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CONTENTS
Section Kxperimenta 7
INTRODUCTION. sevanuomonyuvennonsnunrmonianaemnnnin ea a
SURFACE CHEMISTRY «. he
Sx Experiment To prepare colloidal solution (nol) of atareh ‘
SRExperiment To prepare a colloidal soluti n of gun “4
3 Experiment To prepare a colloidal solution of exe albumin \
A. Experiment Toprepare colloidal solution of ferric hydroxide (Hw/OH)) ;
5. Experimont To prepare colloidal solution of aluminium hydroxide (AN(OW)] :
6. Experiment To prepare colloidal solution of arsenious sulphide (Ass8,} 1
7. Experiment To study the dialyas of solution containing sodium chloride through a eelhoph ane
parchment paper . sof pe r
8. Experiment To study the “ifectiveneas of different common oils (caster oll, cotton weed oi, enn
oil, kerosene oil, mustard oil) in forming emulsions -
o.Experiment To compare the offectivenoss of a number of emulsifying agents in tor
emulsions... .
@ Viva Voce
B. (CHEMICAL KINETIC!
‘NqEiperiment To study the effect of concentration on the rate of the
thiosulphate and hydrochloric acid. vs
SQ .Experiment To study the effect of temperature on the rate trent be
and HCl.
8. Experiment To study the rate “of reaction of iodide ions with piped peroxide at room temperatur
using different concentrations of iodide ions.....
4, Experiment _Tostudy the rate of reaction between potassium iodate KIO, and'sod jum sulphite (Na, Sc
in acidie medium at room temperature using different concentrations of KIO
ion between sod
een sodium thios
1» Viva Voce
THERMOCHEMISTRY,
“SeExperiment — To determine the water equivalent (W) of calorimeter.
iment To determine the enthalpy of dissolution of copper sulphate or F potassium nitra
3. Experiment To determine the enthalpy of neutralisation of the reaction between strong acid (H
and strong base (NaOH). 0.00
4. Experiment To determine the enthalpy change dus
between acetone and chloroform.
ig the interaction (Hydrogen bond format
# Viva Voce
D. ELECTROCHEMISTR'
SeExperiment To study the variation of cell potential in Zn |Zn** | Cu’* | Cu with change in concentra’
of electrolytes (CuSO, or ZnSO,) at room temperature a
eViva Voce i Se 3 i “
E. CHROMATOGRAPHY....., seen
*SeeFxperiment Separate the coloured components present in the mixture of red and blue inks '
a ascending paper chromatography and find their R, values ; ‘
periment Separate the coloured components prsnt in the given grasslower by ascending pane
EB matography and determine their Ry values...
sparate Co** and Ni% ions present in th di
1 given mixture by using ascending p#
chromatography and determine their R, values. ;
}
8. Experiment
© Viva Voce
(6)
Scanned with CamScanner%
PREPARATION OF INORGANIC COMPOUN
‘To prepare erystals of Mohr's salt
1. Bxperiment
g. Experiment To prepare cr ystals of Potash
3. Experiment To prepare cr tals of potassium trioxalatoferrate (ITI)
fe Viva Voce
PREPARATION OF ORGANIC COMPOUNDS .. a a 60
Heereriment Topprepare a sample of acetanilide frem aniline
9 Experiment To prepare a sample of dibenzalacetone 6
Experiment Topreparea sample of p-nitroaotanilide 6
{Experiment To prepare aniline yellow from aniline
e Viva Voce Be tone
TEST FOR THE FUNCTIONAL GROUPS: fs 66 - 80
UNSATURATION, ALCOHOLIC, PHENOLIC,
PRESENT IN ORGANIC COMPOUNDS:
atenYDIG, BETONIC, CARBOXYLIC AND AMINO (PRIMARY) GROUPS
a 7
[Experiment Identify the functional group preset in the given organic compound
1¢ Viva Voce a .. .
STUDY OF TESTS OF CARBOHYDRATES, FATS AND PROTEINS
‘To test the presence of carbohydrate in the given food sample
41, Experiment
2 Experiment To test the presence of ol or fat in the given food sample
GExperiment To test the presence of proteins inthe given food sample
fe Viva Voce enmnnnnns
‘VOLUMETRIC ANALYSIS...
“Se Experiment To prepare 250 mL oi solution of oxalic acid from erystalline oxalic acid.
NeExperiment Toprepare x solution of Mohr's salt (Ferrous ammonium sulphate). Using this solution
find out molarity strength of the given KMnO, solution 99
YY Experiment To prepare x solution of oxalic acid. With the help of this solution, find out molarity
and strength of the given KMnO, solution... 102
Viva Voce Sree ea vs - 108
QUALITATIVE ANALYSIS ..
Determination of one cation and one anion in a given salt.
Cations: Pb?*, Cu, As*, Fe**, Mn®*, Zn®*, Co”, Ni®, Ca’*, Sr”*, Ba”, Mg’, NH
‘Anions: C03, S*, SO, $0}, NO;, CI, Br, I", POs, C}, CH;COO™
(Note: Insoluble salts excluded)
@ Viva Voce ernnnsnn :
INVESTIGATORY PROJECT:
1. Project Dialysis of sols... eau wn
2 Project Study of the dialysis of water samples from different sewages
and identification of different ions in resulting solutions 160
3. Project Coagulation or precipitation of colloidal solutions ... 163
4. Project Surface tension... 165
5. Project Preparation of 80a «1... : am
6. Project Foaming capacity of different soaps... 175
mM
Scanned with CamScanner‘EXPERIMENT 1
AIM
To prepare colloidal solution (sol) of starch.
THEORY
‘Starch forms a lyophilic sol with water (dispersion medium). The process of sol formation can be accelerated
by heating. So the sol can be prepared by heating starch and water at about 100°C. This sol is quite stable
and is not affected by the presence of any electrolyte impurity.
APPARATUS
Beakers (250 mL and 50 mL), glass rod, filter paper, funnel, burner, wire gauze, tripod stand.
CHEMICALS REQUIRED
Soluble starch = 1 g, Distilled water
2 Add a few ml. distilled water to it and mix thoroughly (Fig A.1).
3. Boil 125 mL water in a 250 mL beaker
“4. Pour the starch paste formed in step 2 to this water; a little at a time and with constant stirring (Fig AZ)
5. Allow it to further boil for 2-3 minute and leave it to cool.
‘the contents of the beaker through a filter paper. The filtrate obtained is a starch sol.
“ih a
fistilled water should be used during preparation of the sol.
‘should not be directly added to boiling water because it form lumps. It should first
f igerteyd va Wi
‘is required while addition ofthe paste to the boiling water.
‘Scanned with CamScannerEXPERIMENT 2
AM
To prepare a colloidal solution of gum.
Note: The experiment to be performed i similar to experiment 1.with a diffrence that i
vetrin place of boiling water; since gum is quite stable in warm water, warm water is to be
' a —aems oc @
aM
To prepare # colloidal solution of egg albumin.
THEORY
gg albumin present
by shaking egg white (eee
APPARATUS
‘Apparatus same as Experiment-1.
"CHEMICALS REQUIRED
Eeg and distilled water.
