UNIT 1 BASIC LABORATORY SKILLS

Structure
1.1 Introduction
Objectives

Laboratory Safety and First Aid

Titrimetric Analysis
Types of Titrat~ons
Apparatus for Titrimetric Analysis
Carry~ngout a Titration

Weighing a Substance
Expression of Concentration
Preparation of Standard Solution
Titrimetric Calculations
Heating Methods
Use of Thermometers
Filtration
Summary
Answers

1.1 INTRODUCTION
In this introductory unit, we shall describe some of the experimenial techniques.
You are going to use these techniques during this laboratory course. Therefore,
you must understand the principles behind these techniques. In some cases, the
required apparatus for an experimental technique will also be discussed.

We shall start with a discussion on laboratory safety and first aid. We shall explain
the main features of titrimetric analysis. We shall then state the method of finding
the mass of a substance using an analytical balance; this discussion will help you in
understanding the method of preparation of standard solution. The use of
thermometers will be illustrated with reference to the determination of melting
point of a substance. Finally the method of filtration will be explained.

Objectives
After studying this unit, you should be able to:

state the measures to be taken under laboratory safety and first aid,
explain the types of titrations and the principle of titrimetric analysis,
discuss the method of using an analytical balance for weighing a substance,
state the different ways of expressing the concentration,
explain the method of preparation of a standard solution
carry out titrimetric calculation using the given data,
 Laboratory skills and state the method o f determination of melting point of a substance, and
Techniques
explain the technique of filtration.

1.2 LABORATORY SAFETY AND FIRST AID

Laboratory is a place for learning the experimental skills. You are strongly advised
to be careful at all times. It is recommended not to perform unauthorised
experiments. This will ensure your safety as well as the safety of your
fellow-students. Even a small accident involving minor injury must be reported to
the counsellor. The following instructions should be observed during the laboratory
work.

i) You must wear a laboratory coat or apron over your clothes while working in
the chemistry laboratory. This will save you from injury and protect your
clothes from damage.

ii) Handle the hot glass carefully; it cools very slowly and may be very hot
without appearing so.

iii) Protect your eyes from any spurting of acid o r a corrosive chemical. In case
of such spurting into the eyes, immediately wash with lot of water and go to
a doctor.

iv) You must not reach across lighted burners as it may result in an accident.

v) Wash your apparatus thoroughly with a washing powder.

vi) While heating substances, do not point the tube towards your neighbour or
to yourself. A suddenly formed bubble may eject the contents violently and
dangerously.

vii) When diluting sulphuric acid, pour the acid slowly and carefully into the
water with constant stirring. Never add water to the acid as it may result in
the liberation of a lot of heat.

viii) Read the label on the bottle carefully before usinglhe required chemical.
Never pour back the unused reagent into the bottle.

ix) Never touch or taste a chemical or solution as most of chemicals are either
corrosive or poisonous.

x) Always bring your container to the reagent shelf and do not take the bottles
to your desk. .

xi) Do not insert the pipette or dropper into the reagent bottles; rhis helps in
avoiding any possible contamination.

xii) Graduated cylinders and bottles are not to be heated because these break
very easily and their volume also changes.

xiii) At the end of the experiment, clean and dry the glass apparatus and wipe off
the top of the working table. Ensure that the gas and water taps are closed
before you leave the laboratory.

Laboratory First-Aid

I If a corrosive substance falls on your skin, immediately wash the spot with large
quantities of water, followed by remedial action indicated below:
 Basic Laboratory Skills
Acid spill : Trea: with sodium bicarbonate or ammonium carbonate (2M) solution;
then apply vaseline or a soothing cream.

Base spill : Treat with acetic acid (1 M) followed by vaseline or a soothing cream. 'M' is a unit for concentration.
You will understand this unit
Bromine : Treat with 2 M ammonia; keep the affected part dipped in dilute sodium inSec.1.5ofthisunjt.

bisulphite solution till bromine is washed off. Finally apply vaseline.

Phenol : Wash with ethanol and then take hospital treatment.

The most common accidents in the chemistry laboratory involve cuts, burns o r fire.
The first-aid to be given in each case is below :

Cuts : If you have a cut, wash the wound well with cold water immediately. If
bleeding is severe, apply pressure directly on to the wound to stop the bleeding.
Then an antiseptic cream can be applied to the wound; it should be followed by
proper dressing of the wound.

Burns : Wash the burnt part with cold water for sometime and then apply Burn01
to it.

Fire : A small fire in a beaker, caused by the vapours of an imflammable liquid can
be extinguished by covering it with a watch glass. If the clothes catch fire, one
should lie on the flow and, fire can be put off by wrapping a thick blanket around
the body.

- - -

During this laboratory course, you will be often doing titrimetric analysis.
Titrimetric analysis generally consists in determining the volume of a solution of
accurately known concentration which is required to react completely with a known
volume of the solution of a substance being estimated. The solution of accurately
known concentration is called the standard solution. The standard solution
contains a definite amount of the solute per litre (dm3) of the solution. The term,
--,
volumetric analysis, is also used in the place of the term, titrimetric analysis.

Titration is the process of adding a standard solution to a test solution (or vice
versa) until the reaction is just complete. The p o h t at which the completion of
reaction occurs. is called the equivalence point o r the end point. Let us explain
these two terms. The stage at which the reacting solutions are used up in their
stoichiometric proportions is called the equivalence point. The detection of
equivalence point is often done using instrumental measurements at various stages
of titration. Conductometer and mV/pH meter are two such instruments used for
the determination of equivalence point. In experiments 2 and 3 of CHE-03 (L)
course, their usage in titrimetric analysis has been illustrated.
Let us now explain the term, the end point. Sometimes it is possible to use a
substance to indicate the completion of titration. Such a substance is called an
1 indicator and the equivalence point determined using an indicator is called the end
point. An indicator indicates the completion of reaction by a ckdnge in physical -
/ property such as colour. The basic requirement for an indicator is that its colour

! should be quite different before and after the end point. Ideally, end point should
be.close to the equivalence point. But the colour change occurs only after the
equivalence point; hence the end point differs at least slightly from the equivalence .
point. A well known example of indicator is phenolphthalein used in acid-base
titration. It is pink in basic solution and colourless in acidic solution. In
I
 Laboratory skills and experiments 1 , 4 , 9 , 10 and 11 of CHE-03 (LJcourse, the use of indicators for
TecMques
titrimetric analysis has been explained.
For carrying out the titrimetric analysis of any given substance, a reaction must
satisfy following conditions:
a) The substance to be estimated must react completely with another of known
strength in stoichiometric proportions.

b) There must be a simple and instantaneous reaction.

c) An indicator may be used for identifying the completion of titration by the
change in colour of the solution. In the absence of indicators, instrumental
method should be available to conduct a titration.
Next let us discuss the types of titrations.

