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Titrimetric Methods of Analysis !

Titrimetric methods are analytical techniques that determine the quantity of a reagent needed to completely react with an analyte. There are three main types: volumetric titrimetry which measures reagents volumetrically, gravimetric titrimetry which measures mass, and coulometric titrimetry which measures charge. A titration involves adding a standard reagent to a solution until the reaction is complete as indicated by an indicator color change. Back-titration determines excess standard reagent by titrating with a second standard. Primary standards are pure reagents used to standardize titrants via titration.

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0% found this document useful (0 votes)
179 views31 pages

Titrimetric Methods of Analysis !

Titrimetric methods are analytical techniques that determine the quantity of a reagent needed to completely react with an analyte. There are three main types: volumetric titrimetry which measures reagents volumetrically, gravimetric titrimetry which measures mass, and coulometric titrimetry which measures charge. A titration involves adding a standard reagent to a solution until the reaction is complete as indicated by an indicator color change. Back-titration determines excess standard reagent by titrating with a second standard. Primary standards are pure reagents used to standardize titrants via titration.

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TITRIMETRIC METHODS

OF ANALYSIS
Titrimetric Methods

• Includes a group of analytical methods that are based


upon determining the quantity of a reagent of
unknown strength that is required to react completely
with the analyte.
Titrimetric Methods
• Volumetric titrimetry
• A type of titrimetry in which the standard reagent is
measured volumetrically.
• Gravimetric titrimetri
• A type of titrimetry in which the mass of the standard
reagent is measured.
• Coulometric titrimetry
• A type in which the quantity of charge in coulombs
required to complete a reaction with the analyte is
maesured.
Good Titrations
Titration?
• A process in which a standard reagent is added to a
solution of an analyte until the reaction between the
analyte and the reagent is judge to be complete.
• Back-titration
• A process in which the excess of a standard solution used
to react with an analyte is determined by titration with a
second standard solution.
aA + tT → products
analyte titrant

indicator = added compound that


undergoes a color change at the eq. pt.
end point = end of titration when
analyte moles are completely consumed
and the indicator changes color
equivalence point = theoretical end of
titration as calculated using
stoichiometry,
e.g. 1 mol H2SO4/2 mol NaOH
titration error = difference between the
end point and the eq. pt. volumes
Equivalence and end Points
• Equivalence point
• Related to the amount (mol/mek)
• End point
• Related to the physical sign that associate with the
condition of chemical equivalence.
The end point is express in range, the range should address
to the equivalence point.
Standard?
• Standard Solution
• A primary standard
• A secondary standard
• Standardization
• A process in which concentration of a volumetric solution is
determined by using it to titrate a known mass of a primary
standard.
"Standardization" = process where the
concentration of the titrant is determined
exactly using a….
"Primary Standard" = ultrapure reagent
where the number of moles is known exactly so
it can be used to accurately measure the titrant
concentration, e.g.
2HCl + Na2CO3 → CO2 + H2O + 2NaCl
?? M primary standard
(MW = 105.99)
99.99% pure
PRIMARY STANDARD
• HIGH PURITY
• ATMOSPHERIC STABILITY
• INDEPENDENT OF HUMIDITY
• MODEST COST
• LARGE MOLAR MASS
Percent Purity Calculations

Weigh accurately a portion of the impure sample


and dissolve it in an arbitrary amount of solvent.

mass analyte
% purity  X100
mass sample
Lab #2 %Purity Calculation

A sample of impure KHP weighing 2.1283 g


required 42.58 mL of a 0.1084 M NaOH solution
for titration to the phenolphthalein end point.
Calculate the %purity of the sample.
Lab #3 Standardization Calculation
A sample of primary standard Na2CO3 weighing
0.3542 g is dissolved in H2O and titrated with
HCl. 30.23 mL of HCl is required to reach the
end point. The reaction is -
2HCl + Na2CO3 → CO2 + H2O + 2NaCl
Calculate the molarity of the HCl.
Back-Titration
Back-Titration = = aa known
known amount
amount ofof excess
excess
standard
standard reagent
reagent is is added
added to
to the
the sample.
sample. Then
Then
aa second
second standard
standard reagent
reagent is
is used
used to
to titrate
titrate the
the
excess
excess of
of the
the first
first reagent.
reagent.
A 0.2178 g sample of impure Mg(OH)2 was
dissolved in 50.00 mL of 0.1204 M HCl (1st
standard reagent). Back-titration of the excess
acid required 3.76 mL of 0.0948 M NaOH (2nd
reagent). Calculate the %purity of the Mg(OH)2.
Titration Types

1. acid-base
HCl + NaOH → H2O + NaCl
2. redox
5NaC2O4 + 2 KMnO4 + 6H+ →
10CO2 + 2Mn2+ +8H2O
3. precipitation
Ag+ + X- → AgX(s)
4. complex formation (EDTA)
ethylenediaminetetraacetic acid
ACID BASE TITRATION
 
• INDICATORS

• 
Titration • a method of analysis that
will allow you to
determine the precise
endpoint of a reaction
and therefore the precise
quantity of reactant in
the titration flask.
• A buret is used to deliver
the second reactant to
the flask.
• An indicator or pH Meter
is used to detect the
endpoint of the reaction.
Doing a Titration
• Begin by preparing your buret by
1. washing with soap and water
2. rinsing with tap and then
distilled water
3. and rinsing with the titrant
solution
• You should check for air
bubbles and leaks, before
proceeding with the titration.
• Be sure the tip of the buret is
filled.
• Never dispense so that liquid is
below the last calibration that
you can read.
• Take an initial volume
reading and record it.
• Before beginning a
titration, you should
always calculate the
expected endpoint
volume.
• Prepare the solution
to be analyzed by
placing it in a clean
Erlenmeyer flask or
beaker.
• If your sample is a
solid, make sure it is
completely
dissolved.
• Add indicator.
• Use the buret to deliver
a stream of titrant to
within a couple of mL of
your expected endpoint.
• You will see the indicator
change color when the
titrant hits the solution
in the flask, but the color
change disappears upon
stirring.
• Approach the endpoint more slowly
and watch the color of your flask
carefully.
• Use a wash bottle to rinse the sides
of the flask and the tip of the buret,
to be sure all titrant is mixed in the
flask.
• Make sure you know what the
endpoint should look like.
• For phenolphthalein, the endpoint is
the first permanent pale pink.
• The pale pink fades in 10 to 20
minutes.
• If you think you might
have reached the
endpoint, you can record
the volume reading and
add another partial drop.
• Sometimes it is easier to
tell when you have gone
past the endpoint.
• If the flask looks like this,
you have gone too far!
Acid-Base Indicators
• An acid-base indicator is a weak acid or a weak base.
• The undissociated form of the indicator is a different
color than the original form of the indicator.
• An Indicator does not change color from pure acid to
pure alkaline at specific hydrogen ion concentration,
but rather, color change occurs over a range of
hydrogen ion concentrations.
• This range is termed the color change interval. It is
expressed as a pH range.
End Point of an Indicator
• should not be confused with the equivalence point of
a titration
• indicator changes color at its endpoint
• equivalence point is the stoichiometric point where
neutralization takes place
• ideally, the end point of the indicator and the
stoichiometric equivalence point should coincide
Some common indicators
Titration curves for strong acid vs. strong base

Running acid into the base Running base into the acid
Titration curves for strong acid vs. weak base

Running acid into the base Running base into the acid
Titration curves for weak acid vs. strong base

Running acid into the base Running base into the acid

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