KONGU ENGINEERING COLLEGE

PERUNDURAI, ERODE -638060

SCHOOL OF CHEMICAL AND FOOD SCIENCES

DEPARTMENT OF CHEMICAL ENGINEERING

18MHL31- TECHNICAL ANALYSIS

LABORATORY

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 KONGU ENGINEERING COLLEGE
PERUNDURAI, ERODE -638052

SCHOOL OF CHEMICAL AND FOOD SCIENCES

DEPARTMENT OF CHEMICAL ENGINEERING

18MHL31- TECHNICAL ANALYSIS LABORATORY

RECORD

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Certified that this is a bonafide record of work done by the above

student in the 18MHL31- TECHNICAL ANALYSIS
LABORATORY during the year 2020 - 2021

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 INDEX

Record
Experiment Page submission Marks Signature
Sl. Name of the experiment
Date No date awarded of the Staff
No.
Experiment No: Date:

UV SPECTROPHOTOMETER - ANALYSIS OF WATER

AIM:
To estimate the amount of iron present in the given samples using spectrophotometer.

PRINCIPLE:
Beer’s Lamberts law states that when a monochromatic light passes through a
homogenous absorbing solution. The decrease in intensity of the radiation is directly
proportional to the concentration and length of the solution. Mathematically it is
given by
T = I/Io =10-KCl
A= Io/I = 10 KCl
Log = log Io/I = KCl
Where,
K= Molar absorption coefficient
C = concentration of the solution in moles/lit
L = Length of the absorbing layer
A = Absorbance / optical density of solution
T = Transmittance of solution
I = Intensity of transmitted light
Io = Intensity of incident light
Keeping the path length (say L = 1cm ) the variation in absorption is with reference to
concentration(c). Iron in the ferric state reacts with ammonium thiocyanate according
to the reaction
Fe 2+ + 6CNS- →[Fe(CNS)6]3-
2+
The colour produced by the reaction between is Fe & CNS- unstable. It becomes
weaker with time because of reduction of Fe 2+ by CNS- ions.
PROCEDURE:
The stock solution of Fe (III) is prepared by dissolving ammonium ion (III) sulphate in
concentrated HCl followed by dilution to 100 ml with distilled water (Solution A). 10ml
of this solution is pipette into another standard flask & made upto 100ml (Solution B ).
This solution contains 0.1 mg, 1ml, 2, 4, 6, 8, 10, & 12ml of this standard are taken in
different 100 ml standard flasks. 5ml of 4N HCl and 10 ml of 40 % ammonium
thiocyanate are added and the volume is made upto 100 ml. By measuring the optical
density of solutions, a standard calibration curve can be plotted with concentration
against the optical density. A blank is prepared using the same quantities of reagents
except for the ammonium thiocyanate. It is diluted upto the mark. The absorbance of the
unknown sample is measured in a photoelectric colorimeter at 480 nm, from the
measured optical density values the amount of ferric ion present in the given unknown
sample is calculated. Repeat the same procedure for another sample.

Observation:
Tabulation:1
Concentration Ferrous 1,10 Hydroxylamine Sodium
(ppm) ammonium phenonthroline hydrochloride acetate (ml)
sulphate (ml) (ml) (ml)

Solution:
1, 10 phennonthroline 0.25gm + 25ml conc.HCl in 250ml standard measuring flask.
Hydroxylamine hydrochloride 25gm in 250ml standard measuring flask.
Sodium acetate 25gm in 250ml standard measuring flask.
Ferrous ammonium sulphate 1.75 gm +1.25 ml conc.H2SO4
Tabulation: 2
S.No Concentration of Fe solution (ppm ) Optical density
RESULT:
The concentration of ferric ion present in the given unknown sample A is =

The concentration of ferric ion present in the given unknown sample B is =

Exp.No: Date:
ESTIMATION OF TURBIDITY OF WASTE WATER BY NEPHLOMETRY

AIM
To estimate the turbidity of the given waste water.
PRINCIPLE
Turbidity is an important parameter for characterizing water quality. It is an
expression of optical property of sample water or waste water containing insoluble
substance which causes light to be scattered rather than transmitted in straight lines.
APPARATUS REQUIRED
Nephlometer, Standard measuring flasks
REAGENTS REQUIRED
Prepare Turbidity free water first by passing distilled water through a membrane
filter (pore size <200 μm). Discard the first 200 ml and use further volumes for
preparation of solutions and dilutions.

PROCEDURE
Take the sample well to disperse the solids thoroughly. Pour the sample into
Turbidity Meter tube after all the bubbles have dispersed. If sample is very cold allow it
to reach the room temperature before testing. Prepare the standard sample of zero
turbidity of dust free distilled water of 0 NTU and similarly prepare the sample of 100
NTU. Now place the water sample whose turbidity is to be determined.

RESULT
Thus the amount of turbidity present in given water waste water is determined and
readings are tabulated.Turbidity of the given water waste water =_____________ NTU
Experiment No: Date:

ESTIMATION OF FERROUS (Fe²⁺) BY POTENTIOMETRIC TITRATIONS

Aim:
To estimate the amount of ferrous ion present in the whole of the given solution
potentiometrically. A standard solution of potassium dichromate of strength 0.1N is
provided.

