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14 CHEL17 - Chemistry Lab Manual PDF
14 CHEL17 - Chemistry Lab Manual PDF
LABORATORY MANUAL
I & II SEMESTER
BRANCH :
BATCH :
PART – A
PART – B
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Experiment -1
Potentiometeric estimation of Ferrous Ammonium Sulphate using standard Potassium
Dichromate Solution
Aim: To determine the amount of FAS present in the given solution using standard K2Cr2O7
Principle: The titration, which involves the determination of end point of redox system by the
measurement of e.m.f. of the cell are called potentiometric titrations. In the case of oxidation
reduction titration of FAS using standard dichromate solution, a standard calomel electrode (SCE)
is used as the reference electrode, whose E0 remains constant. The potential and reduced forms of
the iron species
Cr6 + 3e- cr3+ -------------------------------------------------------------------
(1.1)
From Nernst’s equation we have
E=E0 + 0.0591 log [Cr6 +]
3 [Cr3 +]
As the oxidation of Fe2+ progress. ΔE value increases slowly in the beginning and then sharply
near the equivalence point.
Procedure: Pipette out exactly 25cm3 of given FAS solution in a clean 100 cm3 beaker and added
1test tube full of dil H2SO4 to maintain acidic media. Rinse the standard calomel electrode and
bright platinum electrode assembly with ion exchange water and immerse them in the reaction
mixture connect the electrode assembly to the potentiometer pH meter (in millivolts position).
Switch on the potentiometer and record the potential. Add standard K2Cr2O7 from the burette in
0.5cm3 quantity at a time and bubble the solution using a glass tube for uniform mixing. Record he
potential value (E) after each addition of K2Cr2O7. Continue the procedure till the potential
increases more rapidly near the equivalence point. Once equivalence is past there will be only a
slight increases in the potential for the successive addition of K2Cr2O7 solution. Plot a graph of
ΔE/ ΔV values (along y-axis) versus volume of K2Cr2O7 (along x-axis). From the graph find out
the volume of K2Cr2O7 solution required for complete oxidation (peak value of sharp curve).
Finally calculate the normality of FAS and amount of ion present in the given solution.
Calculations:
Normality of K2Cr2O7 Solution = ‘N’ (given)
Volume of K2Cr2O7 Solution
corresponding to the equivalence point = ……… cm3 from graph
Result:
1) The volume of K2Cr2O7 solution corresponding to the equivalence point = ……………….. cm3
2) Normality of given FAS solution = ……………….N
3) Amount of FAS present in litre =………………g/litre
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Experiment 2
Colorimetric estimation of copper
Aim: To estimate the amount of copper present in given solution by colorimetric method.
Principle: When a monochromatic beam of light of intensity (Ia) passes through a transparent
medium, part of light is reflected (Ir), part of it is absorbed (Ia) a remaining part is transmitted (It).
Therefore, I0 = Ia+ Ir + It
In the case of glass and aqueous solution Ir is very negligible
Hence, I0 = Ia+ It
The ratio of intensity of the transmitted light (It ) to intensity of incident light (I0 ) is called
transmittance (T). The negative logarithm of T is called absorbance (A) or optical – density
(O.D.).
Therefore T=It / Io
- log T= log Io/It = A
According to Beer-Lambert’s law “The decrease in the intensity of transmitted light is directly
proportional to thickness of the absorbing medium and concentration of the solution”.
i.e. A = εct
Where ε is the molar extinction co-efficient, which is constant for given substance at a given
wavelength. t is the path length (thickness). If path length is kept constant then, A α C. Therefore
plot of absorbance versus concentration gives a straight line passing through the origin as shown in
the figure. The absorbance of series of standard solution is measured using photoelectric
colorimeter at 620nm and plotted against volume of copper sulphate solution to get calibration
curve. By knowing the absorbance of test solution, the concentration copper can be determined
from the calibration curve.
A deep blue coloured cupraammonium complex ion is formed when Cu2+ ions are mixed with
NH3 according to the following reaction. 4NH3
C u2+ + 4NH3 [Cu (NH3)4 ]2+ ………………… (2.1)
Procedure:
Prepare a standard CuSO4 solution by dissolving 1gm of CuSO4 in 250 cm3 of ion exchange water
in a standard flask. Transfer 5, 10, 15, 20 & 25 cm3 of copper sulphate solution (stock) from a
burette into number of 100 cm3 of volumetric flasks. Add 5 cm3 of 1:1 ammonia solution to each
of the flasks. Dilute the solution with ion exchange water up to the mark and mix well, prepare the
blank solution by diluting 5 cm3 of ammonia solution taken in a 100 cm3 of volumetric flask
making it up to the mark with ion exchange water. To the test solution given in 100 cm 3 of
volumetric flask also add 5 cm3 of ammonia solution and dilute up to the mark with ion exchange
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water and mix well. Measure the absorbance of the solution including test solution against blank
at 620nm using photoelectric colorimeter. Draw a graph of absorbance on y-axis versus volume of
copper sulphate solution on x-axis to construct curve and calculate the amount of copper in the test
solution.
Observation:
0 Blank 5
1 5 5
2 10 5
3 15 5
4 20 5
5 25 5
6 Test solution(X) 5
Calculation:
Result:
Volume of CuSO4 in test solution ……… cm3 (v .from graph)
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Weight of copper in the given test solution …………mg
Experiment 3:
Conductometric estimation of HCI using standard NaOH solution
Principle:
The conductivity of the solution is related to the mobility of ions which in turn related with the size
of the ions. When a mixture of acids like a strong acid (HCl) and weak acid (acetic acid) are
titrated against a strong base (NaOH), strong acid reacts first followed by a weak acid. When the
titration of strong acid and strong base are carried out, there is a decrease in conductivity as highly
mobilized hydrogen ions are replaced by sodium ions.
NaOH + HCl NaCl + H2O
When the whole strong acid is consumed, base reacts with weak acid and conductivity increases as
unionised weak acid becomes the ionised salt.
CH3COOH + Na+ + OH- CH3COO- + Na+ + H2O
After both the acids are consumed, there is a steep increase in conductivity which gives the end
point and this increase in conductivity is due to the fast moving hydroxyl ions from the base. From
this, amount of base consumed for acid and in turn, the amount of acids present is calculated.
