Chemistry Lab Manual-1

Chandigarh University, Gharuan
Applied Chemistry Lab Manual (for IT students)

Subject code: ACP-156
Index
Serial Page
Name of the experiment
No. no
1. Determination of temporary and permanent hardness of given hard water sample by
2
volumetric analysis.
2. To determine the amount of residual chlorine present in given water sample. 11
3. 16
To determine viscosity of the given liquid by Ostwalds Viscometer.
4. Calibration of the pH meter. Determination of the pH of the buffer solutions and an
21
unknown solution.
5. To study the synthesis of Aspirin (acetylsalicylic acid) using different acid and base
25
catalysts.
6. Preparation of polymer (making of plastic) from potato starch. 30
7.
34
Determination of strength of an unknown solution of strong acid by titrating it against
NaOH solution conductometrically.
8. To determine (a) max of a solution of cobalt chloride (b) verify Beer-Lambert law and apply
39
it to find the concentration of given unknown solution by UV spectrophotometer
9. To separate and identify the amino acids in a mixture by thin layer chromatography and
47
find out Rf value of amino acids
10. Determination of heat of neutralization of sodium hydroxide solution against the solution of
51
hydrochloric acid.
11. Project 59
Signature of Subject Coordinator: Signature of HOD (Applied Science):

Date of issue:
Applicable to: 1 st year Engineering students (IT group)
Number of pages: 59
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EXPERIMENT No. 1
Aim: Determination of temporary and permanent hardness of given hard

water sample by volumetric analysis
Pre-preparation/ Prerequisite
Student is advised to understand the following aspects before carrying out the
experiment
Fundamentals of hardness of water.
Concept of temporary and permanent hardness of water and their calculation
Concept of complexometric titration.
Effect of buffer solution on the pH of a solution.
Outcomes of this Experiment

At the completion of the experiment student will be
1. Able to acquire the skill to find out hardness of any water sample.
2. Able to acquire the skill to perform complexometric titration.
3. Able to analyze the hardness (in ppm) value of any water sample.
Teaching Learning Activities

1. Learning about the complexometric titration, different types of hardness of water.
2. Titration, noting the concordant reading and calculation of temporary and permanent hardness
of water.
3. Viva voce examination during experimentations.
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Apparatus: Burette, Burette stand, Conical flask, Measuring cylinder, Dropper
Requirement: Standard Hard water, Hard water sample, N/50 EDTA solution, Buffer
solution (pH~10)
Indicator: Eriochrome Black-T indicator
End Point: Wine red to blue (when EDTA solution in burette)
Chemical Reaction:
M+2 + In [M-In]
(from hard water) blue colour Wine red colour
[M-In] + EDTA [M-EDTA] + In

Wine red
colour Colour less blue colour
Theory: Hardness is the property of water due to which it does not form lather with a soap
solution. Hardness is of two types:
1. Permanent or Non-Carbonate hardness is due to the presence of chlorides (Cl -), Sulphates
(SO42-) and Nitrates (NO3-) of Calcium (Ca2+) or Magnesium (Mg2+) metals. This hardness cannot
be removed just by boiling water.
2. Temporary or Carbonate hardness is due to the presence of bicarbonates (HCO 3-) of Calcium
(Ca2+) or Magnesium (Mg2+) metals. This hardness can be removed just by boiling water.
Amount of hardness can be estimated by two methods.
Soap titration method
EDTA titration method
In this experiment EDTA titration method has been used. When Eriochrome Black-T Indicator is
added to hard water sample at pH~10, maintained with buffer solution (NH 4Cl+NH4OH) then the
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indicator combines with Mg2+ and Ca2+ ions to produce wine red colored complex which is less
stable.
When EDTA is added from the burette, it combines with all metal ions to form the respective
Metal-EDTA complexes and indicator become free. As a result of which blue colour appears in
the titration flask at the end point.
Observations:
Titration 1:
Standard Hard water v/s EDTA:
Volume of standard hard water taken for each titration =10ml
Solution in burette = N/50 EDTA Approx.
Sr. No. Initial Reading Final Reading Volume Used (ml)
Concordant Reading = V1
Titration 2:
Sample Hard water v/s EDTA:
Volume of sample hard water taken for each titration =10ml
Titration 3:
Boiled water v/s EDTA:
Volume of boiled water taken for each titration =10ml
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1
Procedure:
Titration 1:
Standardization of EDTA solution:
Wash the glass apparatus with distilled water. Rinse and fill the burette with EDTA and note
down initial burette reading. Pipette out 10ml of standard hard water in the titration flask. To this,
add approx. 5ml of buffer solution and 3-4 drops of Eriochrome Black-T indicator. Wine red
color is obtained. Now titrate it against EDTA till wine red color changes to blue color. Note
down the final burette reading. Repeate the above procedure 2-3 times for getting concordant
reading.
Titration 2:
Determination of total hardness:
Fill up EDTA solution in the burette and note down initial burette reading. Pipette out 10ml hard
water sample in a washed titration flask. To this add approx. 5ml of buffer solution and 3-4 drops
of Eriochrome Black-T indicator as a result of which wine red colour solution is obtained. Now
titrate it against EDTA till wine red color changes into blue color which is the end point. Repeat
the titration 2-3 times for getting concordant reading.
Titration 3:
Determination of permanent hardness:
Take 100 ml of hard water sample in a 500 ml beaker and boil gently for half an hour .Cool and
filter it. Pipette out 10ml of this water and titrate it with EDTA solution in the same manner as in
step 1 and 2. Take three concordant readings.
Calculations:
For the standardization of EDTA:
1ml of S.H.W = 1 mg of CaCO3
Vol. of S.H.W taken for titration = 10ml
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Let concordant volume of EDTA used = V1
V1 ml of EDTA = 10 ml S.H.W
10ml of S.H.W = 10 mg of CaCO3
V1 ml of EDTA = 10 mg of CaCO3
1 ml of EDTA = 10/ V1 mg of CaCO3
Determination of total hardness of hard water sample:

Vol. of water sample taken for titration = 10 ml
Vol. of EDTA solution used = V2 ml
V2 ml of EDTA = 10 ml of water sample
10ml of water sample = V2 ml of EDTA
10 ml of water sample = V2 * 1 ml of EDTA
10 ml of water sample = V2 * 10/V1 mg of CaCO3
1 ml of water sample = V2/10 * 10/V1 mg of CaCO3
1000ml of water sample = V2/V1 *1000 mg of CaCO3
Total Hardness of water Sample = V2/V1 *1000 ppm
Determination of Permanent Hardness
Vol. of hard water taken after boiling and filtering =10 ml

Let vol. of EDTA solution used = V3ml
10 ml boiled water = V3 ml EDTA
= V3*10/ V1mg of CaCO3
1 ml boiled water = V3/10 *10/ V1 mg CaCO3
1000 ml of boiled water =V3/V1 *1000 mg of CaCO3
Permanent hardness of water = V3*1000/ V1 ppm
Temporary hardness of hard water sample = Total hardness- Permanent hardness =X ppm
Total of hard water sample = X1 ppm
Permanent hardness of water sample = X2 ppm
Temporary hardness of Water sample = X3 ppm.
Standard result: Total hardness 150-300ppm
Deviation (if any): For moderately hard water, total hardness will be in the range of 75-150 ppm
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and for very hard water, total hardness > 300 ppm
Sources of error: 1. Personal error like taking burette reading incorrectly.
2. Spattering of chemicals
3. Leakage in burette.
Precautions
1. The glass apparatus should be cleaned and rinsed with distilled water.
2. Lower meniscus of burette should be read.
3. End point should be observed correctly.
4. The amount of indicator added should be same each time.
Significance:
1. Hardness tells the category/quality of water:
If hardness < 75ppm : Soft water
If hardness 75-150ppm : Moderately hard water
If hardness 150-300ppm : Hard water
If hardness above 300ppm : Strongly hard water
2. Hard water is not suitable for use in boilers because it leads to the formation of scales by which
chocking of pipes occurs and then there is a chance of explosion of boilers.
3. Water fit for domestic purpose should have hardness around 300ppm.
The concentration of Ca2+ in freshwater is generally in the range of 0 to 100mg/L. The
recommended upper level for drinking water is 50mg/L but higher levels do not cause health
risks. If the calcium ion concentration in freshwater drops falls below 5mg/L, the ability of the
water to support life is dramatically decreased.
According to the National Soap and Detergent Association, a powdered detergent with phosphate
will perform well in hard waters.
Results and Discussion

A buffer of pH 10 was added in the titration process since the EDTA and EBT have
polyprotic properties, therefore unstable; and only a single endpoint is needed to be observed
(EDTA can be protonated up to six while EBT is usually up to three). At a lower pH, the increase
in the concentration of hydronium ion may interfere with the complexation of the EDTA with the
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calcium and magnesium ions. If the pH is increased, the sharpness of the endpoint is also
increased; therefore, the endpoint will be too sharp for a feasible titration. Also, the use of too
much buffer would make the system very resistant to pH change, therefore, the endpoint will
not be as sharp as predicted or the end point will not be observed.
Another reason for using pH 10 where the calcium and magnesium ions are being analyzed is
that it satisfies one of the optimum conditions for complexometric titration of these two metal
ions: the minimum pH of the solution. For calcium, the minimum solution pH for it to
complexate with EDTA is 7.3 while for magnesium, it is10. Therefore, the minimum solution pH
of the environment where the reaction occurs is at pH 10. At this pH, Ca-EDTA is stable and any
magnesium present will not interfere with the reaction. In this experiment, EBT (Eriochrome
Black-T) was used as the indicator. Most complexometric titrations are performed with
indicators which are themselves chelating agents and whose metal complexes have a different
color from the reagents. Indicators having this special property are called metallochromic
indicators.
VIVA-VOCE
Q1: On boiling how temporary hardness (carbonate hardness) is removed, explain?
Ans: Temporary hardness of water is due to presence of bicarbonate salts of calcium and
magnesium i.e., calcium bicarbonate and magnesium bicarbonate. These salts are soluble in
water. On boiling, these salts are converted into carbonates and hydroxides of Ca and Mg which
are insoluble in water and can be easily separated by filtration.
Ca(HCO3)2
Calcium bicarbonate CaCO3 + H2O + CO2
Calcium Carbonate
(Soluble in water)
(insoluble in water)
Mg(HCO3)2 Mg(OH)2 + 2CO2