Principle:
Potentiometric titrations depend on measurement of emf between reference
electrode and an indicator electrode. When a solution of ferrous ion is titrated with a
solution of potassium dichromate, the following redox reaction takes place.
K₂Cr₂O₇ + 6FeSO₄ +7H₂O→K₂SO₄ +Cr₂(SO₄)₃ +3Fe₂ (SO₄)₃ +7H₂O
Fe²⁺→Fe3+ + е‾
During this Fe²⁺ is converted into Fe 3+, whose concentration increases. At the
end point, there will be a sharp change due to sudden removal of all Fe²⁺ ions.
This potential is sensitized by platinum electrode dipped into the solution.(To
complete the cell, a reference electrode namely saturated calomel electrode (SCE) is
introduced in to the solution, the electrodes are connected to the potentiometer). Near the
vicinity of the endpoint , the potential changes drastically.
A graph can be drawn for emf vs volume of potassium dichromate from
which end point can be found out. Usually, titration is continued even after the end point.
To know the end point accurately, another graph dE/dV vs volume of potassium
dichromate added can be plotted .
Procedure:
The given ferrous ion solution is made up to 100 ml standard flask. 20 ml of ferrous salt
solution is pipette out into a 100 ml beaker. 20 ml of dilute sulphuric acid (1 N) is added
to it, the electrode are introduced into this solution. Standard potassium dichromate is
taken in the burette. Potentiometer reading is noted for 0 ml addition of potassium
dichromate. For each addition of potassium dichromate, the solution is stirred and
potentiometer reading is noted. Similarly, readings are noted for the addition of each 1 ml
of potassium di chromate. Graph is drawn by plotting emf vs volume of potassium
dichromate added. From the graph, the end point is noted. The amount of ferrous ion
present in the whole of the given solution can be calculated. Repeat the same for sample
B

Tabulation:
Volume of ferrous ion solution= 20 ml.
S.No Volume of Emf(volts) ∆E(volts) ∆V(ml) ∆E/∆V
potassium (volts/ml)
dichromate
Result:
The amount of ferrous ion (Fe2+) present in the whole of the solution A = ________ gms
The amount of ferrous ion (Fe2+) present in the whole of the solution B = ________ gms

Experiment No: Date:

DETERMINATION OF SODIUM BY FLAME PHOTOMETER

AIM:
To determine the amount of sodium present in the given water samples.

PRINCIPLE:
 Flame emission spectrometer is a type of atomic emission spectroscopy. It is
mostly applicable for analysis of alkali and alkalis earth metals. In this spectroscopy the
sample solution of sodium salt is neutralized in to flame, which may produce solid
residue upon solvent evaporation. This solid residue undergoes electronic excitation. Due
to unstable nature of exited state, excited atoms come back to ground state by emission of
adsorbed energy as visible radiation. By measuring the wavelength and intensity of
emitted radiation, we can do quantitative analysis respectively.

CHEMICAL REQUIRED:
NaCl, Distilled water, Flame photometric, volumetric flask, pipette.

PROCEDURE:
Preparation of standards solution for calculations curve. Dissolve exactly 2.542
gm of Nacl in water to make up to 1 liter. This contains 0.1mg per ml (100 ppm). Dilute
this to 2, 4, 6 …….. 20 ppm solutions.

ESTIMATION OF Na BY FLAME PHOTOMETRIC:

First switch on the digital flame photometric by the air compressor with the
required value (10 bars). Open the gas from the cylinder (after the instrument is warmed
up for 10 min). Initially allow the ion-free water to aspirate into flame and set the digital
values as 100. Now the instruments is said to be calibrated. After the calibration of the
instrument, no adjustment should be made. Introduce the solution containing different
concentration of NaCl of the flame and find out the intensity of emitted light of each
solution. Plot a calibration graph between concentration and intensity of NaCl solution
which passes through the origin. Finally introduce the sample of unknown solution
containing sodium in to the flame and find out the intensity of emitted radiation. From the
intensity, the concentration of unknown solution can be determined. Repeat the same for
another sample.

Tabulation:

S.No Concentration of NaCl Solution Flame Intensity

(ppm)
RESULT:
The amount of sodium in the given sample A is _______
The amount of sodium in the given sample B is _______
Experiment No: Date:

Determination of reaction rate constant of acid catalyzed hydrolysis of ester

Aim:
Determination of reaction constant of acid catalyzed hydrolysis of ester
Theory:
The hydrolysis of ethyl acetate catalyzed by dil.HCl can be represented as:
CH3COOC2H5 (aq) + H2O(l) CH3COOH(aq)+ C2H5OH(aq)
In the above reaction the concentration of water being in excess, is very high and
practically remains constant during the reaction. Concentration of H + which catalyzes the
reaction also remains constant. Thus the rate of reaction only depends upon the
concentration of the ester i.e.it is a first order reaction.
Rate=k [CH3COOC2H5]
Reactions of the above type in which one of the reactant is present in large excess, are
though bimolecular but follow th kinetics of first order are called pseudo unimolecular
reactions.
The value of rate constant is calculated from the equation of first order reaction.