1.3.1 Types of Titrations

There are four main types of titrations as given below.
a) Neutralisation titratlon or acid-base titration

Neutralisation titration involves the titration of a base with an acid. The reaction
essentially involves the combination of hydroxyl ions with the hydrogen ions to .
form water. A typical example is the titration of sodium hydroxide against
hydrochloric acid.

b) Precipitation titration

Precipitation titration results in the formation of a precipitate. An example for this

type is the titration of silver nitrate against sodium chloride.
c) Oxidation-reduction titration

Oxidation-reduction titration involves the change in the oxidation number or

transfer of electrons among the reacting substances. The principal oxidising agents
are potassium permanganate, potassium dichromate, iodine and potassium iodate.
The reducing agents are ferrous and stannous compounds , oxalic acid and sodium
thiosulphate.

A typical example of this type is the titration of potassium permanganate against

ferrous ammonium sulphate.
d) Complexometric titration

In complexometric titration, a complexing reagent forms complex ions with metal

ions like ca2+ and M ~ ~Sodium
+ . salt of EDTA(ethy1enediamine tetraacetic acid)
is often used as a complexing reagent in titrations.
The complexing reagent is also
HOOCCH2
called a ligand. A complex ion is a
metal ion with one or more ligands
\
N-CH2-CH2-N
/CH2C00H
bonded to it. H o o c c A 'cHzcooH
EDTA
\ Before trying to know how titrations are carried out, let us know some of the
apparatus used during titrations.
L

1J3.2 Apparatus for Titrimetric Analysis

The apparatus for titrimetric analysis is of three principal kinds:
(i) Volumetric flasks (ii) pipettes and (iii) burettes.
Let us discuss each of them.
i) Volumetric Flasks &sic hboratory skills

Volumetric flas'ks are used for the preparation of standard solutions and for
diluting the sample to known volumes. The volumetric flasks have a flat bottom,
pear shaped body and long narrow neck. These have a ring engraved around
their neck. When filled up to this ring, the volumetric flask contains the volume
of the liquid marked o n it. T h e volumetric flasks are of varying capacities such

++
as 100 cm3, 200 cm3, 250 cm3, etc. As an example, 100 cm3 flask is illustrated in
Fig. 1.1.

Fig. 1.1 : 100 cmJ volumelric flask.

In Sec. 1.6, we shall see the use of volumetric flasks in preparing a standard solution.
ii) Pipettes

Pipettes are used to transfer known volume df a liquid from one container to
another. A pipette usually consists of a narrow tube with a bulb in the middle. The
ring mark engraved on the stem indicates the length to which the liquid level must
be drawn to get exactly the volume of the liquid marked on the bulb. Some pipettes,
known as graduated pipettes, are calibrated so that any volume upto its maximum
capacity can be transferred. The pipettes of volume 1 cm3, 2 cm3, 5 cm3, 10 cm3,
20 cm3 and 25 cm3 are used commonly. As an example, 20 cm3 pipette is indicated
in Fig. 1.2 (a).

Fig. 1.2 : a) pipette; b) handllng a pipette

c) draining out the pipetbd solution.

Before using a pipette for transferring a liquid for estimation, it ha: to be

thoroughly washed with a good quality detergent, followed by pleniy of water and,
~sbarrtorysuls and finally with distilled water. It is then to be rinsed with a solution which is to be
TahnIqucs
pipctted. For rinsing, the solution is taken in a clean dry beaker. The pipette is
dipped into the solution and the solution is sucked into the pipette to fill it about
half its volume. The upper rip of the pipette (the suction end) is closed by the
. finger tip. The pipette is then taken out ad held horizontal between the two hands
. and rolled gently. This ensures the wetting of the walls of the pipette. Make sure
that the solution in the pipette does not reach the suction end. The solution is then
drained into the sink and the process is repeated. This completes the rinsing
process. Now we can use the pipette for transferring the solution for estimation.
The solution is drawn through the pipette past the ring mark. The suction end is
closed by the tip of the index fii~ger(Fig. 1.2 (b)). By rolling the finger-tip slightly,
excess liqbid is allowed to drain out until the meniscus descends to the ring mark.
Now the liquid in the pipette is allowed to drain out into the receiving vessel (Fig.
1.2 (c)). By touching the walls of the receiving vessel with the tip of the pipette, the
last drop is also transferred. Do not blow out the last drop.
iii) Burettes
Burette is a common device for measuring precisely the volume of a liquid used
during titration. There are two well-known types of burettes. The first type consists
of a calibrated tube with a narrow end to which a glass tubing is attached by means
of a rubber tubing. To the rubber tubing, a spring-clip is attached. When you press
the clip, the liquid flows out of the burette. In another type of burette, a stopcock is
used instead of sprin clip. The burette is graduated, the zero being at the top.
9-
Mostly we use 50 cm burette. For some titrations, we use 5 cm3 burette. A 50 cm3
burette is shown in Fig. 1.3 (a).

Flg. 1.3 : a) Burette (with II slopcock) b) using a p~lmllaxcard

c) eye level for burette rcadlng.
 Basic Laboratory Skills

Fig. 1.5 :Analytical balance;

(1) beam (2) pans (3) pointer (4) scale (5) rider-carrier (6) levelling screws (7) arrest-hob (8) rider.

graduated, with the zero of the scale at the center of the beam, with major divisions
reading 1 mg and the subdivisions reading 0.2 mg. Both ends of the beam are thus
graduated. So an analytical balance can weigh only up to an accuracy of 0.2 mg (or
0.0002 g). The balance is fixed inside a glass case. A rider-carrier is attached to the
case which is parallel to the balance beam and is slightly above it. An arrest-knob
for the beam-control is o n the outside of the balance case. The balance case is
supported on levelling screws. You will be provided with a set of weight box and
fractional weights (Figs. 1.6 (a) and (b)) for use on analytical balance.
'-.