Procedure:
Transfer the mixture of strong acid and weak acid into a clean 100 cm3 beaker. Fill the burette
with the standard NaOH solution. Dip the conductivity cell into the test solution so that the
electrodes are completely immersed in the acid solution. Connect the conductivity cell to the
instrument and record conductance. Add NaOH in an interval of 0.5 ml with uniform stirring and
measure the conductance after each addition of NaOH at various stages of neutralization. After
complete neutralization, determine the amount of acid present in the given mixture based on the
volume of alkali consumed. Volume of base consumed for strong acid and weak acid are
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determined by plotting a graph between conductance and volume of base added, where first end
point corresponds to strong acid and second end point corresponds to weak acid.
1. Estimation of HCl
Result :
1.Normality of given HCl=………………………N
2. Amount of HCl present / dm3 =…………………………..g
3. Normality of given CH3COOH =………………………N
4. Amount of CH3COOH present / dm3 =…………………………..g
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Experiment 4:
Aim: To determine the pKa value of given weak acid using pH meter.
Principle:
Strength of acid is generally expressed in terms of acid dissociation constant (Ka) since strong
acids dissociates completely in aqueous solution, it is not meaningful to determine, Ka value of
strong acids as the concentration of undissociated form is small and negligible Hence,
determination of pKa is appreciable only to weak acids as they undergo incomplete dissociation.
Weak acid HA dissociates as
HA (aq) +H2O H3O+ (aq) +A- (aq)
Therefore, Ka = [H3O+] [A-] / [HA]
PKa is determined by measuring variation of pH during the addition of base to the weak acid
solution. During the titration of weak acid against base the pH of the solution increases only
marginally in the beginning then rapidly and then very sharply near the equivalence point. Once
the equivalence point is over, pH again increases only marginally on addition of excess base. The
titration curve is obtained by plotting variation of pH for successive amount of base added.
According to Henderson-Hasselbach equation,
PH=pKa+log10 [salt ] / [acid]
At half equivalence point, [Salt] = [acid]
Therefore pH at half equivalence point gives pKa value of weak acid. i.e., pH=pKa at equivalence
point.
Procedure: Pippette out 25cm3 of given weak acid a clean 100cm3 beaker (if necessary 25cm3 of
ion exchange water to be added). Rinse a glass electrode-calomel electrode assembly with ion
exchange water and immerse the same in the acid. Switch on the pH meter and record the pH.
Add standard NaOH from the burette in quantity of 0.5cm3at a time and bubble the solution using
glass tube for mixing. Record the pH of solution after each addition of NaOH. Continue till the
equivalent point till pH reaches 10-11. Tabulate the reading and plot a graph of pH of Y axis v/s
volume of NaOH added on X-axis. Similarly draw one additional graph of ΔPH/ΔV against
volume of NaOH, and determine the equivalence point Ve. Determine the pH at half
equivalencepoint. This gives pKa value of the acid.
Calculation:
According to Henderson-Hesselback equation,
PH=pKa+log10 [salt]/[acid]
At halt equivalence point, [salt]/[acid]
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Volume of
∆V pH ∆pH ∆pH /∆V
NaOH (V)
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
Result:
Volume of NaOH at equivalence point Ve =………………………cm3
Therefore Volume of NaOH at half equivalence point = Ve/2 cm3
pH at half equivalence point =
Therefore pKa value of weak acid =
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Experiment 5:
Aim: To determine the viscosity co-efficient of a given organic liquid using Ostawald’s
viscometer.
Principle: A liquid flowing through a cylindrical, tube of a uniform diameter moves in the form
of molecular layers. The layer close to the wall of the cylinder is almost stationary and the layer at
the central axis moves faster than any other intermediate layers. Every intermediate layer exerts
viscous or friction on its adjacent moving layer in opposite direction. This frictional property is
called viscosity. Viscosity co-efficient is defined as the tangential force per unit area required to
maintain unit viscosity gradient between any two successive layers of a liquid, one unit distance
apart. The viscosity co-efficient of liquid is given by Poisseuilie’s formula.
η = πpr4t ………………………. (6.1)
8vl
Where V = volume of liquid of viscosity (η ) flowing in time t, through a capillary tube of radius r
and length l, P = pressure (hydrostatic pressure) of liquid = hdg. Where h cm is the difference in
the height between the levels of the liquid in the two arms of Ostawld’s viscometer, d is the density
and g is the acceleration due to gravity.
When the same volume of two different liquids (one being water) are test using the same
viscometer and if the co-efficient of viscosity of one (say, water) is known, η1 of the other liquid
can be easily determined.
ηl = dl tl ηw millipoise
dw tw
Procedure: Clean the viscometer with chromic acid and then was with water. Finally rinse with
acetone and dry it. Clamp the viscometer vertically to a standard and immerse in water bath to
maintain constant temperature. Transfer a known volume (say 10 cm3) of the given organic liquid
whose viscocity co-efficient is to be determined using pipette into the viscometer (say A) using a
rubber tube from the other arm suck the water up. Allow the liquid to flow down freely through
the capillary tube start the stop clock when the Water level just crosses the upper mark. Stop the
stop clock when the water level just crosses the Mark (Say B) below the bulb. Record the time of
flow of liquid in second repeat trial with same water two more times. Empty the viscometer and
rinse the viscometer and pipette twice with acetone and dry it. Repeat the above procedure by
taking same volume of distilled water (10 cm3) and find out the time of flow of water in seconds
for three trials. Finally find the mean time of flow of water (tw) and the liquid (tl).
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Observation & Calculation
Liquid tl =
Water tw =
ηl = dl tl ηw
dw tw
=…………………..millipoise
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Experiment 6:
Determination of amount of sodium present in the given sample of water using flame
photometry
Introduction:
Flame photometry is the measurement of intensity of the light emitted when a metal is introduced
into a flame. The wavelength of the colour tells us what the element, and the color intensity gives
the concentration of the element. Flame photometry is also named as flame emission spectroscopy
because of the use of a flame to provide the energy of excitation to atoms introduced into the
flame.
Flame photometry is used for the determination of elements such as Na, K, Li, Ca, Mg, Sr, and Ba.
The measurement of these elements is very useful in medicine, agriculture and plant science.