Magnesium bicarbonate Magnesium Hydroxide
(Soluble in water) (insoluble in water)
Q2: What is a relationship among various units
of hardness?
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Ans: 1ppm = 1mg/l = 0.1Fr (French) = 0.07Cl (Clark)
Q3: Why hardness expressed in equivalent of CaCO3?
Ans: It is because Mol. Wt. of CaCO 3 is 100 so calculations are easy. Further, it is the most
insoluble compound that gets precipitated during water treatment.
Q4: Why the pH value adjusted to about 10?
Ans: At higher pH, CaCO3 or Mg(OH)2 may get precipitated and the indicator may change its
color. At lower pH value Mg-Indicator complex becomes unstable and a sharp end point
cannot be obtained.
Q5: What are the methods for determination of hardness and why EDTA method is
preferred one?
Ans: Hardness can be determined by i) O-Hehners method ii) Soap solution method iii)
EDTA method. Out of these three, EDTA method gives best results because it is less time
consuming and easy to perform.
Q6: How permanent hardness of water can be removed?
Ans: Permanent hardness of water can be removed by i) Lime-soda process ii) Zeolite process
iii) Ion-Exchange resin
But the colour change from wine red to pure blue is not sharp with calcium indicator
complex. Mg2+ ions have to be added if not present in the hard water.
Q8: Why hard water does not form lather with soap?
Ans: Soaps are sodium and potassium salts of higher fatty acids. On treating soap with hard
water, Ca2+ and Mg2+ present hard water form insoluble Ca 2+ and Mg2+ soaps in the form of
scum . So later is not formed till all the hardness causing cations are removed from water.
2C17H35COONa + Ca2+ (C17H35COO)2Ca + 2Na+
Sodium stearate ppts. of calcium stearate
(Soap) (insoluble in water)
Q9: Why disodium salt of EDTA is used for determination of hardness of water and not
EDTA?
Ans: EDTA cannot be used as such because of its limited solubility whereas its disodium salts
are soluble and also obtained in highly pure form.
Q10: Why complexometric titration using EDTA is not carried out in acidic medium?
Ans: Complexometric titration using EDTA is not carried out in acidic medium because the
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complexes of EDTA with divalent metal are stable in basic solutions.
Q11: Which complex out of the two (Ca 2+-EBT or Mg2+-EBT) Or (Ca2+-EDTA
orMg2+-EDTA) is more stable and why?
Ans: (Ca2+ -EDTA or Mg2+-EDTA) is more stable because EDTA is a hexadentate ligand and
has six coordination sites to entrap the metal ion and hence forms a very stable 1:1 complex
with metal ions quickly.
Q12: What is buffer?
Buffer is solution of known pH which resists the changes in pH when small amount of acid or
alkali is added to it.
Q13: What is an acidic buffer? Give an example.
Ans: It is a solution of a mixture of weak acid and its salt with a strong base. [CH 3COOH +
CH3COONa] is an example of acidic buffer.
Q14: What is a basic buffer? Give an example.
Ans: It is a solution of a mixture of weak base and its salt with a strong base. [NH 4OH +
NH4Cl] is an example of basic buffer.
10 | P a g e
EXPERIMENT No.2
Aim: To determine the amount of residual chlorine present in given water

sample
experiment.
Concept of specification of drinking water
Concept of chlorination technique for purification of drinking water.
Idea of Iodometric titration.
Effect of residual chlorine in drinking water.

1. Able to understand the specification of drinking water and chlorination technique.

2. Able to acquire the skill to perform iodometric titration .
3. Able to acquire the skill to calculate amount of residual chlorine in a given sample of drinking
water.

1. Learning about the iodometric titration and recording of observations
2. Calculation of the amount of residual chlorine in a given sample of drinking water..
Apparatus: Burette, Burette stand, Titration flask, Measuring Cylinder, Beakers, Dropper.
11 | 5 0
Requirement: 10% KI Solution, Hypo solution (N/10), Chlorinated water sample
Indicator: Freshly prepared starch solution.
End Point: Disappearance of blue colour.
Chemical Reaction:
Cl2 + 2KI 2 KCl+ I 2
I2 + 2Na2S2O3 Na S O6
2 4 + 2NaI
I2 + Starch Solution coloured complex
Theory:
Chlorination of municipal water supply is done in order to make it free from germs and other
coloured impurities. Chlorination can be done either by directly passing Chlorine gas, by adding
bleaching powder or Chloramines. Any of these methods give nascent oxygen in the water which
performs the bleaching action.
CaOCl2 + H2O Ca (OH) 2 + Cl2

Cl2 + H2O HOCl +HCl
HOCl HCl+[O]
[O] + germs germs are killed by oxidation
Nascent oxygen has powerful germicidal properties. However excess of free chlorine in drinking
water produces unpleasant smell and taste which affects the digestive system. The amount of free
chlorine in water is determined Iodometrically by treating a known sample of water with excess
of KI solution and then titrating the liberated iodine against hypo solution.
Procedure: Pipette out 20 ml of water sample into a titration flask. Add 10 ml of 10% KI
solution. Shake it vigorously. Reddish brown colour will appear in the flask. Now fill the burette
with standard hypo solution and note down initial reading. Run hypo solution from the burette
until the solution becomes pale yellow. Now add 2ml of freshly prepared starch solution in the
titration flask. The colour of the solution changes to deep blue. Now again run hypo solution
from burette until the solution becomes colorless. This is the end point of the titration. Note
down the final reading. Repeat the experiment three times and take the concordant reading.
Observations:
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Sr.No. Initial Reading Final Reading Vol. Used (ml)
Concordant Volume = V1 ml
Calculation:
1. Determination of free chlorine present in water sample.
N1 V1 = N2 V2
(Hypo) (Water Sample)
1/10 x V1 = N2 x 20
N2 = 1/10 x V1/20
2. Strength of free chlorine present in water sample