PROCEDURE
: 1. Break egg and separate the yolk (yellow part) from albumin (colourless part
Penn ne eis in g beak and dd to it cgglaliznin ig waall amiss st Snort
~~ continuous stirring. The process should take about 20 minute.
q 3. Filter the contents and the filtrate obtained is egg albumin sol.
in the egg white is required to make this sol. The sol is quite stable and can be prepared
«rae with cold water. Being stable, it is not affected by the presence of traces of
ons
1L Cold water should be used because in hot water precipitation of egg albumin takes place.
p Yellow yolk should be separated from egg albumin before making the sal
Z _Adtion of egg albumin to water should be dane very slowly. :
mee
a
cae sca
iy eae
‘Scanned with CamScanner4 of catalyst: A catal
al
(iw) en
the re
Fig. B12: Effect of catalyst on activation energy
‘Techniques involved in monitoring a Reaction
Depending upon the reaction; one of the following techniques may be used to monitor the reaction frit rp
(a) Titration: If either reactant or product are acid or base or they undergo redox reaction. their quan
can be estimated using titration method.
(b) Measurement of volume of gas: The reactions where gases are evolved, the volume of the gas emnn
in unit time can be recorded. _
(@) Ifcoloured products are obtained, their optical density can be measured using photometer, as the reiting
progresses.
(d) In case there is change in optical activity, it can be monitored using polarimeter.
AIM.
To study the effect of concentration on the rate of the reaction between sodium thiosulphate »»¢
hydrochloric acid.
THEORY
The reaction between sodium thiosulphate with hydrochloric acid involves formation of colloidal sulphur
26 Together with” Chemistry Lab Manual—12
Scanned with CamScannerNa,S,0, (ag) + aC) 4 Sie) 2 NaCl (ag) + 80, @) + H,0
$,0}1ag) + 2H"%(ag) ——» Sis) + 80, 4) + 10
This colloidal sulphur gives milky appearance and as the reaction proceeds, « stage comes when due to enough
precipitation of sulphur the salution becomes opaque, A reverence point taken #8 an ink mark on the backround
become invisible at this stage of the reaction. At difforent concentrations of reactants, the time is noted when
the mark becomes invisible. (The reaction beaker is kept on the mark and viewed from the top),
APPARATUS
Three burettes, beakers (100 mL), stop watch, test tube,
CHEMICALS REQUIRED
0.1M Na,S,0; 1M HCl, distilled water
PROCEDURE
1. Label 5 beakers as A, B,C, D and E.
2. Fill three burettes with thiosulphate solution, HCI and distilled water respectively
3. Add 10, 20, 30, 40, 50 mL. 0.1M thiosulphate from the burette to the 5 beakers as A, B,C, D and &.
Add 40, 30, 20, 10 mL distilled water to A, B, C and D respectively. (No water in beaker E).
Take 5 mL HC! from the burette, in a test tube.
Put a (X) cross mark on a white tile or white paper and keep beaker A on the mark (Fig. B.3)
Add 5 mL HCI from the test tube, swir! once into it and start the stop watch,
View from the top. Stop the watch when the cross mark becomes invisible, Note down the time taken
for the mark to just vanish from the sight.
9. Repeat the same procedure with beakers B, C, D, and E by adding 5 mL HCI to each. Note down the
time taken in each case and record your observations
oe
px
View from top eye View from top eye
A A
Na$,0, |
Soliton + HCI Colota sulphur
Taapee Tielpaper
Cross mark Cross mark
on theipaper disappears
|
|
| Fig. 8.3: Stuy of rato of reacton between NaS,0, and a HCI
OBSERVATIONS
‘Scanned with CamScannersee)
Plot a graph between volume of thiosulphate (which will be proportional to ite concentra
and time taken in second. It would be a straight sloping line ation in the tin
RESULT
The rate of the reaction between sodium thiosulphate and hydrochloric acid increases
concentration of thiosulphate. 7 Seared
ote. The reaction can be studied by keeping the volume (conc.) of thiosulphate constant and
Varying the
volume (cone.) of HCl
PRECAUTIONS
1. Since we are studying the effect of change of cone
for all the sets.
The cross mark is to be viewed from the top
other factors as temperature, mark should be
and not from the side.
3. Start the stop watch immediately after the fall of the last drop of the acid
4. In case sulphur remains sticking to the flask, wash with cone. HNO, followed by repeated washing with
water.
EXPERIMENT | 2
gp eed a —_
AM
To study the effect of temperature on the rate of reaction between sodium thiosulphate and
HCL
THEORY
cal reaction inereases by inerease in temperature. It has been found that fr a
the rate constant is nearly doubled. The temperature
Generally the rate of chemi
‘us equation (discussed in introduction)
chemical reaction, with rise in
dependence of rate of a chemical
Increasing the temperature of the substani
greater than activation energy.
temperature by 10°,
| reaction is explained by Arrheni
‘ce increases the fraction of molecules which collide with energies
APPARATUS
100 mi beaker, burette, tripod stand, stop watch, wire gauze, thermometer, burner, test tube
CHEMICALS REQUIRED
0.1M sodium thiosulphate, 1M HCI, cone. HNO,
PROCEDURE
1. Take 50 mL. of 0.1M Na,S,O, solution in a beaker, srmometer.
Let the temperature be T °C.
2. Place the beaker on a cross mark put on a white paper or tile.
‘Add 5 mL HCI (already measured HCI kept in a test tube) to it ani
4. Observe the cross mark. When the cross mark just becomes invisible stop the watch and
‘Wash the beaker with conc. HNO, and then thoroughly with water.
5. Again take 50 ml of 0.1 MNa,S,0, in the beaker, heat the contents on a wire gauze, kept on the tripod
stand. Heat it to (T + 5)°C.
‘Add 5 mL of HCl and similarly note the time taken for the spot to become invisible.
Take a few more readings at the difference of 6°C each time.
note its temperature with the help of a the
.d immediately start the stop watch.
note the time
2
28 Together with® Chemistry Lab Manual—12
Scanned with CamScannera} axis and temperature along ve
vizontal M Vertical zig
and HCL inereases with th
jum thiosulphate increase
10 temperaties
EXPERIMENT a)
the rate of reaction of iodide ions with hydrogen pero,
trations of iodide ions.
at
To study
different concent
THEORY
tn acidic medium, hydrogen peroxide oxidises iodide ions to iodine
2) + H,0, + 2H* ——> I, + 2H,0
I, + F ——> Ij @olyhaide ion)
‘The rate of the reaction can be followed by measuring the time taken for the appearance of blue colour with
starch solution due to the formation of starch -1, complex. The method is modified and the reaction is monitored
by adding sodium thiosulphate. This is done to improve the effectiveness of the observations and is called
‘nmaitor reaction’. A definite amount of sodium thiosulphate and starch is added to the reaction mixture and
the iodine produced reacts with thiosulphate to give I” ions.
I, + 28,0,> —> 8,02 + or
Hence, iodine does not give blue colour in the beginning and is consumed by thiosulphate ions. This oseurs
‘il the entire amount of thiosulphate gets consumed. After that, the production of I, gives blue colour
1, + Starch —— Starch ~ I, complex
This reaction is called indicator reaction.
The time taken for the appearance of blue colour depends on:
(i) Amount of thiosulphate added. sroxide.
