15 - Chel17 27 - Lab - Manual.2016-17

Dept.
of Chemistry,
AIT
PART A
(Instrumental Experiments)
Dept. of Chemistry,
AIT
Observations and Calculations:

E
Volume of
Potential
3
K2Cr2O7 ( cm ) E (mV)
0.0
0.5
0.5
1.0
0.5
1.5
0.5
2.0
0.5
2.5
0.5
3.0
0.5
3.5
0.5
4.0
0.5
4.5
0.5
5.0
0.5
5.5
0.5
6.0
0.5
6.5
0.5
7.0
0.5
7.5
0.5
8.0
0.5
8.5
0.5
9.0
0.5
9.5
0.5
10.0
0.5
E
V
Volume
of K2Cr2O 7
Equivalence point
Volume of K2Cr2O7
Normality of the potassium dichromate = 0.5

3
From the graph: ---------
K Cr O
N
FAS
cm of 0.5N K2Cr2O7 is required to oxidize

V
0.5 ........
K Cr O
V
FAS
Amount of FAS in 1 dm3 of the given solution = N FAS
25 cm FAS.
25
X Equivalent weight of FAS
X 392 =
g
2
Dept. of Chemistry, AIT
GRAPH
SHEET-1 NO.
Experiment 1
Potentiometric estimation of FAS using standard K2Cr2O7 solution
Theory: Redox titrations can be carried out potentiometrically using platinum-calomel electrode
combination. For the reaction,
Reduced form
Oxidized form + n electrons
The potential is given by Nernst equation,
0.0591
[Oxidized form]
E = E0 +
log
n
[ Reduced form ]
Where E is the standard potential of the system. The potential of the system is thus controlled by the
ratio of the concentration of the oxidized to that of the reduced species present. As the reaction
proceeds, the ratio and hence the potential changes more rapidly in the vicinity of the end point of the
titration. This may be followed potentiometrically and a plot of change in potential against volume
(titration curve) is characterized by a rapid increase in potential at the equivalence point. The rapid
increase in the potential at the equivalence point is explained as follows:
The reaction that takes place
in the3+determination of Fe 2+
2+
is Fe Fe + e
Cr2O72- + 14H+ + 6e 2Cr3+ + 7H2O
Prior to the equivalence point, the potential is determined by the Fe 3+/ Fe2+ system and the potential is
given by the equation,
Ecell = EFe
2+
=E
0.0591
log
= 0.75 V + 0.0591
log
[Fe3+]
[Fe2+]
[Fe3+]
[Fe2+]
The potential of the solution will be around 0.75 V (since the contribution to the potential by the
second term is negligible). At the equivalence point the potential is determined by both E 0Fe2+ and
E0Cr2O72- and is given by
2- 2-
at the equivalence point the potential is determined by Cr2O7

equation,
0.0591 log Cr2O7
Ecell = Ecr = E0Cr2O7 2- / Cr3+ +

+
1.33V +
0.0591
6
6
log
Cr O
Cr
Cr
/Cr
3+
system given by the
And hence at equivalence point potential rises steeply. In the experiment, the potential of the cell is
determined with reference to saturated calomel electrode.
PROCEDURE:
Pipette out 25.0 cm3 of ferrous ammonium sulphate solution into a beaker. Add one test tube-full of
dilute sulphuric acid. Immerse the Platinum-calomel electrode assembly into the solution and connect
the electrodes to a potentiometer. Measure the potential. Fill the burette with standard potassium
dichromate solution. Add 0.5 cm3 of K2Cr2O7 to the beaker. Stir the solution carefully and measure the
potential after 10 seconds. Continue the procedure till the potential shows a tendency to increase
rapidly. Further take 6 more readings. Determine the end point by differential method i.e., by plotting
E/V against volume of potassium dichromate as shown in the figure. Calculate the normality of the
FAS solution and determine the amount of FAS in the given solution.
Result:
1. Equivalence Point
2. Normality of FAS =
=
3
3. The amount of FAS present in 1 dm of solution =
********
3

Volume of CuSO4
solution ( cm3 )
Absorbance
A
B
S
O
B
A
N
C
E
5
10
15
Vol.of test soln.

Vol. of CuSO4 (cm3)
20
Test Solution
1cm3of the stock solution contains = 4.2 mg of CuSO4.5H2O

1 molecule of CuSO4.5H2O 1 atom of Cu
249.54 mg of CuSO4.5H2O
63.54 mg of Cu
4.2 mg of CuSO4.5H2O=
63.54 4.2
249.54
= 1.069
mg of Cu
mg of Cu
From graph, Volume of CuSO4 in test solution = ---------
cm3
The amount of copper present in the test solution = --------- 1.069

=
mg of Cu
GRAPH
SHEET-1 NO.
Experiment 2
Colorimetric estimation of copper
Theory: When a monochromatic light of intensity I 0 is incident on a transparent medium, a part I a is
absorbed, a part Ir is reflected and the remaining part It is transmitted.
I0 = Ia + Ir + It
For a glass-air interface Ir is negligible. Therefore,
I0 = Ia + It
It / I0 = T, called the transmittance, log 1/T= log I0/It is called the absorbance or optical density A. The
relation between absorbance A, concentration c (expressed in mol lit -1) and path length t (expressed in
cm) is given by Beer - Lamberts law,
A = log I0/It = ct
Where
is the molar extinction coefficient and constant for a given substance at a given wavelength.
If the path length (cell thickness) is kept constant, then, A c. Hence a plot of absorbance against
concentration gives a straight line as shown in figure (calibration curve). The absorbance of the
colored solution is measured using a spectrophotometer at a wavelength where the absorbance is
maximum.
A series of standard solutions containing cupric ions is treated with ammonia to get deep blue
cuprammonium complex and is diluted to a definite volume.
Cu2+ + 4[NH3] Cu[NH3]42+
Deep blue
The absorbance of each of these solutions is measured at 620 nm since the complex shows maximum
absorbance at this wavelength. The concentration is plotted against absorbance to get a calibration
curve. A known volume of the test solution is treated with strong ammonia and diluted to the same
volume as above. The absorbance of this solution at 620 nm is measured and weight of Cu in the test
solution is determined from the calibration curve.
PROCEDURE:
Fill a burette
with the given copper sulphate solution (stock solution). Withdraw
5.0, 10.0, 15.0 and
3
20.0 cm3 of the copper
sulphate
solution
into
separate,
labeled
50
cm
volumetric
flasks from the
burette. Add 5 cm3 of ammonia solution to each of them and make up to the mark with ion exchange
water. Stopper the flasks and mix the solutions well.
To the test solution taken in a 50 cm 3 volumetric flask, add 5 cm3 of ammonia solution and
make up to
3
the mark with ion exchange
water.
Mix
well.
Prepare
a
blank
solution
by
diluting
5
cm
of
ammonia
solution in a 50 cm3 volumetric flask to the mark with ion exchange water and mixing well.
After 10 minutes, measure the absorbance of the solutions against blank at 620 nm using a
colorimeter. Draw a calibration curve by plotting weight of copper against absorbance. Using the
calibration curve determine the weight of copper in the test solution.
Note: Ammonia should be added to all the solutions including the test solution at the same time
Result:
The given test solution contains =
mg of Cu
********
Dept. of Chemistry,
AIT

Volume of NaOH
cm3
Conductance
Volume of NaOH
cm3
-1cm-1
0.0
5.5
0.5
6.0
1.0
6.5
1.5
7.0
2.0
7.5
2.5
8.0
3.0
8.5
3.5
9.0
4.0
9.5
4.5
10.0
5.0
10.5
Conductance
-1cm-1
C
o
n
d.
.
V1
Volume of NaOH
From graph: Volume of NaOH required to neutralize HCl
cm3 (Say v1)
cm3 (Say v2)
Volume of NaOH required to neutralize both HCl and CH 3COOH =

Volume of NaOH required to neutralize CH3COOH = (v2 - v1 )
cm3
Normality of NaOH = 1
Normality of HCl
Normality of NaOH Volume of NaOH

Volume of HCl
Therefore, the weight of HCl/dm3 = Normality of HCl x Eq. mass of HCl

=
Normality of CH 3COOH
x 36.5 =
Normality of NaOH Volume of NaOH

Volume of CH3COOH
Weight of CH 3COOH /dm3 = Normality of CH 3COOH x Eq. mass of

=
V2
x 60
CH3COOH
GRAPH
SHEET-1 NO.
Experiment 3
Conductometric estimation of HCl and CH3 COOH in a mixture using standard NaOH
Theory:
The neutralization point in acid-base titrations is determined by a change in the color of the
indicator. Such a determination can also be carried out by conductometric titration. In conductometric
titrations, there is a sudden change in conductance of the solution near the neutralization point.
However, the change is not sharp and hence the neutralization point is determined graphically by
plotting conductivity against titre values. The principle underlying conductometric titrations is the
replacement of ions of a particular conductivity by ions of different conductivity during titration.
When hydrochloric acid is titrated against sodium hydroxide the following reaction occurs:
NaOH + HCl
NaCl + H2O
The addition of sodium hydroxide to hydrochloric acid decreases the conductance of the latter because
highly mobile H+ ion (mobility: 350 ohm-1m-1) are replaced by the less mobile Na + ion (mobility: 50
ohm-1m-1). This trend continues till all the H+ ions of HCl are replaced i.e., the acid is neutralized and
end point is reached. Further addition of NaOH raises the conductance steeply due to the presence of
free OH- ions (mobility: 198 ohm-1 m-1). A typical titration curve is shown in the figure.
PROCEDURE:
Fill a microburette with the standard NaOH solution. Pipette out 50 cm 3 of the given acid mixture into
a clean 100 cm3 beaker. Wash and immerse the conductivity cell into the beaker. Connect the cell to
the conductivity bridge and measure the conductance of the solution. Add 0.5 cm 3 NaOH solution
from the burette. Stir the solution gently and measure the conductance. Continue the measurement of
conductance after each addition of 0.5 cm3 of NaOH. The conductance initially decreases and then
rises moderately. Continue addition of NaOH. The conductance rises sharply. Continue taking
readings till the initial reading is observed.. Plot a graph of conductance versus volume of NaOH.
From the graph, find the neutralization points and the volumes required to neutralize the acids. From
this calculate the amount of HCl and acetic acid present in 1 liter mixture.
Result: 1. Normality of HCl
2. Weight of HCl
3. Normality of CH3COOH
4. Weight of CH3COOH
*******
7
Observations and Calculations

Volume of NaCl
(cm3)
I
n
Emission Intensity
(Candella)
e
n
s
i
t
y
5
10
15
20
Volume of NaCl (ml)
Test Solution
From graph, Volume of NaCl =
ml (Say X)
1ml of NaCl contains 0.0001g of NaCl

X ml of NaCl contains = X x 0.0001 g of NaCl
= -------------
g of NaCl (say Y)
58.5 g of NaCl contains 23 g of Na

