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 68C.

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 0.5828M.

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.

PROCEDURE

A. Distillation of the Home Tap Water

1. 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.
2. 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.
3. The first 20 drops or so of the distilled water collected was discarded as the 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

1. 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.
2. 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.
3. 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 CaCO 3 prepared is recorded in the lab
notebook.
4. 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 NH 3 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 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.
1. The burette was filled up with more EDTA solution.
2. 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.
3. 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.
4. 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.
5. 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.
RESULTS

A. Distillation of Home Tap Water

1. Temperature at the start of collecting the distillate = 34 C
2. Temperature at the end of collecting the distillate = 102 C
3. Experimental boiling range for collected sample = 68 C

B. Standardisation of the EDTA solution

1. Concentration of standard Ca2+ solution = 0.1 M
2. Volume of the standard Ca2+ solution = 250 mL

Rough 1 2 3
Final reading of EDTA solution (mL) 7.1 7.1 - -
Initial reading of EDTA solution (mL) 50.0 50.0 - -
Volume of EDTA solution (mL) 42.9 42.9 - -

C. Hardness of Water
1. Concentration of EDTA = 0.1 M

Water sample Lab tap water Lab Deionized 0.1 M

distilled water NaCl
water
Final reading of standard EDTA 49.7 mL 45.5 mL 35.6 mL 38.0 mL
Initial reading of standard EDTA 50.0 mL 49.7 mL 45.5 mL 45.5 mL
Vol of standard EDTA used (mL) 0.30 mL 4.2 mL 9.9 mL 7.5 mL
Vol of water sample (mL) 25 mL 25.0 mL 10.0 mL 25.0 mL
[Ca2+ + Mg2+] (mol/L) 710-4 0.098 0.2308 1.7510-6
Hardness (ppm) 700.8 9808 57750 17496

CALCULATIONS
FOR STANDARDISATION OF THE EDTA SOLUTION
Concentration of standard Ca2+ solution = 0.1 M
Volume of the standard Ca2+ solution = 250 mL
To calculate the number of moles of Ca2+ = Molarity of Ca2+ Volume of Ca2+
= 0.1 M 2510-3 L
= 2510-3 moles
When,
1 mol of Ca2+ = 1 mol of EDTA

Therefore;
2510-3 moles of Ca2+ = 2510-3 moles of EDTA

For the roughly calculation, the volume of EDTA used is 42.9 mL

 Number of moles of EDTA
Molarity of EDTA = Volume of EDTA

25 103 moles
= 42.9 103 L
= 0.5828 M
Therefore, the average of concentration of EDTA is 0.5828 M.

FOR HARDNESS OF WATER

i. Lab Tap Water
No of mole of EDTA = Molarity of EDTA Volume of EDTA
= 0.5828 M 310-4 L
= 1.7510-4 moles
1 mol of EDTA = 1 mol of Ca2+ and Mg2+
1.7510-4 moles of EDTA = 1.7510-4 moles of Ca2+ and Mg2+

Number of Moles
So, the calculation for [Ca2+ + Mg2+] = Volume
4
1.75 10 moles
= 3
25 10 L
= 710-4 M
Meanwhile, the calculation for the hardness (ppm);
Mass of CaCO3 = Number of mole of CaCO3 Molar Mass
= 1.7510-4 moles 100.09 g/mol
= 0.01752 g
Weight of the solute 6
10
Ppm (w/v) = Volume of the solution

0.01752 g 6
10
= 25 mL

= 700.8 ppm
Therefore, it is hardness (soft)

ii. Lab distilled water

No of mole of EDTA = Molarity of EDTA Volume of EDTA
= 0.5828 M 4.210-3 L
= 2.4510-3 moles
When
1 mol of EDTA = 1 mol of Ca2+ and Mg2+
2.4510-3 moles of EDTA = 2.4510-3 moles of Ca2+ and Mg2+

Number of Moles
2+ 2+
So, the calculation for [Ca + Mg ] = Volume

2.45 103 moles

= 25 103 L
 = 0.098 M
Meanwhile, the calculation for the hardness (ppm);
Mass of CaCO3 = Number of mole of CaCO3 Molar Mass
= 2.4510-3 moles 100.09 g/mol
= 0.2452 g

Weight of the solute

106
Ppm (w/v) = Volume of the solution
0.2452 g 6
10
= 25 mL

= 9808 ppm
Therefore, it is hardness (soft).

