 mL) = 0.007M(25.0 mL) (0.007 M)(25.0 mL) 1

Ma = 4.9157 x 10-3 M Ma (35.35 mL) = 0.007 M (25.0 mL)

= 0.004916 M Ma = 4.9505 x 10-3 M

= 0.004951 M

[( 0.004916 ) + (0.004951 )] M
Average molarity of EDTA =
2
= 4.9335 x 10-3 M = 0.004934 M

Part C: Hardness of water

i. Lab tap water (l.t.w)

2+¿
Mg 0.0019 L EDTA
2+¿ ×
0.004934 mol EDTA 1mol EDTA 0.025 LCa
2+¿
2 +¿ Mg ¿
¿
M l .t . w = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.0003749 M

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

2+¿
Mg 0.0019 L EDTA
2+¿ ×
0.004934 mol EDTA 1 mol EDTA 0.025 LCa 2+¿ Mg
2+ ¿
¿
¿
M l .d .w = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.0003749 M

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

2+¿
Mg 0.00165 L EDTA
2+¿ ×
0.004934 mol EDTA 1mol EDTA 0.025 LCa 2 +¿ Mg
2+ ¿
¿
¿
M h .t . w = ×1 mol Ca ¿
¿
1 L EDTA
 ¿ 0.0003256 M

iv. Distilled home tap water (d.h.t.w)

2+ ¿
Mg 0.0002 LEDTA
2+¿ ×
0.004934 mol EDTA 1 mol EDTA 0.025 LCa 2+ ¿ Mg ¿
2+¿ ¿
M d . h .t . w = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.00003947 M

v. Deionized water (d.i)

2+ ¿
Mg 0.0058L EDTA
2+¿ ×
0.004934 mol EDTA 1 mol EDTA 0.025 LCa 2+ ¿Mg
2+¿
¿
¿
M d . i= ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.001145 M

vi. 0.1M NaCl

2+ ¿
Mg 0.00085 L EDTA
2+¿ ×
0.004943 mol EDTA 1 mol EDTA 0.025 L Ca 2+ ¿Mg
2+¿
¿
¿
M NaCl = ×1 mol Ca ¿
¿
1 L EDTA
¿ 0.0001681 M

Hardness of water samples (ppm CaCO 3 ¿:

i. Lab tap water

Ca2 +¿ 1 mol CaCO3

0.0003749 mol × ¿
1L 2+¿ 100.1 g CaCO 3 1000 mgCaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 gCaCO 3
¿ 37.5275 ppm
ii. Lab distilled water
Ca2 +¿ 1 mol CaCO3
0.0003749 mol × ¿
1L 2+¿ 100.1 g CaCO 3 1000 mgCaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 gCaCO 3
¿ 37.5275 ppm
iii. Home tap water

Ca2+¿ 1 mol CaCO3

0.0003256 mol × ¿
1L 2+ ¿ 100.1 g CaCO3 1000 mgCaCO3
1 mol Ca × × ¿
1mol CaCO 3 1 g CaCO3
¿ 32.5926 ppm
iv. Distilled home tap water
Ca 2+¿ 1 mol CaCO3
0.00003947 mol × ¿
1L 2+¿ 100.1 g CaCO3 1000 mgCaCO3
1 mol Ca × × ¿
1mol CaCO 3 1 g CaCO3
¿ 3.9179 ppm
v. Deionized water

Ca 2+¿ 1 mol CaCO3

0.001145 mol × ¿
1L 2 +¿ 100.1 g CaCO3 1000 mgCaCO 3
1 mol Ca × × ¿
1 mol CaCO3 1 g CaCO3
¿ 114.6145 ppm
vi. 0.1M NaCl

Ca2 +¿ 1 mol CaCO3

0.0001681 mol × ¿
1L 2+¿ 100.1 g CaCO3 1000 mg CaCO3
1 mol Ca × × ¿
1 mol CaCO3 1 g CaCO3
¿ 16.8268 ppm
Discussion

This experiment is aiming for three objectives which are to purify water sample by distillation, to
standardize EDTA solution and to analyze hardness of water samples by titration with EDTA.
First and foremost, the experiment is to distill the sample, which the sample used is tap water. As
the potion of life is water thus the need for water for very nature of life and health preservation
has motivated man to devise methods to preserve his purity and wholesomeness (Verma &
Kushwaha, 2013). Therefore this experiment is to distill the water where the initial temperature
when the sample collected was 96.0 oC and the final reading of the temperature taken was 99.0
o
C. Here, after the average of the temperature recorded, it stated that the boiling range applied to
collect the sample is 97.5 oC.