Y g of NaCl contains
g of Na
----------
(SayZ)
= Z x 1000 mg of Na
GRAPH
SHEET-1 NO.
Experiment 4
Flame photometric Estimation of Sodium
Theory
Sodium, potassium, calcium and lithium and other common elements impart characteristic s with the
Bunsen flame. The intensity of the emitted flame varies with the amount of element introduced. This
forms the basis of flame photometry.
When a solution containing a compound of the metal to be investigated is aspirated into a flame, the
following processes occur.
i) Solvent evaporates leaving behind a solid residue.
ii) Vaporization of the solid coupled with dissociation into its constituent atoms, which are
initially in the ground state.
iii) Some gaseous atoms get excited by the thermal energy of the flame to higher energy
levels.
The excited atoms which are unstable quickly emit photons and return to lower energy state i.e.
ground state. Flame photometry involves the measurement of emitted radiation.
Schematically it is represented as:
Evaporation
Vapourisation
Dissociation
M +X MX
MX
M (gas) + Gas
Thermal excitation
M (g) Flame emission, h
The relationship between the ground state and excited state populations is given by the Boltzmann
N1/No = (g1/go)e- E/kT where
equation:
N1 = Number of atoms in the excited state
No = Number of atoms in the ground state
g1/go = ratio of statistical weights for ground and excited states
E = Energy of excitation = h
k = the Boltzmann constant, T = Absolute Temperature
From the above equation, it is evident that the ratio N 1/No is dependent upon both the excitation
energy E and the temperature T. An increase in temperature and a decrease in E will both result in a
higher value for the ratio N1/No.
PROCEDURE:
1.
2.
3.
4.
5.
Transfer 5, 10, 15, and 20 ml of standard NaCl solution (which is prepared by weighing
accurately 2.542 g NaCl into a 1 litre volumetric flask and dissolving the crystals and
diluting the solution up to the mark with distilled water and mixwell. The solution gives
1 ppm/ml) into 50 ml standard volumetric flasks and dilute up to the mark with distilled water.
Place the distilled water in the suction capillary of the instrument and set the instrument to
read zero.
Place each of the standard solutions in the suction capillary and record the emission intensity.
Dilute the given test solution up to the mark and shake well and place the solution in the
suction capillary and record the emission intensity.
Draw a calibration curve by plotting the Emission intensity (y-axis) against volume of NaCl
solution (x-axis).
From the calibration curve, find out the volume of the given test solution and calculate
the amount of Na.
Result:
The test solution contains = -----------
mg of Na
********
9

Volume of
NaOH ( cm3)
pH
pH
pH
V
0.0
0.5
0.5
1.0
0.5
1.5
0.5
pH
V
Vol. of NaOH
Equivalence point
2.0
0.5
2.5
0.5
3.0
0.5
3.5
0.5
4.0
0.5
4.5
0.5
pH
5.0
0.5
pKa
5.5
0.5
6.0
0.5
6.5
0.5
7.0
0.5
7.5
0.5
8.0
0.5
8.5
0.5
9.0
0.5
9.5
0.5
10.0
0.5
Vol.of NaOH
Half equivalence point
From the graph: Volume of NaOH at equivalence point = ----------
cm
Volume of NaOH at Half equivalence point = ---------- cm

pKa value of the given weak acid =
10
GRAPH
SHEET-2
NOS.
Experiment 5
Determination of pKa value of weak acid using pH meter
Theory: In the titration of an acid with a base, the pH of the solution increases gradually at first, then
more rapidly, until at the equivalence point, there is a very sharp increase in pH for a very small
quantity of added base. Beyond the equivalence point, the pH increases only slightly on addition of
excess base. The titration curve obtained by plotting changes in pH against volume of the base added.
Just as the pH is a measure of the hydrogen ion concentration, pK a is a measure of the dissociation
constant (Ka) of an acid. The pKa value of an acid can be calculated using Henderson -Hasselbalch
equation,
pH = pKa + log [salt]/[acid]
Where pKa = -log Ka
At half equivalence point, [salt] = [acid] and hence pH = pK a . Thus pH at half equivalence point
gives the pKa of the weak acid.
PROCEDURE:
Pipette out 25.0cm3 of the given weak acid into a beaker. Immerse a glass electrode - calomel
electrode assembly into the acid and connect the cell to a pH meter. Measure the pH of the acid. Fill a
microburette with the sodium hydroxide. Add NaOH with an increment of 0.5 ml to the beaker. Stir
the solution carefully and measure the pH after each addition. After the rapid increase in pH, take 6
more readings by adding NaOH.
Plot a graph of pH/V against V and determine the equivalence point. Plot a graph of pH (ordinate)
against the volume of sodium hydroxide added (abscissa). Determine the pH at half equivalence point.
This gives the pKa of the weak acid.
Result:
pKa value of the given weak acid =
********
11
Mark
A
Mark
B
Constant
temperature
bath
Time flow in seconds

Trial 1
Trial 2
Trial 3
Average
Test liquid
(tl)
Water (tw)
Liquid no.
Lab temperature
dw = Density of water
w = Viscosity coefficient of water =
dl = Density of liquid
= -------------- g cm
-3
------------ millipoise
= -------------- g cm
Coefficient of viscosity of the given liquid l
-3
w dl tl
dw tw
12
Experiment 6
Determination of Viscosity coefficient of organic liquid by Ostwalds viscometer
Theory: Viscosity arises due to internal friction between moving layers of molecules. A liquid flowing
through a cylindrical tube of uniform diameter is expected to move in the form of molecular layers. A
layer close to the surface is almost stationary while that at the axis of the tube moves faster than any
other intermediate layer. A slow moving layer exerts a friction on its nearest moving layer. This
property of a liquid by which it opposes motion between layers is called viscosity. The coefficient of
viscosity is defined as the tangential force per unit area required to maintain a unit velocity gradient
between any two successive layers of a liquid situated unit distance apart. The
coefficient of viscosity of a liquid is given by Poiseuilles formula,
4
pr t
8v l
Where v = volume of the liquid, r = radius of the tube, l = length of the tube, p is the pressure
difference between the two ends of the tube, is the coefficient of viscosity of the liquid and t is the
time of flow. If equal volumes of two different liquids are allowed to flow through the same capillary
under identical conditions, then
t1 d1
=
. (1)
tw dw
The time (t1) taken by the test liquid to flow through a certain distance in the capillary is determined.
The time (tw) taken by a water to flow through the same distance is measured. Coefficient of viscosity
of the test liquid is calculated from the densities (d l and dw) of the test liquid and the water and the
coefficient of viscosity of the water. The viscosity measurement is carried out in Ostwalds
Viscometer shown in figure. Viscosity is a temperature dependent property and hence the
measurements are carried out at constant temperature.
PROCEDURE:
Fix the dry viscometer vertically to stand in a constant temperature bath (beaker containing water).
Transfer a known volume (say 10 cm 3) of water into the wider limb by clean pipette. Allow the
viscometer to stand for some time so that the liquid attains the bath temperature. Suck the water above
the upper mark A of the viscometer. Allow it to flow freely through the capillary. When the level of
water just crosses mark A, start a stop clock. Stop the clock when the water just crosses the lower
mark B. Note the time of flow in seconds (t w). Repeat to get agreeing values. Pour out the water, rinse
the viscometer with acetone and dry it. Repeat the experiment with exactly the same volume of the
liquid whose viscosity is to be determined and find the time of flow (t l seconds). Calculate the
coefficient of viscosity of the liquid using Eq. (1).
Note: Dry the viscometer thoroughly before conducting the experiment with test liquid
Result: The viscosity co-efficient of the given liquid = --------------- millipoise
********
13
PART-B (VOLUMETRIC EXPERIMENTS)

Weight of weighing bottle + FAS crystals
Weight of empty weighing bottle
Weight of FAS crystals transferred
Normality of FAS =
Weight of FAS transferred 4
X 4
=
Equivalent mass of FAS
392
=
FAS
in burette
Final burette
reading
Initial burette
reading
Volume of
FAS run down
(cm3)
Trial 1
Trial 2
0.0
0.0
Back titre value =
Trial 3
0.0
(say z)
Indicator
and color change
Ferroin
Bluish green to
reddish brown
cm3 (say y)
cm3 (say x)
Blank titre value = y + 10 =
Volume of FAS equivalent to oxidizable impurities = (x-y) cm3 =

1000 cm3 of 1 N FAS solution = 1 equivalent of oxygen
cm3
= 8 g of oxygen
(x - y) cm3 of z N ferrous ammonium sulphate solution
8 x - y z
g of oxygen
1000
That is 25 cm3 of waste water = 8 x - y z g of oxygen
1000
1000 cm3 of the wastewater sample
COD of the wastewater sample
8(x y)z
g of oxygen
25
8000(x y)z mg of oxygen

25
=
14
Experiment 7
Determination of chemical oxygen demand (COD) of waste water - redox titration
Theory: Chemical oxygen demand is a measure of the oxygen equivalent of organic and inorganic
materials in a water sample that can be oxidized by a strong chemical oxidant. This parameter is
important for industrial waste studies. COD is expressed as mg of oxygen required to oxidize
impurities present in 1000 cm3 of waste water.
The oxidizable constituents of waste water include straight chain aliphatic compounds,
aromatic hydrocarbons, straight chain alcohols, acids, pyridine and other oxidizable materials. Straight
chain compounds and acetic acid are oxidized more effectively in presence of silver ions (added as
silver sulphate) as catalyst. However, the silver ions become ineffective in presence of halide ions
(present in waste water) owing to the precipitation of silver halide. This difficulty is overcome by
treating the waste water with mercuric sulphate before the analysis for COD. Mercuric sulphate binds
the halide ions and makes them unavailable.
A known volume of the waste water sample is treated with known excess of acidified
potassium dichromate. Unreacted dichromate is titrated against standard ferrous ammonium sulphate
solution using ferroin indicator. A blank titration without the water sample is performed. COD of the
water sample is determined from the difference in the titre values.
This is a redox titration
PROCEDURE:
Preparation of standard solution of FAS (Mohrs salt)
Weigh out accurately about 4.0 grams of ferrous ammonium sulphate into a 250 cm 3 volumetric flask.
Add one test-tube full of dilute sulphuric acid and swirl the flask to dissolve the crystals. Dilute the
solution up to the mark with ion exchange water. Mix the solution well. Calculate the normality of
ferrous ammonium sulphate.
Back titration: Pipette out 25.0 cm3 of the waste water sample into a 250 cm 3 conical flask. Add 10.0
cm3 of standard potassium dichromate using a pipette followed by one-test-tube full of 1:1 sulphuric
acid (containing silver sulphate and mercuric sulphate) Add 2-3 drops of ferroin indicator and titrate
against the ferrous ammonium sulphate solution until the solution turns from bluish green to reddish
brown.
Blank titration: Pipette out 10.0 cm3 of potassium dichromate solution. Add one test-tube full of 1:1
sulphuric acid followed by 2-3 drops of ferroin indicator and titrate against the ferrous ammonium
sulphate solution till the solution turns from bluish green to reddish brown.
Result:
1. Normality of FAS =
2. COD of the given waste water sample = ------------ mg of oxygen per litre
********
15

Na2S2O3 in burette
Trial 1
Final burette
reading
Initial burette
reading
Volume of Na2S2O3
run down (cm3)
0.0
Trial 2
Trial 3
0.0
0.0
Disappearance
of blue color
Weight of brass sample (w) =

Normality of sodium thiosulphate =
Indicator color
change
Starch towards
the end point
g
0.2
(say y)
cm3 (say x)
Volume of sodium thiosulphate required =
1000 cm3 of 1 N sodium thiosulphate = 1equivalent of Cu

