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THEORY- (a) Mohrs salt having the formula FeSO4.(NH4)2SO4.6H2O has mola
mass 392gmol-1. It is a primary standard.
Its equivalent mass is 392/1 = 392 as its n factor is 1 as per the following
reaction:
Fe2+ Fe3+ + e-
PROCEDURE:
1. Weigh a clean dry bottle using a chemical balance.
2. Add 4.9g more weights to the pan containing the weights for the
weighing bottle.
3. Add Mohrs salt in small amounts to the weighing bottle, so that the
pans are balanced.
4. Remove the weighing bottle from the pan.
5. Using a funnel, transfer the Mohrs salt to the volumetric flask.
6. Add about 5ml. of dilute H2SO4 to the flask followed by distilled water
and dissolve the Mohrs salt.
7. Make up the volume to the required level using distilled water.
(b) THEORY-
1. The reaction between KMnO4 and Mohrs salt is a redox reaction and th
titration is therefore called a redox titration.
2. Mohrs salt is the reducing agent and KMnO 4 is the oxidizing agent.
3. KMnO4 acts as an oxidizing agent in all the mediums; i.e. acidic, basic
and neutral medium.
4. KMnO4 acts as the strongest oxidizing agent in the acidic medium and
therefore dil. H2SO4 is added to the conical flask before starting the
titration.
IONIC EQUATIONS INVOLVED:
Reduction Half:
Oxidation Half:
PROCEDURE1.
2.
3.
4.
on it.
5.
Note down the initial reading of the burette.
6.
Run down the KMnO4 solution into the conical flask drop wise
with shaking.
7.
Stop the titration when a permanent pink colour is obtained in
the solution.
8.
This is the end point. Note down the final burette reading.
9.
Repeat the experiment until three concordant values are
obtained.
10.
BURE
INITIAL
READIN
GS
FINAL
VOLUME
OF KMnO4
USED (ml)
10
18.8
8.8
18.8
27.7
8.9
27.7
36.5
8.8
Using formula:
N1M1V1 = N2M2V2
Where N1=5 (for KMnO4), V1=8.8mL
, M1 =?
0.01M
1.79g/L
Volumetric analysis 2
Volumetric Analysis Acid-Base Titration
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The organic compounds containing the acidic group are analyzed by this titration. This is based on the
neutralization reaction between acid and base. An acid-base indicator is used to detect the end point
which indicates the completion of reaction between acid and base by changing the color of the mixed
solution.
The selection of indicator is very important in acid-base titration because the equivalence point is
determined by the stoichiometric of the reaction whereas the endpoint is measured by changing the color
from indicator. The reaction is neutralized but it is not necessary to come to the end point at pH = 7. The
completion of the reaction depends on the strength of acid and base.
For example: The acid-base titration between HCl (strong acid) and NaOH (strong base) in which
phenolphthalein indicator is used.
To determine the concentration of HCl, we take 20 ml of HCl and neutralize it with 0.150M of NaOH.
The steps for titration process are given below.
1. The titrant, NaOH solution of known concentration, is added from the burette.
2. 20ml HCl is taken in volumetric flask with the help of pipette and 2-3 drop of phenolphthalein
indicator is added.
3. The solution is color less due to the acidic medium.
4. The solution of NaOH is added to the HCl drop by drop. As it comes in the contact with HCl acid,
the color of solution becomes pink which quickly disappears. This is due to the formation of OHions from NaOH which reacts with indicator and changes the color. The solution becomes color
less again due to the neutralization of OH- ions with H+ ions (from HCl).
5. After adding more NaOH, the equivalence point of titration is reached when the equal number of
OH- ions and H+ ions react. At this point the pH of the solution in the flask is equal to 7 and the
indicator is colorless.
6. After this, adding more NaOH drop by drop in the solution makes the solution pink from color less
as the solution becomes basic now. So, indicator changes its color in basic medium. This
permanent change shows the end point of titration. Note this reading which is the volume of base
required to neutralize 20 ml of HCl acid. If 50ml is the volume of NaOH (end point reading from
burette).
Now to calculate the concentration of HCl ;
HCl + NaOH NaCl + H2O
the molar ratio is 1:1 for this reaction
So mole of HCl = moles of NaOH
(molarity = moles/ volume)
For example, titration of HCl and NaOH. At the initial stage of titration, the pH changes very slowly and
increases up to pH= 4. But with addition of small amount of alkali like 0.01 mL approx., pH value reaches
to about 7. This shows the neutralization of acid. Further addition of small amount of alkali increases the
concentration of hydrogen ions and the pH value rises to about 9. There is a rapid increase of pH from
about 4 to 9 when the end point approaches. Indicators like methyl orange, methyl red and
phenolphthalein could be used for these kind of neutralization reactions which show the color change
within the pH range of 4 to 10.
For example, titration of acetic acid against NaOH. The end point of this titration lies between pH 8 and 10
due to the formation of sodium acetate and water. So, phenolphthalein is a good indicator for this.
For example, the titration of ammonium hydroxide with HCl. The end point is in the range of 6 to 4 which
shows the acidic pH of solution. Methyl orange is a good indicator for this titration.