\t) Initial rate of formation of iodine which dopends on the concentration of iodide ions and hydrasen bene
Ue amount and the concentration of thiosulphate is kept constant then the differences in he aBPHI CT,
alse 1a elou Would depend on the concentration of I~ and H,O,. Further, ifthe comeentt
“° Kept constant, the rate of the reaction with variable concentrations of iodide ion ae
Chemical Kinetics
ee |
Scanned with CamScanneralent of calorimeter: Water
id water
aod by nai
ns are explained in experiment 1
sation or dissolution|
details explained in
the
lorinetee
exyeris 2 neti
et 2 an 3, So
me
a ivalent (W) of calorimeter.
qo determine the water equ
Rubber stopper
Scanned with CamScannerApparatus
Styrofoam block in which a beaker can be fitted or polythene bottle or thermos flask, thermometer
Thermometer
‘styrofoam block
Beaker with water
a wo) °
DOODTa Od G|
20 e Doooeng of
PROCEDURE
1, Take 100 mL distilled water in the calorimeter in which a thermometer and stirrer are inserts
Note down the temperature of water kept in the calorimeter (¢,°C).
3. Heat 100 mL of water in another beaker to 10-20°C higher than that of room temperature. N
the temperature of this water (t,).
4. Put this 100 mL warm water into the calorimeter without any delay.
5. Stir the contents and note down the temperature after mixing (¢;°C).
OBSERVATION
‘Volume of water taken in calorimeter = 100 mL, Temperature of water = t
Volume of warm water added = 100 mL.
‘Temperature of warm water = t,°C, Temperature after mixing = ty
CALCULATION
Heat given out by hot water = Heat taken by bottle and cold water
100(t, — t;) = (100 + W) (ty - ty)
(tt)
+W= ae
100 100g
(t,t)
W = |100 7; 75 ~ 100
RESULT
‘The water equivalent of calorimeter is W =
36 Together with® Chemistry Lab Manual—12
Scanned with CamScannerEXPERIMENT &
AIM
‘To determine the enthalpy’ of dissolution of copper sulphate or potassium nitrate,
THEORY
enthalpy of dissolution is defined as the enthalpy change per mole of « solute when dissolved in pure solvent to
eye a salution of specific concentration, Enthalpy of dissolution of a solute in a solvent varies with concentration
‘and the temperature
APPARATUS
Calorimeter set-up with 2 holes (one for thermometer and another for stirrer), beakers, thermometer, stirrer,
‘measuring cylinder.
(CHEMICALS REQUIRED
iydrated copper sulphate or potassium nitrate and distilled water.
PROCEDURE
1, Calculate the water equivalent of calorimeter as experiment - 1
2, Take 200 mL of distilled water in the calorimeter and fix the cover with 2 holes in it. Insert thermometer in
one hole and stirrer in the other. See that the thermometer dips in the wat
of water.
3. Weigh a known weight (7g) of CuSO,.5H,0 and put it in the calorimeter. Put the cover back quickly.
4, Stir it, but the speed of stirring should not be high and vigorous. Stirring will also increase the
temperature and introduce error in the temperature reading.
5, Note down the temperature (f;) when the substance just dissolves.
OBSERVATION
ter. Note down the temperature
eight of hydrated copper sulphate = w g, Volume of water taken = 200 mL, = 200 g, Temperature of water = °C
‘Temperature of water after CuSO,.5H,O is added = ¢,°C, Water equivalent of calorimeter = W g (already
calculated in Experiment—1
CALCULATION
‘Assuming density and specific heat of the solution to be same as that of water, heat evolved or absorbed for
dissolution of w g of the solute.
@ = (W + 200) (t, ~ t2) cal = (W + 200) (¢, ~ f,) x 4.2 J = (W + 200) at x 4.2 J
For 4 moles of the solute dissolved, heat change = (W + 200) at x 42.J
(M = molecular mass of solute) (w = weight of solute)
For 1 mole of the solute dissolved, heat change HE 20d aE J
Heat of dissolution = (W+200)A8tx42xM_ y
For determining the heat of dissolution of potassium nitrate, dissolve 5.5 g of KNO, in 200 mL. of water.
RESULT
‘The enthalpy of dissolution of hydrated copper sulphate in water i8 0... Shmol at ¢,°C.
Theromochemistry 37
Scanned with CamScannerPRECAUTIONS
1. Stir the mixture thoroughly to dissolve the solute
2. Rate of stirring should not be very high as fast stirring may lead to increase in the temperaty,,
solution,
3. High precission thermometer should be used.
EXPERIMENT (3
AIM
To determine the enthalpy of neutralisation of the reaction between strong acid (HCD and sy
base (NaOH).
THEORY
‘When acid reacts with base heat is evolved. Enthalpy of neutralisation is heat evolved when one gram equiv.
of an acid is completely neutralised by a base in dilute solution. The enthalpy of neutralisation of strong
For more details see introduction of this unit.
by strong base is constant with the value 57.1 kJ/mol
APPARATU:
As in Experiment-2.
CHEMICALS REQUIRED
0.2M HCI and 0.2M NaOH solution.
PROCEDURE
1. Take 100 mL of 0.2M HCI in calorimeter and note down it's temperature.
Also, note down the temperature of 100 mL of 0.2M NaOH solution taken in another beak.
2
solutions should have same temperature otherwise wait for them to attain same temperature.
‘Transfer NaOH to HCI quickly, put the lid of calorimeter back, stir and record the temperatur
mixture at small intervals till it becomes constant.
Record the highest temperature reached.
3.
4.
OBSERVATIONS
Initial temperature of acid and base
Rise in temperature = (¢ ~ )°C
Mass of the mixture of the neutralisation
Water equivalent of calorimeter = W g
-C, Final temperature of the mixture
= 200 g (Assuming the solution to have same de:
CALCULATION
Heat evolved during neutralisation of 100 mL of 0.2M HCI = (200 + W) x dt x 4.2 J
Heat evolved during neutralisation of 1000 mL of 1M HCl = 1200-4 Wear ed 2 x 1000 y
Enthalpy of neutralisation = - 200-+W)+Asn4.2 yy
RESULT
‘The enthalpy of
f neutralisation of HCI with NaOH is ...
PRECAUTIONS
‘As in Experiment ~ 2.
36 Together with® Chemistry Lab Manual—12
ad
Scanned with CamScannerPR (a) |Hylg)| H’ (aq) is assigned a zero potential at all temperature cnmrenrndinm
| a= Chis
Ay ota dotlrn
oF yeh oh
| Fig D4: Stanctart tyes saci
HY (ag) + —> Lay
‘At 298 K the emf of the cell, standard hydrogen electrode | second half coil comatraeted ty +
‘hydrogen electrode as anode and other half cell as cathode, gives the reduction genes
the concentrations of the oxidised and the reduced forms of the species ar: E
equal to standard electrode potential.
= eee 2
sae
AIM
To study the variation of cell potential in Zn | Zn” | Cu” | Cu with change in concentration of eleetrolyi=
(CuSO, or ZnSO,) at room temperature.
THEORY
When Zn rod is dipped in ZnSO, solution and Cu rod in CuSO, solution and the solutions are connected internal
with salt bridge and externally the rods with connecting leads, the emf generated due to the redox reaction ca
be measured with the help of voltmeter connected in the outer circuit. The reactions that occur are
Anode (oxidation) Zn(s) ——+ Zn” (aq) + 2
Cathode (reduction) Cu (aq) + 2° + Cu (3)
Overall reaction. Zn (s) +
‘The cell potential of the cell, when the concentration of the solution and/or the temperature varies is gv
by Nernst Equation.
2.303RT
Baa = Eng - 7 hog @
Where E, = cell potential, E%,, = standard cell potential, n = no. of electrons, T = temperature ar
@ = reaction auotient. For Daniell eet Q = [28° and n =2
3°
‘The cell potential decreases with time because concentration of Zn“* (zine sulphate) increases and that of Cu
(copper sulphate) decreases and ultimately falls to zero.