(One equivalent of Cu = atomic mass of copper = 63.54)
Therefore, 1000cm3 of 1 N sodium thiosulphate = 63.54 g of Cu
x cm3 of y N sodium thiosulphate =
Percentage of copper in the brass sample
g of Cu (say a)
a 100
w
16
Experiment 8
Determination of percentage of copper in brass - iodometric titration
Theory: Brass is an alloy of copper and zinc. It also contains small amounts of tin, lead and iron. The
percentage composition of a typical brass alloy is Cu: 50-90 % Zn: 20-40 % Sn : 0-6 % Pb: 0 - 2 % Fe
: 0 - 1%
The amount of copper present in brass can be determined iodometrically. A solution of brass is made
by dissolving the sample in minimum amount of nitric acid. Excess nitric acid is destroyed by boiling
with urea. The solution is treated with ammonia to remove any mineral acid and acidified with acetic
acid. Then potassium iodide is added. The potassium iodide reduces cupric ions to cuprous ions
liberating equivalent amount of iodine. And cuprous iodide is precipitated.
2Cu2+ + 4KI
Cupric
Cu2 I2+ 4K+ + I2
Cuprous iodide
The liberated iodine is titrated against sodium thiosulphate using starch as indicator towards the end
point.
2+ 2I 2S2O32- + I2 S4O6
Thiosulphate
Tetrathionate
Starch forms a blue complex with iodine. The end point is detected by a sharp disappearance of the
blue color. The volume of sodium thiosulphate required is a measure of the amount of copper present.
Note: i) Brass solution should not contain mineral acids as they would oxidize iodine to iodic acid and also
decompose sodium thiosulphate (hence the solution is neutralized with aqueous ammonia and acidified with
acetic acid) .
ii) Starch is invariably added near the end point when the concentration of iodine is low. At high iodine
concentrations a water insoluble starch- iodine complex is formed which results in error in the end point.
PROCEDURE:
Dilute the given Brass solution in 250 cm3 volumetric flask up to the mark with ion exchange water.
Mix well.
Estimation of copper:
Pipette out 25 ml of above prepared brass solution into a clean conical flask Add aqueous
ammonia drop wise until a pale blue precipitate. [Cu(OH) 2, is formed] Dissolve the precipitate by
adding test tube of dilute acetic acid. Add one test-tube-full of 10 % KI. Titrate the liberated iodine
against standard sodium thiosulphate solution till the mixture turns straw yellow. Add 1dropper starch
indicator and continue the titration till the blue color just disappears and a white precipitate is left
behind. Repeat the titration for concordant values.
Result:
Percentage of copper in Brass = ----------
********
1
7
Dept. of Chemistry,
AIT

Weight of weighing bottle + K2Cr2O7 crystals
Weight of empty weighingbottle

bottle
Weight of K2Cr2O7 crystals transferred
Weight of K2Cr2O7 transferred 4
X 4
Normality of K2Cr2O7 =
=
Equivalent mass of K2Cr2O7
49
=
K2Cr2O7
in burette
Trial 1
Trial 2
(say y)
Indicator & color change
Trial 3
K3[Fe(CN) 6]
(External)
Final burette
reading
Initial burette
reading
0.0
0.0
0.0
No blue or green color
with indicator
Volume of
K2Cr2O7 run
down (cm3)
Weight of haematite ore in 250 cm3 of the given solution (w) =
1.6 g
Volume of potassium dichromate required = . cm3.(say x)

1000 cm3 of 1 N K2Cr2O7 = 1 equivalent of Fe
(1 equivalent of Fe = atomic mass of Fe = 55.85)
1000 cm3 of 1 N K2Cr2O7 = 55.85 g of Fe
x cm3 of y N K2Cr2O7 =
g of Fe (say a)
25.0 cm3 of haematite solution contains a g of

Fe 250 cm3 of the solution contains 10 a g of Fe
Percentage of iron in the given haematite ore sample =
10a
w
X 100
=
18
PROCEDURE:
Preparation of standard solution of K2Cr2O7:
Experiment 9
Estimation of percentage of iron in haematite ore solution by external indicator method

Theory: Haematite is an important ore of iron containing mainly Fe 2O3 and a small amount of silica
(SiO2). A known weight of the ore is digested with hydrochloric acid and the insoluble residue mainly
containing silica is removed by filtration. The filtrate is diluted to 250 cm 3 and is supplied for the
estimation.
Iron present in the solution as Fe 3+ (ferric) ions is reduced to Fe 2+ (ferrous) ions using
stannous chloride (SnCl2) in hot condition in presence of concentrated HCl. The excess stannous
chloride is oxidized to stannic chloride, by treating the cooled solution with mercuric chloride. The
ferrous ions in the resulting solution are titrated against standard potassium dichromate using
potassium ferricyanide as external indicator. Potassium ferricyanide produces an intense deep blue
color with ferrous ions due to the formation of ferroferricyanide complex. The end point is noticed
when the indicator fails to form deep blue or green with drop of the test solution.
2Fe3+ + Sn2+ 2Fe2+ + Sn4+
SnCl2 + 2HgCl2 Hg2Cl2
+ SnCl4
Mercuric chloride
Cr2O72-
Mercurous chloride
Fe2+ Fe3+ + e 6
+ 14H+ + 6e 2Cr3+ + 7H2O
Adding (1) and (2),

6Fe2+ + Cr2O7
2-
........(1)
........(2)
+ 14H+ 6Fe3+ + 2Cr3+ + 7H2O
Weigh out accurately about 1.0 g of potassium dichromate crystals and transfer it into a 250 cm 3
volumetric flask. Dissolve in ion exchange water, make up to the mark and mix well. Calculate the
normality of potassium dichromate.
Estimation of Iron:
Pipette out 25.0 cm3 of the haematite solution into a clean conical flask. Add T T of concentrated
HCl and heat the solution to boiling. Add stannous chloride to the hot solution drop wise till the
yellow solution just turns colorless. Add 2 drops in excess to ensure complete reduction. Cool, and
rapidly add T T of mercuric chloride followed by 2 T T ion exchange water. A silky white
precipitate of mercurous chloride is formed.
Place a number of drops of freshly prepared potassium ferricyanide indicator on a wax paper. Add a
few cm3 of potassium dichromate from the burette to the conical flask and mix well. Using a clean
glass rod withdraw a drop of the solution from the flask and bring it in contact with a drop of the
indicator on the wax paper. The color of the indicator turns deep blue. Add 1 cm 3 of the potassium
dichromate and again bring a drop of the titrated solution in contact with a fresh drop of the indicator.
If the blue color develops, continue the titration by adding increments of 1 cm 3 at a time and testing as
above till a drop of the mixture fails to produce a blue color with the indicator (clean the glass rod
after every test).
Repeat the titration with another 25.0 cm 3 of the haematite solution. In the next trial, add most of the
potassium dichromate required at a stretch and then titrate drop wise. Mix the contents of the flask
after every addition and test a drop of the titrated mixture with a drop of the indicator as described
above till the color of the indicator drop fails to develop blue or green color. Repeat for agreeing
values.
Note: (i) SnCl2 should be added drop wise to the hot solution (ii) Mercuric chloride should be added rapidly in
cold condition. A large excess stannous chloride reduces mercuric chloride to mercury (grey precipitate).
Formation of a grey precipitate on the addition of HgCl 2 indicates that a large excess SnCl 2 has been added in
which case the trial has to be discarded. (iii) Potassium ferricyanide forms a blue precipitate with Fe(II).
Hence, the titration has to be stopped when the titrated solution just fails to produce a color with the indicator.
Result:
1. Normality of K2Cr2O7 = ------------ 2. Percentage of Fe in the haematite ore sample = ------------
********
1
9
Dept. of Chemistry,
AIT

Weight of weighing bottle + EDTA crystals
Weight of empty EDTA crystals transferred
Molarity of EDTA =
Weight of EDTA transferred 4
X 4
=
Molecular mass of EDTA
372
=
EDTA in burette
Trial 1
Final burette
reading
Initial burette
reading
Volume of EDTA
run down cm3
0.0
Trial 2
Trial 3
0.0
(say z)
Indicator &
color change
Eriochrome
Black T
0.0
Wine red to
blue
Calculations
Volume of EDTA required to react with 25.0 cm3 of water sample =
cm
(say x)
1000 cm of 1 M EDTA = 100 g of CaCO3 (Molecular mass of CaCO3 =100)

x z 100
x cm of z M EDTA
1000 1
g of CaCO3
=
=
(say a)
25.0 cm of the water sample contains a g of CaCO3

a 10 6 ppm of CaCO
25.0
10 6 cm3 ( 1 million cm3 ) of hard water contains
Total hardness of the given water sample
ppm of CaCO3
ppm of CaCO3
20
Experiment 10
Determination of total hardness of water - complexometric titration
Theory: Hardness of water is due to the presence of dissolved salts of calcium and magnesium. The
total hardness is determined using ethylenediaminetetraacetic acid (EDTA) and is expressed in terms
of parts per million (ppm) of CaCO3. EDTA is a hexadentate ligand and forms complexes with Ca 2+
and Mg2+ ions. The molecule represented as H 4Y has two easily replaceable hydrogen atoms. EDTA
has the structure
HOOC - CH2
CH2 - COOH
N - CH2 -CH2 - N
HOOC - CH2
CH2 - COOH
The ionization in solution is represented as

H4Y
H2Y2- + 2H+
The anion formed in the above ionization forms complex with metal ion M 2+ which can be
represented as:
M2+ + H2Y2MY2- + 2H+
where M2+ is Ca2+ or Mg2+.
The total hardness of water can be determined by titrating a known volume of water against
standard EDTA solution at a pH of 10 using eriochrome black-T as indicator. The color of the free
indicator at pH 10 is blue. Eriochrome black-T forms a wine red complex with M 2+ which is relatively
less stable than MY2-. On titration EDTA first reacts with free M 2+ ions and then with the M2+indicator complex. The latter gives a color change from wine red to blue at the equivalence point.
Such indicators are referred to as metal-ion indicators. Since the reaction involves the release of H +
ions, a buffer mixture (NH3 - NH4Cl) is used to maintain a pH of 10. The free acid (EDTA) is only
sparingly soluble; hence the more soluble disodium salt, Na 2H2Y, is used for preparing the reagent.
PROCEDURE:
Preparation of a standard solution of disodium salt of EDTA: Weigh accurately about 2.0 g of
disodium salt of EDTA crystals using an analytical balance. Transfer the crystals carefully into a
funnel placed over a 250 cm3 volumetric flask and find the weight of the emptied weighing bottle.
Add ion exchange water through the funnel to ensure that all the crystals run down into the flask. Add
test tube of NH3. Wash the funnel with ion exchange water and remove the funnel. Dissolve the
crystals by gently swirling the flask. Dilute with ion exchange water and make up to the mark. Stopper
and invert the flask several times to give a homogeneous solution. Calculate the molarity of EDTA.
Determination of total hardness of water sample Using a pipette transfer 25.0 cm3 of the given
water sample into a clean conical flask. Add 2 cm 3 of NH3 - NH4Cl buffer and 1-2 drops of
eriochrome black-T indicator. Titrate against EDTA till the color of the solution changes from wine
red to blue. Repeat the experiment for agreeing values.
Result:
1. Molarity of EDTA =
2. Total hardness of the given water sample = ----------
ppm of CaCO3
********
2
1
Dept. of Chemistry,
AIT

Weight of weighing bottle + EDTA crystals
Weight of EDTA crystals transferred
Weight of EDTA transferred 4
Molarity of EDTA =
X 4
=
Molecular mass of EDTA
372
EDTA in
burette
Trial 1
Final burette
reading
Initial burette
reading
0.0
Trial 2
Trial 3
0.0
(say z)
Indicator &
color change
Patton &
Reeders
indicator
0.0
Volume of EDTA
run down (cm3)
Wine red to
blue
Weight of cement sample in 250 cm3 (w) = 0.6 g