Flame photometry is also successful in determining certain transition elements, such as Cu, Fe and
Mn. Flame photometry is a simple, rapid method for the routine determination of elements that
can be easily excited.
Principle:
When a liquid sample containing a metallic salt solution is introduced into a flame the
processes involved in flame photometry are complex, but the following is a simplified version of
the events.
The solvent is vaporized, leaving particles of the solid salt.
The salt is vaporized or converted into the gaseous state.
A past or all the gaseous molecules are progressively dissociated to give free
neutral atoms or radicals.
These neutral atoms are excited by the thermal energy of the flame.
The excited atoms, which are unstable, quickly emit photons and return to lower
energy state, eventually reaching the unexcited state.
The measurement of the emitted photons i.e., radiation, forms the basis of flame
photometry.
When flame photometry is employed as an analytical tool, the wavelength of the radiation
coming from a flame tells us about the elements which are present in that flame. Also, the
intensity of the radiation enables us to know the amounts of those elements present.
The intensity of the light radiation emitted in proportional to the number of atoms in the exited
level, the atom fall back to their ground state by emitting the difference between the excited and
ground state, in the form of light radiation. The intensity of the light radiation is proportional to the
number of atoms in the flame or concentration of the solution fed into the flame. Thus the
concentration of the solution is related to the intensity of the excited radiation. The sequence of
changes taking place at the flame, when metal salt solution may be as follows.
M+ X- M+ X- MX MX M (gas) + X(gas)
Solution Mist Solid Gas
Absorption of heat
M+ (gas)
Flame emission
M (gas)
The intensity of the excited radiation, measured as detector response is related to the concentration
by an expression similar to Beer’s law.
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E = k c
Where E is detector response,
k is constant
is the efficiency of atomic excitation
C is concentration of the solution.
Procedure:
Draw out the standard solution of sodium chloride from burette 5, 10,15 and 20 ml into four
different 100ml standard flask, make up the solution up to the mark with distilled water and shake
well for uniform concentration. Take the first standard solution in a small beaker and aspirate into
the flame of the flame photometer. The flame emission intensity of the standard is measured by the
flame photometer using sodium filter (598nm).The same procedure is repeated for all standard
solution. Plot the graph emission response versus concentration of the solution. From the plot
compare the concentration of sodium in the water sample.
Observation and Calculation:
Weight of the sodium per ml of the solution =
Solution of sodium Concentration of Emission response
chloride sodium chloride
5
10
15
20
Unknown
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PART – B Experiments
Experiment 1: Determination of total hardness of a sample of water
1. Aim: To estimate the total hardness of given water sample using standard Na2EDTA solution.
2. Principle: The hardness of the water is generally due to the presence of traces of calcium and
magnesium salts in water. The total hardness can be determined by titrating the sample against
disodium salt of Ethylenediaminetera acetic acid (Na2EDTA ) at pH-10 using Erichrome black-T
as an indicator.
EDTA forms complexes with a large number of cat ions including Ca2+ and Mg2+ ions. EDTA is
only sparingly soluble hence the more soluble disodium salt of EDTA (Na2EDTA) is used to
prepare a standard solution.
The structure of Na2 EDTA is as shown below
HOOCCH2 CH2COOH
N - CH2 - CH2-N
NaOOCH2C CH2COONa
Na2 EDTA
It has two easily replaceable hydrogen atoms and the resulting ion after ionization may be
represented as H2y2-. The latter forms complexes with metal ions as follows.
M2+ + H2 Y2- MY2- + 2H+ ---------------------------(1.1)
Where M is Ca or Mg2+
2+ 2+
Since the reaction involves the liberation of H+ ions, there is a decrease in the pH of reaction
mixture. in addition Erichrome black-T tends to polymerize in acidic media and gives reddish
brown product. Hence the pH of solution is maintained at 10, using NH3-NH4Cl buffer during the
course of titration. The hardness of water is usually expressed in terms of ppm of CaCO3.
3. Procedure:-
4. Observations
Part 1. Preparation of standard Na2 EDTA solution.
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Weight of weighing bottle + Na2 EDTA salt (w1) =…………….….g
I II III
Burette reading
Final reading
Initial reading
Volume of Na2 EDTA
Solution run down in cm3
Let the volume of EDTA consumed by 25 cm3 of hard water = x cc
5. Calculation:
1000 cm3 of I M EDTA = 100g of CaCO3 (Molecular mass of CaCO3 = 100)
1000
= a ( say)
25 cm3 of hard water sample contains a g of CaCO3
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Experiment 2:
Determination of Percentage of calcium oxide in the given sample of cement solution
Aim: To determine the percentage of calcium oxide in the given cement solution
using standard Na2 EDTA.
Principle: Cement may be defined as “a material possessing adhesive and cohesive properties and
capable of bonding material like bricks, stones” etc. Cement contains silicates of calcium,
magnesium, iron, aluminum etc., calcium oxide is the major constituent of cement (60-70%). In
the estimation of calcium oxide in cement, a known quantity of latter is weighed and treated with
conc. Hydrochloric acid. The insoluble silica is filtered off. The clear filtrate contains calcium,
magnesium, iron and aluminium. The latter two (Fe,Al) present in the filtrate are precipitated as
their hudroxides by addition of NH4OH and NH4Cl. Calcium ion can be determined by titrating
the resulting filtrate against Na2 EDTA solution at PH of 12-14 using patton & Reeder’s Indicator.
In this method, diethylamine and glycerol are added to maintain the pH and to get sharp end point
respectively.
Procedure:-
Part 1. Preparation of standard solution of Na2 EDTA
Weigh accurately about ‘w’gram (say 1 gm) of Na2 EDTA using an electronic balance and transfer
the crystals carefully into funnel over a clean 250ml volumetric flask. Wash down the crystals with
ion exchange water and add one test tube of 1:1 NH4OH solution to dissolve the crystals
completely. Dilute the solution exactly up to the mark with ion exchange water. Shake the solution
well to get uniform mixing.
Observations
Part 1. preparation of standard solution of Na2 EDTA
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Part 2. Determination of calcium oxide.