42 Together with® Chemistry Lab Manual—12
Scanned with CamScanner=
on simplification Nernst equation reduces to Kgy = Hy ~ 2° toy @. at T= 208 K with the value of
p= 8314 JK? mol"! and F = 96500 coulomb .
APPARATUS
jing Toads, voltmeter, pinch-coek, rubber tube, measuring
100 mL beaker, salt bridge, or glass tube com
cylinder, Key, measuring flask,
CHEMICALS REQUIRED
KCI, agar-agar, Zn and Cu strips, ZnSO, (1M), CuSO, (IM, 0.5 M, 0.25 M and 0.125 M).
PROCEDURE
‘A. Construction of Salt Bridge
1. Take about 30 cm long glass tube and bend it twie ht angles to make U tube.
2, Take 3 g of agar-agar, 30 g of pure potassium chloride in a beaker and add 100 ml. of water, wa
‘all the solid dissolves to give a clear solution.
3, Fix about 1m rubber tube to one end of the U-tube. Dip the
prepared in step 2. Suck to fill the U-tube with this solution close the
that the solution does not run back. Allow it to cool down, The solution will s
of the U-tube with cotton plugs. The salt bridge is ready
rm till
ther end of the U-tube in warm solution
rubber tube with pinch cock so
wet like a gel. Plug the ends
Pinch cock
‘Agar-agar + KCI Rubbertubing |
+ Water
Fig, 0.2: Construction and filing the sat bridge
‘When salt bridge is not in use, keep its open ends in saturated solution of KCL.
B. Construction of the cell
Cathode
Potassium chioride solution
Copper strip
Layne
Copper sulphate sluton
Fig. D.3: Assembly ofthe eletrochemicol col Zn(s) [2n"(a) I] Cu (ag Cu (s) |
1. Clean the copper and zinc electrodes with sand paper.
2. In two beakers take 1M ZnSO, and 1M CuSO, solutions separately (560 mL volume of each)
Electrochemistry 43
Scanned with CamScannertrips in solution of that
3, Immerse the metal s
1 of voltmeter to the cop)
4, Connect one terminal
the help of connecting
5, Place the salt bridge in
6; Insert the key to complete t]
7, Note down the voltmeter rea
8, Repeat the procedure with different
down your observations in tabular form
Note. 0.5M, 0.25M, 0.125M coppe
OBSERVATIONS
wires.
the beakers such
he circuit (Fig. D8)
1 concentration:
1
05
0.25
les
RESULT
Cell potential decreases with decrease in
‘Note. There would be some difference in
current during measurement and also we are
PRECAUTIONS
1, Electrodes should be cleaned by sand paper.
metal.
por plate and other
that it connects both th
ding that gives the ©
+ sulphate solution can be prepared
concentration of copper sulphate.
the measured and calculated values
alculating using concentration values inste
to zine plate with a key in series win,
\e solutions.
mf of the cell.
5 of CuSO, but same n of ZnSO,. Note
1M concentral
by
because voltmeter draws some
.ad of activities.
2. There should not be any air bubble in the salt bridge.
i 3. Use a new salt bridge for every cell.
4. Each voltmeter reading should be taken
[viva
after sti
irring the solution.
VOCE |
Q.1. What is electrochemistry?
‘Ans. Electrochemistry is the study of production of
electricity from chemical reactions and the use of
‘electrical energy to bring about non-spontaneous
‘chemical reactions.
”. What is a Daniell cell?
Daniell cell is an electrochemical cell which is
constructed by dipping zine electrode in ZnSO,
and copper electrode in CuSO, solution. The
two solutions being connected internally by salt
bridge and externally by connecting wires. It is
represented as Zn\Zn**|Cu*"|Cu.
What do you understand by E.M.F.?
EMF, or electromotive force is the difference
of potential which causes the flow of current
from one electrode to another electrode in
an electrochemical cell. In fact e.m/f. is the
cell potential of the cell when no current is
drawn.
Q.4. What is meant by an electrode?
‘Ans. A metal or carbon rod by which an electr
current passes into or out of a cell is called «
electrode.
Q.5. What are the names of anode and cathode of «
Daniell cell?
Ans. Zn strip acts as anode whereas Cu strip ct
as cathode.
Q.6. What is a galvanic or voltaic cell?
Ans. It is an electrochemical cell in which electrics!
‘energy is produced by a spontaneous chemic#!
ea Daniell cell is a specific galvan
cell.
44 Together with® Chemistry Lab Manual—12
pd
Scanned with CamScannerAIM
Separate the coloured components present im the misture of xed and tue inks by aecemting 907~
chromatography and find their R, values.
APPARATUS
Gas jar, glass rod, filter paper strip (Whatman filter paper 1), jar cover, fine capillary taibe,
CHEMICALS REQUIRED
A mixture of red and blue inks, alcohol and distilled water.
PROCEDURE
1. Take a Whatman filter paper strip (20 x 2 em) and draw a line with pencil above 4 ex: from one «:
2. With the help of fine capillary tube, put a drop of the mixture of red and blue inks at the point F
centre of the line, Let it dry in air. Put another drop on the same spot and dry again. Hepest =
times, so that the spot gets loaded with the mixture.
48 Together with® Chemistry Lab Manual—12
Scanned with CamScannera
fe crromatographic paper
lq —— Whatrnan fiter paper
Criginal ne about 4 em above the edge
Point to put the spot ofthe mixture
Fig. E. 4: Spotting of the mixture
3. Suspend the filter paper vertically in a gas jar containing thy
jr euch a way that the pencil line (and the spot) remains above the solvent I
of alcohol and water.
Cover the jar and keep it undisturbed. The solvent will rise along
‘After the solvent has risen about 12-15 cm you will observe two
on the filter paper.
Take the filter paper out of the jar and mark the distance that the solvent has risen on the paper with
a pencil. This is called the solvent front. Measure this using scale.
Dry the paper. Put pencil marks in the centre of the blue and red spots.
[Also measure the distance of the two spots from the original line.
Calculate the R, values of the blue and red inks by using the formula:
Distance travelled by the blue or red ink from the point of application
Distance travelled by the solvent from the original line
1e solvent (eluent) with the help of a glass rod
level. Solvent is a mixture
with the mixture of red and blue inks
different spots of blue and red colour
ame
R=
OBSERVATIONS AND CALCULATION
1 | Red ink + Blue ink ‘A cm (Red ink)
2. _| Red ink + Blue ink | B cm (Blue ink)
PRECAUTIONS
1. Always make use of a fine capillary tube.
2 Keep the jar undisturbed and covered during the experiment.
3. A spot should be small and rich in mixture
4. Allow the spot to dry before putting the strip in the jar.
5. Keep the strip erect. Do not let it to be curled.
6 Do not allow the spot to dip in the solvent.
Chromatography 49
‘Scanned with CamScannerSame as in experiment-1.
as developing solvent.
50 Together ewith® Chemistry Lab Manual—12
Scanned with CamScannerMolecular mass
n factor a
factor is no, of electrons 2° released oF gsined per formula uni,
C. Formulae used during titration calculation 4
N,V, = N:Vy or myMyV; = meMlaVe Si
Strength = N x Equivalent mass
: Strength = M x Molecular mass
% purity = Calculated strength 199
oe Given strength
Equivalent masses of some redox reagents
Equivalent mass =
MnO; + 8H" + 5e~
+ Mn?" + 4,0
Potassium
permanganate
(acidic medium)
Potassium
permanganate
(basic medium)
‘Oxalic acid
MnO; + 2H,0 + 3e~
+ MnO, + 40H"
C,07 —> 2C0, + 3e”
Sodium oxalate 02> 200, + 2e°
igs Fe Fe +e"
(hydrated)
| Ferrous
ammonium,
sulphate
Mohr's salt)
Fe» Fe* +e"
AIM
M . "
‘To prepare 250 mL of solution of oxalic acid from erystalline oxalic acid.