Ylg. 1.6 :a) Weight box ~ n a b) rrnciiunal weights.

 Laborntory Skills and Using an Analytical Balance for Weighing
Techniques
Before using a balance for weighing, we have to examine whether the balance
functions properly. For this, first the side doors of the balance are to be closed. The
arrest-knob is to be slowly,and carefully turned counter-clockwise. When the
arrest-knob is turned fully to the left, the pointer starts swinging around the centre
of the scale. The first two swings are ignored. Then, starting with the third swing,
the extreme positions of the swing are noted for at least two more swings. The
readings.of the swings to the left and to the right must be equal o r can differ by one
unit only during each swing. If the readings to the left and right are much different,
the balance must be adjusted by means of the screws, for which you may request
your counsellor.

After adjusting the balance (if necessary), we come to actual weighing. For this
purpose, we use a glass or a plastic weighing bottle, Fig. 1.7. First of all, the
weighing bottle is weighed on a rough balance to find its approximate mass to the
nearest gram. Then the left side door of the analytical balance is opened and the
weighing bottle is kept on the left side pan and the door is closed. Through right
side door, weights equal to the approximate mass of the weighing bottle are
Fig. 1.7 :Weighing bottle. transferred to the right side pan from a weight box with the help of forceps and,
the right side door is closed.

The arrest knob is once again turned to the left and the movement of the pointer is
seen. If it moves more to the left, then the weights transferred are in excess of the
Always use forceps to transfer
the weights, Refrain from using mass of the bottle. In that case, some weights have to be removed . O n the other

sufficient and, we need to add more weights. Arrest the movement of the beam by
turning the arrest-knob fully towards the right and, open the right side door to add
or remove some weight(s), as the case may be. Recheck the movement of the
pointer by using the arrest-knob. Continue this process till the addition of 1 gram
weight makes the right hand pan heavier while its removal makes it lighter, e.g., if
the weight is say 15.5 g, then weight would be lighter and 16 g weight would be
heavier. After this, the fractional weights marked in mg, have t o be added in
decreasing order till the two sides are balanced. Do not use fractional weights less
than 10 mg; you should use a rider in such cases. A rider (Fig. 1.6 (b)) is a thin
A rider is used for mass metallic wire suitably bent to be seated on the beam of the balance. It is normally
adjustments be'ow mg(O.O1g). put on the right hand side of the beam with the help of the rider carrier. By varying
the position of the rider on the beam, the two pans are balanced.

Mass of the object =(Weights added in grams)

+(fractional weights added x 0.001) g
+(main division of the rider position x 0.001) g
+(subdivision of the rider position x 0.0002)g

Let us illuktrate the use of this formula. Suppose that while weighing an object, the
weights added to the right side pan are 15 g, 200 mg and 2 x 20 mg. Let the rider
position be 2 on the main divisions and 3 on the subdivisions.

Then the mass of the object

= 15 g + (240 x 0.001) g + (2 x 0.001) g + (3 x .0002) g

= 15.2426 g
Before filling the burette with a liquid, it has to be washed, first with a detergent,
followed by plenty of water and distilled water. 11 is then rinsed with the liquid
which is to be taken in it. For rinsing it, fill the burette to half its volume with the
liquid, rotate it repeatedly keeping it horizontal between the two hands; then drain
out the liquid. The burette is then vertically mounted on the stand and is filled
with the liquid through a funnel. After taking out the funnel, the meniscus is
adjusted to any definite graduation mark in the burette by drawing out the necessary
volume of the liquid through the stopcock (or spring clip). It is not necessary for the
meniscus to be at zero mark, since the volume delivered from a burette can be obtained
simply by noting the difference between the initial and final readings.

To avoid error in burette reading, you may make use of a parallax card. Parallax a

card is a small piece of cardboard covered with white paper in which the lower half
is blackened with ink. While reading a burette, adjust the dividing line at the same
level as the meniscus as shown in Fig. 1.3 (b).

In order to avoid the parallax, view the position of the burette such that the front
and rear levels of the liquid coincide, Fig. 1.3 (c). For accurate titration results, the
volume of liquid used for titration should neither be too large nor too small. Titre
value is obtained by noting the difference between the intial burette reading and
final burette reading (after titration).

1.3.3 Carrying out a Titration

In general, during titration, a standard solution taken in the burette, is added A solution for which the
concentration is known
dropwise to a test solution in the conical flask (Fig. 1.4).
accurately is called a standard
solution.

White paper
(for observing
colour change)

Fig. 1.4 : DeLivery of a Uquld rrom a burette

11
 Laboralory Skills and The purpose of the titration is to find the concentration of the test solution. The
Techniques
equivalence point (or the end point) is determined. The volume of the standard
solution delivered through the burette for attaining the equivalence point is known as
the titre value. From the titre value, the concentration of the standard solution and the
volume of the test solution, it is possible to calculate the concentration of the test
solution. The calculation part will be discussed in Sec. 1.7. In the next section, we shall
discuss weighing of a substance. This will help us in understanding Sec. 1.6 in which the
prcparation of standard solution is going to be discussed.

EAQ 1
Define the term, titrimetric analysis.