Referring the second objectives, the standardization was undergo two trial titration which the
result secured 35.60 mL and 35.35 mL, after the calculation the average mL of EDTA solution
used was 35.48 mL, this equal to 0.004934 M, as the concentration obtained 0.007 M with 25.0
mL used for the standard Ca2+ solution standardize with EDTA solution. Specifically in the
nature of other metal ions as EDTA, it is a non-selective complexing agent forming stable
complexes with most metal ions (Nagaraj et al, 2015).

As well in term of hardness titration process, again the EDTA solution was used to titrate the
decided samples which are six different type of water samples are collected form multi source.
Hardness (hard water) is one of the growing issues with water quality worldwide as water
occupies a minimum of 70 per cent of the earth's surface according ( Ahn et al, 2018). As the
molarity of the EDTA solution was identidfied, this help to acquired the water harness
concentration especially in term of part per million formula. From the calculation, deionized
water distilled water was recorded as the hardest water from all water samples as it obtained the
highest concentration of Ca2+ ions (114.6145 ppm), followed by lab tap water and lab distilled
water with data recorded (37.5275 ppm), home tap water jotted (32.5926 ppm), 0.1 M NaCl
(16.8268 ppm) and lastly, distilled home tap water recorded (3.9179 ppm). This indicates that
deionized water contained the highest Ca2+ ions in the solution with data jotted 114.6145 ppm.
According form my research, it stated that the existence of Ca 2+ and Mg2+ have affected the water
hardness and the total hardness was equal the sum up of magnesium and calcium hardness.
Conclusion

In a nutshell, this experiment was successful as the three main objectives were achieved where
the water sample was purified by distillation process and it recorded 97.5 oC. The concentration
of standardized EDTA solution was obtained 0.004934 M. and the water hardness are identified
as the greatest concentration of Ca2 + ions (114.6145 ppm) in the deionized water, accompanied
by lab tap water and lab distilled water with recorded data (37.5275 ppm), home tap water jotted
(32.5926 ppm), 0.1 M NaCl (16.8268 ppm) and finally distilled home tap water (3.9179 ppm)
was recorded. Hardness (soft) have for samples distilled home tap water (3.9179 ppm), 0.1 M
NaCl (16.8268 ppm), home tap water (32.5926 ppm) and lab tap water and lab distilled water
(37.5257 ppm) while hardness (medium) recorded with dionized water (114.6145 ppm)

References

K. C. Verma & A. S. Kushwaha. (2013). Demineralization of drinking water: Is it prudent?

Medical Journal Armed Forces India, 377-379.
M. K. Ahn., R. Chilakala., C. Han. & T. Thenapali. (2018). Removal of Hardness from Water
Samples by a Carbonation Process with a Closed Pressure Reactor. Journal of Water, 1-
10.
P. Nagaraj., B. T. Gopalakrishna. & K. G. Chandrashekara. (2015). Indirect complexometric
determination of Mercury(II) using L-Cystine as a selective masking agent. International
Journal of Chemical Studies, 27-29.
Questions

1. Why should the water in the condenser flow uphill during distillation?

To prevent the condenser from being too hot on its inner surface, the flow of cool water should
be upward. If it gets too hot, then the distillate will evade from the system as it vapors.

2. Compare the hardness between i) lab tap water and lab distilled water ii) home tap
water and home distilled tap 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. Meanwhile, for home tap water it 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 0-60 ppm is termed soft, 60-120 ppm is medium hard,
120-180 ppm is hard and above 180 ppm is very hard. Classify the water samples that you
analysed in the experiment.

Hardness (soft):

 Distilled home tap water (3.9179 ppm)

 0.1 M NaCl ( 16.8268 ppm)
 Home tap water (32.5926 ppm)
 Lab tap water and lab distilled water (37.5257 ppm)

Hardness (medium):

 Deionized water (114.6145 ppm)

4. Do you think there should be a correlation between conductance and hardness result?
Explain your anwer.

Conductivity should have high water hardness intensity because calcium density is easier to
calculate than the concentration of calcium ions. The amount of conductivity due to sodium can
be subtracted from the overall conductivity found with electrolytes.

5. Suggest any ways you can think of to improve any parts in this experiment.

The only way to improve in this experiment is during Part C of the experiment, at least 3
measurements for the hardness of water samples would have been taken to achieve a more
reliable read.