Volume of EDTA required to react with 25.0 cm3 of the cement solution =
1000 cm3 of 1M EDTA = 56.08 g CaO
y cm3 of z M EDTA =
cm3 (say y)
(Molecular mass of CaO = 56.08)
56.08 y z g of CaO (say a)

1000
25.0 cm3 of cement solution contains a g of CaO

250 cm3 of cement solution contains 10a g of CaO
10a 100
Percentage of CaO in the cement sample
22
Experiment 11
Determination of percentage of calcium oxide in cement Rapid EDTA method

Theory: Cement contains calcium, aluminium, magnesium, silica and small quantities of iron. A
known weight of the cement sample is treated with acid and the insoluble residue mainly containing
silica is removed by filtration. Iron and aluminium in the filtrate are precipitated as their hydroxides
and filtered. The resulting solution containing calcium and magnesium is diluted to 250 cm 3 and
supplied for estimation.
Calcium ions present in the solution is determined by titrating a known volume of the
cement solution with EDTA. The solution is treated with diethylamine to maintain the pH at 1214.
4N sodium hydroxide is added to precipitate the Mg present in the solution as magnesium hydroxide
so that Mg does not interfere in the estimation of Ca 2+. The solution is then titrated against standard
EDTA using Patton and Reeders indicator. Glycerol is added to get a sharp end point.
PROCEDURE:
Preparation of a standard solution of disodium salt of EDTA: Weigh accurately about 2.0 g of
disodium salt of EDTA crystals using an analytical balance. Transfer the crystals carefully into a
funnel placed over a 250 cm3 volumetric flask and find the weight of the emptied weighing bottle.
Add ion exchange water through the funnel to ensure that all the crystals run down into the flask. Add
test tube of NH3. Wash the funnel with ion exchange water and remove the funnel. Dissolve the
crystals by gently swirling the flask. Dilute with ion exchange water and make up to the mark. Stopper
and invert the flask several times to give a homogeneous solution. Calculate the molarity of EDTA.
Preparation of a standard solution of disodium salt of EDTA:
Estimation of CaO: Pipette out 25.0 cm3 of the given cement solution into a clean conical flask. Add
test tube of 1:1 glycerol with constant shaking of the contents of the flask followed by test tube
of diethylamine (so as to bring the pH of the solution to 12). Add 1/2 test-tube of 4 N sodium
hydroxide and mix the solution thoroughly. Add 2-3 drops of Patton and Reeders indicator. Titrate
against the EDTA solution till the color changes sharply from wine red to blue.
Note: The titration should be performed very slowly near the end point.
Result:
1. Molarity of EDTA = -----------2. Percentage of Calcium oxide in the given cement sample = -----------
********
23

V1 ml
Burette
readings
Trail 1
Trail 2
V2 ml
Trail 3
Trail 1
0.0
0.0
Trail 2
Trail 3
Final burette
reading
Initial
burette
reading
0.0
0.0
0.0
0.0
Volume of
HCl run
down in cm3
CALCULATION:
Alkalinity of water is expressed as parts of equivalent CaCO 3 per million parts of water.
1000 ml 1N HCl = 50 g of CaCO3
1 ml 1N HCl = 50 mg of CaCO3
Estimation of Phenolphthalein alkalinity (P):
V1 ml 0.1N HCl = V1 x 0.1 x 50 mg of CaCO3
( say a)
25 ml of water sample contains a mg of CaCO3
1000 ml water sample contains = a x 40 mg of CaCO3

=
Phenolphthalein alkalinity (P) = .. mg/l of CaCO3
24
Experiment 12
-
-2
Determination Of Alkalinity (OH , CO3 & HCO3) of water sample using standard
HCl Theory:
The acidity of water sample is its capacity to neutralize a base where as its alkalinity
is measure of its capacity to neutralize acids. Natural water may be acidic or alkaline
depending upon the source of water and the extent and nature of pollutants from industry and
municipal sanitary disposal. If highly alkaline water is used in boiler for steam generation
leads to precipitation of sludge, deposition of scales, and cause caustic embrittlement.
Knowledge of kind of alkalinity present in water and their magnitudes is important. In
calculating the amount of lime and soda needed for water softening. In maintaining a pH
range where acids produced by hydrolysis of salts like MgCl 2, FeCl 2 etc. and coagulants
[Al2(SO4)3, Fe2 (SO4)3,] may be effectively neutralized. In corrosion control, and in internal
conditioning of boiler-feed water. Caustic alkality of industrial waste has to be neutralized
before discharging them into rivers or other receiving waters. Water containing in excess of
alkaline earth concentrations are not suitable for irrigation purposes. The alkalinity of water
sample may be determined volumetrically by titrating it with a standard acid to an arbitrary
pH using an indicator. At the end point, when the color changes from pink to colorless, the pH
is lower to about 8.3. the volume of acid(V 1ml) used up to this point corresponds to the
complete neutralization of hydroxides and conversion of all the carbonate into bicarbonates.
-
OH + H
Co3
-2
H2O (i)
+
+ H HCO3 (ii)
The alkality measured upto this point is called Phenolphthalein Alkalinity . Beyond the
phenolphthalein alkalinity end point, titration is continued using methyl orange indicator.
-
HCO3 + H H2O + CO2 (iii)

The color changes from yellow to orange red occurs at a pH of about 4.5 and additional volume
of acid (v2 ml) used corresponds to the complete neutralization of all the bicarbonates whether
present originally or obtained from carbonates (Reaction ii). The total volume (v 1 + V2) ml used
in the two titrations, therefore, corresponds to the neutralization of hydroxide, carbonate and
bicarbonate. Thus, a measure of total alkalinity, also called Methyl orange Alkalinity .
Alkalinity is expressed as parts of equivalent CaCO 3 per million parts of water.
From the measurement of phenolphthalein and methyl orange alkalinity, it is possible
to calculate the magnitudes of various forms of alkalinity. The possible combinations of ions
causing alkalinity in water are Hydroxides only, Carbonates only, Bicarbonates only,
Hydroxide and Carbonate, Carbonate and Bicarbonate.
The possibility of hydroxide and bicarbonate ions together is ruled out, because they
combine instantaneously to carbonate. Thus, OH and HCO3 ions cannot exit together.
-
OH + HCO3
Co3
-2
+ H2O
25
Estimation of Methyl orange Alkalinity (M):

V2 ml 0.1N HCl = V2 x 0.1 x 50 mg of CaCO3
( say b)
25 ml of water sample contains b mg of CaCO3

1000 ml water sample contains
= b x 40 mg of CaCO3
Methyl orange Alkalinity (M) = .. mg/l of CaCO3

From the value of P and M, calculate the type and amount of alkalinity in water by using
following reference table.
Alkalinity Hydroxide
(ppm)
P=0
0
P=1/2M
0
P<1/2M
0
P>1/2M
2P-M
P=M
M
Water
sample
1
Carbonate
(ppm)
0
2P
2P
2(M-P)
0
Bicarbonate
(ppm)
M
0
M-2P
0
0
Hydroxide (ppm)
Carbonate (ppm)
2P-M =
2(M-P) =
Bicarbonate (ppm)
0
26
PROCEDURE:
Dilute the hydrochloric acid given in 250 ml volumetric flask up to the mark with ion
exchange water and mix well.
Pipette out 25 ml water sample into a conical flask. Add one drop of phenolphthalein
indicator. Titrate against std. HCl until the pink color just disappears. Record the volume of
acid consumed as V1 ml. to the same solution add 2-3 drops of methyl orange indicator and
titrate further until the color changes from yellow to orange red. Record the additional
volume consumed as V2 ml. repeat the procedure two more time to get concurrent readings.
This whole procedure is repeated for different samples of water.
RESULT: Alkalinity of water sample is
i) Hydroxide =.. ppm
ii) Carbonate =.. ppm
iii) Bicarbonate =.. ppm
********
27
OUTLINE OF PROCEDURES
INSTRUMENTAL EXPERIMENTS:
Experiment 1: Determination of pKa value of a weak acid:
Pipette out 25cm3 of the given weak acid into a clean beaker. Immerse the glass electrode- calomel electrode assembly
into the acid. Connect the electrodes to a pH meter and measure the pH. Add NaOH from a microburette in increments
of 0.5 ml and measure the pH until there is a sharp rise in the pH. Take 4 more readings. Plot the graph of pH/V
Versus Volume of NaOH and pH Versus Volume of NaOH. From the graph report the pKa value of the given weak acid.
pH
pH
V
pKaa
volume of NaOH
Equivalence point
V ol. of NaOH
Half eq.point
Experiment 2 : Colorimetric estimation of copper

Fill a burette with copper sulphate solution. Draw out 5, 10, 15 and 20 ml of the solution into 4 separate 50ml standard
flasks. Add 5 ml of ammonia solution to the flasks and to the flask containing the test solution. Dilute all the solutions
up to the mark with ion exchange water. Prepare a blank by taking 5 ml of ammonia solution in a 50ml standard flask
and diluting up to the mark. Shake well. Measure the absorbance of all the solutions against the blank at 620nm. Draw
a calibration curve and determine the weight of copper in the test solution,
A
B
S
O
B
A
N
C
E
Vol.of Test solution

Vol. of CuSO4 (cm3)
Experiment 3 : Conductometric estimation of HCl and CH3COOH in a mixture

Pipette out 50ml of the acid mixture into a clean beaker. Immerse the conductivity cell into the acid. Connect the cell to
a conductivity bridge and measure the conductivity. Add NaOH solution from a microburette in increment of 0.5ml and
measure the conductivity. The conductivity initially decreases and later starts increasing moderately finally rapidly.
Take readings till initial reading. Plot a graph of volume of NaOH against conductivity and estimate the amount of HCl
and acetic acid in the given solution.
C
o
n
d.
.
V1
V2
Volume of NaOH
28
Experiment 4: Potentiometric estimation of FAS

Pipette out 25ml of FAS solution into a beaker. Add 1 test tube of dil. H 2SO4. Immerse the platinum-calomel electrode
assembly into the mixture. Connect the electrodes to a potentiometer and measure the potential. Add K 2Cr2O7 solution
form a microburette in increments of 0.5ml and measure the potential after each addition until there is a steep rise in
the potential. Take 4 more readings. Plot a graph of E/V versus volume of potassium dichromate. From the
equivalence point obtained calculate amount of FAS present in one liter solution.
E
V
equivalence point
Volume of K2Cr2O7
Experiment 5: Determination of viscosity coefficient of a liquid.