Color change on acidic
Range of color
side
change
side
Methyl Violet
Yellow
0.0 - 1.6
Violet
Bromophenol Blue
Yellow
3.0 - 4.6
Blue
Methyl Orange
Red
3.1 - 4.4
Yellow
Methyl Red
Red
4.4 - 6.3
Yellow
Litmus
Red
5.0 - 8.0
Blue
Yellow
6.0 - 7.6
Blue
Indicator
Bromo thymol
Blue
Phenolphthalein
Colorless
8.3 - 10.0
Pink
Alizarin Yellow
Yellow
10.1 - 12.0
Red
1. pH indicator - This is a substance which shows the chemical change by changing the color.
2. A potentiometer - This is used to measure the electrode potential of the solution. These are
used for redox titration. They show the end point with changing potential of the working electrode.
3. pH meter - It is a ion-selective electrode. In pH meter the potential of electrode depends on the
amount of H+ ion present in the solution. The pH of the solution can be measured in the whole
titration. This gives more correct result than indicators.
4. Conductance - The conductivity of solutions is also changed in titration and it depends on the
ions present in the solution, mobility of ions and ions concentration.
5. Color change - In the redox reactions, the color of solution changes without use of indicator. This
is due to different oxidation states of the product.
The volumetric analysis can be categorized into four types which are based on the type of reaction
involved in the process.
Types
Chemicals to be analyzed
Reagents to be used
Indicators to be used
Acid / Base
acid or base
alkali or acid
pH indicator
compound containing
Precipitation
conductivity
Redox
Complexometric
reducing or
oxidizing agent
redox indicator
complexing agent
Some important points should be remembered in doing volumetric analysis to get the accurate results.
1. All the equipments like burette, beaker, pipette and volumetric flask should be washed properly
with distilled water before taking them in use as the presence of any other chemical can be the
reason for wrong measurement.
2. The process of filling the pipette should be accurate to avoid excess addition of solutions.
3. The flask should be shaking well after adding the indicator and also the titration flask with addition
of each drop of solution from burette.
4. The addition of acid should be drop wise.
5. Contamination should be avoided.
6. The indicator should not be used in excess.
7. The flask should be removed as the indicator changes color.
8. Sometimes, an air bubble in the nozzle of the burette can be the reason for altering the readings,
so, it must be removed before taking the initial reading.
9. The burette should not be leaked during titration.
10. Keep eyes in the level of the liquid surface during the time of taking the burette reading or
measuring flask and pipette etc.
11. Lower meniscus and upper meniscus are always read in case of color less and colored solutions
respectively.
12. Do not blow through the pipette to expel the last drop of solution from it; simply touch the inner
surface of the titration flask with the nozzle of the pipette for this purpose.
13. Index finger should be used for pi-petting the solution.
Solved Examples
Question 1: Calculate the concentration of HCl acid if 50ml of HCl is required to neutralize 25ml of 1.00M
NaOH in acid base titration.
Solution:
HCl + NaOH -> NaCl + H2O in this chemical reaction the molar ratio is 1:1 between
HCl and NaOH. So mole of HCl = moles of NaOH
[molarity = moles/volume]
MHCl x volume of HCl = MNaOH x volume of NaOH
MHCl = $\frac{M_{NAOH}
MHCl = 25.00ml1.00M50.00ml
MHCl = 0.50 M HCl
So the concentration of HCl is 0.50 M.
Question 2: The titration curve of ammonia and HCl are given below. Find out all the unknown species A,
B, C and D.
Solution:
At point A, the pH is highly basic so its NH3. At point B, NH3 and NH4 + ammonium ions are in
the buffering region.
C = NH4+. This is equivalence point at which all the NH3 has been protonated and water molecules starts
to take acidic protons.
D =H3O+ more acidic solution.
A = NH3
B = NH3 and NH4+ buffering solution
C = NH4+
D = H3O+
Question 3: Find out the molecular weight of the unknown mono protic acid whose 5 gm is neutralized
with 26.23 ml of a 1.008 M NaOH solution in 150.2 ml of solution.
Solution:
Moles of NaOH = Molarity of NaOH x Volume of NaOH
So moles of NaOH = 1.008 x .02623 = 0.026439moles
As the acid is mono protic so the molar ratio of acid and base is 1:1.
So mole of mono protic acid = moles of NaOH
Question 4: If the 20 ml of an unknown acid is required 30ml of 0.125 N NaOH to get the equivalence
point. Find out the normality of the unknown acid.
Solution:
equivalents of acid = equivalents of base
Vacid Nacid = Vbase Nbase
So Nacid = (30.0ml)(0.125N)(20.0ml)= 0.1875 N
experiment 3
ALCOHOL
Preliminary Test:Experiment
Observation
No Effect
Or
Pink colour of Bromine
water changed to
colourless.
Inference
Compound is saturated.
Or
Compound is unsaturated.
Confirmatory Test:Experiment
Warmed with acetic acid
and a few drops of
concentrated sulphuric
acid.
Observation
Fruity smell is formed.
Exp. 4
ALDEHYDE
Preliminary Test:-
Inference
Alcohol confirmed.