...…(1)
Where Co- Concentration of ester,
(Co-x)- Concentration of ester at a time t.
Since acetic acid is formed as a result of hydrolysis, the kinetics of the reaction
can be followed by determining the amount of acetic acid produced at definite intervals
of time. For this known amount of esters and mineral acids are mixed and equal volume
of the reaction mixture are withdrawn at definite intervals. The reaction mixture so
withdrawn is titrated against standardized alkali(NaOH) using phenolphthalein. The
volume of alkali used for each titration corresponds to the amount of acid used as catalyst
and the amount of acetic acid produced at that time. The final reading is taken after
keeping the remaining reaction mixture in water bath for 24 hrs or keeping it in hot
water at 50-60 0C for about 30 minutes.
Let V0 -Volume of NaOH used at time t=0
Vt - Volume of NaOH used at time t
V∞ - Volume of NaOH used at time t=∞
Now, V0 - The amount of HCl present in the reaction mixture.
Vt - The amount of HCl present in the reaction mixture + acetic acid produced at time t
V∞ - The amount of HCl present in the reaction mixture + acetic acid produced after
the completion of the reaction.
Therefore,
Amount of acetic acid produced when the hydrolysis is completed = V∞-V0 …….
(2)
Amount of acetic acid produced at time t = Vt-V0
……(3)
Further,
V∞-V0=Initial concentration of the ester, C0 ……(4)
(V∞-V0)-(Vt-V0)=(V∞-Vt)-concentration of ester at time t, C0-x …..
(5)
Using equation (4) and (5) in equation (1) we get,

..…(6)

The value of k is determined using equation (6) for the different sets of values
corresponding to different intervals of time.
From equation
………(7)

Apparatus required:
50 ml burette,100 ml conical flasks, 250 ml conical flask, graduated pipette, stop watch,
thermometer, water bath and thermostat.

Chemicals required:
Ethyl Acetate, Hydrochloric Acid(0.5 N),Phenolphthalein indicator, sodium
hydroxide(0.1N), ice cubes(prepared from CO2 free water)

Procedure:

1. Take 50 ml of 0.5 N HCl into 250 ml conical flask and 10 ml of ethyl acetate in a
test tube.
2. Cork both of them and place them in a thermostat maintained at room
temperature. Let
3. In the mean time, rinse and fill a burette with 0.1 N NaOH solution. Fix it on a
Burette stand. Also arrange five conical flasks of 50 ml capacity and put 25 ml of
ice cold water in one of them.
4. Now pipette out 5 ml of the ester kept in the thermostat and transfer it to a conical
flask containing hydrochloric acid. Start the stop watch when nearly half of the
volume of ester is added.
5. Mix the contents quickly and at once pipette out 5 ml of the reaction mixture into
the conical flask containing 25 ml of ice cold water. This freezes or arrests the
reaction (due to lowering of temperature)
6. Now titrate it quickly against 0.1 N NaOH using phenolphthalein as indicator.
Appearance of light pink color marks the end point. The titer value represents Vo.
7. Similarly, after a time interval of 10 minutes, again pipette out 5 ml of the
reaction mixture into a conical flask in which 25 ml of ice cold water has already
been added. Titrate it against(0.1N) NaOH as before using phenolphthalein as
indicator.
8. Repeat the process of pipette 5 ml of reaction mixture into a conical flask
containing phenolphthalein and 25 ml of ice cold water and titrating it against(0.1
N) NaOH after every 10 minutes for 1 hour. Each of the titer value from second
onwards constitute Vt. (The titer value require for each titration after t minutes
correspond to volume of alkali used to neutralize hydrochloric acid and acetic
acid formed after time t)
9. To obtain the volume of NaOH required when the hydrolysis is complete, the
corked flask containing the reaction mixture is kept in a water bath at a
temperature of 50-60 0C for about 30 minutes to 1 hour. [To save time, this can be
done just after first reading by with drawing 20 ml of reaction mixture in a
separate flask and keeping it in water bath at 50 -60 0C for 30 minutes to 1
hour].Cool the conical flask to room temperature and titrate 5 ml of this mixture
against (0.1N) NaOH as above . In this titration, there is no need to add ice cold
water. The last titer value represents the infinite reading V∞.
Observation:

Room temperature= ………0C

S.No Time(min) Burette Reading(ml) Titer Value log (V∞-Vt)

(ml)

Initial Final
Calculations:

The value of k is calculated according to the first rate expression,

1. The value of k are calculated at different intervals of time t

(i) k=……………sec-1
(ii) k=……………sec-1
(iii) k=……………sec-1

2. A graph between t versus is plotted . A straight line is

obtained .Value of k is also calculated from the graph

k= -2.303 x slope = ………….sec-1

Result:

k (by calculation) =………….sec-1

k (by graphical method) =………….sec-1

Experiment No: Date:

DETERMINATION OF SODIUM BY FLAME PHOTOMETER

AIM:
To determine the amount of sodium present in the given water samples.

PRINCIPLE:
Flame emission spectrometer is a type of atomic emission spectroscopy. It is
mostly applicable for analysis of alkali and alkalis earth metals. In this spectroscopy the
sample solution of sodium salt is neutralized in to flame, which may produce solid
residue upon solvent evaporation. This solid residue undergoes electronic excitation. Due
to unstable nature of exited state, excited atoms come back to ground state by emission of
adsorbed energy as visible radiation. By measuring the wavelength and intensity of
emitted radiation, we can do quantitative analysis respectively.

CHEMICAL REQUIREDS:
NaCl, Distilled water, Flame photometric, volumetric flask, pipette.