SAQ 2
You are given a solution of sodium hydroxide of known concentration and you are
asked to find out the concentration of given hydrochloric acid solution. Indicate a
method based on each of the following :

i) determination of end point

ii) determination of equivalence point

In the next unit, we shall discuss

SI units for various physical - - -- - - - - - - -

quantities. 1.4 WEIGHING A SUBSTANCE

Mass is the quantity of matter of
which the object is composed. The internationally accepted unit (SI unit) of mass is kilogram. One gram is
Mass of an object is same, one-thousandth part of one kilogram whereas o n e milligram is one-thousandth
irrespective of the location where part of o n e gram. In this laboratory course, you would b e measuring mass
it is weighed.
from a few milligrams t o grams. YO~Jwould b e using analytical balance for
Throughout this laboratory weighing.
course, w e u s e an analytical
balance to find the mass of an
An analytical balance (Fig. 1.5) can b e used for finding masses to a precision limit
object.
of 0.2 mg. As we proceed with the study of this laboratory course, you will notice
Weight of an object is the force
exerted on it by gravitational
that many experiments involve at least one measurement of mass. Hence the
attraction. The gravitational force accuracy of your experiment will depend largely on your skill of using the analytical
and the weight differ at different balance. The analytical balance actually compares the unknown mass of a sample
locations o n the earth. A spring with a standardised mass.
balance is used to find the weight
of an object. In an analytical balance, (Fig. IS), two pans are suspended from the ends of the
balance beam. A pointer is attached to the center of the balance beam and it
projects down to a scale at the base. The upper edge of the balance beam is
 Basic Laboratory Skills
You have, s o far, seen how to weigh an object, such as a weighing bottle, accurately.
If we want to weigh a substance in the weighing bottle, we make use of the method
of weighing by difference. For this, the weighing bortle is first approximately
weighed. The substance to be weighed is put into the bottle (a little more than Mass of the substance (m g)
required) and weighed accurately (x g). T h e substance is transferred into a = (Mass of the bottle wlth
volumetric flask and the bottle is again weighed accuracy O, g). The difference substance (x g))
between the two masses, i.e., (x-y) g is the exact mass of the substance transferred - (mass of t h e bottle after
(m g)- transferring the substance Cy g))
i.e., m =(x-y) g
You are advised to observe following precautions for getting accurate results during
You w ~ l see
l the way of entering the
weighing : data for weighing towards the end
of Sec. 1.6.
a) Ensure that your balance is in good condition. In case there is any
malfunclioning, it may be reported to the counsellor.

b) Clean the pans. Never release the beam arrest-knob abruptly as this may
damage the balance and you may not get reliable results.

c) Arrest the beam before adding o r removing either the sample o r the weights.

dj Never place the hot objects for weighing on the balance. An object must be
cooled to attain the room temperature before weighing.

e) Always shut the doors of the balance before raising the pans using the
arres t-knob.

f) Handle the sample with a piece of paper. The weights must be picked with
forceps only.

g) Avoid jerks to the balance.

Having learnt in general about some apparatus t o be used in the experiments of

this lab course, let us now understand the various terms and concepts used in many
of the experiments. Before proceeding to the next section, try the following SAQ's.

SAQ 3
What is the precision limit of an analytical balance ?

SAQ 4
What is the mass of a substance if the following weights are needed to weigh it ?

g mg position of rider
10
5 200 6.1
1,nburatorj Skill!. anid
~ecdni~ues
1.5 EXPRESSION OF CONCENTRATION
The term 'concentration' refers to the relative amounts of a solute and a solvent in
a solution. Solute is the dissolved substance in a solution. Solvent is the substance
in which the solute is dissolved. Solution is the homogeneous mixture of a solute
and a solvent. Before we discuss the different ways of expressing the concentration
The number of 12catoms in of a solution, let us explain a few terms used in quantifying a substance.
0.012 kg (i.e., 12 g) of lLcis
equal to 6.022 x
Mole, denoted as mol, is the amount of a substance that contains as many
elementary entities as in 0.012 kg of 'Fc isotope of carbon. The mole may be of
atoms, ions, molecules, electrons or any other entity. The number of elementary
entities in a mole of any substance is fixed and is given by a constant called the
Avagadro number, N A , which equals 6.022 x

Relative molecular mass (molecular weight) denoted as Mr is the mass of one

Relative molecular mass is molecule in atomic mass unit (a.m.u.) relative to 1112th the mass of pure 12c
since it a isotope (12.000 a.m.u.). We find the relative molecular mass by multiplying the
ratio.
atomic mass of each element in the molecule by its subscript in the formula and
then adding the total for each element to get the grand total, e.g., one molecule of
C 0 2 has relative molecular mass of 44, which is calculated as :

Although SI unit of molar mass is [(I2 x 1) + (16 x 2)] = (12 + 32) = 44

kg mol-', it is more convenient to
use g mol-' for titrilnetric Molar Mass, denoted by symbol (M,), is the mass of one mole of a given
calculations. substance. It is numerically equal to the relative molecular mass but is expressed in
g mol-' units. The following illustration explains this point.

The relative molecular mass of oxalic acid dihydrate [(COOH)2.2Hz0] crystals is

I t is better to use the phrase equal to 126. Hence, the molar mass of oxalic acid dihydrate crystals = 126 g mol-l.
'amount of a substance' rather
than 'number of moles of a Amount of a substance is given by the ratio of the mass of the substance to its
substance'. molar mass.

Mass
Amount of a substance =
Molar mass

Thus the amount of substance having mass equal to molar mass is called mole. Let
us now see various methods of expressing the concentration of a solution.

Molarity .

For titrimetric purposes, we express concentration in terms of molarity denoted by

symbol M. Molarity is defined as the amount present in one dm3 of the solution. It
can be expressed as follows:

Amountof solute
Molarity =
Volume of solution in dm3

Thus, if you dissolve 126 g of oxalic acid dihydrate (molar mass = 126 g mol-l) in
water and make up the volume to 1 dm3, then the solution would be 1 M.

The molarity of a solution containing m g of the solute in V cm3 of a solution can

be calculated as folkows :

Let the molar mass of the solute be M, g mol-l.

Using Eq. 1.1,

 Basic Laborntory Skills
amount of a solute =
Mass -
- mg
Molar mass M, mol-'

Volume of the solution = v c m 3

Since ZOO0 cm3 = 1 dm3,
. .
1dm3
Volume of the solution = vcm3 x
1000 c n 3

Using Eqs. 1.1 to 1.4,

Amount of solute
molarity of solution =
Volume of solution in dm3
m mol
=- x 1
Mm V

1000 m mol dm-3

i.e., molarity = - . . . (1.5)
M m v

By substituting the volume of a solution in cm3 unit in the above expression,

molarity of a solution can be calculated.