Pipette out 10ml of the given liquid into the wider limb of a dry viscometer. Suck the liquid into the narrow limb.
Allow the liquid to flow freely through the capillary. When the level of the liquid just crosses the upper mark start the
stop clock. Stop the clock when the level of liquid just crosses lower marks. Determine the time (in seconds) required
by the liquid to flow between the two marks. Repeat for agreeing values. Pour out the liquid, rinse the viscometer with
acetone and dry the viscometer. Determine the time required by same volume (10ml) of water to flow between the
same marks. Repeat for agreeing values and calculate the viscosity coefficient of the given liquid using the following
formula.
l = w t 1 d1 =
t w dw
dw = Density of water
d
= Density
of liquid
---------- millipoise
w = Coefficient of viscosity of water

tl = Time flow of liquid
tw = Time flow of water
l = Coefficient of viscosity of the given liquid

Experiment 6: Flame photometric estimation of Na
Transfer 5, 10, 15 & 20 cm3 of standard NaCl solution into 4 separate 50 ml standard flasks and dilute up to the mark
with distilled water. Set the Emission Intensity to zero using ion exchange water. Now measure intensity for all the
above prepared solutions. Dilute the test solution up to the mark in the standard flask with distilled water record the
intensity. Draw a calibration curve by plotting the Intensity against volume of NaCl.
From the calibration curve determine the weight of NaCl and hence the weight of Na in the test solution.
I
N
T
E
N
S
I
T
Volume of test solution
y
Volume of NaCl
Experiment 6: Flame photometric estimation of K

Transfer 5, 10, 15 & 20 cm 3 of standard KCl solution into 4 separate 50 ml standard flasks and dilute up to the mark
with distilled water. Set the Emission Intensity to zero using ion exchange water. Now measure intensity for all the
above prepared solutions. Dilute the test solution up to the mark in the standard flask with distilled water record the
intensity. Draw a calibration curve by plotting the Intensity against volume of KCl.
From the calibration curve determine the weight of KCl and hence the weight of K in the test solution.
I
N
T
E
N
S
I
T
Volume of test solution
y
Volume of KCl
29
VOLUMETRIC EXPERIMENTS:
Experiment 7: Determination of COD of waste water sample
Weigh out about 4.0 g of FAS crystals into a funnel placed over a 250ml standard flask. Add 1 test tube of dil.H 2SO4
and dissolve the crystals. Dilute the solution up to the mark. Shake well.
N FAS
Weight of FAS 4
Equivalent weight of FAS ( 392)
Burette: Standard FAS solution

Conical flask: 25 ml waste water sample+ 10 ml standard K2Cr2O7 + 1 test tube of 1:1
H2SO4. Indicator: ferroin
End point: blue green to reddish brown.
Perform a blank experiment under similar conditions but without the waste water sample.
From the difference in the blank and back titre values, calculate the COD of the waste water sample.
Experiment 8: Determination of percentage of copper in brass
Dilute the given Brass solution in 250 cm3 volumetric flask up to the mark with ion exchange water. Mix well.
Burette: Standard Na2S2O3 solution
Conical flask: 25 cm3 brass solution + 1:1 ammonia drop wise till a slight ppt. + test tube acetic acid to dissolve the
ppt. + 1 test tube 10% KI
Indicator: Starch towards the end point
End point: Disappearance of blue color.
From the titre value calculate the percentage of copper in the given brass sample.
Experiment 9: Determination of percentage of iron in haematite
Weigh out about 1.0 g of K2Cr2O7 crystals into a funnel placed over a 250ml standard flask. Add ion exchange water.
Dissolve the crystals, and dilute the solution up to the mark. Shake well.
N K2Cr2O7
Weight of K2Cr2O7 4
Equivalent weight of K2Cr2O7 ( 49)
Burette: Standard K2Cr2O7 solution

Conical flask: 25ml haematite solution + test tube of Conc. HCl, boil + SnCl 2 drop wise in hot condition till the
solution turns colorless + 2 test tubes water , Cool + test tube HgCl 2 at a stretch, .
Indicator: K3Fe(CN)6 (external)
End point: Indicator fails to turn blue color with test solution drop.
From the titre value calculate the percentage of iron in the haematite sample..
Experiment 10: Determination of total hardness of water;
Weigh out about 2.0 g of EDTA crystals into a funnel placed over a 250ml standard flask. Add ion exchange water to
run down the crystals into the flask. Add test tube of ammonia solution, dissolve the crystals. Dilute the solution up
to the mark. Shake well.
MEDTA
Weight of EDTA 4
Molecular mass of EDTA (372)
Burette: Standard EDTA solution

Conical flask: 25ml hard water sample + 5ml of NH3-NH4Cl buffer
Indicator: Eriochrome Black T
End point: wine red to blue.
From the titre value calculate the total hardness of the water sample.
30
Experiment11 : Determination of percentage of CaO in cement

Weigh out about 2.0 g of EDTA crystals into a funnel placed over a 250ml standard flask. Add ion exchange water to
run down the crystals into the flask. Add test tube of ammonia solution, dissolve the crystals. Dilute the solution up
to the mark. Shake well.
MEDTA
Weight of EDTA 4
Molecular mass of EDTA (372)
Burette: Standard EDTA solution

Conical flask: 25ml cement solution + 5ml of diethyl amine + 5ml of glycerol + test tube of 4N NaOH
Indicator : Patton & Reeders indicator
End point: wine red to blue.
From the titre value calculate the percentage of CaO in cement.
Experiment 12: Determination of Alkalinity (OH-, CO3-2 & HCO3) of water sample using standard HCl
Dilute the given HCl in 250 cm3 volumetric flask upto the mark with ion exchande water. Mix well.
Burette: Standard HCl solution
Conical flask: 25 cm3 of the water
sample Indicator: Phenolphthaleien
End point: Pink to colorless
Indicator: methyl orange
End point: yellow to light orange

From the titre value calculate the alkalinity (OH-, CO3-2 & HCO3) of the given water sample.
31
VIVA VOCE
(The questions given below are only model questions. The students are expected to learn the principle
behind each experiment.)
INSTRUMENTAL EXPERIMENTS:
Experiment 1: Potentiometric estimation of FAS

1. What is potentiometer titration?
The determination of the equivalence point of titration on the basis of potential measurements is
called a potentiometric titration.
2 Explain the principle of potentiometeric titration?
Principle involved in potentiometric titration is the measurement of emf between two electrodes, an
indicator electrode, and a reference electrode. Potential is measured as the titration is in progress. The
equivalence point of the reactions is indicated by a sudden change in potential.
Potentiometry essentially involves the measurement of change in potential as a species in solution is oxidized
or reduced. When a reducing agent is titrated against an oxidizing agent the potential gradually changes in the
beginning but changes rapidly near the end point.
3. What is the relation between potential at an electrode and the concentration of the active species in
the solution? Explain in brief the potentiometric estimation of FAS
Nerst equation gives the relations between the potential at an electrode and the concentration of the active species in
the solution
E EO 0.0591 log oxidizedspecies

reducedspecies
n
initially, when dichromate is added from the burette, Fe2+ is oxidized to Fe3+. As more and dichromate is
added, the concentration of oxidized species (Fe3+) increases and the concentration of reduced species
(Fe2+)decreases. Hence the second factor in the Nernst eqn. increases and potential increases. At equivalence
point once all the ferrous ions are oxidized to ferric ions, the potential increases sharply because the potential
is now due to both ferrous/ ferric system and dichromate / chromic system beyond this, there is no change in
potential because redox reaction is complete.
4. What are the electrodes used in the potential metric estimation of FAS?
The electrodes used in the determination of FAS potential metrically are calomel electrode (reference
electrode) and Platinum electrode ( indicator electrode)
5. What is an indicator electrode?
The electrode whose potential is dependent upon the concentration of the ion to be determined is
termed as indicator electrode. Example: Platinum electrode.
6. Name the reaction that occurs during the titration?
Reaction between FAS and K2Cr2O7 is a redox reaction, in acidic medium is given below:
6FeSO4 + 7H2SO4 + K2Cr2O7
3Fe2(SO4)3 + K2SO4 + Cr2(SO4)3 + 7H2O
7. Explain the potential at equivalence point?

At equivalence point, the redox reaction is complete and the potential due to both ferric ferrous
system and dichromate chromic system are maximum.
8. What are the advantages of potentiometer titration?
1. Turbid, fluorescent, opaque or colored solutions can be titrated.
2. Mixture of solutions of very dilute solutions can be titrated.
3. The results are more accurate because the actual end point is determined graphically.
9. Why is sulphuric acid added?
Sulphuric acid is added because the oxidation reaction with dichromate takes place in acidic medium
Note: in the preparation of a solution of FAS ( COD experiment) Sulphuric acid to avoid the formation of
ferric hydroxide
32
Experiment 2: Colorimetric estimation of copper

1. What is wavelength?
The distance between two adjacent peaks or troughs of waves is called wavelength. It is represented by .
2. Give the range of wavelength in the Visible region?
Visible region consists of radiations of wavelengths between 400nm and 750nm.
3. What is frequency?
It is the number of times a wave passes through a given point in one second. It is represented by .
4. What is colorimetry?
Colorimetry is a method of determination of concentration from the intensity of the colour.
5. What is a photoelectric colorimeter?
It is a device, which measures the amount of light absorbed by colored solution using a photocell.
6. Name the Law on which colorimetric estimation is based .
Colorimetry is based on Beer-Lamberts law.
7. What do you mean by wavelength of maximum absorption (max)?
Each and every colored species absorbs light to a maximum extent at a particular wavelength. This is known
as wavelength of maximum absorption (max).
8. What do you mean by monochromatic light?
Light of single wavelength is known as monochromatic light.
9. What is the difference between electromagnetic light and monochromatic light?
Electromagnetic light consists of radiations of many wavelengths while monochromatic light consists of
single wavelength.
10. Why are filters used in colorimetric experiments?
In colorimetric experiments filters are used to obtain desired monochromatic light i.e., selected spectral
range.
11. State Beers law.
Beers law states when a monochromatic light is incident on a transparent medium. the intensity of a
beam of monochromatic light decreases exponentially as the concentration of the absorbing substance
increases arithmetically.
12. State Lamberts law.
Lamberts law states the intensity of transmitted light decreases exponentially as the thickness of
the absorbing medium increases arithmetically.
16. State Beer-Lamberts law.
Beer-Lamberts law states the amount of light absorbed is directly proportionally to the concentration of
the solution and path length.
A = log Io/It = c l
Where = Molar extinction coefficient, c = concentration, l = path length
A c [ as and l as constant]
Molar extinction coefficient is a constant for a given substance at a given wavelength for a unit path
length and unit molar solution.
17. What is transmittance (T)?
Transmittance is the ratio of intensity of transmitted light to that of incident light
18. What is absorbance?
log 1/T = log Io/It is called absorbance (A) or optical density.
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Dept. of Chemistry,
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19. Explain the principle involved in estimation of copper by colorimetric method?

Copper in the form of cupric ions when treated with ammonia produces a blue colored
Cuprammonium complex.
Cu2+ + 4 NH3
[Cu(NH3)4]2+ The
cuprammonium complex has a maximum absorbance at 620nm.
A series of standard solutions of copper are treated with an optimum amount of NH 3 solution and diluted to
a definite volume. The absorbance of the standard samples is measured at 620nm using a colorimeter and the
absorbance are plotted against concentration to get the calibration curve. A known volume of the test
solution is also treated with the same optimum amount of ammonia and diluted to the same volume. The
absorbance of the sample is measured at 620nm. Then, the concentration of copper in the test solution is
evaluated using the calibration curve.
20. Why is ammonia added to copper sulphate solution?
Why is the same amount of ammonia added in colorimetric determination of copper?
Ammonia is added to get Cuprammonium sulphate [Cu(NH 3)4]SO4 (dark blue complex) same amount of
ammonia is added to nullify the absorbance due to a any coloring impurities present in ammonia.
21. What is a calibration curve?