PROCEDURE:
Preparation of standards solution for calculations curve. Dissolve exactly 2.542
gm of Nacl in water to make up to 1 liter. This contains 0.1mg per ml (100 ppm). Dilute
this to 2, 4, 6 …….. 20 ppm solutions.
ESTIMATION OF Na BY FLAME PHOTOMETRIC:
First switch on the digital flame photometric by the air compressor with the
required value (10 bars). Open the gas from the cylinder (after the instrument is warmed
up for 10 min). Initially allow the ion-free water to aspirate into flame and set the digital
values as 100. Now the instruments is said to be calibrated. After the calibration of the
instrument, no adjustment should be made. Introduce the solution containing different
concentration of NaCl of the flame and find out the intensity of emitted light of each
solution. Plot a calibration graph between concentration and intensity of NaCl solution
which passes through the origin. Finally introduce the sample of unknown solution
containing sodium in to the flame and find out the intensity of emitted radiation. From the
intensity, the concentration of unknown solution can be determined. Repeat the same for
another sample.

Tabulation:

S.No Concentration of NaCl Solution Flame Intensity

(ppm)
RESULT:
The amount of sodium in the given sample A is _______

The amount of sodium in the given sample B is _______

Experiment No: Date:

DETERMINATION OF CHEMICAL OXYGEN DEMAND (COD) OF WASTE

WATER
AIM:
To determine the chemical oxygen demand (COD) of a given sample using K 2Cr2O7
and to compare the result
APPARATUS REQUIRED:
Burette, Pipette, Conical flack, Beaker, Round bottomed flask, Condenser, Water
bath.

CHEMICALS REQUIRED:
N/4 of K2Cr2O7, N/4 of Mohr’s salt solution, Ferrion indicator, Sample solution,
HgSO 4, Silver sulphate Reagent.

THEORY:
The chemical oxygen demand (COD) is defined as the amount of oxygen required
to oxidizing the organic matter content of a sample with a strong chemical oxidant under
acidic conditions.
A known amount K2Cr2O7 is added to the measured amount of the sample & the
mixture is boiled with concentrated H2SO4. The organic matter gets completely oxidized
to produce CO2 & H2O.
CXHYOZ + (X+Y/4-Z/4) O2 XCO2 + Y/2 H2O.
The excess of K2Cr2O7 remained after the reaction is titrated against standard Mohr’s salt
solution using ferrion indicator. The dichromate consumed gives the O2 required for the
oxidation of organic matter.

INDICATOR: Ferrion indicator.

END POINT: Blue to wine red or colourless to red.

PROCEDURE:
Take 20 ml of the given sample in a round bottomed flask and add 1 gm of HgSO 4 and
some broken porcelain pieces and immerse the flask in cold water (it is an exothermic
process) and slowly add 25 ml silver nitrate reagents with continuous shaking. Add 25 ml
of K2Cr2O7 (0.25 N) to this solution and mix it properly.
Attach the reflux condenser and reflux for 2 hours .Wash the condenser with distilled
water, cool the flask and dilute 300 ml by distilled water. Add 2-3 drops of ferrion as
indicator and titrate against 0.25 N Mohr’s salt solution till the end point from blue to
wine red. Record the volume of Mohr’s salt solution consumed. Let it be ‘X’ ml. Perform
a blank titration using distilled water in place of sample solution and repeat the above
procedure and find the volume of Mohr’s salt solution consumed. Let it be ‘Y’ ml.

OBSERVATION:
Volume of sample taken = 20ml.
Tabulation-1:
a. For sample (A) solution:
 Vol. of solution taken Burette reading(ml)
Vol. of the titrate used.
S.NO in the titration
Initial reading Final reading (final-initial readings)ml
flask(ml)

b. For sample (B) solution:

Vol.of solution taken Burette reading(ml)
Vol. of the titrate used.
S.NO in the titration
Initial reading Final reading (final-initial readings)ml
flask(ml)

c. For distilled water(blank titration)

Vol.of solution taken Burette reading(ml)
Vol. of the titrate used.
S.NO in the titration
Initial reading Final reading (final-initial readings)ml
flask(ml)

CALCULATION:
Vol. of Mohr’s salt solution consumed for sample A = X1 ml =
Vol. of Mohr’s salt solution consumed for sample B = X2 ml =
Vol. of Mohr’s salt solution consumed for distilled water = Y ml =
Vol. of K2Cr2O7 to oxidized the organic matter present in water sample (A) = Vol .of
Mohr’s salt solution equivalent to k2cr2O7 = (Y- X1) ml =
V1N1 = V2N2
N1(A)× 50 = 1/4(Y- X1)
Vol. of k2cr2O7 to oxidized the organic matter present in water sample (B) = Vol .of
Mohr’s salt solution equivalent to k2cr2O7 =(Y- X2)ml =
V1N1 = V2N2
N1(B)× 50 = 1/4(Y- X2)
COD of sample (A) = N1(A)×equivalent weight of O2 = N1(A)× 8 gm/lit= N1(A)×8×1000
mgm/lit.
The COD of the given sample (A) is = mgm/lit.
COD of sample (B)= N1(A)×equivalent weight of O2 = N1(B)× 8 gm/lit= N1(B)×8×1000
mgm/lit.
The COD of the given sample (B) is = mgm/lit.

RESULT:
The COD of the given sample A is = mgm /lit
The COD of the given sample B is = mgm /lit

DETERMINATION OF BIOLOGICAL OXYGEN DEMAND (BOD) OF GIVEN

SAMPLE WATER

AIM:
To determine Biologiacal Oxygen Demand (BOD) of a given sample of water.

APPARATUS:
Burette , pipette, conical flasks, beakers.
CHEMICALS:
MgSO4 SOLUTION (22.5 g/l) CaCl2 solution (27.5g/l) FeCl3 solution (0.25g/l),
phosphate buffer solution ,BOD bottles, Na2S2O3.

