PRINCIPLES & APPLICATIONS OF

INSTRUMENTS & TECHNIQUES

INTRODUCTION . . .

 Titration is a technique to determine the

concentration of an unknown solution.

 Titration is the slow addition of one solution of a

known concentration (called a titrant or titrator) to a
known volume of another solution of unknown
concentration (called a titrand or analyte) until the
reaction reaches neutralization, which is often
indicated by a color change.

 Also known as Titrimetry or Volumetric Titration.

Elements of Titration . . .
 The standard solution: the
solution of known
concentration.
An accurately measured
amount of standard solution is
added during titration to the
solution of unknown
concentration until the
equivalence or endpoint is
reached.

 The analyte: the solution of

unknown concentration is
known as the analyte.
During titration the titrant is
added to the analyte in order to
achieve the equivalence point
and determine the
concentration of the analyte.
 The equivalence point: the point when the reactants are
done reacting.
The equivalence point is the ideal point for the
completion of titration. At the equivalence point the
correct amount of standard solution must be added to
fully react with the unknown concentration.

 The end point: it indicates once the equivalence point

has been reached. It is indicated by some form of
indicator which varies depending on what type of titration
being done. For example, if a color indicator is used, the
solution will change color when the titration is at its end
point.
Equivalence point & End point are not
necessarily equal.

 An endpoint is indicated by some form of indicator at

the end of a titration.

 An equivalence point is when the moles of a

standard solution (titrant) equal the moles of a
solution of unknown concentration (analyte).
 The calibrated burette: it is the main
piece of equipment required for a titration
method. Calibration is important because
it is essential for the burette to be as
accurate as possible in order to dispense
very precise amounts of liquid into the
sample.

A burette is a long cylindrical piece of

glass with an open top for pouring in the
titrant. At the bottom there is a carefully
formed tip for dispensing.

Burettes usually have a plastic stopper

that can easily be turned to deliver mere
fractions of a drop of titrant, if needed.
Burettes come in many sizes and are
marked in millilitres and fractions of
millilitres.
 The Indicator: the use of an indicator is key in performing a
successful titration reaction. The purpose of the indicator is to show
when enough standard solution has been added to fully react with
the unknown concentration.
Indicators must only be added to the solution of unknown
concentration when no visible reaction will occur. Depending on the
solution being titrated, the choice of indicator can become key for the
success of the titration.
Titration with an Indicator . . .
MATERIALS . . .

~Erlenmeyer flask or Beaker

~Excess amount of standard solution (titrant)

~A precisely measured amount of analyte; this will be

used to make the solution of unknown concentration

~Indicator

~Calibrated Burette

~Burette Stand
PROCEDURE . . .

Obtain all necessary materials and clean all

necessary items with distilled water

Measure out a precise amount of analyte &

make up the solution of unknown
concentration

Quantitatively transfer the analyte into a

beaker or Erlenmeyer flask

Add additional distilled water until the

analyte is fully dissolved. Measure and
record volume of aqueous solution

Add four to five drops of the appropriate

color indicator into the beaker
Swirl the beaker in order to mix the aqueous
solution of the analyte and the drops of
indicator

Fill the burette with an excess amount of

titrant, the standard solution of known
concentration and should be in aqueous form

Clamp the burette carefully to a burette stand.

The tip of the burette should not be touching
any surfaces

Place the beaker containing the aqueous

solution of unknown concentration under the
burette

Record the initial volume of the burette. Make

sure to measure at the bottom of the
meniscus
Turn on the stopcock (tap) of the burette so that
standard solution is added to the beaker. This
should cause a color change so be sure to swirl the
beaker until the color disappears

Repeat the above step until the color does not

disappear. This means you have reached the
endpoint

Stop when you've reached endpoint, which is the

point when the reactant within the solution of
unknown concentration has been completely
neutralized

Measure and record your final volume of the burette.

Calculate the volume of standard solution used by
subtracting the initial volume measurement from the
final volume measurement of the burette

Now perform the necessary calculations in order to

obtain the concentration of the unknown solution
TYPES Of Titrations . . .
 There are many types of titrations with different
procedures and goals.

Acid – Base titration

Redox titration
Gas phase titration
Complexometric titration
Back titration
Karl Fischer titration
(Potentiometric)
Acid – Base titration:

 Acid-base titrations depend on the neutralization

between an acid and a base when mixed in solution.

 In addition to the sample, an appropriate indicator is

added to the titration chamber, reflecting the pH
range of the equivalence point.

 The acid-base indicator indicates the endpoint of the

titration by changing color.
The final solution after titration should be neutralized and
contain equal moles of hydroxide and hydrogen ions. So
the moles of acid should equal the moles of base:
Some common Indicators used in acid –
base titration:
Redox titration:
 Redox titrations are based on a reduction-oxidation
reaction between an oxidizing agent and a reducing
agent.

 A potentiometer or a redox indicator is usually used to

determine the endpoint of the titration.

 Some redox titrations do not require an indicator, due to

the intense color of the constituents.

 For instance, in permanganometry a slight persisting pink

color signals the endpoint of the titration because of the
color of the excess oxidizing agent potassium
permanganate
Titration CURVES . . .
 The graphs of titration curves effectively show the
relationship between the pH of the solution of
unknown concentration as the standard solution is
added to it in order to reach neutralization.
 In biodiesel: Waste vegetable oil (WVO) must be
neutralized before a batch may be processed. A
portion of WVO is titrated with a base to determine
acidity, so the rest of the batch may be properly
neutralized. This removes free fatty acids from the
WVO that would normally react to make soap
instead of biodiesel.

 Kjeldahl method: A measure of nitrogen content in a

sample. Organic nitrogen is digested into ammonia
with sulfuric acid and potassium sulfate. Finally,
ammonia is back titrated with boric acid and then
sodium carbonate.
 Winkler test for dissolved oxygen: Used to determine
oxygen concentration in water. Oxygen in water
samples is reduced using manganese(II) sulfate,
which reacts with potassium iodide to produce
iodine. The iodine is released in proportion to the
oxygen in the sample, thus the oxygen concentration
is determined with a redox titration of iodine with
thiosulfate using a starch indicator.

 Vitamin C: Also known as ascorbic acid, vitamin C is

a powerful reducing agent. Its concentration can
easily be identified when titrated with the blue dye
Dichlorophenolindophenol (DCPIP) which turns
colorless when reduced by the vitamin.
 Ester value (or ester index): A calculated index. Ester
value = Saponification value – Acid value.

 Acid value: The mass in milligrams of potassium

hydroxide (KOH) required to neutralize carboxylic
acid in one gram of sample. An example is the
determination of free fatty acid content. These
titrations are achieved at low temperatures.

 Saponification value: The mass in milligrams of KOH

required to saponify carboxylic acid in one gram of
sample. Saponification is used to determine average
chain length of fatty acids in fat. These titrations are
achieved at high temperatures.
 Benedict's reagent: Excess glucose in urine may
indicate diabetes in the patient. Benedict's method is
the conventional method to quantify glucose in urine
using a prepared reagent. In this titration, glucose
reduces cupric ions to cuprous ions which react with
potassium thiocyanate to produce a white
precipitate, indicating the endpoint.