Strength = Normality x Eq. Wt. of Chlorine
= N2 x 35.5 g/L
= N2 x 35.5 x 1000 mg/L or ppm
= x ppm
Result: Strength of free chlorine present in water sample = x mg/L or ppm
Standard result: The amount of residual chlorine in normal drinking should be around 5 ppm.
Deviation (if any): Higher values can be obtained (up to 30-40 ppm) if excess of chlorine is
added for the treatment of drinking water.
Sources of error: 1. Personal error like taking burette reading incorrectly.
2. Spattering of chemicals
Precautions:
Shake the solution vigorously so that KI solution is thoroughly mixed with water sample.
Use only freshly prepared starch solution.
13 | 5 0
Note the end point carefully.
Read the burette readings carefully.
Significance:
A chlorine dosage higher than break point chlorination means that the chlorine demand of all the
chlorine reactive materials has been completely met. The extra amount of chlorine present in
water is known as residual chlorine.
Result and Discussion:
Chlorine will liberate free iodine from potassium iodide (KI) solutions at pH 8 or less. The
liberated iodine is titrated with a standard solution of sodium thiosulfate (Na 2S2O3) with starch as
the indicator. Titrate at pH 3 to 4 because the reaction is not stoichiometric at neutral pH due to
partial oxidation of thiosulfate to sulfate.
For maximum accuracy, iodometric titrations using starch indicator should be performed at
sample temperatures less than 20 C (68 F). A back titration is recommended for waters
containing potential chemical interferences. In this case, a known amount of thiosulfate is added
in excess of the chlorine in the sample. The amount of unreacted thiosulfate is titrated with a
standard iodine solution. Then, the total chlorine is calculated, based on the thiosulfate
equivalency in the sample. When mixed with chlorine-containing water, sodium thiosulphate
reacts with the chlorine according to the equation
Na2S2O3 + Cl2 + H2O > Na2S04 + S + 2HCl
Sodium thiosulphate also reacts with hydrochloric acid (produced in the previous reaction) to
form breakdown products such as sulphur, salt and water:
Na2S2O3 + 2HCl > 2NaCl + H2O + S + SO2
The dose required will vary with the pH of the water, but is approximately 2 to 7 parts sodium
thiosulphate per one part chlorine. It is important to note that sodium thiosulphate will also bind
the chlorine in chloramines, thereby releasing ammonia. It is important to note that sodium
thiosulphate will also bind the chlorine in chloramines, thereby releasing ammonia.
VIVA VOCE QUESTIONS
Q1: Why freshly prepared starch solution is used as indicator?
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Ans: Starch solution is hydrophobic colloid and is not stable when allowed to stand for a longer
duration. A gelatinous mass appears if it is kept for longer time. It is to be freshly prepared.
Q2: What is the effect of overdose of chlorine added to the water for chlorination?
Ans: Excess of chlorine produces an unpleasant taste and odour. Moreover, its excess produces
an irritation on mucus membrane. Excess of chlorine also interferes with the enzymatic activity
of the digestive system.
Q3: Why is boiled water not 100% safe for drinking?
Ans: Boiling kills only the existing germs in water, but does not provide any protection against
further possible contamination during storage.
Q4: What is the significance of break point chlorination?
Ans: Break point chlorination is the amount of chlorine which is required to kill all the germs
and remove all the impurities present in given amount of water. Amount of chlorine higher than
break point chlorination remains in the water as free or residual chlorine which may impart
unpleasant odour and taste to water and makes it unfit for drinking. Therefore from the
knowledge of break point chlorination we can know the amount of chlorine required to be added
in the water to make it free from harmful bacteria and germs.
Q5: What is iodometric titration?
Ans: In iodometric titrations, an oxidizing agent is allowed to react in neutral medium or in

acidic medium with excess of KI to liberate free iodine.
KI +oxidizing agent I2
Free iodine is titrated against a standard reducing agent usually with sodium thiosulphate.
15 | 5 0
EXPERIMENT NO. 3
Aim:-To find out the viscosity of a given liquid using Ostwalds Viscometer
experiment.
Concept of viscosity.
Factors affecting viscosity
Concept viscosity coefficient
Description of Ostwald's viscometer

1. Able to understand the terms like viscosity and viscosity coefficient of a liquid
2. Able to acquire the skill to perform experiment with Ostwald viscometer.
3. Able to calculate the viscosity of a given liquid.