Final reading
Initial reading
Calculation
Molarity of EDTA = Z M
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Experiment 3:
Determination of percentage of copper in the given sample of brass using standard sodium
thiosulphate solution
Aim: To determine the percentage of copper present in the given sample of brass
Principle : Brass in an alloy of copper and zinc. It also contains small quantities of tin, lead and
iron. The composition of typical brass is, copper –60-90%, zinc -20-40%, tin-0-6%, lead- 0-2%,
iron -0-1%. Brass solution is prepared by dissolving the sample in minimum amount of 1:1 nitric
acid. Excess HNO3 is removed by boiling with urea until all reddish brown fumes are expelled.
The clear blue solution obtained is called brass solution.
3Cu + 8 HNO3 3Cu (NO3)2 + 4H2O + 2NO---------- (3.1)
2NO+ O2 2NO2 (reddish brown fumes)----------- (3.2)
In acid medium the Cu2+ ions react excess of potassium iodide to iodine. If iodine is estimated by
titrating against standard sodium thisoulphate solution using starch as indicator towards the end
point.
2Cu2+ + 4KI Cu2I2 + 4K+ +I2 ------------------------(3.3)
cuprous iodide
I2 + Na2S2O3 2Nal +Na2S4O6------------------------- (3.4)
sodium thiosulphate sodium tetrathionate
Procedure :
part 1. Preparation of brass solution
Weigh accurately 'w' g ( say 0.12g ) of given brass sample and transfer it into a clean conical flask.
add ¼ test tube of 1:1 HNO3, Boil the contents of flask till the alloy dissolves completely by
keeping a glass funnel over the mouth of the conical flask. Add one test tube of ion exchange water
and boil gently till all the brown fumes of oxides of nitrogen are expelled completely. Add one
gram of urea and continue boiling for some more time to expel all the fumes. Cool the contents of
the flask to room temperature by keeping under (tap) running water. Transfer the contents of the to
250 ml volumetric flask. Wash the conical flask 3-4 times with distilled water and transfer the
washings in the volumetric flask. Dilute the solution exactly up to the mark with ion exchange
water. Shake the solution well to get uniform mixing.
Observation
Weight of brass sample w = ------------------g
Initial reading
Volume of Na2S2O3
solution run down in cm3
Calculation
Weight of brass =wg
Normality of Na2S2O3 = 0.05 N
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Experiment 4:
Determination of percentage of iron in the given sample of haematite ore
(External indicator method)
1.Aim : To determine the percentage of iron in the given sample of haematite ore solution by using
standard (Fe2O3)
2. Principle: Haematite ore is a chief ore of iron, contains mainly ferric oxide (Fe2O3) with small
amount of silica (SiO2) Haematite ore solution is made by dissolving the ore in dilute HCl. The
insoluble silica is filtered off. The clear filtrate contains FeCl3 .the ferric ions (Fe3+) present in
haematite ore solutions are reduced to ferrous ions (Fe2+) by adding stannous chloride (SnCl2)
under hot condition in the presence of HCl, the excess stannous chloride is removed by the
addition of mercuric chloride (HgCl2).
2FeCl3 + SnCl2 2FeCl2 + SnCl4------------------(4.1)
Ferric chloride. stannous chloride ferrous chloride stannic chloride.
The resulting ferrous ions is titrated against standard K2Cr2O7 using potassium ferricyanide as an
external indicator.
Fe2+ + Cr2 O7 2- + 14H+ 6Fe3+ + Cr3+ +7H2O----(4.3)
Ferrous ferric
Final reading
Initial reading
Volume of K2Cr2O7
Solution run down in cm3 (X)
5. Calculation :
Weight of haematite ore in the given solution = w1 g
1 cc of 1 N K2Cr2O7 = 0.05585 g of Fe
x cc of Y N K2Cr2O7 = 0.05585X x X Y g of Fe
= a g of Fe (say)
250 cc of solution contains 10 a g of Fe
Percentage of Iron in haematite sample = 10 a X 100
W1
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Experiment 5:
Determination of Total Alkalinity of a given Water Sample using standard Hydrochloric
acid.
Principle:
Alkalinity of water is due to the presence of hydroxide (OH -) carbonate (sodium or potassium
carbonate) and bicarbonate (sodium or potassium carbonate) or temporary hardness (calcium
bicarbonate or magnesium bicarbonate). There are five alkalinity conditions are possible in a water
sample. These conditions can be estimated by titrating water with standard acid using
phenolphthalein (P) and methyl orange (M) indicators.
i) Phenolphthalein End Point: The titration of the water sample with a standard acid up to
phenolphthalein end point marks the completion of reactions given below. The amount
of acid consumed corresponds to hydroxide plus one half of the carbonate present.
OH- + H+ → H2O
-3 +
CO 2 + H → HCO3 -
ii) Methyl Orange End point: Titration of the water sample with a standard acid to methyl
orange end point marks the completion of all three reactions.
OH- + H+ → H2O
CO 2-3 + H+ → HCO3 -
HCO -3 + H+ → CO2 + H2O
Hence , the amount of the total acid consumed correspond to the total alkalinity and the amount of
acid used after the phenolphthalein end point corresponds to one half of carbonate plus all the
carbonates.
The alkalinity in water can be due OH-only or carbonate only or bicarbonate only or due to their
combinations, but OH- and bicarbonate cannot exist together because they combine
instantaneously to form carbonate ions
From the two titre values the different alkalinities are calculated. It is given in the table (1)
If, [P] = O; only bicarbonate ion is present (OH- and carbonate are absent)
[P] = M; only hydroxide ion is present (alkalinity due to OH- =P=M)
[P] = 1 / 2 M; only carbonate ion is present. (Since half of carbonate neutralization reaction takes
place with phenolphthalein indicator, while complete carbonate neutralization takes place when
methyl orange indicator is used. Therefore, alkalinity due to carbonate=2P)
[P] < 1 / 2 M; Carbonate and bicarbonate ions are present.( Alkalinity due to carbonate =2P and
therefore alkalinity due to bicarbonate = M-2P.
[P] > 1 / 2 M; hydroxide & carbonate ions are present.(half of the carbonate is equal to M-P.
Therefore alkalinity due to carbonate =2(M-P), and alkalinity due to OH- = M- 2(M-P)=2(P-M)
Alkalinity values are expressed in term of milligram per litre as calcium carbonate.
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Reagents Required:
Hydrochloric acid (0.02N), Phenolphthalein (0.5%), Methyl orange (0.5%)
Titration - I
Standardisation of HCl
(STD. NaOH VS HCl)
Wash the Burette with water and rinse with HCl. Then fill it with HCl. Pipette out 25ml of Std.