THEORY:
The BOD in a water sample is directly related to the extent of pollution by sewage or
other oxygen demanding waste. If the oxygen in water is less than BOD, the
decomposition of microorganisms takes place anaerobically (in absence f oxygen) and
hence produce highly objectionable end products including H2S, NH3 & CH4.
Therefore sufficient oxygen must be present or supplied externally to maintain aerobic
conditions so that organic matter decomposes into acceptable products. To know the
amount to oxygen required by the given sample , the determination of BOD is necessary.
Polluted waters will continue to absorb oxygen for many months ,till the oxidation gets
completed and hence it is not practical to determine this ultimate oxygen demand which
would require an extended period of time .As a result , it has become standard practice to
simply measure the oxygen over a shorter period 5 days. This is known as 5 days BOD
test.BOD5 is the total amount of oxygen consumed by micro organisms during the first
five days of bio degradation.
In its simplest from BOD5 would involve diluting a known volume of sample water with
a known volume of pure water, whose oxygen content is already known. Let it be D 1.This
is kept for 5 days at 20°C in a stoppered bottle, away from light. The dissolved oxygen is
measured after the period of incubation. Let it be D2.The different between the original
oxygen content and residual oxygen content will indicate the oxygen consumed by the
water sample in five days in organic matter present in water sample. Thus BOD 5 is given
by:

BOD5 = D1-D2 × Volume of sample water after dilution

Volume of sample water before dilution
Where,
D1 =D.O of the sample in mg/L at the start of the experiment
D2 = D.O of the sample in mg/L after 5 days
= Loss of oxygen in mg/Lx Dilution factor.
The dilution of the waste water sample with pure water is necessary because
 waste water contains more oxygen demanding material and hence the dissolved
oxygen may not be sufficient to decompose it aerobically.
PROCEDURE:
Preparation of dilution water :
1. Take 1000ml of distilled water in a bottle .add 1ml each of phosphate
buffer (pH = 7.2), CaCL 2 (27.5g/L), MgSO4 (22.5g/L)
& FeCL3 (0.25g/L).

2. Water is aerated by passing compressed air through a diffusion tube until it

is completely saturated.

DETERMINATION:
3. Take about 5ml of the sample and dilute it to 300ml with dilution water
prepared above (or any appropriate dilution)

4. The dilution sample is taken in two bottles filled upto the neck.

5. The dissolved oxygen in one bottle is determined immediately and in the

other bottle after 5 days of incubation. The procedure for determining the
DO is the same as given in experiment number: 5.

OBSERVATION:
I. Determination of DO in bottle No – 1
S.NO Vol.of solution taken Burette reading(ml) Vol. of the
in the titration Initial reading Final titrant used.
flask(ml) reading (final-initial
readings)ml

II. Determination of DO in bottle No –2

S.NO Vol.of solution taken Burette reading(ml) Vol. of the

in the titration Initial reading Final titrant used.
flask(ml) reading (final-initial
readings)ml

Volume of sample taken for each titration=100ml

Normality of Na2S2O3 Used =N/100

CALCULATIONS:
Volume of the sample before dilution = 5ml
Volume of the sample before dilution = 300ml
i. D.O in bottle no.-1:
 (Hypo) (O2 in sample)
N1V1 = N2V2
1/100 × V1 = V2 × 100
N2 = V1/10000

Strength of dissolved oxygen = N2 × Eq. wt

(D1) = V1 / 10000 × 0.8 g/ L
= 0.8 V1 ppm

ii. D.O in bottle no.-2:

Similarly find D.O in bottle no.-2

Let it be D2
iii. BOD = D1-D2 × Volume of sample after dilution mg/L

Volume of sample before dilution mg/L

RESULT:

BOD of the given water sample = ppm

Experiment No: Date:
Determination of co efficient of viscosity of the given liquid by Ostwald’s Viscosity
Method

Aim:
To determine the coefficient of viscosity of the given liquid by Ostwald’s Viscosity
Method

Theory:
The Ostwald’s Viscometer method is based on Poiseuille’s equation. This relates the rate
of flow of a liquid through a capillary tube with the co efficient of viscosity and is
expressed by the equation.

…………………(1)

Where V- volume of liquid of viscosity flowing in time t through the capillary tube of
radius r and length l
P-hydrostatic pressure of the liquid

Thus the determination of absolute viscosity by means by Poiseulle’s equation involves

the determination of V, r, t, l and P.
The method is however tedious and laborious one. Hence a simpler method is used
wherein we compare the viscosities of two liquids. If the co efficient of viscosity of one
liquid is known, then that of the other can be calculated.
If t1 and t2 are the flow time required to flow for equal volume of two liquids through the
same liquid of capillary tube then from equation (1), we have

…………………(2)

…………………(3)
(or)

Now,
P= h ρ g ……………………….(5)
Where,
 h is the height of the liquid column( it is constant for all the liquids if taken for
identical points and taken in equal volumes for a particular set of observations)
g is acceleration due to gravity
ρ is the density of the liquid
Since in this case for two liquids h and g are the same hence,

This will give us the relative viscosity of the given liquid. Relative viscosity has no
units.
The absolute viscosity is given by,

Apparatus Required:

1. Ostwald’s viscometer,
2. Stop watch,
3. Specific gravity bottle,
4. 10 cm3 pipette,
5. Distilled water,
6. Rubber tubing.