Calibration curve is obtained from the plot of optical density (absorbance: A) of series of standard solution
against concentration of solution.
22. Name the coloring agent used in estimation of copper by colorimetry?
Ammonia is used as coloring reagent
23. Why is estimation of copper done at 620nm wavelength?
The estimation of copper is carried out at 620nm wavelength because, the cuprammonium complex shows
maximum absorbance at 620nm.
24. What is a blank solution?
A blank solution is one, which contains all the reagents except the analyte.
25. What precaution must be taken to get accurate results in colorimetric experiments?
1. Appropriate filter (wavelength) should to be selected for taking reading.
2. Cuvette or Neslers tube should be cleaned thoroughly and outer surface of it should be free from
coloring matter.
3. Before taking each reading of the sample it should be set to minimum (zero) absorption against
blank solution
26. List the advantages of colorimetric determinations.
1. Colorimetric determinations give more accurate results at low concentration solutions when
compared to titrimetric or gravimetric analysis.
2. The method is extensively used to estimate metals like Cu, Fe, Ni, etc and also biological
substances.
Experiment 3: Conductometric estimation of hydrochloric acid and

acetic acid in a mixture using standard NaOH
1. What is an electrolyte?
Electrolyte is a substance, which can dissociate into ions in aqueous solution.
2. State Ohms law?
Ohms law states that the current, I(ampere), flowing in a conductor is directly proportional to the applied
electromotive force (volt) and inversely proportional to the resistance R(ohm) of the conductor.
I= E / R
3. What is conductance?
The reciprocal of resistance is called the conductance.
4. What is the unit of conductance?
The unit of conductivity is ohm-1m-1.
5. What is a conductivity cell or what is a cell?
A cell is a device, which produces an electromotive force and delivers an electric current as the result of a
chemical reaction.
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Dept. of Chemistry,
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6. What is specific conductivity?

It is the conductivity of a solution placed between two platinum electrodes of 1cm2 area and kept 1cm apart.
7. What is equivalent conductivity?
It is the conductivity of the solution which contains 1 gram equivalent of solute, when placed between
two electrodes 1cm apart.
k 1000
c
and
=kV
Where, V= Volume containing 1 gram equivalent of solute

c= Normality of solution.
8. What is molar conductivity?
It is the conductivity of a solution, which contains 1 gram molecular weight of a substance, when
placed between two electrodes of 1cm2 area and kept of 1 cm apart.
9. What is the principle involved in conductometric titration?
The principle involved in conductometric titration is conductance of the reaction mixture is measured at
various stages of addition of sodium hydroxide using conductivity meter. The conductivity initially decreases due to
the replacement of more mobile H+ by less mobile Na+ and reaches a minimum value which indicates the complete
neutralization of HCl.The conductivity then increases moderately because the neutralization of acetic acid begins.
Since acetic acid is a weak acid, the conductivity increases moderately when NaOH is added. Finally the
conductivity increases sharply because the neutralization of both the acids is complete, and further addition of NaOH
leads to increase in the conductivity due to increase in the number of Na + and OH-. A plot of conductance verses
volume of sodium hydroxide added results in three straight lines. The point of intersection of the first two lines
indicates the neutralization point of HCl. The volume of sodium hydroxide corresponding to this point is the volume
required for neutralization of HCl. The point of intersection of the two lines indicates the neutralization point of both
HCl and acetic acid. The volume of sodium hydroxide corresponding to this point is the volume required for
neutralization of both HCl and acetic acid.
10. Explain the variation in conductivity at equivalence point.

The addition of sodium hydroxide to hydrochloric acid decreases the conductance because of
replacement of highly mobile H+ ions by the less mobile Na+ ions. This continues till all the hydrogen ions
of HCl are replaced and the end point is reached. A further addition of sodium hydroxide increases the
conductance because of the neutralization of acetic acid. The increase is moderate because acetic aicd is a
weak acid and is partially ionized. Once the acetic acid is also neutralized, the conductivity increases
sharply due to increase in the concentration of OH- ions .
11. What are the advantages of conductometric titration?
1. The method is accurate in dilute as well as more concentrated solutions.
2. It can also be employed with coloured solutions.
3. Mixture of acids can be titrated more accurately.
4.
Acidic organic reagents like phenol, can be titrated conductometrically.

sodium hydroxide) vs volume of sodium hydroxide.
Experiment 4: Flame photometric estimation of Na / K

1. Explain the principle of flame photometry in brief.
Flame photometry is based on the atomic spectra arising due to emission of light when atoms are
excited in a flame. When the analyte ( NaCl or KCl) is aspirated into the flame, the solvent ( water)
evaporates, the solid (NaCl or KCl) dissociates into atoms. Some of the atoms absorb thermal energy of the
flame, get excited and move to higher energy state.. the excited atoms are unstable and return to ground state
by emitting the energy as photons. The wavelength of the emitted light characteristic of elements and helps
in identifying the element (qualitative analysis) and the intensity of the emitted light is a measure of the
concentration of the atom and is used in quantitative nalysis.
2. What is the colour imparted to flame by sodium?
Sodium imparts golden yellow colour to the flame.
3. What is the colour imparted to flame by potassium?
Potassium imparts violet (lilac) colour to the flame.
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Dept. of Chemistry,
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4. In what region of electromagnetic spectrum is flame photometry conducted?

Flame photometry is conducted in the visible region
5. What is the basis of flame photometry?
It is based on the measurement of intensity of light emitted when a color is introduced into a flame. The
wavelength of the color tells us the element and the color intensity tells us how much of the element is
present.
6. Why the flame photometer is also called flame emission spectroscopy?
Because using a flame provide the energy of excitation to atoms introduced into the flame.
7. Give the sequence of events that occur in flame photometry.
Liquid sample containing element aspirated into a flame
droplets resulting in the formation of residue
and emission of radiation from atoms
Formation of the liquid droplets
Decompose of residue into neutral atoms
Evaporation of
Formation of excited atoms
wave length and intensity of emitted radiation measured by flame photometry
8. What are the applications of flame photometry?

a) Qualitative analysis: used to detect elements of groups I & II of the periodic table
b) Quantitative analysis: used for the rapid quantitative determination of the elements in group I &
II of the periodic table
c) Carry out simultaneous analysis
d) Used in the analysis of biological fluids and tissues. In these elements like Na, K, Al, Ca, Co and Fe
are detected. Also used for determining Na, K, Al, Ca, Co and Fe in soil analysis
9. What are the factors that influence the intensity of emitted radiation in a flame photometer?
a) Viscosity the addition of substance which increases the viscosity of the solution (e.g. Sucrose)
decreases the intensity of the light emission. This decreases results, due to a reduction in the
efficiency atomization.
b) Presence of acids decreases the light intensity. This decrease arises due to the disturbance of the
initial dissociation equilibrium.
c) Presence of other metals alter the intensity of emitted radiation.
10. What are the limitations of flame photometry?
a) It does not provide information about the molecular form of the metal present in the original
sample.
b) It cannot be used for the detection of the halides or the inert gases.
c) Only few elements can be analyzed
d) Only liquid samples may be used
11. What are the advantages of this spectroscopy?
a) Well understood technique
b) Low running cost and maintenance costs
c) Measurements is possible in a wide range of fluid systems
Experiment 5: Determination of pKa of weak acid using pH meter

1 What is a weak acid? Give Examples
The acid, which ionizes to a small extent in aqueous solution is called weak acid Example: Acetic acid,
chloroaceticacid acid, formic acid etc.,
2. Define degree of dissociation ()
Degree of dissociation = No. of molecules of the electrolyte which ionizes
Total No. of molecules of the electrolyte
3.
What Ka of an weak acid?

Ka is dissociation of a weak acid
Ka( CH3COOH) = [H3O+] [CH3COO- ]
[CH3COOH]
4.
What is pKa of a weak acid?

It is the negative logarithm to the base 10 of dissociation constant.
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Dept. of Chemistry,
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5. What information does pKa give?

pKa is a measure of the strength of a weak acid. Higher the value of Ka smaller is the value of pKa
value. Therefore, an acid with lower pKa value is relatively stronger than the one with higher pKa value.
6. How are pH and pKa related?
The relation between pH and pKa is given by Henderson-Hasselbalch equation,
pH pKa log
salt
[ acid ]
7. Name the electrodes used in pH measurement

The electrode consists of combined glass electrode (indicator electrode) and calomel electrode
(reference electrode).
8. What type of electrode is glass electrode?
Glass electrode is an ion selective electrode.
9. Define pH of a solution?
The pH of a solution is the negative of the logarithm (to the base10) of the effective concentration or
activity of hydrogen ions. Mathematically,
pH = - log10[H+] or [H+] = 10-pH
10.
Explain the pH
scale. pH ranges from
0 - 14
if pH of the solution lies between 0 to < 7 then solution is acidic.
if pH of the solution is 7 then solution is neutral.
if pH of the solution lies between >7 to 14 then the solution is basic.
11. What is an ion selective electrode?

Ion selective electrode is an electrode which is sensitive to a specific ion and develops a
potential proportional to the concentration of the ion.
12. What is the trend observed in pH titration of weak acid vs sodium hydroxide and why?
The pH value increases slowly with the addition of sodium hydroxide till the neutralization point
(equivalence point). At this point there is a sudden rise in pH. The sodium hydroxide added in excess
after the equivalence point produces slight increase in pH.
When weak acid is+titrated against sodium hydroxide, the H+ ions are neutralized by OH- ions, this
results in a decrease in H ion concentration and hence
the pH value increases gradually; after the
equivalence point addition of base increases the OH- ion hence pH of the solution increases suddenly, further
addition of sodium hydroxide produces slight increase in pH.
13. Why does the pH increase suddenly at the equivalence point?
At equivalence point, H+ ions of the weak acid has been neutralized by the OH- ions of added sodium
hydroxide (base); further addition of base increases the OH- ions hence pH of the solution increases
suddenly.
14. What is the significance of plot of pH/V vs. volume of NaOH?
The plot of pH/V vs volume of NaOH is used to find out the equivalence point.
15. What is the significance of plot of pH vs. volume of NaOH?
The pH at half equivalence point is found out from the graph obtained by plotting pH vs. volume of NaOH
and pH at half-equivalence point gives pKa value of the weak acid.
16. Explain the principle of pKa determination from the pH values?
At half-neutralization point i.e., when the acid is exactly half-neutralized, half of the acid (acetic acid)
forms salt (sodium acetate) and hence the concentration of acid and salt are equal. Therefore, the pH at
half-neutralization point is equal to pKa of the weak acid.
Mathematically, at half-equivalencePoint
[salt] = [acid]
by Henderson-Hasselbalch equation, i.e.,
salt
because,
pH pKa log
acid
l
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Dept. of Chemistry,
AIT
Experiment 6: Determination of viscosity coefficient of a liquid using Ostwalds

viscometer
1. Define viscosity of a liquid?
Viscosity arises due to internal friction between moving layers of molecules. A moving layer exerts a
drag or friction on its nearest moving layer backward
2. What is viscosity coefficient of a liquid?
The viscosity co-efficient of a liquid is defined as the tangential force per unit area required maintaining a
unit velocity gradient between any two successive layers of a liquid situated unit distance apart.
3. What is the unit of viscosity coefficient?

