Volumetric Analysis Precautions

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4.

3 Volumetric analysis
Learning outcomes
To understand the apparatus used in
volumetric analysis and correct
titrimetric procedure.

Students should know


the following key
words:
Volumetric analysis,titration,standard
and non standard solutions

Volumetric analysis
A titration is a lab procedure where a
measured volume of one solution
(burette) is added to a known volume
(flask) of another solution until the
reaction is complete

Standard solutions

A standard is a solution of precisely known


concentration
It must be available in a highly pure state
It must be stable in air
It must dissolve easily in water
It should have a fairly high relative
molecular wt
It should under go a complete and rapid
reaction

Non standard solutions


Sodium

hydroxide absorbs carbon


dioxide from atmosphere
HCl can produce chlorine gas in
reactions and liberate hydrogen
when exposed to air
Nitric acid can act as an oxidising
agent interfering with reactions
Sulphuric acid absorbs water form
the air

Na2CO3
1 mole

2HCl 2NaCl + H2O + CO2


2 moles
2 moles
1 mole
1
mole

EQUIPMEN
T

Apparatus used
Burette
Volumetric
Beaker
Pipette
Funnel
Indicator
White

tile

flask

Burette titration procedures

Precautions when using


equipment
Burette must be vertical, use and then
remove funnel, check meniscus, rinse
with de-ionised water and then given
solution.
In using a Pipette rinse with de-ionised
water first and then with given
solution. Check meniscus. Do not blow
out remainder of liquid into flask and
keep tip of pipette in contact with flask

Precautions
Conical

flask should not be rinsed


with solution it is to contain and swirl
In using a Volumetric flask the last
few cm must be added so that the
meniscus rest on calibration mark
Invert stoppered flask to ensure
solution is homogeneous/uniform

Why is a conical flask, rather


than a beaker, used in the
experiment?
To

allow easy mixing of the contents,


by swirling.

Why is the funnel removed


from the burette after
adding the acid solution?
So

that drops of solution from the


funnel will not fall into the burette.

In using a burette, why is it


important
(a) to rinse it with a
little of the solution it is
going to contain.
(b) to clamp it
vertically. (c) to have
the part below the tap
full?

Solution (a) Rinsing

To remove any residual water, and


so avoid dilution of the acid solution
when it is poured into the burette.

Solution (b) clamp vertically


To

enable the liquid level to be


read correctly

Solution (c) Full tap

To ensure that the actual volume of


liquid delivered into the conical
flask is read accurately.

The following procedures were


carried out during the
titration:
The sides of the conical flask

To ensure that all of the


acid added from the
burette can react with
the base.
To ensure complete mixing
of the reactants

Why is a rough titration carried out?

To find the approximate end-point.


This information enables the
subsequent titrations to be carried
out more quickly.

Why is more than one accurate


titration carried out?

To minimise error by getting


accurate readings within 0.1 cm of
each other.

Calculation example

Volume of acid Va
(cm3) is the
titration figure from
burette
The concentration
of acid is Ca (mol)
na is the mol of full
balanced equation
per litre

Volume of base is
Vb (cm ). Usually
placed in the
conical flask.
Cb is the
concentration of
the base
na is the mol of full
balanced per litre

Calculations
USE

FORMULA Va. Ca = Vb. Cb


na
nb
Va = 37 cm
Ca is unknown
na = 2
Vb = 25 cm
Cb = 0.1 mol
nb = 1

Va. Ca = Vb. Cb
na
nb
37 cm Ca =
0.1mol

25 cm

Ca = 25 2 0.1
mol/L
37

= 0.13

EXAM QUESTIONS

Look out for dilution factors e.g vinegar


Choice of indicator
Type of vol flask given 1L OR 250 cm as
you have to adjust in your calculations
Take titre reading from burette and given
vol of solution is taken from conical flask
USE FORMULA Va. Ca = Vb. Cb
na
nb

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