Description:

(1) Ostwald’s Viscometer: It consists of a capillary tube connected at its upper end
with a bulb A and its lower end with a U-tube provided with a bulb B. Bulb B is
of larger size than A . Marks X and Y are etched on the capillary tube above and
below the bulb A. the bulbs are necessary to maintain the hydrostatic pressure
during flow of liquid. Through the capillary, the liquid flow with the measurable
speed.
(2) Relative density bottle: the density o iquid is conveniently measured by means
of a relative density bottle or specific gravity bottle. It is a round bottomed glass
vessel,fitted with a glass cork containing a fine capillary

Procedure:
1. Clean the viscometer with chromic acid(K2Cr2O7 + Conc H2SO4) and then wash it
several times with distilled water. It is finally washed with alcohol and ether and
then dried.
2. Attach a piece of clean rubber tube to the end C and clamp the viscometer
vertically in air.
3. Now introduce a sufficient volume of the given liquid with the help of a pipette in
bulb B so that the bend portion of the U-tube and more than half of the bulb B are
filled up.
4. Through the rubber tube, suck up the liquid until it raises above the mark X.
Make sure that there is no air bubbles inside the liquid.
5. Now allow the liquid to fall freely through the capillary up to the mark X. Start
the stop watch and note the time t1 for the flow of liquid from mark X to mark Y.
6. Repeat the experiment thrice. The values should be concordant.
7. Remove the liquid, clean and dry the viscometer again.
8. Repeat the experiment by taking same volume of distilled water and note down
the time taken t2 for flow of water from mark X to Y. Repeat thrice.
9. Weigh the relative density bottle and note down its weight.
10. Fill it with the given liquid and weigh it again.
11. Remove the liquid, wash it with chromic acid and then with distilled water and
dry in the oven. Now fill it with distilled water and weigh it.

Observation:
Room temperature = °C
S.No Given Liquid Water
Time of flow Mean Time of flow Mean

Weight of empty specific gravity bottle = ………….. g

Weight of empty specific gravity bottle + given liquid = ………….. g
Weight of empty specific gravity bottle + distilled water = ……………g

CALCULATION:

Density of solution )=
1
Density of water( 2 )=

Relative viscosity of the given liquid=

Absolute viscosity=
RESULT:

The relative viscosity of the given solution is ________at ______°C

The absolute viscosity of the given solution is_________Pascal at ______ °C
Experiment No: Date:

DETERMINATION OF BOILING POINT AND MELTING POINT

AIM:
To determine the boiling point of a liquid and to determine the melting point of a
solid.

MATERIALS USED:
Match box, Isopropyl Alcohol/Benzene, thermometer, powdered acetamide/Urea,
beaker,
2 closed-end capillary tubes (melting point tubes) and heat source

PROCEDURE:
I. Boiling point
1. Make a test tube assembly by using the following directions and illustration.
a. Place about1 ml of Isopropyl alcohol in a 10-12 mm diameter test tube.
b. Using a small rubber band, attach a thermometer to the outside of the
test tube. The thermometer bulb should be even with the test tubes
bottom.
c. Insert an inverted closed end capillary tube into the test tube.

2. Mark a water bath assembly by using the following directions and illustration.
a. Half fill a 100 ml or larger beaker with warm tap water. (Note: a water
bath is used if the boiling point of the material is expected to be less
than the boiling point of water; otherwise, an oil bath is needed.)
b. Place the above test tube assembly in the water bath so that the surface
level of the alcohol in the test tube is beneath the surface level of the
water bath.
c. Place the beaker on the wire stand and stirring frequently to insure even
heating, carefully heat the water bath with your heat source until the
water bath boils and a rapid stream of bubbles continuously
emerges from the capillary tube. (Note: if an oil bath is used, the oil
does not boil; the stream of bubbles from the capillary tube is the sole
indicator that the liquid in the pipette or test tube is boiling.)
 d. Remove the heat source and begin observing the stream of bubbles.
e. When the last bubble emerges from the capillary tube, record the
temperature.

3. Reheat the water bath and repeat the cooling process two more times. Record
the temperature reading after each trial and average all three trials.

4. The published boiling point of benzene is 79-810C.

5. Calculate the error between the observed boiling point and the published value
of the boiling point.

II. Melting Point

1. a. Push the open end of a capillary tube into the powdered urea.

b. Move the powdered to the closed end of the capillary tube by tapping it on
the table. Repeat until the powdered urea occupies 1-2 mm of the capillary
tube end.
c. With rubber bands, attach the capillary tube to a thermometer and align the
bulb of the thermometer with the closed end of the capillary tube.
d. Make a water bath as before by half filling a 100 mL beaker with warm tap
water.
e. Place the thermometer/capillary tube assembly in the water bath so that the
surface level of the urea is beneath the surface level of the water bath.
f. Place the beaker on the burner stand and, stirring frequently to insure even
heating, carefully heat the water bath with your heat source.

2. Note the temperature at which the urea melts. Remove heat source.
3. Let the urea cool and recrystallize. Repeat the procedure two more times and
average the results.

4. The published melting of urea is completed. Compare your experimental

result with the accepted (published) value.

5. Calculate the present error.

Clean-up:
Dispose of the used capillary tubes by putting them in your trash can. If any
isopropyl alcohol is left in your test tube, you may pour it down the drain with
water.
RESULT:

1. Melting point of the given sample (urea) = __________

2. Boiling point of the given sample (benzene) = ___________

Experiment No: Date:

CONDUCTOMETRIC TITRATIONS-MIXTURE OF ACIDS

Aim:
To determine the amount of strong acid and weak acid in a mixture of acids(HCl and
CH3COOH) using conductivity bridge. A standard solution of 0.02 N NaOH is provided.