The viscosity co-efficient is expressed as Pascal second (Ps) 1Ps =1Kg m-1 S-1.
4. Define density of a liquid.
The density of a liquid is the mass of its unit volume.
5. What is the unit of density?
The density of the liquid is expressed in terms of gram/cm 3.
6. Name the formula used in the determination of viscosity coefficient of a liquid.
The formula is Poiseuille formula = pr4 t /8 v l
Where = Viscosity co-efficient of the liquid, v = volume of the liquid, r = radius of the tube, l = length of the
tube, p = hydrostatic pressure (pressure difference between the two end of the tube), t = time of the flow of
the liquid of volume v.
7. Why should the viscometer be fixed vertically to the stand to record the flow time of liquid and water?
Viscometer should be fixed vertically to the stand to record the flow time of liquid and water to reduce
the tangential force (to minimize the error).
8. Why should viscometer be dried before the time flow measurements of other liquid?
The viscometer should be dried to avoid the formation of emulsion, which changes the rate of flow
of the liquid.
9. Why is acetone used for cleaning viscometer?
Acetone is a good solvent and also has a low boiling point. it is miscible in water and organic
solvents and helps in drying the viscometer quickly.
10. Why is the laboratory temperature recorded for the determination of viscosity of the liquid?
Temperature has a marked influence on the viscosity of the liquid,
11. What are the factors that affect the viscosity of a liquid?
1. Viscosity increases with increase in molecular weight.
2. Polar compounds are more viscous than the non-polar ones.
3. Presence of Hydrogen bonds increases the viscosity.
4. Temperature has marked influences on the viscosity of a liquid. Viscosity
decreases with rise in temperature.
12. Why is the same volume of water & liquid are used in the determination of viscosity coefficient of a
liquid?
The same volume of water and liquid are used to eliminate the volume factor. The viscosity coefficient
of a liquid is determined with reference to that of water.
13. Why same viscometer is used to measure the flow time of water and liquid?
Same viscometer is used to measure the flow time of water and liquid to maintain constant volume
and Radius (r), length of the tube (l) and hydrostatic pressure (p).
14. How is fluidity of a liquid related to viscosity?
Fluidity of a liquid is the reciprocal of viscosity co-efficient. It is a measure of the ease with which the
liquid flows.
15. How is viscosity of a liquid related to its mobility?
Viscosity of a liquid is inversely proportional to its mobility.
Note: Poiseuielle formula is applicable for steady stream lined flow. The capillary in the Ostwalds viscometer
ensure steady stream lined flow.
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Dept. of Chemistry,
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VOLUMETRIC EXPERIMENTS:
Experiment 7: Determination of COD of waste water sample

1. Define chemical oxygen demand (COD).
COD is the amount of oxygen required for oxidation of inorganic and organic impurities in 1 litre of waste
water by strong oxidizing agent such as acidified potassium dichromate.
2. Define Biological oxygen demand (BOD).
It is defined as the amount of oxygen required for the biological oxidation of the organic matter in 1 litre of
waste water under aerobic conditions 20 0C and for a period of 5 days.
3. What is the role of silver sulphate in the determination of COD?
Silver sulphate catalyses oxidation of straight chain organic compounds, aromatics and pyridine.
4. What is the role of mercuric sulphate in the determination of COD?
Mercuric ions of mercuric sulphate bind the halide ions present in waste water to form mercuric chloride
and prevent the precipitation of silver halide.
5. Name a few oxidizable impurities in waste water.
Waste water contains organic impurities such as straight chain aliphatic compounds, aromatic
hydrocarbons, straight chain alcohols etc.
6. Name the indicator used in COD experiment.
Ferroin (Ferrous 1, 10- phenanthroline sulphate)
7. What is the colour change at the end point in the determination of COD?
Colour change: bluish green to reddish brown.
8. Why is sulphuric acid added during the preparation of standard FAS solution?
Sulphuric acid is added to prevent the hydrolysis of ferrous sulphate into ferrous hydroxide.
9. Name the general groups of organic compounds that are not oxidized in the COD test.
Aromatic hydrocarbons and pyridine are not oxidized in COD test.
10 Mention a few applications of COD test. What are the limitations of COD test?
1. The COD test is extensively used in the analysis of industrial wastes.
2. It gives the extent of pollution in effluents from industries.
3. The COD test is extensively used in the analysis of industrial wastes.
4. It gives the extent of pollution in effluents from industries.
Limitations: Inability to differentiate between biologically oxidisable and biologically inert organic matter.
11. What is the chemical formula of Mohrs salt?
Mohrs salt is FAS, Ferrous ammonium sulphate, FeSO4. (NH4)2SO4.6H2O. It is a double salt.
12. Why COD value is greater than BOD value?
COD value contains both organic and inorganic impurities.
Experiment 8: Determination of percentage of copper in brass

1. What is an alloy?
An alloy is a homogeneous mixture of two or more metals (eg. Bronze- an alloy of copper and tin) and in
some alloys a non-metallic element like carbon is also present ( eg. Steel is an alloy of iron and carbon).
2. What are the constituents of brass?
The major constituents of brass are copper and zinc. The minor constituents are tin, lead and iron. The
approximate composition of brass is Cu: 50-80%, Zn: 20-40%, Sn: 0-6% and Fe: 0-1%.
3. What is the role of urea in the preparation of brass solution?
Urea is added to remove the oxides of nitrogen, and destroy excess of nitric acid.
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Dept. of Chemistry,
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4. Why is ammonium hydroxide added to the brass solution in determination of copper in brass?
Brass solution is treated with dilute ammonium hydroxide to neutralize the mineral acids.
5. Name the compound formed when ammonium hydroxide is added to brass solution.
When ammonium hydroxide is added to brass solution a pale blue precipitate of cupric hydroxide is formed.
6.
Why should the mineral acids be neutralized?

The mineral acids
a. liberate iodine from KI (more thiosulphate consumed)
b. convert iodine to iodic acid (less thiosulphate consumed)
c. decompose Sodium thiosulphate (more thiosulphate consumed)
7. Why is acetic acid added to brass solution in determination of copper?

Acetic acid is added to neutralize the excess of ammonium hydroxide and also make the solution slightly
acidic (pH 4-5.5). Iodine is liberated from KI at slightly acidic pH.
8. Why is potassium iodide added to the brass solution?
In determination of copper in brass, potassium iodide quantitatively reduces cupric ion to cuprous iodide
with the liberation of equivalent amount of iodine.
Cu2I2
2Cu2+ + 4KI
+ 4K+ + I2
Cupric
Cuprous iodide
9. Why does the color of brass solution turn brown upon the addition of potassium iodide solution?
Blue solution of brass turns brown on addition of potassium iodide solution due to the liberation of iodine.
10. What is the composition of the white precipitate left at the end point in the determination of copper in
brass?
A white precipitate of cuprous iodide is left at the end of the titration in estimation of copper in brass.
11. Write the reaction involved in estimation of percentage of copper in brass.
2Cu2+ + 4KI
Cu2I2
+ 4K++ I2
Cupric
Cuprous iodide
The liberated iodine is titrated against sodium thiosulphate using starch as indicator.
+ 2 I+ I2
2S2O32S4O62thiosulphate
tetrathionate
12. Mention the difference between the iodometric and iodimetric titration?
Iodometric titration is the titration carried out with liberated iodine. Iodimetric
titration is the titration carried out with standard solution of iodine.
13. Why is starch indicator added towards end?

If starch is added in the beginning when the concentration of iodine is high, water insoluble, stable complex
will be formed and amount of thiosulphate consumed will be lesser than actual value. If it is added near the
end point, the concentration of iodine is low, a water soluble complex is formed and amount of thiosulphate
consumed will be equal to actual value.
14. Though both zinc and copper are present in brass, the experiment helps in determination of copper
in brass. Explain.
Copper can be reduced by KI and liberated iodine is a measure of amount of copper ions. Zinc does not react
with KI.
15. Name the brown gases when brass is treated with nitric acid.
Oxides of nitrogen are liberated when nitric acid is added to brass
16. How do you prepare Brass solution?
Weigh out accurately the given brass sample and transfer it into a conical flask. Dissolve in test tube of
1:1 HNO3. Add 1 spatula of urea and 1 test tube water. Boil for few minutes to expel the nitrous fumes.
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Dept. of Chemistry,
AIT
Experiment 9: Determination of iron in haematite

1. What are minerals?
Naturally occurring metallic compounds are known as minerals.
2. What is an ore?
The mineral from which a metal can be extracted profitably is known as ore.
3. Name a few ores of iron.
Haematite (Fe2O3), Magnetite (Fe3O4), syderite and iron pyrites (FeS2) are the ores of iron.
4. What is the main constituent of haematite ore?
The main constituent of haematite ore is ferric oxide (Fe2O3) and silica (SiO2)
5. What is the role of stannous chloride in the determination of percentage of iron in haematite ore?
Stannous chloride reduces ferric (Fe3+) ions to ferrous (Fe2+) ions.
6. Why is mercuric chloride added in the determination of percentage of iron in haematite ore?
Mercuric chloride is added to convert excess stannous chloride to stannic chloride.
SnCl2 + 2HgCl2
Hg2Cl2 + SnCl4
7. Name the indicator used in the determination of percentage of iron in haematite ore?
Potassium ferricyanide K3Fe(CN)6 is used as an external indicator.
8. What is the color of K3Fe (CN) 6 with ferrous ion?
Potassium ferricyanide produces an intense deep blue color with ferrous ion due to the formation
of ferroferricyanide complex.
9. Explain the color of the indicator drop before the end point and at the end point?
Before the end point, the indicator forms a blue complex with ferrous ions. At the end point, all the ferrous
ions are oxidized to ferric ions. The indicator fails to give blue color with a drop of the titrated solution at
the end point.
10. Why can potassium ferricyanide not be used as an internal indicator in the analysis of haematite ore?
Potassium ferricyanide combines irreversibly with ferrous ions to form a deep blue colored
ferroferricyanide complex. This blue color persists throughout the titration; hence end point cannot be
determined.
11. What is the reaction that takes place during the titration?
Acidified potassium dichromate oxidizes ferrous ion to ferric ion and itself gets reduced to chromic ion.
12. Explain the calculation of equivalent weight of potassium dichromate?
2-
Cr2 O7
14H 6e 2Cr
7H 2 O
Six electrons are required to reduce one molecule of dichromate to chromic ion,
molecular mass (294)
Equivalent massof potassium dichromate
49 6
Experiment 10: Determination of total hardness of water

1. What is a standard solution? How is it prepared?
A standard solution is a solution whose concentration is known. A standard solution of a substance is
prepared by dissolving a known weight of the substance in a known volume of water.
2. Define normality and write the formula used to calculate normality.
Normality is the number of gram equivalents of a solute in 1 dm3 of the solution.
Weight of the substance dissolved in 1 liter
Normality of a Solution =
Equivalent weight of the substance
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Dept. of Chemistry,
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3. In the formula for normality calculations why is the factor 4 used?

Normality3 is number of gram equivalents of a solute in 1 dm 3 of the solution. Since the solution is prepared
in 250 cm , the factor 4 is used.
Weight of the substance dissolved in 250 ml x 4
Normality of a Solution =
Equivalent weight of the substance
4. What is a decinormal solution?
A decinormal solution contains 1/10th gram equivalent weight of a solute in 1dm3 of the solution.
5. Define Molarity.
The molarity of a solution is the number of gram moles of the solute present in one dm3 of the solution.
6. When does normality become equal to Molarity?
For some substances, molecular weight is equal to equivalent weigh. The normality of a solution of
such substance is equal to molarity, e.g. HCl, NaOH.
7. Define Molality?
The molality of a solution is the number of moles of the solute dissolved in one kg of the solvent.
8. Give the structure of EDTA disodium salt of EDTA
EDTA is ethylene diamine tetraacetic acid
HOOC-CH2
CH2COOH
Disodium salt of EDTA

HOOC-CH2
NCH2CH2 N
HOOC-CH2
CH2COONa
NCH2CH2 N
CH2--COOH
NaOOC-CH2
EDTA (H4Y)
CH2--COOH
Na2 EDTA (Na2H2Y)
9. Indicate the ethylene moiety in EDTA

HOOC-CH2
CH2COOH
N CH2CH2 N
HOOC-CH2
ethylene moiety
CH2--COOH
10. Indicate the diamine moiety is EDTA

HOOC-CH2
CH2COOH
N
HOOC-CH2
Diamine moiety
CH2--COOH
11. Indicate the tetraacetic acid moiety is EDTA

HOOC-CH2
CH2COOH
NCH2CH2 N
HOOC-CH2
tetraacetic acid moiety
CH
12. What is hard water?