‘THEORY
Oxalic acid is 00H
j OOH
tandard. Its erystals are available with high degree of purity. It is neither deliquescent "°°
sie stored for long without change in concentration, Its solution is stable and does
a dicarboxylic 91,0 and molecular mast 126
cid having molecular formula as {
| primary s
Its solution
on exposure to light
os 7 wh® Chemistry Lab Manual—12
Scanned with CamScanneradding water. This is done to prevent h
EXPERIMENT
AIM
Prepare x solution of Mohr’s salt (Ferrous ammonium sulphate). Using this solution, find out the
molarity and strength of given KMnO, solution.
THEORY
The reaction between KMnO, and Mobr's salt is a redox reaction and the titration is therefore called redox
titration KMnO, acts as oxidising agent and Mohr's salt as reducing agent. KMnQ, can act as oxidising agent
in acidic, neutral and alkaline medium. However, the medium used for volumetric titration is acidic medium.
‘The reaction in acidic medium is MnO; + 8H’ + Se” —» Mn®* + 4H,0.
Dil H,$0, - 4Nv 11,80, is used to provide acidic medium, Cone, HNO, can't be used as it itself is an oxidising
gent and would oxidise Mohr’s salt or Oxalic acid used as reducing agent in the titration. (Hence, the reaction
will not be quantitatively using KMnO, as required by the aim of titration), HC! can also not be used to
Provide aciaie medium as it will get oxidised by KMnO, to evolve Cly,
2MnO; + 16H’ + 10Cl —> 5Cl, + 2Mn” + 8H,0.
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Alkaline medium, also cannot be used for the titration as MnO, (brown solid) formed interferes,
observation of end point
MnO; + 2H,0 + 8° —» MnO, + 401
‘The titration between Mohr's salt and KMn, is fast enough at room te NAM saci. 4
No separate external indicator is required for the titration a8 hanya PES GH.S6 due en
of KMn0, after the equivalence point imparts pink eolour to the # 10,
present.
(Min®* ions are also light pink but appear colourless in dilute wolu
‘As (KMn0,) reacts with Mohr's salt Mn?* ions are predict a
‘as catalyst for the reaction, Hence in the beginning of titrati
emperature
tions).
1n ions produced in the fest stage ty
takes time to be consumed jn,
but later the colour of KMnO, fades away faster.
APPARATUS AND CHEMICALS REQUIRED ME tbe, coca,
Mohe’s salt crystals, standard measuring flask, weighing bottle, funnel, burette, pipette, :
weight boxes, beakers and KMnO, solution,
TONIC REACTIONS
Molecular equation is:
QKMn0, + SH,SO, + 10FeSO,(NH,),S0,6H,0 — K,SO, + 2MnSO,
‘MnO, + 8H* + 5e° —> Mn” + 4,0,
(Fe? —> Fe +e] x5
+ 5Fe(SO,), + 68H,0 + 100vH,
MnO, + 8H* + 5Fe”* —» 5Fe"* + 4H,0 + Mn”
PROCEDURE ;
‘A. Preparation of standard solution as discussed in previous experiment.
B. Titration of KMnO, solution against x ‘Mohr's salt solution.
1. 10 mL Mohr’s salt solution to be taken in conical flask, 10 mL. of dil H,SO, is also added
2. KMn0, solution is taken in the burette.
3. Perform the titration as discussed under ‘Process of titration’.
4. Record your observations as under.
OBSERVATIONS AND CALCULATION
A. Preparation of standard solution of Mohr’s salt
Calculation of weight to be weighed to prepare 100 mL, x solution of Mohr’s salt.
Weight 1000
Form pee Weight Ce, 000s
See rsiemntan Weight,” Vda
Weight of empty weighing bottle = y g (say) 11.820 g
Weight of bottle + Mohr's salt = (x + y) g (11.820 + 1.96) g = 19.78 g
B. Titration between KMnQ, solution and Mohr’s salt solution
Solution to be taken in the pipette = Mohr’s salt, Volume of the pipette = 10 mL
Dil. H,SO, to be added is 10 mL,
Indicator — KMnO, self indicator
Colour change ~ From colourless to light. pink
Weight 1000, weight = 1%
1
20 392“ 100
100 Together with® Chemistry Lab Manual—12
Scanned with CamScannerOBSERVATION TARLE,
Burette Readings
Reading
Rend
8 are assumed)
' 0, used (in rt) |
Final Volume of KMn0,
Reading, baie. .|
116 10.5
21.8 | 10.3
82.1 | cag
424 103
RV (Say) Coneordant reading = 10.3 ml
h
used. th = MV,
perm KMn0, ~ Mobrissali
n=5 nel
Pagar, * M, 1-610
Mromo, = “Mots Mrvonrssait* Viohes salt” 20 = 0.0097 M
Pxatno, * Viwino, 5x 10.3,
4 Strength
= (Molarity x Molecular weight) g/L.
Calculated strength of KMnO,
0.0097 x 158 = 1.53 WL.
RESULT
‘The molarity and strength of KMnO, is found to be 0.0097 M and 1.53 g/L.
Note: The titration between oxalic acid and KMn0,
in the reaction and procedure involved. Also,
Reaction would be
is to be done in a similar way with the following change
note that the ‘n’ factor of oxalic acid is 2.
(MnO, + 8H" + 5° —, Mn® + 4H,0) x 2
(C,07° — 200, + 21 « 5
2Mn0; + 16H" + 5C,0}- —+ 2Mn* + 8H,0 + 10CO,
Molecular reaction is 2KMnO, + 5C,H,O, + 3H,SO, —> K,SO, + 2MnSO, + 10CO, + 8H,0
Change in the procedure
Since, the reaction is very slow at room temperature; the titration is done at
60-70°C.
For this the contents of conical flask, i.e. (oxalic acid + dil. H,SO,) to be heated
over the Bunsen flame by placing conical flask on the wire gauze kept on a
tripod stand.
Tocheck the temperature is 60-70°C touch the conical flask on the back of your
hand. The moment the touch becomes unbearable, start the titration.
Donot overheat the conical flask as oxalic acid on overheating will get decompose 7
10 CO, before undergoing reaction with KMnO, and hence, accurate volumetric Wires
: ig. IAT: Checking the
analysis would not be moon temperature of Oxale Ace
Ta pr? CO, + CO + HO
i OOH beta
Different possible Aims and the Calcul Required.
