ABSTRACT

The distillation is the process of common purification for liquids. Home tap water will be distillated and will
compare with the hardness of the non-distilled tap water to determine the effectiveness of the distillation
procedure. When doing the distillation, the boiling range for collected sample of temperature was taken,
this is around 68˚C. The standardization of the EDTA solution is added of Eriochrome Black T indicator. The
EDTA solution must be the fresh solution one, to ensure that the experiment was successful. When doing
the titration part, make sure that dropwise of the titrant is added to the solution before the endpoint. It is
to make sure that to prevent the overshoot of the endpoint. The average concentration of the EDTA
solution is

4.889 X 10¯ᶾM.

The hardness of water is determined by the titration of lab tap water, lab distilled water, deionized water
and 0.1 M NaCl. The water sample can be classified by the hardness (soft) and also hardness (medium).
The hardness (soft) is from lab tap water, lab distilled water, home tap water and deionized water.
Meanwhile, for the hardness (medium) is only 0.1 M NaCl.

OBJECTIVE

1. To purify water sample by distillation.

2. To standardize EDTA solution.

3. To analyses hardness of water samples by titration with EDTA.

INTRODUCTION

In this experiment, we will carry out about distillation process. The home tap water has been distilled and
then the hardness of the non-distilled tap water are compared to that of the distilled tap water to
determine the effectiveness of the distillation process, which is been used the titration to determine the
hardness of water sample. Water containing high concentration of Ca2+, Mg2+, Fe2+, or Fe3+ ion is called
hard water. Ca2+ and Mg2+ are the most common sources of hardness in water. Calcium ion and
magnesium ions react with soap to form a precipitate when sticks to stinks, bathtubs, and fabrics. They can
form large amounts of insoluble calcium carbonate, magnesium carbonate, and iron (III) carbonate when
heated and form scale inside pipes, tea kettles and water heaters. Scale build up can impede water flow.
Water softening using ion exchangers can remove the hard water ions to produce soft water. Soft water
produced by ion exchangers contains sodium ion (Na+) instead.

About distillation process, it is the most used technique for the purification of liquids. The liquid is placed
in a distilling flask and is heated to its boiling point. The vapour those, leaving behind higher boiling
impurities still in the flask; are passed along a condenser which condenses the vapour back to liquid form
and is collected in a different flask. Low boiling impurities can also be separated similarly. Boiling will
happen when the vapour pressure of a substance equals the confining pressure. Normal boiling point
occurs when the confining pressure equals the atmospheric pressure.

Hard water can be softened by other methods such as by ion exchange. When hard water is passed through
a home water softener, the calcium and magnesium ions in the water are replaced by sodium ions. In other
cation exchange resins, the cations in the sample are replaced by the hydrogen ions while the anion
exchange resins, replace the anions in the sample with hydroxide or chloride ions. If both hydrogen and
hydroxide resins are used, the yielded hydrogen and hydroxide ions reacts with each other to produce
water i.e. deionized water. Deionized water is more superior to distilled water.

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). Hardness is more commonly expressed in
units of ppm rather than molarity because of the low concentration value of these ions.

METHOD

A. Distillation of the Home Tap Water

A typical distillation apparatus is illustrated and was referred to the figure as a guide to assemble
the distillation apparatus. The 250 mL round bottom flask is used for the distilling flask and a 250 mL conical
flask for the receiver to collect the distillate. The apparatus was clamped adequately and at strategic places
to avoid breakages.

The distilling flask was filled about two thirds with home tap water. A couple of boiling chips is added to
the flask to prevent bumping and the tap is turned on. The water flows uphill was checked in the condenser
and the mercury bulb of the thermometer also has been checked it is lower than the junction of the
condenser with the distillation column. The Bunsen flame is carefully turned on and it was started heating
the distillation flask. When boiling occurs, condensation is followed and was started to collect water in the
receiving flask. While waiting for the distillation process, the titration for standardizing the EDTA has been
set up.
 The first 20 drops or so of the distilled water collected was discarded as they might contain volatile
impurities and the impurities form the distillation glassware. The temperature on the thermometer was
read as soon as it was started to collect 1 mL of the distillate. The distillation process is continued and was
kept a watch on the distilling the flask so as not to let it dry. The flame is turned off when have collected
enough of the distillate or before the sample flask is dried. The temperature is recorded when stop the
distillation.

B. Standardisation of the EDTA solution

A 50 mL burette is cleaned and the insides were rinsed with distilled water. The stopcock was
opened and drained completely into a “waste” beaker. The burette was ensured clean and there are no
‘reagent spot’ in the interior. Finally the burette was rinsed with the EDTA solution and it was discarded.

