Volumetric Analysis
Science of Medicines
Aims for today
01 02 03
I can identify I can explain I can describe
the equipment the steps for a some potential
used in a titration errors in an
titration titration
Volumetric
Analysis
• Volumetric analysis is a quantitative
technique.
• It uses very precise volumes of
accurately known concentrations to
determine the concentration of an
unknown solution
Standard Solutions
• Solutions with an accurately
known concentration are called
standard solutions.
• They can be primary standards –
made up from a solid
• Or they can be secondary
standards which have been
titrated against a primary
standard to determine their
concentration accurately
3 important pieces of equipment
Burette - to measure
accurately the volume of a
solution (titrant) added. The
scale can be read to an
accuracy of half a division.
This is the titre.
Pipette - to deliver an accurate
volume of a solution. This is
the aliquot.
Volumetric flask - to make up
an accurate volume of a
Titration
• A titration is stopped at the end
point This needs to be as close as
possible to the equivalence point
• End point: when the indicator
undergoes a permanent colour
change
• Equivalence point: the point at
which the exact mole ratio of
reactants is present.
• If the indicator is chosen carefully,
the end point is an approximation
of the equivalence point.
Choosing Acid-Base Indicators
• Weak acid-strong base is usually greater than pH 7 which
makes phenolphthalein most suitable
• Strong acid-weak base is usually less than pH 7 which
makes methyl orange and methyl red the most suitable
Acid-Base Indicators
• Acid-base indicators change
colour at a specific pH range
• They are usually weak acids or
bases themselves and when
they change into their
conjugate form a distinct colour
change occurs
• These are found in the data
booklet
Common Acid-Base Indicators
pH range
Colour at Colour at
Indicator for colour
lower pH higher pH
change
methyl orange red yellow 3.1 – 4.4
methyl red red yellow 4.4 – 6.2
litmus red blue 5.0 – 9.0
bromothymol
yellow blue 6.0 – 7.6
blue
phenolphthalein colourless pink 8.3 – 10.0
Steps of a Titration
Step 1 – A known volume of one of the solutions is measured using a
pipette and transferred into a conical flask. The volume measured by
the pipette is called an aliquot.
Step 2 – The other solution is dispensed slowly into the titration flask
from a burette until a permanent colour change is seen – this is the end
point.
Step 3 – The equivalence point is the point during the titration when
the solutions have been mixed in the mole ratio shown by the reaction
equation. The volume of solution delivered by the burette is known as
the titre.
Step 4 – To minimise errors, the titration is repeated several times and
the average titre found which have concordant results – within 0.1
mL of each other.
Sources of Error and Uncertainties
• There are a range of different types of errors, that do not
include mistakes. Mistakes are incorrect use of equipment
or reading scales incorrectly. Errors can be:
• Systematic errors, they are errors that are always
biased the same way, i.e. they are always either too high
or too low. Like a pipette that always delivers 20.2 mL
rather than 20.0 mL
• Random errors on the other hand sometimes have a
value that is too high or sometimes have a value that is
too low. Like determining the precise reading on a burette.
• When reading scales or equipment, the last digit can be
Sources of Error – Titrations
Effect if the substance being
Situation analysed is in the … Comments
Burette Titration flask
Rinsing water The burette solution is
left in the Underestimated Overestimated diluted with more water,
burette so more is used
Rinsing water The solution aliquot in
left in the Overestimated Underestimated the titration flask is
pipette diluted
Indicator
chosen The chosen indicator is
Overestimated Underestimated
changes too critical
soon
Sources of Error – Titrations
Effect if the substance being
Situation analysed is in the … Comments
Burette Titration flask
All the necessary
measurements are made
Water in titration No effect No effect
before the chemicals are
mixed with this water
Concentration of Fewer moles of the standard
standard solution solution than expected, so
Overestimated Overestimated
lower than more moles of the
calculated substance
Concentration of More moles of the standard
standard solution solution than expected will
Underestimated Underestimated
higher than be used, so less moles of
calculated the substance
Extension –
Stoichiometric
Calculations
Changing the Concentration Units
• Mass per unit volume
• Grams of solute dissolved in each L of solution (g/L
or gL-1)
× molar mass
molL-1 gL-1
÷ molar mass
Example 1
1.00 L of a 2.00 M solution of NaCl contains 2.00
mol of dissolved NaCl. Calculate the concentration
in gL-1.
V = 1.00 L
C = 2.00 M or molL-1
C (gL-1) = C(molL-1) M
= 2.00molL-1 × (23.0 + 35.5) gmol-1
= 117 gL-1
Other Ways to Express Concentration
These are used for very low concentrations as in the case of air
pollution.
• Parts per million (ppm) grams per million grams
ppm = mg L-1 = μg mL-1 = mg kg-1 = μg g-1
• Parts per billion (ppb)
% (m/v)=
ppb = μg kg = μg L
-1 -1
These are used for commercial products.
• Percent mass/volume (% m/v) grams per 100 mL
• Percentage mass (% m/m) gram per 100 g
• Percentage volume (% v/v) mL per 100 mL
Knowing the Equivalence Point
Example 1
HCl (aq) + NaOH (aq) NaCl (aq) + H2O (l)
n(HCl) : n(NaOH) is 1 : 1
The equivalence point is reached when the number of
moles of the reactants are equal.
Example 2
2HCl (aq) + Ca(OH)2 (aq) CaCl2 (aq) + 2H2O (aq)
n (HCl): n (Ca(OH)2) is 2 : 1
So, the equivalence point is reached when
n (HCl) = 2 n (Ca(OH)2)
Volumetric Calculations
Stoichiometry plays a key role:
1. Write a balanced equation
2. Find the number of moles of the known
3. Use the ratio to find the number of moles of the
unknown
4. Find the concentration of the unknown
Often a dilution needs to be taken into account
somewhere along the process
Example 2 Hint – use multiple colours of
highlighters when reading the question
to group the pieces of information
together
A solution of sodium hydroxide is titrated against 0.350 molL-1 solution
of sulfuric acid. If 12.75 mL of sulfuric acid is required to neutralise a
20.00 ml aliquot of sodium hydroxide, what is the concentration of the
sodium hydroxide?
V = 20.00 mL V = 12.75 mL
C=? C = 0.350molL-1
n( NaOH ) 2 n = CV
n( H 2 SO 4) 1 n = 0.350 × 12.75 × 10-3
n = 0.00446 mol
n(NaOH) = 2 × 0.00446
= 0.00893 mol
C(NaOH) = n 0.00893 0.446molL 1
V 20.00 10 3