EXPERIMENT 5

PREPARATION OF DISTILLED WATER AND

DEIONISED WATER
Structure

5 . Introduction
Objectives -.
-

5.2 Principle
5.3 ~e~uirements
5.4 Procedure
Preparation of Distilled Water
Preparation of Deionised Water
5.5 Summary

5.1 INTRODUCTION
You require large quantities of pure water for various purposes such as
preparation of solutions for analysis and also as a reaction medium in a
laboratory. You have studied in Unit 6 of this course that the tap water is an
impure form of water due to the presence of dissolved solids or gases in it, and
thus it is unsuitable for experiments. Pure water can be obtained either by
distillation or by demineralisation or deionisation of tap water, as discussed in
Unit 6.

In this experiment, you will study the working of a distillation still and a
deioniser which are used [or preparing distilled water and deionised water,
respectively.

Objectives
After performing this experiment, you should be abIe to:
prepare distilled water and deionised water,
use a distillation still and a deioniser,
explain the working of a distillation still and a water deioniser unit,
recharge a water deioniser unit, and
use and descale the distillation still.

5.2 PRINCIPLE
Distilled water is essentially condensed steam. Tap water is boiled in a water
still and the steam, which contains only water molecules, is condensed back
into liquid. The dissolved gases present in tap water are boiled out and the
dissolved solids remain in the boiler.
+
Deionised water or demineralised water is obtained by passing tap water
through ion exchange resins. Ion exchange resins are complex organic
polymers which contain replaceable H' and OH- ions attached to them. The
resins having H' ions are known as cation exchange resins and the resins
having OH- ions are known as anion exchange resins, respectively. When both
Basic Experiments H+ and OH- ions are incorporated into a single resin, such resin is tenhed as a
in Chemistry mixed bed resin. As their names indicate, the cation exchange resins and the
anion exchange resins exchange their H+ and OH- ions with the cations (e.g.,
~ a ' ,ca2+,M ~ " , etc.) and the anions (e.g., C1-, HCO; ,SO:-, etc.) present in
tap water:

R-H + ~ a 'd RNa + H+

2R-H + ca2' d R2Ca + 2H+
2R-H + M ~ *------+
+ R2Mg + 2H+

R'-OH + C1.- d RrCl + OH-

R'-OH + HCO; -+RrHC03 + OH-

H' + OH- H20

Thus, after passing tap water first through a bed of cation exchange resins and
then through a bed of anion exchange resins pure water (free from ionisable
impurities) is obtained. The purity of the deionised water is monitored by a
electrical conductivity meter. As you know, pure water is a very poor \

conductor having a conductivity of less than 30 microsiemens per centimetre.

But, water containing ions is a better conductor. Therefore, an increase in the
conductivity of the water coming out of the deioniser indicates that some of the
impurities in the feed water are passing straight through the bed of the resin,
which has become exhausted.

The exhausted cation exchange resin can be recharged by passing a 30%

solution of commercial hydrochloric acid through it. The H+ ions replace the
metal cations and the cation exchange resin is charged again:
RNa + H+ 4 RH + ~ a +
R2Ca + 2 ~ ' ----+
2RH + ~ a "

The resin is finally flushed with pure water to remove excess of acid from it.

The exhausted anion exchange resin can be similarly recharged by passing a

8% solution of sodium hydroxide through it. The OH- ions replace the anions
and the resin is recharged:

R'C1 + OH-
I
*R'OH + C1-
&So4 + 20H- 2RrOH + SO:-
The resin bed is finally flushed with pure water to remove excess of alkali
from it.

Thus, pure water can be conveniently prepared by distillation or by using a

deioniser. But, ion-exchange resins are expensive, deionisation is an expensive
means of producing pure water.

5.3 REQUIREMENTS - - -

1. Water still 1 No.

 Experiment 5
2. Deioniser Unit 1 No.
3. 30% Hydrochloric acid
4. 8% Sodium hydroxide

,,5.4 PROCEDURE
5.4.1 Preparation of Distilled Water
Take a water still. Although designs of stills vary, they all have the same
basic features as shown in figure given below.

Cooling w a l e ? cut.

Condenscf
I-

C o o l ~ ~ rw;llov
y In

O t , l l ~ llor cli.;l!!led W:~IPI/--

1
Boiler

Cunslanl level device -

Fig.5.I: A water still.

The still is normally plumbed into the cold water supply. If it is not,
connect the still into the cold water tap by means of plastic or rubber
tubing. Wire the tubing on to the tap and the connecting points on the
still so that any increase in water pressure will not blow the tubing off.
When using a still, turn on the cold water supply before heating, and
after use turn off the heating before the water supply. This prevents the
boiler accidently boiling dry. Electrically heated stills usually have a cut-
out-device incorporated in the element, similar to electric kettles.
When distilled water is being produced, adjust the rate of flow of the
feed water so that the waste water is merely warm to the touch.
If the tap water is hard, you will need to descale your still at intervals, the
frequency depending on the hardness of the water. Do not allow the scale
to accumulate as it reduces the efficiency of the boiler and it can cause
localised "hot spots" on electric heating element which may damage
them. Although the scale, consisting mainly of metal carbonates, is
soluble in mineral acids, but you should not use mineral acids on metal
heating elements or in metal boilers. Instead a solution of citric acid
should be left to stand in the boiler overnight.
Basic Experiments 5.4.2 Preparation of Deionised Water
in Chemistry
A deioniser unit generally consists of two low density polythene cylinders
which are filled with cation and anion excharge resins. The cylinders are
connected in series by means of flexible tubes and a hard rubber multivalve
block incorporating four rubber diaphragm valves. The cylinders are firmly
mounted on a mild steel tubular PVC coated frame work supported on a mild
steel under frame having wheels for easy movement of the unit from place to
place.

Some deioniser units consist of only a single cylinder filled with a mixed bed
ion-exchange resin which is capable of exchanging both the cations and
anions.

The frontal panel, which is made of mild steel, is fitted with the multi valve
block and a conductivity meter, which is connected to a 2201230 volt single
phase AC line and a conductivity cell. The conductivity cell is fitted in the
treated water outlet line of the anion exchanger. The conductivity meter has a
range of 0-40 microsiemens/cm.

Go through the instructions about operating and recharging the deioniser unit.
The instructions are given in the manufacturer's manual of the unit. Operate
the unit accordingly. See that the conductivity of the deionised water is below
30 microsiemenslcm. If it is more, it indicates that the resins have been
exhausted. Recharge the resins as per the instructions given in the manual.

5.5 SUMMARY
In this experiment, you would have performed the following:
handled and operated a water still,
prepared distilled water,
descaled the water still,
operated a water deioniser unit and prepared deionised water,
recharged the resins of the deioniser unit.