Though molarity is accepted nowadays as the way of expressi~~g concentrations,

another related term, viz, normality is still in use. Here equivalent mass is used in
C
place of relative molecular mass. Normality is defined as the number of gram
equivalents of the solute per dm3 of the solution. In other words,

Normality =
Numberofgram equivalentsofsolute -
- Mass
Volume of solution(in dm3) Equivalent mass x volumeof solution(in dm3) W e a r e not discussing the
methods of arriving a t the
The molar mass of a substance is an inherent property. It is independent of the equivalent masses of substances,
nature of the chemical reaction ir may be undergoing. Hence, a given solution since we a r e not going to use
containing a known amount of the solute will have the same molarity independent in Our

of the type of chemical reaction. Normality, on the other hand, can change as the
equivalent mass of a substance depends on the chemical reaction involved in the
titration. For example, KMnO, can have equivalent mass of 158.04 g, 52.6 g or 31.6
g depending on the reaction conditions. In the light of the above, it is advisable to
I;se molarity rather than normality. We would be using molarity in all the
titrimetric experiments. However, percentage, formality and molality, are some
other ways of expressing concentration. These are briefly explained here.

Percentage

The percentage of a solute in a given solution can be expressed in three different

ways depending upon the nature of the solute and the solvent. Let us illustrate by
taking some examples.

(a) If we take 10 g of, say, NaCl and dissolve it in water to make a solution of
volume 100 cm" then we get a 10% mass by volume, i.e., 10% m/V solution
of NaCl in water.
(b) If instead of preparing 1(X) c m h f solution, we add enough watcr (to 10 g of
NaCl) to prepare 100 g of solution, then we get 10% mass by mass, i.e. 10%
m/m solution of NaCl in water.

(c) In cases where the solute is also a liquid, it is possible to represent

concenlration as volume by volume. For examplc, if we mix 10 cm%f
methanol (solute) with enough H 2 0 (solvent) to prepare 100 cm3 of thc
solution, then we gel IU46 volume by volume, i.e. 10%) VV/ solution of
methanol in water.

W e shall use percenlage units for denoting the concentration of solutions in Units
5, 12 and 13 of this course.

Formality

For certain ionic compounds, e.g., NaC1, which are completely dissociated in
solution, it is less accurate to talk in terms of (molecules or) molar mass. Here, it is
more appropriate to talk of formality than of normality o r molarity. Formality is
defined as the number of gram formula masses dissolved per dm3 of the solution.

Mass
Formality of a solution (F) = - --
of the substance in gram unit
Gram formula mass

1
X ... (1.6)
Volume of the solution in dm%nits

The gram forniula mass of a substance is obtained by multiplying the atom'ic mass
of each element by its s u h ~ c r i p in
t the formula and the11 adding lhc tolal for cach
element tu get the grand total. Thus, o n e gram formula mass of sodium chloride
= [(I x 23) +
( 1 x 35.45)] g = 55.45 g

Molality

T h e molality of solution is the number of moles of the solute per kilogram of the
solvent contained in a solution. It is given by the following expression :

m , x 1000
Molality = -
m2 X M ,

whcre.
m 1 = p a s s of the solute (in g)

I"
nl2 = ass of the solvent (in g)
M , = Molar mass of lhe solute (in g mol-')
I
The molality scale is useful for experiments in which depression of freezing point,
elevation of boiling point, and relative lowering of vapour pressure, a r e measured.
For example, we shall see its use in Unit 8.

Calculate the molarity of a sodium hydroxide solution, if 500 cm3 of the solution
contains 2 g of solute.
 Basic Laboratory Skills

1.6 PREPARATION OF STANDARD SOLUTION

You may recall that a standard solution is one for which the concentration is
known accurately. A standard solution may be prepared by dissolving an accurately
weighed, pure stable solid (solute) in an appropriate liquid solvent. Preparation of
a standard solution is generally the first step in any quantitative experiment; hence
it is important to know how to prepare a standard solution.

Primary and Secondary Standards

In titrimetry, certain chemicals are used frequently in known concentrations as

reference materials. Such substances are classified as primary standards or
secondary standards. A primary standard is a substance of sufficient purity. A
standard solution can be prepared by weighing a quantity of the primary standard
directly, followed by dissolution and dilution to give a definite volume of the
solution. The following specifications have to be satisfied for a substance to qualify
as a primary standard:

1) It must be easily available and easy to preserve.

It should not be hygroscopic nor should it be otherwise affected by air. Hygroscopic substances are
2)
those which have a tendency to
It should be readily soluble in the given solvent. absorb moisture.
3)
Some of the available primary standards for titrations are given below along with
their relative molecular mass (M,) values:

Potassium hydrogen phthalate (KHP), C8H504K Mr = 204.2

(an acidic substance)

Anhydrous sodium carbonate, Na2C03 Mr = 106

(a basic substance)

Potassium dichromate, K2Cr207 (an oxidising agent) Mr = 294.2

Arsenic (111) wxide, As203 (a reducing agent) M, = i97.6

Potassium iodate, K103 (an oxidising agent) Mr = 214.0

Sodium oxalate, Na2C204 (a reducing agent) Mr = 134.0

Solutions prepared from the primary standards are called pri~liarystandard

solutions.

Substances which do not satisfy all the above conditions, are known as secondary
standards. In such cases, a direct preparation of a standard solution in not possible.
Examples are alkalies and various inorganic acids. These substance cannot be
obtained in pure form. Therefore, concentration of these substances is to be
Alkalies (sodium hydroxide and
determined by titrating them against primary standard solutions. This process is potassium hydroxide) are
called standnrdisation and, the solution so standardised is called a secondary hygroscopic. Further, these absorb
standard solution. Now let us discuss the method of preparation of a standard carbon dioxide from air and, some
solution. part of the alkalies get converted
into carbonates. Hence, alkalies
To prepare a standard solution of volume, V cm3, of known molarity, M mol dm-3, cannot be used as primary
standards.
the mass of the solute required, m g, of molar mass Mmcan be calculated by
rearranging Eq. 1.5 as follows:
 LPboraiory S k i b and
Techniques Molarity. M,, .V.
Mass of the solute ( m ) =
1000

T h e solute is weighed in a n analytical balance a s explained before (Sec. 1.4),

transferred into a volumetric flask with the help of a funnel and dissolved in a small
quantity of the solvent. T h e solution is then made u p to the mark by carefully
adding the solvent. This can b e done using a wash bottle o r with a pipette. It is then
shaken thoroughly to get a homogeneous solution.