1. Learning about the different parameters that affect the viscosity of a liquid.
2. Handling of Ostwald viscometer by each student.
3. Recording of Observations.
Apparatus: Ostwalds viscometer, Stop watch, Clamp stand, Rubber tubing

Requirement: Distilled water, Unknown liquid
Diagram:
16 | 5 0
Fig: Ostwalds viscometer
Theory:
Viscosity is the property of a liquid by virtue of which it offers resistance to flow when a stress is
applied over it. In the process of flow the molecule comprising the fluid move against one
another and viscosity arises from what can be termed as the frictional effect of relative motion.
When the liquid is flowing in a circular tube, the flow pattern is called streamlines or viscous or
laminar. The Ostwalds Viscometer method is based on Poiseuilles equation. This relates the rate
of flow of a liquid through a capillary tube with the coefficient of viscosity and is expressed by
the following equation:-
= r4tP /8Vl ..1
Where, V = Volume of the liquid
= viscosity
t = Time of Flow of liquid
r = Radius of Capillary Tube and l = length
P = Hydrostatic pressure of the liquid
Thus the determination of the absolute viscosity by Poiseuille's expression involves the
determination of V,r, t, l and P. The method is however tedious. Hence, a simpler method is used
wherein we compare the viscosities of the two liquids. If the coefficient of viscosity of one liquid
is known, then that of the other can be calculated. If t1 and t2 are the flow times required to flow
17 | 5 0
for equal volumes of two liquids through the same length of a capillary tube then from equation
(1) we have
1 = r4t1P1 /8Vl
2 = r4t2P2 /8Vl
Or 1/2 = t1P1/t2P2 2
P = hdg 3
Where H = height of the liquid column
g = acceleration due to gravity
d = density of the liquid
Since in this case for two liquids h and g are same hence, 1/ 2 = t1d1 /t2d2
Or 1 = d1/d2 X t1/t2 X 2
Procedure:
Wash the viscometer with chromic acid (K2Cr2O7 + Conc. H2SO4) and then rinse it with
distilled water for 2-3 times. Introduce a sufficient volume of distilled water through the
pipette of Bulb B such that the bent portion of tube and half or a little more than half of Bulb
B gets filled. Clamp the viscometer in vertical position. Suck up the distilled water from Bulb
A in such a way that the level rises above the upper mark C and then allow it to flow under
its own weight. Count the time of flow of distilled water by starting the stopwatch as the
meniscus just reaches the mark C and stopping the watch as the meniscus just passes the
lower mark D.Take at least 3 readings with given liquid. Remove distilled water and
introduce the given liquid in the viscometer in the same manner as did with distilled water.
Repeat the same procedure to take 3 readings for noting down the flow time of the given
liquid.
Observations:-
S.No Time of flow of water (t1) (sec.) Time of flow of given liquid (t2) (sec.)
18 | 5 0
1
Mean Time =sec Mean Time =.sec
Coefficient of viscosity of water 1 = 17.26 poise

Coefficient of viscosity of given liquid 2 = _____ poise
Density of water d1 = 0.99 g/ml
Density of given liquid d2 = 0.79 g/ml
Calculation:
We know
1/2 = d1/d2 X t1/t2
2 = [(t2 x d2) / (t1 x d1)] x 1 poise
Result: The coefficient of viscosity of a given liquid ispoise.
Standard result: Depends on the nature of the unknown liquid. About 5% deviation from the
standard result is accepted.
Sources of Error: 1. Personal error like taking reading incorrectly.
Precautions:
1) The viscometer should be thoroughly cleaned before use. Viscometer should be strictly
kept in vertical position
2) Observe accurately when the meniscus of liquid and water are just passing the upper
and lower mark.
3) Same volume of water and liquid must be taken in the viscometer. There should be no
air-bubble inside any of the bulbs.
VIVA-VOCE
Q.1: What is the CGS unit of coefficient of viscosity?

Ans: The CGS unit of coefficient of viscosity is poise.
19 | 5 0
2. Define viscosity of a liquid.
Ans: Viscosity is a measure of the resistance of a fluid to deform under shear stress. It is
commonly perceived as "thickness", or resistance to flow. Viscosity describes a fluid's
internal resistance to flow and may be thought of as a measure of fluid friction.
3. Name the apparatus to measure the viscosity of a liquid?
Ans: Viscosity can be measured with the help of an apparatus known as viscometer.e.g.
Ostwalds viscometer, Redwood viscometer
4. What is the effect of temperature on viscosity of liquid?
Ans: The viscosity of a liquid is directly affected by temperature because heat causes molecules
to move farther apart and low temperature causes molecules to come closer together. At
lower temperatures the viscous material will be thicker and at high temperatures it will be
thinner.
5. What are the various factors that affect the viscosity?
Ans: 1) Increase in temperature results in a decrease of viscosity by about 2 % per degree.
2) The presence of solutes, lyophilic colloids and other suspended impurities tend to
increase the viscosity of liquids.
3) Polarity also affects the viscosity (polar compounds are more viscous than the non-
polar).
4) Hydrogen bonding in a molecule also increases the viscosity.
5) Branched chain compounds possess greater viscosity than straight chain ones.
6) Increase in molecular weight increases the viscosity of the liquid.
6. What is viscosity index?

Ans: Viscosity index is the variation of a liquid with temperature.
20 | 5 0
EXPERIMENT No. 4
Aim: Calibration of the digital pH meter. Determination of the pH of the

buffer solutions and an unknown solution
experiment
Fundamentals of pH of the solutions.
Concept of acidic and basic nature of a solution
Concept of buffer solution.
Effect of temperature on the pH of a solution.

1. Able to understand the terms like pH, pOH, acidic, basic & neutral solutions practically.
2. Able to acquire the skill to measure the pH of the solution using pH meter.
3. Able to acquire the skill to classify the samples as acidic, basic or neutral based on the pH value
4. Able to operate and calibrate the pH meter.
5. Able to analyze the results of the experiments.