NaOH in a clean conical flask. Add 1-2 drops of phenolphthalein as indicator. This pink coloured
solution is titrated with HCl taken in the burette; the end point is the disappearance
of pink colour. Repeat the titration to get the concordant value.
Titration II
Estimation of Alkalinity
Burette is filled with HCl. Pipette out 50ml of water sample into a clean conical flask. Add 1-2
drops of phenolphthalein indicator. This pink colored solution is titrated against HCl taken in the
burette till the pink colour disappears. Note this point as (P).
To the same colourless solution add 1-2drops of methyl orange indicator. This yellow coloured
solution is titrated against HCl from the point (P). The end point is colour change from yellow to
red orange. Note this point as (M).
Repeat the titrations to get the concordant value.
Standardisation of HCl
Burette : HCl solution
Conical flask : 25cm3 of NaOH + Indicator
Indicator : Phenolphthalein
End Point : Colourless to pale pink
Final reading
Initial reading
Volume of HCl
Solution run down in cm3 (X)
Calculation:
Volume of NaOH Solution V1 = 25 ml
Strength of NaOH Solution N1 = __________ N (given)
Volume of HCl V2 = ______ ml (ConcordantValue)
Strength of HCl N2 = V1 N1/V2
25X -----------
------
=--------------------------------N
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Estimation of alkalinity
Burette : HCl solution
Conical flask : 50cm3 of water + Indicator
Indicator : Phenolphthalein and methyl orange
End Point : pink color just disappears and Yellow to reddish brown
Final reading
Initial reading P
M
Volume of HCl P
Solution run
down in cm3 (X) M
1/2M = ____________ml
Calculation:
Volume of water sample taken =50 ml
Concentration of the standard HCl solution =X N= 0.02 N
Volume of acid consumed for phenolphthalein end point =V1 ml
Extra volume of acid used to methyl orange end point = V2 ml
Concentration of phenolphthalein alkalinity = V1 * X
100
Phenolphthalein alkalinity in terms of CaCO3 equivalents, P = V1 * X *50 g/l
100
P = V1 * X *50 *106 ppm
100 *1000
Methyl orange alkalinity in terms of CaCO3 Equvivalents,M = (V1+ V2) * X *50 g/l
100
Result:
(i) Alkalinity due to OH ion = ------------------- ppm.
(ii) Alkalinity due to CO3 ion = ----------------- ppm.
(iii) Alkalinity due to HCO3 ion = -------------- ppm.
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Experiment 6 :
Determination of Chemical oxygen demand (COD) of the waste water sample.
1.Aim: To determine the chemical oxygen demand of the given waste water sample.
2. Principle: The chemical oxygen demand is a measure of the total quantity of oxygen required
for the complete oxidation of the organic matter (both biological and chemical) present in
industrial waste water sample. It is defined as the number of milligrams (mg) of oxygen required
to oxidize the organic impurities present in 1 litre of wastewater sample. It is important and
quickly measured parameter for water treatment plants, industrial water sample etc. Wastewater
contains organic impurities such as straight chain aliphatic compounds, aromatic hydrocarbons,
alcohols, acids, pyridine and other easily ox disable impurities. Straight chain compounds, acetic
acid etc. can be oxidized more effectively by the addition of silver sulphate (Ag2SO4) as a catalyst.
But silver sulphate reacts with chlorides present in the sample to form precipitate which are only
partially oxidized by this procedure. This difficulty is over come by adding mercuric sulphate
(HgSO4) tothe sample.
A known volume of waste water sample is treated with known excess volume of K2Cr2O7 is
titrated against standard FAS using ferroin as a indicator. Blank titration is conducted with the
same volume of K2Cr2O7 solution. The difference in the titre values is used to calculate COD of
the given waste water sample.
Procedure:
Part 1. Preparation of standard FAS solution
Weigh accurately about “W”gm (Say about 4.9gms) of Ferrous ammonium sulphate into 250cm 3
volumetric flask. Add 1 t.t of dil H2SO4 and dissolve the crystals. Dilute the solution upto the
mark with ion exchange water. Mix the solution well for uniform concentration.
4. Observation
Part I Preparation of standard FAS (Mohr’s Salt) Solution
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Normality of FAS = W x 4
equivalent weight of FAS (392.14)
Therefore, Normality of FAS = ……………………….N
Final reading
Initial reading
Volume of FAS
Solution run down in cm3 (X)
Let the volume of FAS consumed in the sample titration be ‘X’ Cm3
Part III Blank titration
Burette : Standard FAS solution
Indicator : Ferroin
Let the volume of FAS consumed for 25cm3 of K2Cr2O7 solution be ‘Y’ Cm3
5. Calculation:
Volume of Mohr’s salt consumed in part A= x cc =
= 8 g of oxygen
Therefore 25 cm of waste water sample = 8 X (y-x) X z X 1000 mg of Oxygen/dm3
3
25
Result:
COD of the waste water sample = ---------------- mg of oxygen/dm3.
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VIVA-VOCE QUESTION AND ANSWERS
Volumetric analysis
Law of volumetrics
Solutions of equal strength always interact in equal volumes, V1N1 = V2N2
Volumetry is the subject which involves estimation of quantities of chemical substances indirectly
by measuring the volume of the solution of that particular substance in a suitable solvent ( water ).
Primary Standards of volumetric estimations: the substances are easily available in pure state
and easily soluble in water and should be very stable .Ex: K2Cr2O7 , FAS, Oxalic acid etc.,
Standardisation of solution means:An approximate weight of the secondary standard substance
is dissolved in a known volume and the exact strength of the solution is found by titrating it against
standard solution of known substance . This process is called Standardization.
Equivalent weight of an acid- The equivalent weight of an acid is the number of parts by weight
of the acid which contain one part (ie., 1.008 parts ) by weight of replaceable hydrogen.
In general equivalent weight of an acid = Mol. Wt. / basicity
Equivalent weight of a base- The equivalent weight of base is the number of parts by weight of
the base which neutralizes one equivalent weight of an acid.
In general equivalent weight of base = Mol. Wt. / acidity
Equivalent weight of an oxidizing agent- The equivalent weight of an oxidizing agent is the
number of parts by weight of it which contain 8 parts by weight (one equivalent) of oxygen
available for oxidation.