Principle:
Solutions of electrolyte conducts electricity due to the presence of ions and their mobility,
when HCl and CH3COOH are titrated against NaOH.

HCl + NaOH NaCl + H2O

 CH3COOH+NaOH CH3COOH+H2O

Procedure:
The given NaOH solution is made upto 100 ml in a standard measuring flask. A 50 ml
burette is washed with distilled water and rinsed with NaOH solution.

It is then filled with the same solution exactly upto the mark. An exactly 20 ml of mixture
of acids(approximately ) 0.1N HCl and 0.1N CH3COOH) is pipette out into a clean 100
ml beaker and add 20 ml of conductivity water. The conductivity cell is inserted into the
solution. Ensure that the electrodes are well immersed in the solution. The two terminals
of the conductivity cell are connected to the conductivity meter. Record the conductance
before the addition of sodium hydroxide. Add each 1ml of NaOH from the burette, stir
well and record the conductance for the addition of each 1ml.

HCl is stronger than acetic acid is neutralized first, since the fast moving H + ions are
replaced by the slow moving Na+ ions. As a result, conductance of the solution decreases.
After the endpoint, addition of sodium hydroxide will react with weak acetic acid which
will increase the conductance slowly. Further addition of NaOH will cause sudden
increase in the conductance.

Plot a graph with volume of NaOH on the x-axis and conductance on the y-axis. The end
point is noted from the graph. From which the amount of HCl and CH 3COOH present in
the given acid mixture is calculated.

TABULATIOIN:

1.20 ml HCl + 20 ml conductivity water & cell constant = 0.969

S. No. Volume of Observed specific Conductivity =
NaOH Conductance Specific Conductance /
(mho) m -1 x 10 -3 cell constant
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.

Calculation:

1. To find normality of HCl:

Volume of mixture of acids (HCl), V1 = 20ml.

Normality of HCl, N1 =X

Volume of sodium hydroxide, V2 =2.5ml(1st end point from graph)

Normality of Sodium hydroxide, N2=0.02N

We know that V1 N1=V2 N2

N1=

Amount of HCl present in 100ml

Of the given solution = N1 x equivalent weight x 100/1000

 2. 20 ml HCl + 20 ml CH3COOH:
S. No. Volume of Observed specific Conductivity =
NaOH(ml) Conductance Specific Conductance / cell
(mho) m -1 x 10 -3 constant
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.

3. To find normality of acetic acid:

Volume of mixture of acids (CH3COOH), V1=20 ml.
Normality of CH3COOH, N1 =X
Volume of sodium hydroxide, V2 =2.3 ml (2nd - 1st end point from graph)
Normality of Sodium hydroxide, N2=0.02 N
We know that, V1 N1=V2 N2

Amount of CH3COOH present in 100ml

Of the given solution = N1 x equivalent weight x 100/1000
Result:
The amount of HCl present in the given acid mixture = __________ gms.
The amount of CH3COOH present in the given acid mixture = __________ gms.

Experiment No: Date:

Analysis of Water: pH, Conductivity, Hardness, Chloride and Sulphate

I. pH METER:

Aim:
To estimate the amount of pH present in 100 ml of the given water sample and to find
the reason for variation in the pH.

PRINCIPLE:
The titration between a strong acid and a strong base to an acid where changes in pH
are recorded by a pH meter. Increasing alkalinity or acidity is a function of pH.

PROCEDURE:

● The given buffer solution is mixed thoroughly in 200 ml of distilled water.

● The pH of the solution is = 9.2

● The pH meter is standardized by this solution.

● The electrode is cleaned in distilled water and then it is inserted in a given

water sample to find pH.

II.CONDUCTIVITY:

Aim:
To find the conductivity of the given water samples
PRINCIPLE:
Solution of electrode conduct electricity due to the presence of ions and their
mobility when HCl and CH3COOH and titrated against CH3COOH will commence next.
Hence a combination of curves is obtained.
HCl + NaOH NaCl + H2O
CH3COOH + NaOH CH3COONa + H2O

Observation:

1. pH of water (sample 1) =
2. Conductivity of water (sample 1) =
3. pH of water (sample 1) =
4. Conductivity of water (sample 1) =

Hardness

S.No Vol. of std Burette Reading (ml) Vol. of EDTA End point & Indicator
Hard water (ml)
(ml) Initial Final

Estimation of EDTA :
Vol. of Sample Burette Reading (ml) Vol. of EDTA End point &
water (ml) (ml) Indicator
 S.No Initial Final

Estimation of Permanent Hardness:

S.No. Vol. of Sample Burette Reading (ml) Vol. of End Point &
Hard Water EDTA (ml) Indicator
(ml) Initial Final

PROCEDURE

● The conductivity meter is standardized.

● The electrode is inserted in the given water sample to find out its
conductivity.

III. HARDNESS
AIM:
To find the total and temporary hardness of the given water sample.

PRINCIPLE:
Ca and Mg ions present in hard water form complexes with EDTA. The completion
of the reaction is indicated by Eriochrome Black-T forms unstable wine red color
complex with calcium and magnesium ions at pH 9-10.
Ca2+/Mg2+ + EBT [Ca2+/Mg2+ - EDTA] + EBT
Wine red color Stable complex Steel blue (unstable)

When EDTA solution is added, it gradually forms a stable complex with calcium and
magnesium ions by breaking the unstable complex. At the end point the EBT complex is
completely replaced by EDTA and the Eriochrome Black-T indicator is left free in the
alkaline medium which produces steel blue color.
[Ca2+/Mg2+ - EBT] + EDTA [Ca2+/Mg2+ - EDTA] + EBT
Wine red color Stable complex steel blue

PROCEDURE:
TITRATION 1:
STANDARDIZATION OF EDTA SOLUTION:

● Burette is washed with distilled water and is filled with EDTA solution.