1. Learning about the different components of pH meter such as electrode.
2. Practice for fixing and operating the pH meter by each student.
3. Recording of Observations.
21 | 5 0
Theory: Most of the chemical and biochemical processes are affected by the acidity and
alkalinity of the medium in which they take place. So, pH measurement is valuable information
for a reaction to occur. pH is a measure of the acidity or alkalinity of a solution; pH of a solution
can be represented as follows,
pH= -log [H+]
In case of water or any neutral solution, pH = 7
For acidic solution, pH < 7
For alkaline solution, pH > 7
Apparatus: Digital pH meter, beaker, tissue paper, distilled water, Buffer tablet (pH 4 and 9),
beaker (100 ml), hydrochloric acid, sodium hydroxide solution.
Procedure:
Standardization of the instrument:
1. Switch on the instrument; wait for 10-15 minutes so that it gets warmed up.
2. Prepare the buffer solution of pH 4 and 9 using buffer tablets
3. Function key was set to stand by position.
4. Temperature of the buffer 7.0 is recorded and the temperature knob is set to the measured
temperature.
5. The electrode is washed several times with distilled water, dried with clean tissue paper
and then immersed in the buffer solution of pH 7.0.
6. Function key is set to pH position and wait for reading to stabilize.
7. Calibrate switch is adjusted to display the correct pH of buffer 7.0 at measured
temperature. After noting the pH value, the pH meter is reset to position.
8. The electrode is washed with distilled water, dried using tissue paper and the n dipped in
a solution of pH 4.0 or 9.0 (Depending on the pH value of the sample).
9. Step 6 was repeated. Now slope control key is adjusted to display the correct value of the
second buffer at measured temperature.
10. Steps 5-9 was repeated with buffer solution with pH 7.0 (adjusting calibrate) and buffers
4.0 and 9.2 (adjusting slope control key) once or more until the pH meter displays the
22 | 5 0
correct values of both buffers without the need of further adjustments. The reading should
be correct within one count.
11. After pH meter is standardized, it is ready for measurement of the pH of the sample.
12. Rinse electrodes with distilled water and dried with tissue paper. Set the function key to
standby position, measure sample temperature and set temperature value on manual
temperature knob. Dip the electrode in sample solution , set meter to pH position, wait for
reading to stabilize and the reading is recorded.
Standard result: pH value depends on the nature of solution taken for analysis. 5%
deviation is accepted from actual result.
Sources of error: 1. Calibration error in pH meter.
2. Personal errors like taking readings incorrectly.
Precautions:
1. In between measurements, always set function key to stand by position.
2. Buffer solution should be prepared only before use. The buffer value is likely to change
due to CO2 absorption and contamination.
3. Always cap the buffer containers tightly to prevent ingress of moisture and CO2
absorption.
4. Used buffer should not be poured back into bottles for reuse. This is likely to cause errors
in measurement due to possible contamination and degradation.
5. The glass electrode should be stored in distilled water.
6. Standardization should invariably be done when changing from acidic range and vice-
versa.
VIVA-VOCE
1. What is the effect of temperature on pH?
Ans. As [H+] increases with increase in temperature, so pH value also increases with
temperature.
2. What are buffers?
Ans. Buffers are solutions of known pH which resist the changes in pH when small
amount of acid or alkali is added to it.
23 | 5 0
3. Give example of one acidic buffer and one basic buffer.
Ans. Acidic buffer: CH3COOH-CH3COONa
Basic buffer: NH4OH- CH3COONH4
4. What is the effect of temperature on pH?
pH value of the solution increases with increase in temperature.
5. Name three electrodes. Which are usually employed to measure pH of a solution?
Hydrogen electrode, Quinhydrone electrode and Glass electrode.
Glass electrode is most suitable for this purpose. Glass electrode is simple, not easily
oxidized and attains equilibrium rapidly.
24 | 5 0
EXPERIMENT No. 5
Aim: To study the synthesis of Aspirin (acetylsalicylic acid) using different

acid and base catalysts
experiment
Fundamentals of catalysis.
Idea about the synthesis and utility of Aspirin
Role of acid and basic catalyst on the reaction rate of synthesis of Aspirin from
salisaldehyde.
Calculation of % yield of a chemical reaction
Characterization of solid product by checking melting point.

1. Able to understand the role of acid and basic catalyst on the rate of reaction practically.
2. Able to acquire the skill to carry out chemical reaction, work up, quenching and isolation of
product by filtration.
3. Able to calculate theoretical and actual yield of a chemical reaction.
4. Able to check the melting point using melting point apparatus. .
5. Able to analyze the % yield of the experiments.