In general equivalent weight of K2Cr2O7 = Mol. Wt. / No. of electrons involved
The reduction of K2Cr2O7 in acid solution K22+ Cr2+6 O7-14 Cr2+3 [ SO4-6]
The change in the oxidation number of two atoms of chromium is from +12 to +6 units of
reduction
1 Mol molecule K2Cr2O7 = O=6 equivalents
Therefore one equivalent weight of K2Cr2O7 =Molecular weight of K2Cr2O7/6=294.6/6=49.1
Equivalent weight of FAS : The equivalent weight of reducing agent is similarly determined by
the change in the oxidation number which the oxidized element suffers.
Consider the conversion of FeSO4 to Fe2 (SO4)3
2(Fe2+ SO4-2) Fe2+3 (SO4)3-6
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Here the change in oxidation number per atom of iron is from +2 to +3 or by 1 unit of oxidation
Mole weight of FAS =1 equivalent.
1 equivalent of FAS = molecular weight of FAS/1 = 392/1
Standard solution of a substance is a solution which contains a known weight of the substance
dissolved in a known volume of the solution.
Normality of a solution is its strength expressed in terms of the number of grams equivalents of
the solute dissolved in 1 dm3 of the solution.
Molarity of a solution is the number of mole molecules of the solute dissolved in 1 dm3of the
solution.
Molality of a solution is the number of mole molecules of the solute dissolved in 1000 g of the
solvent.
Indicator is a substance which indicates the end point of a volumetric reaction by a change of
colour of the solution.
Internal indicators are the substance which are added to the titration flask to indicate the change
of color during volumetric titration. Ex: Phenolphthalein, Eriochrome Black-T, Ferroin, etc.,
External indicators are the substances used as indicators when a tiny drop of the solution from
the flask is removed out and tested for color change externally. Ex: Potassium ferricyanide.
The determination of concentration of acid by standard alkali is known as acidimetry and the
reverse process is known as alkalimetry.
The reagent undergoing reduction is called oxidizing agent, i.e., oxidizing agent gains electrons
and reduced to lower valance state Ex; KMnO4 , K2Cr2O7
A substance ( reducing agent) which undergoes oxidation is called a reducing agent i.e., reducing
agent loses electrons and is oxidized to higher oxidation valence state. Ex: FAS, SnCl4
K2Cr2O7 as such is not an oxidizing agent . However , in the presence of acidic medium or a
reducing agent, it is an oxidizing agent because 3 oxygen atoms ( 6 equivalents) are available for
oxidation of reducing agent and the oxidation state of Cr changes from 6+ to 3+.
POTENTIOMETRICTITRATION-ESTIMATION OF FAS USING STANDARD
POTASSIUM DICHROMATE SOLUTION
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The potential that is developed when an element is in contact with a solution containing its
own ions in 1M concentration at 298 k is called standard electrode potential
4. What is potentiometer?
It is a device or circuit used for measuring the emf between the two electrodes
10. What is the reaction occurring between FAS and potassium dichromate?
6FeSO4 + 7H2SO4 + K2Cr2O7 → 3Fe2(SO4)3 +K2SO4 + Cr2(SO4)3 + 7H2O
Acidified potassium dichromate oxidizes ferrous sulphate to ferric sulphate and itself gets
reduced to chromic sulphate
11. Why sulphuric acid is added to FAS solution during emf measurement?
In presence of sulphuric acid , potassium dichromate oxidizes ferrous ion(Fe+2) to
ferric ion (Fe+3)
12.Why the colour of the solution changes to green on adding potassium dichromate ?
Due to formation of green coloured chromic sulphate.
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COLORIMETRIC DETERMINATION OF COPPER
2. What is colorimetry?
Chemical analysis through measurements of absorption of light radiation in the visible region of
the spectrum (400-760nm) with respect to a known concentration of the substance is known as
colorimetry
6. What is wavelength?
The distance between any two successive peaks or troughs of waves is called wave length. It is
represented by λ
8. What is frequency?
It is the number of waves passing through a point per second. It is represented by ν
22. Name the complex obtained when ammonia is treated with copper sulphate solution
Cuprammonium sulphate, [Cu (NH3)4]SO4 a dark blue colour complex
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23. Why is ammonia added? Why is that same amount of ammonia added?
Ammonia is added to get cuprammonium sulphate [Cu(NH3)4]SO4 a dark blue complex. Same
amount of ammonia is added to nullify the absorbance due to any colouring impurities present
in ammonia.
2. What is conductance?
Reciprocal of resistance is called conductance.
3. What is a cell?
A device, which produces an EMF and delivers electric current as the results of a chemical
reaction.
10. Which of the above conductivity is measured during the conductometric titration ?
Specific conductance.
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16. Why are the slopes of curves before and after neutralization point not exactly the same ?
Before the neutralization point, the conductivity is mainly due to the highly mobile H+ ions
and after the end point, it is mainly due to OH- ions, which are less mobile compared to H+
ions. As a result, magnitude of decrease in conductivity is more before the neutralization
point compared to that after the neutralization point.
18. What are the advantages of conductometric titration over visual potentiometric titrations?
i). Accurate for both dilute and concentrated solutions.
ii). Can be employed for colored solutions.
iii). Very weak acids such as boric, phenol (cannot be titrated potentiometrically) can be
titrated.
iv). Mixture of acids can be titrated more accurately.
5. What is meant by pH ?
pH is defined as negative logarithm to base 10 of hydrogen ion concentration. pH = - log10[H+]
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8. How is the measurement of pH made?
The measurement of pH is made by determining the emf of the cell containing glass electrode
and the calomel electrode immersed in the test solution. The emf of the cell is expressed by the
equation E = K + 0.0591 pH, where K is a constant.
12. What are the electrodes used in the measurement of pH and determination of pKa?
Glass electrode (indicator electrode) and calomel electrode (reference electrode).
In this case, glass electrode acts as anode & calomel acts as cathode.
1. What is viscosity?
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. This property of a liquid by
which it retards or opposes motion between the layer is called viscosity.