In preparing a standard solution of conccntration, say, around 0.1 M, the mass of

the substance weighed need not he exactly equal to the mass required for 0.1 M. It
can be slightly less o r more, but the weighing must be accurate. F r o m the mass of
the solute actually taken, molarity of the solution can bc calculated using Eq. 1.5.

In t h e example given below, we show how to enter the data for

weighing potassium hydrogen phthalate (for preparing a standard solution) and,
calculation of molarity of the solution.
Preparation of 250 cm3 of a standard solution of potassium hydrogen phthalate
Approximate mass of the weighing bottle = rill = ........... g
Mass of the weighing bottle + potassium hydrogen phthalate = nl2 = ............ g
Mass of the bottle after transferring the salt = m3 = ............... g
Mass of potassium hydrogen phthalate = m2 - ni3 = m = ................ g
Molar mass (M,,) of potassium hydrogen phthalate =204.2 g mol-'
Volume of potassium hvdrogcn phthalate solution prepared = 250 cm3
Molarity of potassium hydrogen phthalate ( M I )is calculated using Eq. 1.5 as,
m x 1 0 0 0 =--
nix4
MI =
M , x 250 204.2
- ..........mol dm-3

SAQ 6
You are asked to standardise the solutions of lollowing substances. Suggest a
primary standard for cach.

(i) hydrochloric acid

(ii) potassium permanganate (an oxidising agent)

1.7 TITRIMETRIC CALCULATIONS

You may be interested to know as to how titrimetric calculation is done. For this
purpose, let us consider the general case of a reaction between two substances, A
and B, yielding C and D, as per the stoichiometric equation:

whcrep, y, r a r ~ ds are rne stoichiometric coefficients. As per Eq. 1 . 9 , ~n1vic.s of A

are required for q moles ol'B for complete reaction. A t any instant, the aniount ol'
a A and B reacted are related as lollows:
 m o u n t of A reacted -
- P_
Amount of B reacted q

Suppose that during titration, VA cm3 of A of molarity M A has reacted with VB cm3
p and q are known, once
of B of molarity MB.
stoichiometric equation is
written.
Amount of A reacted = Molarity of A x volume o t A in dm3
(using Eq. 1.2)
=MA-VA/lOOO . . . (1.11)
[since V A is given in cm3 units] .

Similarly, amount of B reacted

= Molarity of B x volume of B in dm3

Using Eqs. 1.10 to 1.12,

M A VA/lOOO p
We get,
MB VB/lOOO = q

Assume that a standard solution of A ( M A known) is available. The volume of A

(VA) required to react with a known volume of B (VB) is found out by titration.
Sincep and q are known from the stoichiometric equation, the molarity of B ( M B )
can be determined using Eq. 1.13. See the following examples.

I (i) The reaction between sodium hydroxide and potassium hydrogen phthalate

Sodium hydroxide and potassium hydrogen phthalate ( K H P ) react according to the

I equatioc:

I COOK
+ NaOH - COONa

COOK
+ H,O
I
By comparison with Eq. 1.9,
p = Coefficient of K H P = 1
q = Coefficient of NaOH = 1

Let the molarities of potassium hydrogen phthalate and sodium hydroxide solutions
be represented as M Iand M 2 . Let the volumes of these two solutions used during
I
neutralisation be Vland V2, respectively.
Using Eq. 1.13,

The tabulation of titration data and calculation method for the standardisation of
sodium hydroxide solution using standard potassium hydrogen phthalate are given
below:
b
Laboratory Skills and Indicator Phenolphthalein
Ttcbnlqurs
Colour change : Colourless to pink

Potassium hydrogen phthalate vs. sodium hydroxide solution

S1. No. (Volume of potassium Burette Reading (Volume of

hydrogen phthalate)/cm3 NaOM) / cm3
Initial Final

Determination of molarity of sodium hydroxide solution

Molarity of potassium hydrogen phthalate = M I = .....tnol dm-3

Volume of potassium hydrogen phthalate solution = V I = 20 cm3

Volume of NaOH solution used (from the above table) = V2 = ..... cm3
Molarity of NaOH solution = M2 = ?
Using Eq. 1.14,
Mi VI = Mz Vz
Ml Vl
Molarity of NaOH solution = M2 = -
v
2
-- ..... moldm 3
Since MI, Vl and V2 are known, M2 can be calculated.

. ii) The reaction between oxalic acid and potassium permanganate in presence
of dilute sulphuric acid

The stoichiometric equation for this reaction is given below :

Here again, p = Coefficient of H2C204 = 5 and

q = Coefficienr of KMn04 = 2

Using Eq. 1.13,

M ~ ~ n v0 ~4 ~ n 0-4

For this case, we do not intend giving the tabulation of titration data. But we
illustrate the use of Eq. 1.15 in the calculation of molarity of oxalic acid. Assume
that 25 cm3 of oxalic acid of unknown concentration requires 20 cm3 of 0.02 M
potassium permanganate for complete reaction.

5 MKM~O
V ,~ ( M ~ O ,
Using Eq. 1.15, MHtCZo4 =
v~2GLo4
 MH C 0 = 0.04 M
2 2 4

Thus the molarity of oxalic acid is 0.04 M.

Based on the study of Secs. 1.3-1.7,we can sum up the steps involved in the
titrimetric estimation of a test solution using primary and secondary standards. T o
illustrate the steps, we consider the estimation of given ferrous sulphate solution.
Assume that oxalic acid is used as a primary standard while potassium
permanganate solution is used as a secondary standard.
Step Illustration

1. Weigh the necessary amount 1. Weigh the necessary amount of oxalic

of the primary standard. acid crystals.

2. Prepare the solution of 2. Dissolve the oxalic acid crystals in

primary standard from the water and make up to known volume
amount weighed in step (i). t o prepare a standard solution.

3. Titraie the secondary standard 3. Titrate potassium permanganate

against the primary standard solution against standard oxalic acid
asing proper medium. From solution in presence of dilute
the titre value, calculate the sulphuric acid. Calculate the
concentration of secondary concentration of potassium
standard (using equation permanganate solution
similar to Eq. 1.13). (using Eq. 1.15)

4. Titrate the secondary standard 4. Titrate potassium permanganate

against the test solution solution against ferrous sulphate
using proper medium. solution in presence of dilute
Calculate the concentration sulphuric acid. Calculate the
of test solution (using concentration of ferrous sulphate
equation similar to Eq. 1.13). solution using the following equation.