1. Learning about the different components of pH meter such as electrode.
2. Practice chemical reaction, work up, quenching and isolation of product by filtration.
by each student.
25 | 5 0
3. Identification of Aspirin by checking melting point of the solid product obtained during
the reaction
4. Calculation of % yield of chemical reaction.
Apparatus: Two Test tubes, Test tube stand, Measuring cylinder (10 ml), two erlenmeyer
flasks (50ml), two beakers (100 ml) and one beaker (500 ml), Dropper,
Requirement: Salicylic Acid (2.0 grams), Acetyl chloride (4 ml), Pyridine (5 drops), Sulphuric
acid (5 drops).
Theory: Aspirin is an analgesic anti-inflammatory drug. It is one of the oldest and widely used
drugs in medicine. Aspirin is synthesized by using acetic anhydride or acetyl chloride to salicylic
acid. Aspirin can be synthesized from salicylic acid by using either acid catalyst or base catalyst.
O OH
O O
CH3
Aspirin
Chemical Reaction:
HO O O OH
OH O Acid O CH3
+
H3C Cl or base catalyst O
Salicylic acid Acetyl chloride Acetylsalicyclic acid
Procedure:
Two thoroughly cleaned test tubes were labeled as A and B. 1.0 gm of Salicylic Acid was
placed in each test tube. 4ml of Acetyl chloride was measured using a 10ml graduated cylinder.
2.0 ml Acetic Anhydride was poured in each test tube.
Sulfuric Acid (5 drops) was added to test tube A with constant stirring. The change was noted
(physical change/temperature change). It has been observed that there was distinct physical
26 | 5 0
change (effervescence with solidification of the reaction mass) immediately after addition of
catalytic amount of sulphuric acid.
Pyridine (5 drops) was added to test tube B with constant stirring. The change was noted
(physical change/temperature change). It has been observed that there was no distinct physical
change immediately after addition of catalytic amount of pyridine.
An 500ml beaker, filled with water, placed on a hot plate was allowed to heat to boiling
temperature. Two test tubes (A and B) were placed into the hot water bath for 5 minutes. After
the 5 minutes, the test tubes were checked to ensure that all solids in the test tubes had dissolved
completely.
Two 50 ml Erlenmeyer flask was taken and 25 ml of distilled water was poured into the
flask. The contents of the two test tubes (A and B) were poured separately into each 50 ml
Erlenmeyer flask. A small amount of distilled water was used to rinse the test tubes to ensure that
all solution was transferred to both flasks. Both flasks were cooled in ice water bath for 10-15
min to ensure complete crystallization. If necessary, a glass stirring rod may be used to scrap the
bottom of the flask to induce crystallization.
The content was filtered; the contents and filter paper were transferred onto the watch
glass. The watch glass and contents were placed in the drawer and allowed to dry for a week.
A week later, the mass of Acetylsalicylic Acid was recorded. The melting point was
recorded. The theoretical melting point of Acetylsalicylic Acid is 136C.
Result:
In both experiment, 1 g Salicylic Acid (M.W 138.12) was reacted with 2mL Acetyl
chloride to afford Acetylsalicylic Acid or Aspirin (M. W 180.157). The following equations help
determine the limiting reagent.
1 mol Salicylic Acid

1 g Salicylic Acid =0.0072mol Salicylic Acid
138.12 g
1mol Acetic Anhydride

2 ml Acetic Anhydride =0.021 mol Acetic Anhydride
102.09 g
In this reaction, Salicylic Acid is the limiting reagent because there are fewer moles and
therefore sets the maximum amount of capable of being made.
The theoretical yield is determined using the equations below.
1 mol Acetylsalicylic Acid

0.0072 mol Salicylic Acid =0.0072 mol Acetylsalicylic Acid
1 mol Salicylic Acid
27 | 5 0
180.157 g Acetylsalicylic Acid
0.0072 mol Acetylsalicylic Acid =1.3 g Acetylsalicylic Acid
1 mol Acetyl salicylic Acid
Limiting Reactant Salicylic Acid
Theoretical Yield 1.3 g
Actual Yield in case of

sulphuric acid (g)
Percent Recovery in case of

sulphuric acid (%)
Actual Yield in case of

pyridine (g)
Percent Recovery in case of

pyridine (%)
The theoretical melting point of Acetylsalicylic Acid is 136C. The recovered

Acetylsalicylic acids in each case were recorded.
Acetylsalicylic Acid Melting Point
Theoretical Melting Point 136C
Recorded Melting Point (in case of sulphuric acid)
Recorded Melting Point (in case of pyridine)
In this experiment, two different catalysts were used (Sulfuric acid and Pyridine) in test
tubes A&B, respectively. The pKa values of Pyridine and Sulfuric acid are 5.25 and -3
respectively. Pyridine was the basic catalyst in this experiment and sulfuric Acid was the acid
catalyst in this reaction.
Sources of error:
1. Personal errors such as reading scales incorrectly.
2. Spattering of chemicals.
3. Impurities in a solid lower the melting point (than the literature value), and also spread
out the range / make it broader (5-10 deg instead of 1-2, for example). If the sample is not
28 | 5 0
properly dried (moisture is still present in the sample) then it may result in lower melting
point.
4. In organic lab unless something is wrong with the procedure or equipment, a substance
generally cannot be observed to melt at higher temperature than its melting point
5. Other reasons for getting wrong melting point may happen due to:
a. Heating the sample too fast. (Heating rate of 1-2 degree per minute is will give good
results. Going faster than five degrees per minute virtually guarantees poor results in
most cases.
b. The sample should be firmly packed in the bottom of the capillary tube to ensure
efficient heat transfer.
Precautions:
All chemicals were disposed off properly. Aqueous filtrates were diluted and flushed
down the drain. The Acetylsalicylic Acid was placed in the appropriate organic waste container.
VIVA-VOCE
Q 1. Why one can get smell of acetic acid from a old bottle of Aspirin?
The reason that a bottle of old Aspirin might smell like acetic acid is because the
acetylsalicylic acid undergoes hydrolysis leaving Salicylic Acid and Acetic Acid. This occurs
when moisture is introduced to the Aspirin. The water molecules in the air react with the Aspirin
causing hydrolysis. The hydrolysis reaction is depicted below:
O OH
O OH
O
OH
O O
+ H2O + HO CH3
CH3
Aspirin Water Salicylic Acid Acetic Acid
Q 2. Why Aspirin is used instead of salicylic acid as an analgesic?
Traditionally, many pains were treated with salicylic acid. Salicylic acid is great for
treating pains; however it is highly acidic and damaging of mucous membranes. One way to get
the benefits of salicylic acid without its irritating characteristics is to add an acetyl group to it.
This new compound is known as Acetylsalicylic Acid, commonly known as Aspirin. This new
compound was first isolated by Felix Hoffmann. Hoffmann wanted to find a medicine that was
as effective at treating pain as salicylic acid, but without the irritating and damaging side effects.
29 | 5 0
He took salicylic acid and found that covering up the acidic part of salicylic acid with an acetyl
group greatly decreases the acidity and damaging side effects. (Hoffman)*
References
*Hoffman, Lucas. "Aspirin 101" 01 April 2000. HowStuffWorks.com.