10. What is the law based on the viscous flow of liquids through capillary tubes?
Poiseuille law
Πρr4t Where Ρ = hgd
η=
8Vl
V = volume of the liquid, r = radius of the tube, l = length of the tube,
ρ = pressure difference between two ends of the tube,
η = the coefficient of viscosity of the liquid,
t = time required for the volume.
12. Why should the viscometer be dried before the measurements are done?
The viscometer should be dried to avoid the formation of emulsion, which changes the rate of
flow of the liquid.
14. Why is viscometer not rinsed with the given liquid or water?
If the viscometer is rinsed with given liquid or water before measuring the flow time, the
volume taken will be more than a definite known volume.
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17. What is fluidity of a liquid?
Fluidity of liquid is the reciprocal of viscosity co-efficient. It is a measure of the ease with
which the liquid flows.
Fluidity (Ө) = 1/ η, η = the viscosity co-efficient.
3. What are the various events that occur, when a solution containing metal atom ion
Atomized through a flame?
Sequence of events taking place are ;
a. Aspiration of liquid sample into a flame.
b. Formation and evaporation of liquid droplets resulting in the formation of residue.
c. Decomposition of residue into neutral atoms.
d. Excitation of atoms and emission of radiation from atoms.
e. Measurement of wavelength and intensity of emitted radiation by flame photometer.
An atomizer, the burner system and an optical system, a photocell, amplifier and recorder.
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Temporary hardness is due to unstable bicarbonates of Ca and Mg, while permanent hardness
is due to more stable Cl – and SO42- of Ca and Mg
9.What is EDTA?
Ethylene diamine tetra acetic acid.
11. How many replaceable hydrogen atoms are present in disodium salt of EDTA?
Two.
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The solution which resists change in its pH value even after adding small amounts of an acid or
base to it.
20 .Why is EBT shows wine red at the beginning and blue colour at the end?
EBT is blue in colour, which is added to hard water with a pH of 10; it combines with a few of
the calcium and magnesium ions to form a weak complex which is wine red in colour as shown
in the equation.
This action frees the EBT from the complex (M-EBT), and the wine red color changes to a
blue colour at the end of titration.
21. Titrations involving EDTA carried out slowly towards the end point. Justify?
Because the rate of formation of the metal complex of EDTA is very slow.
1. What is cement?
Cement is a lime based building material used to bind together coarse aggregates.
12. Which is the indicator used in the determination of CaO in cement solution?
Patton and reeder’s reagent (Calconcarboxylic acid; IUPAC name : Naphthalenecarboxylicacid,3-
hydroxy-4-[(2-hydroxy-4-sulfo-1-naphthalenyl)azo]-;3-hydroxy-4-[(2-hydroxy-4-sulfo-1-
naphthalenyl)azo]-2-Naphthalenecarboxylicacid).
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DETERMINATION OF PERCENTAGE OF COPPER IN BRASS USING STANDARD
SODIUM THIOSULPHATE SOLUTION.
1. What is Brass?
Brass is an alloy
2. What is an alloy?
An alloy is a homogeneous mixture of two or more metals
2NO + O2 ⇆ 2NO2
2NO2 + H2O ⇆ HNO2 + HNO3
8. What is the bluish white precipitate formed after adding ammonia solution?
Cupric hydroxide
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Acetic acid is added to neutralize the excess of ammonium hydroxide and to make the solution
slightly acidic.
12. Although copper ions are blue in colour in the beginning become colorless after the end
point? why?
At the beginning of the titration Cu2+ ions present (blue) which are reduced to Cu+ ions
(colorless) state.
13. Why do you get blue color when starch indicator is added?
Triiodide in the solution reacts with the amylose of starch gives a blue color.
15. What is the reaction that occurs between iodine & sodium thiosulphate?
2Na2 S2O3 + I2 Na2 S4O6 + 2NaI
sodium thiosulphate sodiun tetrathionate
1. What is an ore?
An ore is mineral, from which a metal can be extracted economically & conveniently
2. What is a mineral?
A mineral is a naturally occurring metallic compound.
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3. What are the main constituents of haematite ore?
Ferric oxide ( Fe2O3)
11. Why potassium Ferro cyanide cannot be used as an indicator in the estimation of Fe
Potassium Ferro cyanide cannot be used as an indicator because Ferro cyanide does not
react with ferrous ion.
12. Why the colour of the indicator drop remains same at the end point?
At the end point there are no more ferrous ions available to react with the indicator, as they
oxidized to ferric ions by the time the end point is reached.
1.What is alkalinity?
It is the capacity to neutralize acid.
6. Write the structure and give the colours for phenolphthalein and methyl orange indicators
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phenolphthalein : pH < 0(orange),
pH ˜ 0−8.2
1. What is sewage?
Sewage is commonly a cloudy dilute aqueous solution containing human & household
waste, industrial waste, ground waste, street washings. Sewage contains organic and
inorganic matters in dissolved, suspended & colloidal states.
3. What is COD?
It is amount of oxygen required for the complete chemical oxidation of both organic and
inorganic matter present in the sample of water by a strong chemical oxidizing agent such as
acidified potassium dichromate.
5. What is BOD?
It is the amount of oxygen required for the complete oxidation of organic matter present in liter
of waste water over period of 5 days at 200 C.
13. Differentiate between blank & back titration. Why blank value is higher than back
value?
Blank titration is done using distilled water instead of test solution (waste water) and back
titration is done using waste water as one of the solvent. Blank titration involves no
oxidation of organic matter.
14. What general groups of organic compounds are not oxidized in the COD test?
Aromatic hydrocarbons and pyridine are not oxidized in COD test.
19. Why is sulphuric acid added during the preparation of std. FAS solution?
Sulphuric acid is added to prevent the hydrolysis of ferrous sulphate into ferrous
hydroxide.
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SYNOPSIS FOR I/II SEMESTER CHEMISTRY PRACTICAL EXAMINATION
PART A
Expt. 1: Potentiometric titration of FAS vs Potassium dichromate:
Instrument: pH meter
Apparatus: burette, 100cm3 beaker, pipette, straw, and electrode assembly
Solutions: FAS, K2Cr2O7 and sulphuric acid
Electrodes: Platinum electrode ( indicator)- calomel electrode (reference ) assembly
Procedure:Pipette out 25ml of FAS into a beaker. Add 2 test tubes of dil.H2SO4. Immerse calomel
electrode-platinum electrode assembly into it. Connect the assembly to a potentiometer and
measure the potential. Add K2Cr2O7 form the burette in the increments of 0.5ml and measure the
potential after each addition. Plot the graph of ∆E/∆V against volume of K2Cr2O7 and determine
the equivalence point.