(Write the balanced equation for

FeS04-KMn04 reaction and verify
this equation).

Based on the study of this section, answer the following SAQ.

SAQ 7
Write an equation similar to Eq. 1.14 for the reaction between sodium carbonate
and h-fdrochloric acid.
laboratory S W and
~echniques 1.8 HEATING METHODS
- --

In this lab course, you will use the follbwing heating devices:

i) burner

ii) water bath

iii) oil bath

Since many of the substances get decomposed at high temperatures or are

inflammable, care should be exercised in using the heating devices.

Direct heating on a burner flame should be avoided as far as possible. Heating on a

burner should be done using a wire gauze. While using a burner, all inflammable
and volatile materials should be removed away from the burner.

A water bath, an oil bath or a sand bath should be used to provide uniform heating.
For temperatures upto 100°C, a water bath is generally employed. The simplest
form of a water bath consists of a beaker containing water. Water is boiled in a
beaker and, the vessel to be heated is kept on the rim of this beaker. If a test tube

'4
or a boiling tube is to be eated, it can be kept immersed in it as such or by
clamping it using a stand. You may be using an electrically heated water bath or a
copper water bath (which can be heated on a burner). These two water baths are
shown in Figs. 1.8(a) and (b).

Each of these water baths is covered with rings, which can be adjusted according to
the size of the vessel to be heated.

(3)

Fig. 1.8 a) : Eleclrically healed waler bath b) copper water balk

 Basic Laboratory Skills
An oil bath o r a sand bath is used when heating is carried out in the range
100-200°C. An oil bath can be made by filling a copper bowl with a liquid like
paraffin oil. A sand bath is a shallow iron plate filled with sand. Both these baths
are heated by means of a burner.

SAQ 8
3
It is proposed to study the miscibility of 10 cm- mhtures of phenol and water at
different volume by volume percentage con~positionsin the temperature range 35°C
and 75°C. Suggest a simple heating arrangement for this experiment.

1.9 USE OF THERMOMETERS

Temperature measures the degree of hotness of a body. Temperature scales such as
celsius scale are, in general, empirical and arbitrary. The thermodynamic scale or Unit (Block 2) of Physical
the kelvin scale, is based on the second law of thermodynamics. It is independent of chemistry course, thermodynamic
the properties of any particular substance. It is defined in terms of the efficiency of scale o f has been
explained.
a thermodynamically reversible heat engine. The temperature in the kelvin scale ( T
K) and that in the celsius scale (t°C) are related as follows :

The kelvin scale of temperature suffers from lack of convenient instruments for
measurement. In this course, we shall use thermometers calibrated in celsius unit.
Typical examples are mercury thermometers. We shall be using 0-360°C and
0-1 10°C thermometers. The former is sensitive to 1°C, whereas the latter is
sensitive to O.l°C. We shall be using thermometers for various purposes. Some of
them are given below :

i) For determining the hea't qpacity and the enthalpy of neutralisation (Unit 7)

ii) For determining the melting point (for estimating the molar mass of a
nonvolatile solute using Rast method) (Unit 8)

/ iii) For obtaining the phase diagram of a given system,(Units 12 and 13)

iv) For studying the rate of a reaction (Units 15 and 16)

To illustrate one of the above mentioned uses of thermometers, we shall discuss the
I method of finding out the melting point of a substance.
I
Determinatioa o f Melting Point

The melting point of a solid is that temperature at which the solid changes into The freezing point of a substance is
that temperature at which a liquid
liquid at one atmosphere pressure. A pure solid.has r sharp melting point. For a
changes into a solida t one \
pure solid, the difference between the temperature at which the collapse of the atmosphere pressure. The freezing-
t crystal is first observed and the temperature at which the sample becomes point of a substance in the liquid
completely a liquid, does not exceed by 0.5"-1.0". But an impure solid melts over a State is the same as its point
in the solid state. This principle is
range of temperatures, depending on the amount of the impurity. Let us now made use of in Unit 8 of this courk.
discuss the experimental details for determining the melting point of a substance.
7C
 \
1
Laboratory Skills and
Melting points are usuallfdetermined in capillary tubes open to the air. A capillar)
Techniques
tube is a thin glass tube about 1-2 mm in diameter. For melting point
Melting point can arso be . determination, a capillary tube of about 8-9 cm long is taken and sealed at one end
determined by keeping the liquid by holding it horizontally into the edge of a small burner flame for a few seconds
bath in while rotating it. The molten glass would seal the capillary. Formation of large
i) a long-necked flask, known a s glass beads should be avoided. Let us now see how the capillary tube is filled.
Kjeldahl flask, or
ii) a 100 cm3beaker. About 25 mg of the dry substance is placed on a clean porcelain plate and finely
powdered with a metal or glass spatula forming it into a small heap. The open end
of the capillary tube is pushed into the powder, when a small amount of the powder
gets into the capillary tube. The solid is shaken down the tube by tapping the closed
end of the tube gently on the work-table. The process is repeated until the length of
the tightly packed material is about 3-5 mm. The outside of the tube is then wiped
clean.

The capillary tube can be heated in a liquid bath or o n an electrically heated metal
block. You may be using Thiele's melting point apparatus (Fig. 1.9), which is a tube
with a closed bent side-arm. O n heating the bent side-arm, the heated.liquid
circulates and rises the temperature of the sample. The tube is filled with the liquid
to just above the bent side-arm. No stirring is required. The bath liquid generally
The attachment of the capillary . used is liquid paraffin, which can be safely heated upto 220°C; above this
tube t o the thermometer through temperature it starts fuming and gets discoloured. Silicone oils, though more stable,
moistening is due to the
are expensive.
phenomenon of surface tension.
You will study the phenomenon
Into the melting point apparatus, the thermometer is fitted through a cork. A
of surface tension in Unit 4 of
this course. section of the cork is cut away, so that the thermometer scale is visible and the
If the arrangement used in your
heated air could escape. The filled capillary tube is moistened with the bath liquid
laboratory for noting the melting which helps in attaching the capillary tube to the thermometer. The filled capillary
point is different from the one tube is attached to the lower end of the thermometer in such a way that the
explained here, you can get the substance is at the level of the middle of the mercury bulb. The thermometer, with
details of using the same from
the capillary tube attached, is then inserted into the bath. Care is taken that the
your counsellor.
open end of the capillary tube is well above the level of the liquid.