A. Preparation of a solution of Mohr's salt containing exactly 17 g of it in 1 litre solution, With the help of
this solution, determine the molarity and strength of KMnQ, solution provided to you
Hint: Weigh exact 4.250 g of Mohr’s salt to make 250 mL. solution, Rest of the procedure and calculations
are same,
Volumetric Analysis 101
Scanned with CamScannerfore starting the titration, Contents of tho
a vel Pee AGsllciacid to Co, ines nical flask should not be overheated as it will lead to
wigan cle oi oing reaction with KMnO, and hence, accurate volumetric
ool (COOH), __hieh tem
and Molecular a
o8l eon:
+ 00, + Co +
eactions TOES
soni IMnO; + 8H* + 56 2
+ 8H" + Ge” —_, Mn 4 41,0) x 2
Ic,0? —> 2CO, + 2] « 6
2MnO," + 16H" + 50,0? a
+ 5C,0;° ——> 2Mn’* + 8H,0 + 1060,
reaction:
Nolecslae
2KMnO, + 5C,H,0, + 3H,80, —, K,S0, + 2MnSO, + 10CO, + 8H,O
appaRATUS AND CHEMICALS REQUIRED
atid oxalic acid, standard measuring flask, weighing bottle, funnel, burette, pipette, test tube, conical flask,
, tripod stand, wire gauze, Bunsen burner, KMnO, solution
procEDURE
M zi ‘
‘A. Prepare =, (100 mL.) solution of oxalic acid by dissolving 0.262 g of oxalic acid to make 100 ml. solution
Please note that dil. H,SO, is not to be added while preparing standard solution of oxalic acid.
i
B, Titration of => solution prepared alone against KMnO, solution (provided in the lab).
1, KMn0, solution is taken in the burette.
2, Pipette out 10 mL of oxalic acid solution to the conical flask and add 10 mL of dil. H,SO, to it
3, Heat the contents of the conical flask over the Bunsen flame by placing conical flask on the wire
gauze kept on the tripod stand. The contents to be heated to 60-70 °C.
To check the temperature, touch the conical flask on the back of your hand. The moment the
touch becomes unbearable, start the titration.
4, Titration is to be performed as discussed under ‘process of titration’
5. Record your observations as under.
OBSERVATIONS AND CALCULATION
A. Preparation of standard solution of Oxalic acid.
me — Weight 1000 _, _1_ Weight 1000 _, Weight -
Molecular Weight == V(in mL) 50 126 100
Weight of empty weighing bottle = y g (say) 11.820 g.
Weight of bottle + Oxalic acid = (x + y) g say (11.820 + 0.252) g = 12.072 g
B. Titration between KMnO, solution and Oxalic acid solution.
Solution to be taken in the pipette = Oxalic acid
Volume of the pipette = 10 mL.
Dil. H,SO, to be added = 10 mL,
Indicator — KMn0, as self indicator, Colour change ~ From colourless to light pink.
252 g
Volumetric Analysis 103
Scanned with CamScannerOBSERVATION TABLE (ADINGE AIK APBUMIED)
05
104
104
04
Bay) Comemndant readion, = 10
MY, lM
Pormnila used KMn0, ” Oxalicncid
mab ned
ar4 410
Moun, » Matte” A taste” Vater = ss = 0018 A
eae Msg” Visbory
IW Sarr Acdece aA
RESULT
‘The molarity and strength of KMnO,
C. Determine the number of water molecules of
2 tatn0, solution. You are aso provided with Mobs salt solution prepared ty disw i: 7
106 gf or students may be asked to prepare 250 ml. of Mohr's salt solution by dis my
49 g of Mohr’s salt.
APPARATUS AND CHEMICALS REQUIRED
KMn0, solution, Mohr's salt solution, dil. H,S0,, beakers, burette, pipette, fannel, test tube, comical “=<
Theory, reactions and procedure as per experiment-2.
solution ia Sound out to be O07 and 12.27 ofl reepectively
crystallisation of Mohr's salt by titrating it agin.
OBSERVATION TABLE (Volume of Mohr's salt pipetted for each titration = 10 ml.)
1
Ez
oon] 3 ‘WA 101
roy 04 405
CALCULATION
Find out Molarity of Mohr’s salt by applying
2AM, . MV, _
KMn0, ~ Mots salt
1s al
5x Ty Fe,(SO,), + 20NH,),SO, + 13,0} 5
2AMnO, + 8H,SO, + 10FeS0,(NH,),S0,6H,0 ——> K,SO, + 2MnSO, + 5Fe(SO,),
+ 10(NH,),SO, + 68H,0
PROCEDURE
1. Prepare s Mohr's salt solution as in experiment-2
2, Perform the titration of this Mohr’s salt solution with KMnO, solution provided in the lab. Titration to
be performed as in experiment 2.
OBSERVATIONS AND CALCULATION
Bein, *Va, 1 yy txt cig tet
ae rr 520 vB
Strength of alkali metal permanganate in the solution
16 g/L. = Molarity x Molecular weight
1.6 4 x (Molecular weight of KMnO,)
Volumetric Analysis 105
ae SC ee
Scanned with CamScanner>»
“Ay !Momic mass of Alkali meta (say a)] + Mass of Mno,)
= Ari = a=.6«5V)- 119
Calculate the value of ‘a’ the atomic mass of alkali metal.
RESULT
‘The atomic mass of alkali metal in alkali metal permanganate is a u.
[FOONs|
and
E, Determine the percentage composition of mixture of sodium oxalate
a (COONa!
oxalic acid . 2H,0 | You are provided with M Kmn0, solution.
(COOH 50
APPARATUS AND CHEMICALS REQUIRED.
Mixture of oxalic acid and sodium oxalate, x KMn0, solution, dil. H,SO,, apparatus for titration as ;,
experiment C.
Chemical Reaction *
FOOH 91,0 + [0] —> 200, + 8H,0 =~
coou
00N:
JOON® | H,S0, + [0] ——> 200, + H,0 + Na,S0,
COONa
Tonic Equation
(MnO; + 8H* + 5e> ——> Mn™ + 4H,O ] x 2
[C,0,° —+ 200, + 2e']x 5 (from both oxalic acid and sodium oxalate
2MnO, + 16H* + 5C,0? ——> 2Mn™ + 10CO, + 8H,O
PROCEDURE
1. Weigh 1 g of the mixture to make 250 mL solution.
2. Perform the titration of this solution with KMnO, as in experiment C.
OBSERVATIONS AND CALCULATION
Volume of the solution of the mixture pipetted out for each titration = 10 mL.
dil. H,SO, added = 10 mL.
CALCULATION
106 Together with® Chemistry Lab Manual—12
Scanned with CamScannerof percentage composition of mixture,
conan jot of (oxalate Hon from oxalic
‘ acid + oxalate ions from sodium oxalate)
Me gg-ehe solution of the mixture = 4 w/t ( 250 ml, solution)
1 1g. was dissolved to make
seth of oxalate ion from oxalic acid in solution = y WL
vate of oxalate ion from sodium oxalate would be = (4 — y) WL
Strength = Mota
xture (total motes of oxalate ions per litre of mixture)
pa 29
Strength
ty « Molecular Weight =» Molarity = Si5jecular weight
s of
ee (moles of oxalate ions por litre from oxalic acid) + (mole
=~. ns per litre from sodium oxalate)
eS kets 4-y
0.005 = ( 3 + (4
2 Sb eos 126 a
no, of moles of
sodium oxalate
alate the value of y, % of oxalic acid
T
the & of oxalic acid in the mixture is and the % of Sodium oxalate in the mixture is ;
fF, You are provided with partially oxidised sample of ferrous sulphite (FeSO,7H,0 - green vitriol)
crystals. Prepare a solution by dissolving 1.4 g of these crystals to make 100 mL solution and determine
the percentage oxidation of the given sample. You are provided with x KMn0, solution.
MATERIALS AND APPARATUS REQUIRED
< KMnO, solution, partially oxidised solid of FeSO,-7H,0 [or FeSO,-7H,0 crystals mixed with small amount
i
of Fe{SO)s, dil. H,SO,, apparatus for titration as per experiment 2.