The EDTA solution was poured into the burette beyond the zero mark, and it was made sure to
close the burette valve earlier. The burette was attached to a burette stand and was checked to make sure
that there is no air bubble trapped in the tip of the burette. When there is presence of air bubble, the
bubble was removed by fully turning the stopcock 360°. The force of the solution coming out from the
burette is now strong enough to push the bubble out. After the bubble was removed, the initial reading is
adjusted. Initial reading does not have to be at 0 and does not waste time trying to bring the level exactly
to the 0 mL mark. The outside of the burette tip was wiped to remove by adhering liquid

there.

25.0 mL aliquots of the prepared standard Ca2+ solution has been pipette and transferred to a 250
mL conical flask. The concentration of the CaCO3 prepared is recorded in the lab notebook.

8 mL of pH 10 ammonia-ammonium chloride buffer, 15 mL of distilled water and 3 drops of

Eriochrome Black T indicator were added into the flask. The solution should be of red wine colour initially
and does not added too many drops of the indicator since this can create problems with seeing the end
point. The sample is immediately titrating with the EDTA solution against a white background until the red
solutions turns to sky blue. The volume of the burette at the end point was recorded and the process was
repeated with at least two more samples.

The above reaction mixture will evaporate NH3 to some extent. This changes the pH of the solution. It is
therefore advisable to carry out the titrations quickly but carefully. The faster the titrations are done, the
better the results will be. However, be careful not to overshoot the endpoint due to excessive haste.
In any titration it is a good practice to sacrifice one sample solution to perform a rough titration. This is to
determine the approximate endpoint and to observe the colour change. In the next subsequent titrations,
dropwise or ½ drop is added at a time of the titrant to the solution in the conical flask about 3 or 4 mL
before the endpoint.

C. Hardness of Water

Water hardness is determined by titration on lab tap water, lab distilled water, deionized water, home tap
water, distilled home tap water and a 0.1 M NaCl.

The burette was filled up with more EDTA solution. A 25 mL pipette with tap water and pipette
25.0 mL of lab tap water were rinsed into a 250 mL conical flask. The content of the pipette has been empty
into the flask, and the last drop off is touched by touching the tip of the pipette onto the interior wall of
the flask. The remaining liquid in the pipette does not blow into the flask as this are deliver more than 25.0
mL.

8 mL of the ammonia-ammonium chloride buffer and 3 drops of Eriochrome Black T were added
into the water sample in the flask. The initial burette reading was recorded to the nearest 0.01 mL. The
stopcock of the burette is turned to release the standard EDTA solution into the water sample in the flask.
The rate of releasing the EDTA solution has been slowed down into the flask when the blue coloured
solution is formed. If the calcium and magnesium in the sample has exhausted, the solution is turned into
blue colour. The titration is stopped and the final reading has been taken. The titration is repeated with
another two more lab tap water samples.

The inside of a 25.0 mL pipette is rinsed with distilled water. A little bit of lab distilled water was
obtained using rubber filler. The filler is removed, tilted and rotated the pipette to rinse the inside of the
pipette with the distilled water. The tainted distilled water is discarding. 25.0 mL of fresh distilled water is
pipette into a clean dry conical flask (rinsing with distilled water is adequate). Buffer and indicator were
added as above and titrate with the standardized EDTA solution to the endpoint and the process was
repeated.

The pipette was rinsed with home tap water or an unknown available. 25.0 mL of the unknown is
pipette into a clean flask. Buffer and indicator were added and it was titrate with the standardized EDTA
solution
RESULT

A. Distillation of Home Tap Water

1. Temperature at the start of collecting the distillate = 88.0°C

2. Temperature at the end of collecting the distillate = 96.0°C

3. Experimental boiling range for collected sample = 80°C

B. Standardisation of the EDTA solution

1. Concentration of standard Ca2+ solution = 0.007 M

2. Volume of the standard Ca2+ solution = 25 mL

Rough 1 2 3
Final reading EDTA solution 35.30 36.1 36.0
Initial reading EDTA solution 0.00 0.00 0.00

Volume of EDTA solution 35.50 36.1 36.0

C. Hardness of Water

1. Concentration of EDTA = 4.889 x 10¯ᶾ M

Water sample Mineral Lab distilled Home tap Distilled deionized 0.1M NaCl
water water water home tap water
water

Final reading of 7.05 3.05 3.35 2.50 6.40 2.10

standard EDTA
Initial reading of 0.01 0.01 0.01 0.00 0.01 0.00
standard EDTA

Volume standard 7.04 3.04 3.34 2.50 6.39 2.10

EDTA used (mL)

Volume water 25.00 25.00 25.00 25.00 25.00 25.00

sample (mL)
[Ca²ᶧ + Mg²ᶧ] 1.38x10¯ᶾ 5.95x10¯⁴ 6.53x10¯⁴ 4.96x10¯ᶾ 1.25x10¯ᶾ 4.11x10¯⁴
(mol/mL)
Hardness (ppm) 138.12 59.55 65.36 48.94 125.08 41.10
DISCUSSION

From the first purpose of this experiment is the purification of the water sample by distillation, which is to
separate the substances and as such can be used for water purification. The experimental boiling range for
collected sample is about 80˚C and the water sample was kept for the other procedure.