● Pipette is rinsed with distilled water and 20ml of standard hard water is pipette out
in to a clean conical flask.

● Add 10-15ml ammonia buffer and 2 drops of EBT indicator.

● Titrate against the EDTA solution.

● The final end point is change of color from wine red to steel blue.

● The final readings are noted and calculated.

TITRATION II:
ESTIMATION OF TOTAL HARDNESS:

● Burette is filled with EDTA and the 20ml of water sample is pipette out in a
clean conical flask.
 ● Add 10-15ml ammonia buffer and 2 drops of EBT indicator.
● Titrate against the EDTA solution.
● The final point is change of color from wine red to steel blue.
● The final reading are noted and calculated.

TITRATION III:
ESTIMATION OF PERMANENT HARDNESS:

● Burette is filled with EDTA solution.

● 250 ml of the given water sample is taken in a 500 ml beaker and boiled off to a
volume of 50 ml and cooled.
● Temporary hardness settles down. The above solution is filtered and again makes
up to 250 ml by using standard flask.
● 20 ml is pipette and titrated to get the end point.

IV. CHLORIDES:
AIM:
To estimate the amount of chloride present in the given water sample.
PRINCIPLE:
Generally water contains chloride ions in the form of NaCl,KCl,CaCl 2 and
MgCl2.The concentration of chloride more than 250 ppm is not desirable for drinking
purpose, total chloride ions can be determined by argent metric methods.In this method
Cl ions solution is directly titrate against AgNo3 with potassium chromate as an indicator.

PROCEDURE:
TITRATION 1:
 ● The given water sample is made up to 100ml in a standard measuring flask.
● 20 ml of water sample is pipette into conical flask and 1 ml of 2% K 2CrO4
indicator solution is added.
● It is titrated against AgNO3
● End point changes of color from pale yellow to reddish brown.

V. SULPHATES:
AIM:
To estimate the amount of sulphate present in the given water sample.

PRINCIPLE:
Barium chloride when mixed with water sample reacts with the sulphate control to
from barium sulphate .

BaCl2 + SO2-2 BaSO4

The BaSO4.2H2O compound contains 32 moles of sulphate and hence the amount of
sulphate in the given water sample can be easily calculated.

PROCEDURE:

● The barium chloride sample is mixed in the given 200ml of water sample.

● The solution is heated; barium chloride reacts with sulphate control in the
water sample to form precipitate of barium sulphate.

● The solution is allowed to settle for 24 hours.

● Then the precipated is filtered using wattmann filter paper.

● The filter paper is then dried.

 ● The amount of barium sulphate deposited is then calculated.

S.NO Vol of water Burette Reading (ml) Vol of AgNo3 End Point &
Sample (ml) (ml) Indicator
Initial Final

Estimation of Chloride:
RESULTS:

1. pH of water =

2. Conductivity of water =

3. Hardness of water

Total hardness =
Permanent hardness =
Temporary hardness =

4. Chloride content in water sample =

5. Sulphate content in water sample =

ATOMIC ABSORPTION SPECTROMETER

AIM:
To estimate the amount of Cu present in the given samples using Atomic Absorption
Spectrometer.
PRINCIPLE:
The most common analysis method for determining the concentration of metal ions in
solution uses the atomic absorption spectrometer. In this method, solutions containing the
metal ion of interest are aspirated into a nebulizer to divide the sample into a fine aerosol.
The aerosolra is then swept into a flame where it is desolvated. The metal containing
particles are then vaporized and atomized. The concentration of metal atoms in the flame
is then determined by rationing the intensity of light incident on the flame with that
exiting the flame at a wavelength specific for the metal of interest. A hollow cathode
containing the metal of interest is an essential component for this experiment. The
concentration of ion is often determined by atomic absorption spectrometer, but
sometimes it is important to know the concentrations of ion and no information on the
oxidation state of the ion measure or the relations between two species of ion. In this
experiment we will utilize AAS to determine the total concentration of copper in the
given sample.

STOCK SOLUTION PREPARATION:

Recommended Standard Materials:
Copper metal strip or wire 99.99 %

Solution Technique:
Dissolve 1 g of copper metal in a minimum volume of 1:1 nitric acid and dilute to 1 litre
to give 1000 mg/l Cu. Flame Emission Wavelength 327.4 nm, Slit width 0.1 nm, fuel:
Acetylene, Support: Air

PROCEDURE:

1. Prepare stock solution as per the given guidelines

2. Prepare sample solutions with known concentration as 1 ppm, 2 ppm, 3 ppm from
the stock solution.
3. Setup the AAS as per the manufacturer guidelines and calibrate it with de-ionized
water
4. Place the samples and note down the absorbance
5. Prepare the unknown sample and place it in the chamber to find the absorbance
and the corresponding concentration.
OBSERVATION:
TABULATION:
S.No. Concentration of Cu solution(ppm) Absorbance
1
2
3
4 Unknown

Calculation:
Concentration of Cu unknown = mg/l

RESULT:
Concentration of Cu ions present in the given unknown sample A= mg/l