MOLECULAR AND IONIC EQUATIONS
Molecular equation:
2KMn0, + 3H,S0, ——> K,SO, + 2MnSO, + 3H,0 + 5{0]
[2FeSO, + H,SO, + [0] —> FeSO), + HO] x 5
2KMn0, + 8H,S0, + 10FeSO, ——> K,SO, + 2MnSO, + 5FeSO,), + 8H,0
MnO, + 5Fe’* + 8H* ——> 5Fe™* + Mn + 4H,0
PROCEDURE
1. Prepare 100 mL of FeSO,-7H,0 (partially oxidised) solution by dissolving 1.4 g of the crystals.
2 Perform the titration as per experiment 2.
OBSERVATIONS AND CALCULATION
. Concordant reading = V mL (say)
Volumetric Analysis 107
Scanned with CamScannerCALCULATION
mY) = AM
Mra wot Via. 8
Maaniy ® Viatany \
Myaoymyo 8 8" V
1
Strength of FGOY THO in the oxidised solution» 555
Note that the calculated molarity and strongth is die to Fe
Already oxidised Pe do not participate in the redox titration,
Strength of partially oxidised sample = M4 g/l, (ax 14g of thin a
Ted, oe ee
100
V = Congortant reacting of ¥
vM
1000 200
0
jolume of KMaO, used
Vx 278 (Molocular woight of FeSO, 711,0)
2+ Jone of the solution oxidised to Po" by Ky,
sample wan dissolved to make 109
solution)
=> Strength of oxidised ferrous sulphate = (14 = y) wh
ey % oxidation we x 100
RESULT
‘The & oxidation of the given sample of green vitriol is %,
[viva voce
QA. What is oxidation? ‘Ans. A reducing agent gets oxidised itself
“Ans. Oxidation may be defined as one of the following: the other substance, eg. Mobr's salt and Ova
acid,
(2) Lass of electrons, eg. Zn —> Zn®* + 2e
Gi) Loss of hydrogen, e.g, H{O —> Hy + 2 0,
water is oxidised 8
(ai) Gain of oxygen, eg C + 0, —> CO,
carbon is getting oxidised.
Q-2. Define a reduction reaction (electronic concept)
Ans. A reaction involving gain of electrons is called
a reduction reaction,
Q.3. What is a redox reaction?
Ans. A reaction where reduction and oxid
occurring simultaneously is called a redox
reaction.
Q44. Give an example of a redox reaction
Ans. In this reaction, Zn is getting oxidised and
CuSO, is getting reduced
CuSO, + Zn —+ ZnSO, + Cu.
Q.5. What is an oxidising agent? Give one example
of an oxidising agent,
‘Ans. An oxidising agent is the one which oxidises the
other substance and get reduced itself, HNO,,
K,Cr,0,, KMnO, are oxidising agents.
Q.6, What is a reducing agent? Give one example of
a reducing agent.
ion is
Q.7. In the following reaction, identify the species ti
is oxidised and the species that is reduces!
Sn + Hg"? —> Sn!* + Hy,”
‘Ans. (i) Sn* is oxidised to Sn** (loss of electron
(ii) Hg’ is reduced to Hy," (or Hg") (gain
celectrons),
Q8. Name some oxidising agent used in redo
reactions.
Ans. KMn0,, K,Cr,0;.
Q.9. What is the oxidation state of Mn in KMo
- KMn0,
+ lore 2x
+t
Q.10, What is the formula of Mohr's salt?
Ans. FeSO,(NH,),S0,6H,0.
Q.11. What change do KMnO, and Mobr's salt uncles
when they react during redox titration done
acidic medin?
Ans, 8H'+ MnO, + be
Fe" —
From Mol’ salt
Q.12 Which out of KMnO, and Mobr's salt act
reducing agent?
»Mn*"+4H,0 (reduction
> Fel +6 (oxidation
108 Jagether with® Chemistry Lab Manual—12
eed
Scanned with CamScannera
nr salt act as reducing agent, sinc
ting oxidised itself from Fo”
it is
Give one example of a redox titration where 1
solution is used
yp solution is used for titrating @ hypo solution
* Lich is sodium thiosulphate solution, ‘The
Feactions would be
28,0? —> 8,0% + 2
Ty + 2° —> 2
Write the reduction reaction where potassium
dichromate acts as oxidising agent.
r,0} + 14H" + 6° —> 2Cr** + 7H,0
What change does oxalic acid undergo during
the redox reaction between it and KMn0,?
00 — 2CO, + 26° (oxidation process)
COO"
Oxalic acid is getting oxidised to CO,, hence
acts as reducing agent.
What is the principle of volumetric analysis?
(oxidation)
(reduction)
Qu
Ans.
Quis.
16.
see In volumetric analysis, concentration of a
solution is determined by allowing a known
‘volume of a solution to react quantitatively with
another solution of known concentration.
What is an indicator?
Substance which changes colour when the
reaction between two reactants is complete, is
called an indicator. It gives different colours in
different medium and helps in the detection of
the end point.
‘What is an equivalence point?
‘The stage of the titration when the reaction is
just complete is called equivalence point.
What is an end point?
‘After the reaction between the substance and
the standard solution is practically complete;
with one extra drop the indicator shows a clear
visual change in the liquid being titrated. The
stage in the titration at which this occurs is
called the end point.
Q.20. What is a titrant?
Ans. The reagent of known concentration is called a
titrant.
Q21. What is a titrand?
Ans. The substance being titrated is called a titrand.
Q22. How are reactions classified in volumetric
analysis?
Ans, The reactions employed in titrimetric,
volumetric analysis falls into two main
classes:
(a) Those in which no change in oxidation
Quit.
Q.18.
Ans,
Qus.
Q.28.
Ans.
Q24.
‘Ans.
Q27.
Q28.
Ans.
Ans.
state occurs; these are dependent upon
the combination of ions, It includes
neutralisation (acid-base) reactions, complex
formation reactions (EDTA-titrations) and
precipitation reactions
change of oxidation state; as redox reaction
between KMnO, and Mohr's salt or Oxalie
acid
What is a standard solution?
A standard solution is one which contains @
known weight of the reagent in a definite volume
of solution
What is a primary standard?
A primary standard is a substan
concentration solution can be prepared by
directly weighing the sample and dissolving it in
given amount of the solution. It's concentration
value is accurate.
Give examples of primary standard solution
ce where exact
. Mobr’s salt solution and oxalic acid solution.
. What are the conditions that a primary standard
solution must satisfy?
‘A primary standard substance should sa
the following requirements
(a) It must be easy to obtain, to purify and to
preserve in pure state.
(b) The substance should be unaltered in
air during weighing, ie. it should not be
hygroscopic nor oxidised by air; nor affected
by CO, ete.
(©) It should have a high equivalent, so that
the weighing errors may be negligible
(d) The substance should be readily soluble
and its solution should be stable
Is KMnO, solution a primary standard?
No.
Why is KMnO, not a primary standard?
KMnO, sample available is usually contaminated
with MnO, and is not pure. Moreover, its
solution is affected by heat and light and slowly
gets decomposed to MnO, on standing,
Why is Mohr’s salt solution a primary
standard?
Mohr’s salt is a double salt having formula
FeSO,(NH,), SO/6H,O. It is available in pure
crystalline form and is a stable salt. It is not
hygroscopic in nature and the concentration of
its solution does not change on keeping for long
time, Its molecular mass is also high and so,
errors involved in weighing are minimised,
Volumetric Analysis 109
Scanned with CamScannerQAK0, What is a secondary standard?