From the volume of Potassium dichromate at equivalence point, calculate normality of K2Cr2O7
and the weight of FAS in the given solution.
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take 5ml of ammonia and make upto the mark with water and mix well. This is blank solution
which doesn’t contain copper sulphate solution. Measure the absorbance of each at 620nm wave
length of these against blank solution. Plot a graph (calibration curve) of absorbance (OD)
against concentration of copper or volume of Copper sulphate solution and determine the
concentration of copper in test solution from the calibration graph.
Procedure: Pipette out 25ml of given HCl and 25 ml of acetic acid solution into a beaker. Immerse
the conductivity cell in it. Connect the cell to a conductometer and measure the conductance in
mho/cm. Add NaOH from the micro burette in the increments of 0.5ml and measure the
conductance after each addition. Plot a graph of conductance against volume of NaOH. Determine
the neutralization points. From the normality and volume of NaOH, required for the neutralization
point, calculate the normality and amount of strong and weak acid in the given mixture by extra
polating graph.
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Report: Volume of NaOH V1 and V2 from the graph =
The Normality of given strong and weak acid =
The weight of strong and weak acid in the given solution=
Procedure:Pipette out 25ml of the given weak acid into a beaker. Immerse the glass electrode -
calomel electrode assembly into it. Connect the electrodes to pH meter and measure the pH. Now
add NaOH from burette in increments of 0.5ml with constant stirring and measure the pH after
each addition of NaOH
Plot a graph of ∆ H/ ∆V against volume of NaOH and determine equivalence point. Note the half
equivalence point of neutralization of weak acid. Plot another graph of pH against volume of
NaOH and determine pka value of the given weak acid using graph as follows.
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Report:
The equivalence point of the given weak acid =
The half equivalence point of the given weak acid=
pH at half equivalence point =
The pKa of given weak acid =
Laboratory temperature:
Density of water: (d w)
Viscosity co-efficient of water: (η w)
Density of given liquid: (d l)
Time flow of liquid: tl
Time flow of water: tw
d l tl w
Viscosity coefficient of liquid
d w tw
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SYNOPSIS FOR I/II SEMESTER CHEMISTRY PRACTICAL EXAMINATION
PART B
Report:-Note down the burette readings in a tabular column and from the volume of Na2EDTA
consumed calculate the hardness of the given water sample in terms of ppm of CaCO3.
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Determination of CaO in given Cement solution .
Part-A: Preparation of a standard solution of di sodium salt of EDTA:
Weigh out the given do sodium salt of EDTA crystals accurately in a weighing bottle and transfer
it into a 250ml volumetric flask. Add 1 test tube of ammonia solution and dissolve it in little
amount of distilled water. And dilute up to the mark with distilled water. Mix well.
Wt. of bottle + Na2EDTA crystals = W1 g
Wt. empty bottle = W2 g
Wt of Na2EDTA crystals = (W1-W2) g
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Report: Note down the burette readings in a tabular column and from the volume of Na2S2O3
consumed, calculate the percentage of copper present in the given brass sample.
Report: Note down the burette readings in a tabular column and from the volume of K2Cr2O7
consumed, calculate the percentage of iron in the given hematite ore.
Determination of Total Alkalinity of a given Water Sample using standard Hydrochloric acid.
Principle:
Alkalinity of water is due to the presence of hydroxide (OH-) carbonate and bicarbonate. There are
five alkalinity conditions are possible in a water sample. These conditions can be estimated by
titrating with standard acid using phenolphthalein (P) and methyl orange (M) indicators.
Reagents Required:
Sulphuric acid (0.02N), Hydrochloric acid (0.1N), Phenolphthalein (0.5%), Methyl orange (0.5%)
Titration - I
Standardisation of HCl (STD. NaOH VS HCl)
Wash the Burette with water and rinse with HCl. Then fill it with HCl. Pipette out 25ml of Std.
NaOH in a clean conical flask. Add 1-2 drops of phenolphthalein as indicator. This pink coloured
solution is titrated with HCl taken in the burette; the end point is the disappearance
of pink colour. Repeat the titration to get the concordant value.
Standardisation of HCl
Burette : HCl solution
Conical flask : 25cm3 of NaOH + Indicator
Indicator : Phenolphthalein
End Point : Colourless to pale pink
Titration II
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Estimation of Alkalinity
Burette is filled with HCl. Pipette out 20ml of water sample into a clean conical flask. Add 1-2
drops of phenolphthalein indicator. This pink coloured solution is titrated against HCl taken in the
burette till the pink colour disappears. Note this point as (P).
To the same colourless solution add 1-2drops of methyl orange indicator. This yellow coloured
solution is titrated against HCl from the point (P). The end point is colour change from yellow to
red orange. Note this point as (M).
Repeat the titrations to get the concordant value.
Estimation of alkalinity
Burette : HCl solution
Conical flask : 25cm3 of water + Indicator
Indicator : Phenolphthalein and methyl orange
End Point :
Result:
(i) Alkalinity due to OH ion = ------------------- ppm.
(ii) Alkalinity due to CO3 ion = ----------------- ppm.
(iii) Alkalinity due to HCO3 ion = -------------- ppm.
Part-A: Preparation of standard solution of ferrous ammonium sulphate (FAS) Weigh out the
given ferrous ammonium sulphate (FAS) crystals accurately and transfer it into a 250ml
volumetric flask. Add 1 test tube of dil.H2SO4, dissolve the crystals, dilute up to the mark and mix
well.
Wt. of bottle + FAS crystals = W1 g
Wt. empty bottle = W2 g
Wt of FAS crystals = (W1-W2) g
Rport: From the difference in the titre values of Part-B and Part-C, calculate the COD of the waste
water sample in mg/lit of O2 or in ppm
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Model Questions
References Books:
1) Laboratory manual in Engineering Chemistry Sudharani, Dhanpatrai
Publishing Company.
2) Vogel’s Text Book of Quantitative Chemical Analysis revised by
G.H.Jeffery, J. Bassett, J. Mendham and R.C Denney.
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General Instructions for Volumetric Analysis
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