For the second objectives is to standardize EDTA solution. We are using 0.007 M of concentration of
standard Ca2+ solution and the volume of it is 25.00 mL. When we are already finished the pipetting, we
get the results of the volume of EDTA solution that we are used for 1st,2nd,3rd experiment which are
35.30,36.10,36.00 mL. Meanwhile, the average concentration of EDTA solution as we have been calculated
is 4.889x10¯ᶾ M.

To analyse the hardness of water samples by titration with EDTA is the last purpose of this experiment. As
you can see at the table data, about four water sample than six we are doing when conduct the experiment
which is lab tap water, lab distilled water, Home tap water, Distilled home tap water, deionized water and
lastly 0.1 M of NaCl. The total amount of Calcium ion and Magnesium ion that react with the EDTA solution
in lab tap water is 1.37 x 10¯ᶾ mol/L and their hardness is 138.12 ppm which is hard. The water hardness is
hard because the theoretical value for very hard water is more than or equal to 450 ppm. Next, for the lab
distilled water, the amount of concentration of Calcium ion and Magnesium ion is about 5.95 x 10¯⁴mol/L.
The hardness of water is also hard, which is 59.55 ppm which is the hardness is medium. For the Home tap
water, the amount of concentration of Calcium ion and Magnesium ion is about about 6.53 x10¯⁴mol/L and
their hardness is 65.36 ppm which is the hardness is medium. Next, the total amount of Calcium ion and
Magnesium ion that react with EDTA solution in Distilled home tap water is 4.89 x 10¯⁴mol/L and the
hardness is 48.94ppm which is the hardness is soft .The concentration of Ca2+ and Mg2+ is 1.25 x 10¯ᶾ
mol/L and the amount of their hardness is 125.08 ppm for water samples of deionized water which the
hardness is hard. Lastly, 0.1 M of NaCl was done by calculate its concentration of Ca2+ and Mg2+ is 4.11 x
10¯⁴mol/L, hence their hardness of water is about 41.10 ppm which the hardness is soft.

The hardness is divided by two parts, which is soft, medium and hard. For hardness (soft), it is Distilled
home tap water and 0.1 M,NaCl. Hence, Home tap water and Lab distilled water is for hardness (medium).

For hardness (hard) are Lab tap water and Deionized water.
As a student, I have found that some errors while doing the experiment by us which is when reading the
scale of the liquid inside the pipette. After that, maybe we are put an extra drops of titrant to the solution
which is to prevent the overshoot of the endpoint, frequently wash the sides of the flask and the burette
tip to ensure all the titrant has gotten into the solution in the flask. Not even that, the EDTA solution that
we are used must be not exposed to the air and it was made sure that the solution is always closed. The
EDTA solution also must be in a fresh solution, not the old solution one.

QUESTIONS

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

The flowing of water should be flow uphill during distillation to prevent the condenser from
becoming too hot on its inner surface. When the condenser become too hot, the distillate will escape as a
vapour from the system.

2. Compare the hardness between (i) lab tap water and lab distilled water and (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 medium hard, 120 – 180
ppm hard and above 180 ppm very hard. Classify the water samples that you analysed in this experiment.

Hardness (soft): Lab tap water, Lab distilled water, Home tap water, Deionized

water

Hardness (medium): 0.1 M 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 combustion 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 the part C, the hardness of water, at least 2 or 3 readings should have been taken to obtain a
more precise reading for the hardness of water samples.

CONCLUSION

As a conclusion, the purification water sample by distillation was achieved. Next, the average value of
standardize the EDTA solution is 4.889 x 10¯ᶾM. Lastly, the analyse hardness of water samples by titration
with EDTA is hardness (soft) include lab tap water, lab distilled water, Home tap water,Distilled home tap
water, deionized water and the hardness (medium) is include 0.1M NaCl, which is their hardness is around
138.12 ppm, 59.55 ppm, 65.360 ppm,48.94 ppm,125.08 ppm and 41.10 ppm.

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