Ans. A substance whose sohation of exact concentration
cannot be prepared by weighing is called a
secondary standard
QL, Can FeSOLTHAO be considered a primary
standart?
Ans, No, it is a secondary standard since it ie
an efforescont salt, Tt will lose water of
crystallization and change its composition
4.82. Why is NaOH a secondary standard?
‘Ans, Because it is deliquescent in nature, ie,, absorbs
moisture from air. Hence, it can't be weighed
accurately,
Q33. Define molarity,
‘Ans. Nolarity is defined as the number of moles of
‘solute present per litre of solution,
Weight
Molecular weight” V
Q.84, Define normality.
‘Ans. Normality is defined as the gram equivalent of
solute present in 1 L of solution.
Weight__, _1000__
N= Faunalent weight ~ VGnml)
Q35. How are molarity and normality related?
Ans, N= nM
n= no. of electrons gained or lost by 1 molecule
during reduction or oxidation reaction it is
undergoing.
Q.36. How will you determine the equivalent weight
of an oxidising agent?
Ans. The equivalent weight of an oxidising agent
" Molecular weight
No.of electrons gained by 1 molecule
e4., Equivalent weight of KMn0,
__ 158 (its molecular weight)
~ 5 (no. of electrons gained)
37, How can M solution be diluted to get 500 ml.
aint
Fy olution?
‘Ans. Use the formula, M,V, = MV,
Take 100 mL of x solution in standard flask
of 500 mL capacity. Make up the volume by
adding water.
Why do buretto nnd pipette should be rng
Qk.
the solution for which they are to hun!
‘Ana. Burotte and pipette should be rinsed hor
so that any drop of water present in 4
‘washing do not affect the concentraiin
doing titration PW
Q.A19, Should a titration flask als0 be ringeyy —|
‘Ana, No; since the rinsing of the titration fay,
increase the volume, will make it oy
the pipetted one.
ut, Why the last drop of the pipette must nr
out?
‘Ams, Because the last drop in the jet of the .,,
fe not eounted in the volume of the pins
| Why should pipette not be held from iy
Bocause the heat of the body may expan,
lass atthe bull, thereby increasing the,
Soho pipette and hence introducing an ,,
asurement of the volume
in me
. Why is it essential to remove the air
from the jet of the burette before st
titration?
Because the air bubbles may escape an
during the titration and thus affecting
volume of the titrant.
Why is upper meniscus read in coloured solutin
like KMn0,?
Because in case of coloured solutions; the
meniscus is not clearly visible
What is anti-parallex card used for?
It is a piece of white paper put on the burs
that helps in reading the burette corre
What is molality?
It is number of moles of solute disolved per iy
of solvent.
Why is dil, H,SO, added to the Mohr’ «
while preparing it’s standard solution?
Dil. H,SO, is added to prevent the hyde
of Mohr's salt.
Can we use dil. HCI or dil. HNO, to p
acidic medium in KMnO, titration? Give res
No, dil. HNO, is itself an oxidising agent whe
HCI gets oxidised to Cl, by KMn0,
2KMnO, + 16HC] —> 2KCI + 2MnC
+5Cl, +
Why is dil,H,SO, added before doing the
between KMnO, and oxalic acid or “bo
salt?
Q.a3.
Ans.
Qa.
‘Ans.
Q.48.
110 agecher with® Chemistry Lab Manual—12
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oO ction of KMnO,
ato act in acidic medium
I ne eaiam is provided by dil. 180,
acide ™ potassium permangnate titrations done
‘adie medium even though it acts ass
‘ng agent in neutral and basic mediums
ol?
can act as an oxidising agent in acidic,
04
ans Oe and neutral medium as following:
e%fq neutral and weakly basic medium, it
‘undergoes the following change.
MnO, + 2H,0 + 3e —~> MnO, + 4011
(p In strongly alkaline medium,
MnO; + & —+ MnO;
Permanganate ion
‘The manganate ion produced further reduced
to MnO, when a reducing agent is present.
MnO} + 2H,0 + 2e° —+ MnO, + 40H
Hence, the complete reaction would be
MnO; + 2H,0 + Se —> MnO, + 40H-
(came reaction as neutral medium)
(© In acidic medium,
MnO, + 8H’ + 5e° —> Mn” + 4H,0
We see that in basic and neutral medium
MnO, a brown ppt. is obtained which will
hinder the observation of the colour change
at the end point. Hence, the acidic medium
is choosen for the titration.
(50. Why do we titrate Mohr’s salt and not FeSO,
with KMnO,?
‘Ans. Because FeSO, gets readily oxidised by air thereby
change in the composition or concentration of
the solution would occur, introducing errors in
the volumetric measurements.
Q51. KMn0, solution bottle develops a brown layer
on glass, why?
‘Ans. Due to the decomposition of KMnO, to MnO,
in presence of light and heat.
(Q52 Why do we heat the oxalic acid solution to
60-70°C in case of oxalic acid-KMn0, titration?
Ans. To increase the rate of reaction as the rate of
the reaction between them is very slow at room
temperature.
53. Why is strong heating at 100°C not recom-
mended?
Ans. On strong heating oxalic acid may decompose
0 CO, and CO thereby change in concentration
of the solution will occur.
54. Mohr’s salt ve KMnO, titration is done in cold
why not in hot?
As (a) The rate of reaction is fairly high at room
temperature, hence there is no need to
heat.
Manganate ion
a
Qs.
Ans.
0.56.
Ans.
Q097.
Ans.
Q58.
Ans.
Ans.
Ans.
Qs.
‘Ans.
Q.62.
Ans.
Q.63.
‘Ans.
Ans,
oxidised to Fe” at high
(b) Fe? get
temperature
the end point?
or Mohr’s salt full
and an extra drop of
the solution.
w
At the end point oxalic acid
4s oxidised to CO, o Fe
KMn0, furnishes pink colour in
What is the colour of Mn”?
Mn” ions are light pink but in
‘ lour at the end point
at happen
dilute
appear
solutions,
colourless, The pink cok
due to MnO; ions and not due to Ma
What is the meaning of auto-catalysis im
ration
to KMnO, 0» oxalic acid titration?
Mn” ions produced during the initial stat
Aitalyse the reaction and the react
t catalysis
eof the
titration, catal;
is fast later. It is called auto~
What is meant by normal solution?
A solution containing 1 gram equivalent of solute
dissolved per litre of solution is called a normal
solution.
What is the equivalent weight of KMnO,
acidic and basic media?
In acidie medium equivalent, weight
Molecular weight _ 158 _ 346
sgt ee
In neutral or feebly basic medium, Equivalent
Molecular weight 2.6.
3
Why is KMnO, solution not filtered through
filter paper?
Filter paper being organic matter reduces
KMnO, and itself gets oxidised.
Why should KMnO, be stored in dark place?
It slowly decomposes on exposure to sunlight
What is a molar solution?
A solution containing 1 g mole of the solute
dissolved per litre of the solution is called a
molar solution.
Which out of molar and molal solution will not
undergo change in concentration with change in
temperature?
Molal solution will not undergo change in cone.
with temperature. Molality depends on weight
of solvent and molarity depends on volume of
solution. With change in temperature weight
remains same but volume changes. Hence, molal
solution's concentration does not change with
change in temperature
weight =
What is the minimum weight that can be
weighed with the chemical balance?
On a usual balance provided with a
ided wi rider we
can weigh 2x 10+ g (with rider) r
Volumetric Analysis 111
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