Flg. 1.9 :Tblele's melting point apparatrb.

 T i e melting poing apparatus is heated with a small flame comparatively rapidly BM~C
LPbomry SUS

till the temperature is about 15" below the melting point of the substance. Later
it is heated slowly such that the rise of temperature is about 2" per minute. The
temperature at which the substance starts to melt and the temperature at which
it has completely liquified are noted. These two temperatures give the melting
range. As said above, for a pure compound, the melting range should not exceed
I 0.5" - 1". In case of an unknown compound, an approximate melting point may
be taken first.

The following precautions must be observed while determining the melting

point:

I 1. The capillary used must be of uniform bore.

,

I 2.

3.
The packing of the substance should be compact and uniform.

A sand bath must be placed below the melting point apparatus, in case the
bath liquid is concentrated sulphuric acid.

4. A section of the cork must be cut away.

5. The heating of the flask must be slow.

6. The substance should be dry.

In the next section, we shall discuss filtration.

1.10 FILTRATION
- -

Filtration is employed for separating a precipitate from a solution. For this, we

make use of a funnel, a circular sheet of filter paper, a stand, a beaker, a glass rod
and a wash bottle. A wash bottle is designed to deliver a fine stream of distilled
water In a controlled way. A typical wash bottle is shown in Fig. 1.10.

Flg. 1.10 :Wash bottle.

The first step in the filtration of a precipitate is to fold the filter paper properly
into halves along any diameter as shown in Fig. l.ll(a). The side holding three
quarters is opened to obtain a cone of the filter paper (Fig l.ll(b).

27
Laboratory SkiU.5 and
Techniques

Tear the corner here

Beaker with
Edges do na meet pmcipitate and
mother liqm

funnel

beaker

(4

F i g 1.11 :a) and b) Folding the fiitcr paper c) tearing the corner d) ZLHration set-up

In order to get efficient filtration, tear off the upper tip of the filter paper cone
(Fig,l.ll(c)) so that the cone fits into the funnel. Also a long stem funnel should
be used. The filter paper cone is fixed in the mouth of the funnel using a little
water. Now the funnel is placed on a stand with its stem touching the side of the
receiving vessel kept for collecting the filtrate. The mixture to be filtered is
poured into the filter paper gently along a glass rod, the lower tip of which rests
on three quarters of the filter paper cone (Fig.l.1 l(d)). The solid particles in the
mixture will be collected on the filter paper, while the filtrate will be collected in
the receiving vessel. At the beginning of filtration, the solid particles should be
allowed to settle down and the liquid should be decanted into the funnel, leaving
most of the precipitate in the vessel. The precipitate should be washed with the
wash-liquid, the solid again allowed to settle down and the l i p @ transferred to
the funnel. This process is repeated to free the precipitate of ot/er ions. Finally
the precipitate is completely transferred t o the funnel using more of
wash-liquid. Usually wash-liquid is water or a liquid in which the precipitate is
insoluble. Wherever quantitative estimation is done, proper filt9r paper is &I k q
*
used as per the advice of the counsellor.
 5 Bash L.barn(or~r
S W

1.11 SUMMARY
In this unit, we discussed the safety measures to b e adopted while working In a
chemistry laboratory. W e explained some of the techniques which a t e useful in
performing the experiments of this course. We also discussed the retevant
calculations and the apparatus for these experiments.

1.12 ANSWERS
Self Assessment Questions

1) Titrimetric analysis consists in determining the volume of a standard solution

which is required t o react completely with a known volume of the solution of
a substance being estimated.

2) i) Titration using phenolphthalein as an indicator

ii) Titration using conductometer o r mV/pH meter. I

3) A n analytical balance can be used for weighing masses to a precision limit of
0.2 mg.

1OOOnz
5) A s per Eq. 1.5, molarity = -
MmV

6) i) Sodium carbonate

ii) sodium oxalate

7 Cog
(from
+ 2 ~ +
(from
- H2C03

Na2C03) HCl)

Let MI and M 2 stand for the molarities of sodium carbonate and hydrpchloric acid,
respectively while Vl and V2 refer to the equivalent volumes of sodiu'm carbonate
and hydrochloric acid, respectively. In comparison to Eq. 1.13.

8) Mixtures of different compositions of phenol and water are t o be taken in

different test tubes and heated in water bath t o study the miscibility ,
temperature in each case.
 UNIT 2 HANDLING OF DATA
Structure
2.1 Introduction

2.2 S1 U n ~ t s
Basic Units
Derived Units
S1 Prefixes
Grammatical Rules for Representing S1 Units

2.3 Some Useful Mathematical Operations

Scientific Notation
Using the Table of Logarithms
Finding the Numbers from their Logarithms

2.4 Significant Figures

Calculation of Significant Figures in a Number
Addition and Subtraction Maintaining Significant Figures
Multiplication and Division Maintaining Significant Figures
Taking Logarithms and Antilogarithms Maintaining Significant Figures

2.5 Laboratory Note Book

2.6 Tabulation of Data and Plotting of Graphs

2.7 Summary

2.8 Answers

2.1 INTRODUCTION
In Unit 1, we studied some of the laboratory techniques which are to be used in
this course. As part of this, we discussed the methods of expression of
. concentration and, titrimetric calculation. These two are, in fact, part of data
handling techniques. Handling of data consists of processing the experimental data
and expressing the values of the physical parameters with proper magnitude and
units. processing of data includes stepwise calculation to obtain the value of a
parameter and representation of results using tables or graphs.

In this unit, we shall discuss the basic and derived SI units. We shall explain the
principles 'to be followed in qxpressing a number in scientific notation. We shall
define the term, significant figure. We shall explain how to maintain significant
- figures while doing qiIculations of various types such as addition. subtraction,
multipllcation, division, taking logarithms and antilogarithms etc. We shall finally
discuss how to record the obseivations, tabulate the data and plot the graphs.

Objectives
After studying this unit, you should be ableto
.
state the SI units of basic and derived physical quantities,
arrive at the SI units of a physical quantity,