Hard water is the sample of water that does not lather with soap easily.
42
13 Name the salts responsible for hardness in water

Bicarbonates of calcium and magnesium impart temporary hardness.
Sulphates and chlorides of calcium and magnesium impart permanent hardness.
14 What is total hardness of water?
Sum of temporary and permanent hardness is total hardness.
15 How can temporary hardness be removed?
Temporary hardness can be removed by boiling.
16 How is permanent hardness removed?
Permanent hardness is removed by chemical processes such as lime soda process.
17 Why is sodium salt of EDTA used?
Sodium salt of EDTA is used instead of EDTA because EDTA is sparingly soluble in water but sodium salt
of EDTA dissolves in water easily.
18 Why is ammonia added during the preparation of a solution of EDTA?
Addition of ammonia facilitates faster dissolution.
19 At what pH is the total hardness of water determined.
The total hardness of water is determined using Eriochrome black T at a pH of 10.5
20 What is a buffer?
Buffer is a solution which resists the change in pH when a small amount of an acid or base is added.
21. Name the buffer used in the determination of total hardness of water
NH3- NH4Cl buffer is used in the determination of total hardness of water
22 Name the indicator used in the determination of total hardness of water
Eriochrome Black T is used in the determination of total hardness of water
23. Why is NH4OH- NH4Cl buffer used in the determination of total hardness of water?
NH4OH- NH4Cl buffer is used in the determination of total hardness of water to maintain a pH of about 10.
24. Why is the solution wine red before the end point and blue at the end point?
Initially metal ions in water form a weak complex with the indicator. The metal ion- eriochrome black-T
complex is wine red at basic pH.
During the titration, EDTA first forms colorless complex with the free metal ions in water. Once all the free
metal ions are consumed, the metal ion Indicator complex breaks and a strong complex of EDTA-metal
ion is formed and free indicator is liberated. Free indicator is blue at basic pH.
(The above answer also explains the principle behind the titration in brief.)
25. What will happen to the pH of the solution if buffer is not added? Justify your answer.
If buffer is not added, the pH decreases. During the titration, the hydrogen in EDTA are replaced by the
metal ions in water. And hydrogen ions are liberated. This causes decrease in pH.
26. What is volumetric analysis?
Determination of the concentration of a solution by titration against a standard solution using a suitable
indicator is called volumetric analysis.
43
27. What is an indicator?
Indicator is a substance, which indicates the end-point of a titration by change of color.

a. Internal indicator: The internal indicator is added directly to the reacting system. Acid-base
indicators like methyl orange, phenolphthalein, metal ion indicators like ferroin, the starch
indicator used in iodometry, are all internal indicators.
b. External indicator: This type of indicator is not added directly to the reacting system, but is used
externally, e.g., potassium ferricyanide in the titration of ferrous salt against acidified potassium
dichromate.
c. Self-indicator: Whenever potassium permanganate is one of the reactants in titrations, at the end
point, the reaction mixture assumes the pink color of the permanganate itself. Potassium
permanganate is a self-indicator.
28. Give a few disadvantages of using hard water in industries
a. In boilers use of hard water leads to scale formation. This decreases the life and efficiency of
boiler and also fuel efficiency
b. In laundries, the salts in water form scum with soap. This results in necessity of use of more
soap. c. In dye industry, it leads to discoloration.
29. How many replaceable hydrogens does disodium EDTA have?
EDTA has two replaceable hydrogen atoms.
30. What type of ligand is EDTA?
EDTA is a hexadentate ligand.
31. What is a ligand?
A ligand is an ion, atom or a molecule that can donate one or more pairs of electrons to the central metal
atom forming coordinate bonds.
32. How is hardness of water expressed ?
Hardness of water is expressed in ppm of CaCO3.
33. Why is hardness of water expressed in terms of CaCO3?
Hardness of water is expressed in ppm of CaCO3 because
a. CaCO3 is the least soluble salt of calcium

b. CaCO3 has a molecular mass of 100.
34. Why is hardness of water expressed in ppm.?
Hardness of water expressed in ppm because the hardness of water has a very low value.
Experiment 11: Determination of percentage of calcium oxide in cement

1. Name the main constituents of cement.
The main constituents of cement are calcium, magnesium, aluminium, silica.
2. What is the function of glycerol in the estimation of calcium oxide in cement?
Glycerol is added to get a sharp end point
3.
What is the function of diethylamine in the estimation of calcium oxide in cement?

Diethyl amine acts as a buffer and maintains the pH 12.5
4. What is the function of 6N NaOH in the determination of calcium oxide in cement?

It is added to mask the magnesium ions in the form of magnesium hydroxide that gives an alkaline
pH around 12.5; hence magnesium ions will not be available to react with EDTA.
5. Name the indicator used in the determination of calcium oxide in cement
Patton & Reeders indicator is used as indicator in the determination of calcium in cement
44
Dept. of Chemistry,
AIT
6. Explain why Eriochrome Black-T (EBT) indicator cannot be used in the estimation of CaO in
cement solution?
Eriochrome Black T enables estimation of both calcium and magnesium ions. When Patton
Reeders indicator is used, calcium can be estimated in the presence of magnesium.
7. Give the IUPAC name of Patton and Reeders indicator?
IUPAC Name: 2-hydroxy-1-(2-hydroxy-4-sulpho-1-naphthylazo)-3-naphthoic acid.
-2
Experiment 12: Determination of Alkalinity (OH , CO3 & HCO3) of water

sample using standard HCl
1. Define alkalinity of water.
Alkalinity of water is a measure of its capacity to neutralize acids.
2. Explain in brief the titration involving determination of total alkalinity of water.
In this experiment, total alkalinity of water is determined. Total alkalinity, At, is the sum of alkalinity due to
hydroxides, Ah, alkalinity due to carbonates, Ac and alkalinity due to bicarbonates, Ab.
When methyl orange is used as indicator, the end point reached when hydroxides, carbonates and bicarbonates
react completely. Hence the end point corresponds to alkalinity due to hydroxides, carbonates and
bicarbonates i.e. total alkalinity.
At = Am.o = Ah + Ac + Ab
Since the aim of the experiment is to determine total alkalinity, methyl orange is used as indicator in this
experiment.
3. Mention an indicator other than methyl orange that can be used to determine the alkalinity of water
Phenolphthalein can be used as an indicator in acid base titrations.
4. Write the reactions that take place during the titration
NaCl + H2O (for hydroxides )
NaOH + HCl
Na2CO3 + HCl
NaHCO3 + NaCl (for carbonates)
NaHCO3 + HCl
NaCl + H2O + CO2 (for bicarbonates)
...(1)
... (2)
... (3)
5. How is alkalinity of a water sample determined?

Alkalinity is determined by titrating a known volume of water sample against a strong acid
using phenolphthalein or methyl orange indicator.
6. How is total alkalinity of a water sample determined?
Total alkalinity is determined by titrating a known volume of water sample against a strong acid
using methyl orange indicator.
7. Name the species that cause alkalinity in water
Carbonates, hydroxides and bicarbonates cause alkalinity in water
8. Definition of an acid?
Acids produce H+ ions in aqueous solutions.
9. Definition of a base?
Bases produce OH- ions in aqueous solutions.
10. What is alkalinity?
It is the capacity to neutralize acid
11. What is the significance of determining alkalinity in water?
The knowledge of alkalinity of water is necessary due to the following
a) For controlling corrosion of boiler
b) In calculating the amount of soda and lime required for water softening
c) To control the alkalinity of water being used for irrigation purposes
d) In neutralizing acidic solutions produced by hydrolysis of salts.
e) The amount of coagulants like aluminium sulphate and ferros sulphate to be added depends upon
the amount of alkalinity in water
45
12. What are the possible combinations of ions causing alkalinity in water?
a) Only hydroxide b) Only carbonate c) Only bicarbonate d) Hydroxide and carbonate e) Carbonate
and bicarbonate together
13. The possibility of hydroxide and bicarbonate is not possible. Why?
The possibility of hydroxide and bicarbonate ions together is ruled out, because they combine
instantaneously to form carbonate. Thus hydroxide and bicarbonate ions cannot exit together. On the
basis of same reasoning, all the three hydroxide carbonate and bicarbonate ions cannot exit
together.
OH- + HCO3-
CO3-2 + H2O
14. What are the indicators used in the determination of alkalinity?

Phenolphthalein and methyl orange
15. What is the working pH of Phenolphthalein and methyl orange indicators?
pH = 8.3 10.0 for Phenolphthalein
pH = 3.1 4.4 for methyl orange
********
Qn: Name the types of buffer?

Ans: Buffers may be
Basic It maintains a basic pH. ex: NH3NH4 Cl maintains pH 10.5
Acidic It maintains a acidic pH ex: acetic acid sodium acetate maintains pH 4.5
Neutral It maintains a neutral pH phosphate buffer
Qn: Name the types of indicators
Ans: Indicators may be
Internal Ex: phenolphthalein, starch, eriochrome black T, ferroin
External Ex: potassium ferricyanide
Self indicator Ex: potassium permanganate
********
46
Graph sheets
6 no.s

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Dept.

Observations and Calculations:

Normality of the potassium dichromate = 0.5

From the graph: ---------

cm of 0.5N K2Cr2O7 is required to oxidize

Amount of FAS in 1 dm3 of the given solution = N FAS

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

at the equivalence point the potential is determined by Cr2O7

Ecell = Ecr = E0Cr2O7 2- / Cr3+ +

system given by the

3. The amount of FAS present in 1 dm of solution =

Dept. of Chemistry, AIT

Observations and Calculations:

Vol.of test soln.

1cm3of the stock solution contains = 4.2 mg of CuSO4.5H2O

From graph, Volume of CuSO4 in test solution = ---------

The amount of copper present in the test solution = --------- 1.069

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Observations and Calculations:

From graph: Volume of NaOH required to neutralize HCl

cm3 (Say v1)

cm3 (Say v2)

Volume of NaOH required to neutralize both HCl and CH 3COOH =

Normality of NaOH Volume of NaOH

Therefore, the weight of HCl/dm3 = Normality of HCl x Eq. mass of HCl

Normality of NaOH Volume of NaOH

Weight of CH 3COOH /dm3 = Normality of CH 3COOH x Eq. mass of

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Observations and Calculations

Volume of NaCl (ml)

From graph, Volume of NaCl =

1ml of NaCl contains 0.0001g of NaCl

58.5 g of NaCl contains 23 g of Na

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Observations and Calculations

Half equivalence point

From the graph: Volume of NaOH at equivalence point = ----------

Volume of NaOH at Half equivalence point = ---------- cm

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Dept. of Chemistry, AIT

Observations and Calculations

Time flow in seconds

Coefficient of viscosity of the given liquid l

Dept. of Chemistry, AIT

Result: The viscosity co-efficient of the given liquid = --------------- millipoise

Dept. of Chemistry, AIT

PART-B (VOLUMETRIC EXPERIMENTS)

Weight of empty weighing bottle

Weight of FAS crystals transferred

Weight of FAS transferred 4

Equivalent mass of FAS

Back titre value =

Blank titre value = y + 10 =

Volume of FAS equivalent to oxidizable impurities = (x-y) cm3 =

(x - y) cm3 of z N ferrous ammonium sulphate solution