iii. Deionized water

No of mole of EDTA = Molarity of EDTA Volume of EDTA
= 0.5828 M 9.910-3 L
= 5.7710-3 moles
When
1 mol of EDTA = 1 mol of Ca2+ and Mg2+
5.7710-3 moles of EDTA = 5.7710-3 moles of Ca2+ and Mg2+

Number of Moles
So, the calculation for [Ca2+ + Mg2+] = Volume

5.77 103 moles

= 3
25 10 L
= 0.2308 M

Meanwhile, the calculation for the hardness (ppm);

Mass of CaCO3 = Number of mole of CaCO3 Molar Mass
= 5.7710-3 moles 100.09 g/mol
= 0.5775 g

Weight of the solute

106
Ppm (w/v) = Volume of the solution
0.5775 g 6
10
= 10 mL

= 57750 ppm
Therefore, it is hardness (soft)

iv. 0.1 M of NaCl

No of mole of EDTA = Molarity of EDTA Volume of EDTA
= 0.5828 M 7.510-3 L
= 4.3710-3 moles
When
1 mol of EDTA = 1 mol of Ca2+ and Mg2+
 4.3710-3 moles of EDTA = 4.3710-3 moles of Ca2+ and Mg2+

Number of Moles
So, the calculation for [Ca2+ + Mg2+] = Volume

4.37 103 moles

= 3
25 10 L
= 1.74810-6 M

Meanwhile, the calculation for the hardness (ppm);

Mass of CaCO3 = Number of mole of CaCO3 Molar Mass
= 4.3710-3 moles 100.09 g/mol
= 0.4374 g

Weight of the solute 6

10
Ppm (w/v) = Volume of the solution
0.4374 g 6
10
= 25 mL

= 17496 ppm
Therefore, it is hardness (medium)

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 68C and the water sample was
kept for the other procedure.

For the second objectives is to standardize EDTA solution. We are using 0.1 M of
concentration of standard Ca2+ solution and the volume of it is 250 mL. When we are already
finished the pipetting, we get the results of the volume of EDTA solution that we are used
which is 42.9 mL. Meanwhile, the average concentration of EDTA solution as we have been
calculated is 0.5828M.

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, deionized water and
lastly 0.1 M of NaCl. We do not have the water sample of home tap water and also distilled
home tap water because we are conducting the experiment in the laboratory room. The total
amount of Calcium ion and Magnesium ion that react with the EDTA solution in lab tap water
is 710-4 mol/L and their hardness is 700.8 ppm. The water hardness is very 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
0.098 mol/L. The hardness of water is also very hard, which is 9808 ppm. About 0.2309
mol/L of concentration of Ca2+ and Mg2+ and the amount of their hardness is 57750 ppm for
water samples of deionized water. Lastly, 0.1 M of NaCl was done by calculate its
concentration of Ca2+ and Mg2+, 1.7510-6 mol/L, hence their hardness of water is very
hardness which is about 17496 ppm. The hardness is divided by two parts, which is soft and
also medium. For hardness (soft), it is include lab tap water, lab distilled water, home tap
water and deionized water. Hence, 0.1 M NaCl is for hardness (medium).

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.

CONCLUSION
As a conclusion, the purification water sample by distillation was achieved. Next, the average
value of standardize the EDTA solution is 0.5828 M. Lastly, the analyse hardness of water
samples by titration with EDTA is hardness (soft) include lab tap water, lab distilled water,
deionized water and the hardness (medium) is include 0.1M NaCl, which is their hardness is
around 700.8 ppm, 9808 ppm, 57750 ppm and 17496 ppm.

REFERENCES
1. Anonymous, (n.d.). Determination of Hardness of Water. Retrieved on April 25,2016
from website
http://chemistry.bd.psu.edu/jircitano/Water05.pdfhttp://chemistry.bd.psu.edu/jircitano/Wat
er05.pdf
2. Gaithersburg, MD., (n.d.). Distilled Vs. Purified Water. Retrieved on April 26,2016 from
website http://www.drinkmorewater.com/distilled-or-purified-water
3. Analytical Chemistry slides notes.
4. Analytical Chemistry Laboratory manual.
5. Aristotle. Meteorology Book II (PDF), The University of Adelaide. Retrieved on
April 27, 2016.
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.