<http://health.howstuffworks.com/medicine/medication/aspirin.htm> 30 January 2013.
EXPERIMENT No. 6
Aim: Preparation of polymer (making of plastic) from potato starch,
experiment
c. General concept of polymer

d. Advantage and disadvantage of conventional polymers
e. Disposal issue of a conventional polymer and necessity of production of
biodegradable polymer.

1. Able to realize the necessity of production of biodegradable polymer.

2. Able to acquire the skill to prepare plastic from potato starch.
3. Get the idea about of the role of plasticizer in the synthesis of plastics.

1. Learning about the terms like biodegradable polymer, plasticizer etc.
2. Preparation of plastic from potato starch with and without plasticizer.
30 | 5 0
Theory: In this activity students will make a plastic from potato starch and investigate the effect
of adding a plasticizer on the properties of the polymer. Starch is made of long chains
of glucose molecules joined together. It contains two polymers: amylose which is straight-
chained and amylopectin which is branched. When starch is dried from an aqueous
solution it forms a film due to hydrogen bonding between the chains. However, the
amylopectin inhibits the formation of the film. Reacting the starch with hydrochloric acid
breaks down the amylopectin, forming more satisfactory film. This is the product that
students make without propane-1, 2, 3-triol. The straight chains of the starch (amylose)
can line up together and although this makes a good film, it is brittle because the chains
are too good at lining up. Areas of the film can become crystalline, which causes the
brittleness.
Section of a starch molecule

(amylose and amylopectin)
Adding propane-1, 2, 3-triol makes a difference due to its hydroscopic (water attracting)
properties. Water bound to the propane-1, 2, 3-triol gets in amongst the starch chains and stops
the crystalline areas from forming, preventing the brittleness and resulting in more plastic
properties, thus acting as a plasticizer. This can be explained to students that the propane-1, 2, 3-
triol acts as a plasticizer.
31 | 5 0
Apparatus: 2 beakers (250 ml), watch glass, hot plate, stirring rod, petri dish, universal
indicator paper, pipettes, measuring cylinder (25 ml and 10 ml).
Requirement: Dilute hydrochloric acid (0.1 M, 10 ml), dilute sodium hydroxide (0.1 M,
about 10 ml), potato starch (8 g) and propane 1, 2, 3-triol (2 ml)
Procedure:
1. Making the plastic film:

a. Put 22 ml of water into the beaker and add 4 g of the potato starch, 3 ml of hydrochloric
acid and 2 ml of propane-1, 2, 3-triol.
b. Put the watch glass on the beaker and heat the mixture using the Bunsen burner. Bring it
carefully to the boil and then boil it gently for 15 mins. Do not boil it dry. If it looks like it might,
stop heating.
c. Dip the glass rod into the mixture and dot it onto the indicator paper to measure the pH.
Add enough sodium hydroxide solution to neutralize the mixture, testing after each addition with
indicator paper. You will probably need to add about the same amount as you did of acid at the
beginning (3 ml).
d. Pour the mixture onto a labelled petridish and push it around with the glass rod so that
there is an even covering.
e. Repeat the process without propane-1, 2, 3-triol.
f. Label the mixtures and leave them to dry out. It takes about one day on a sunny windowsill,
or two days at room temperature.
Results:
Students should be able to see a difference in the two films that they make. The one without the
propane-1, 2, 3-triol is far more brittle, the one with it shows more plastic properties.
Precautions:
1. Do not let the mixture boil to dry, or it pops and has a tendency to jump out of the
beaker. For this reason, students should wear eye protection at all stages.
2. If too much water is used, then their polymer wont solidify and remains a liquid.
32 | 5 0
VIVA-VOCE
1. Define a polymer.
Ans: A high molecular mass giant molecule formed by linking together of a large number of
small molecules of monomers.
2. Define thermoplastic and thermo setting plastic

Ans: A polymer, which can be softened on heating and hardened on cooling reversibly.
Example, PVC.
A polymer which during moulding process get hardened and once set, it cannot be
softened again.
Example, Phenol formaldehyde resin
3. What is addition polymerization?

Ans: Addition polymerization is a reaction that yields a product which is exact multiple of
the original monomeric molecule. Example: polyethene
4. What is condensation polymerization?

Ans: Condensation polymerization is an intermolecular combination though different
functional groups present in the monomer, with the elimination of small molecules like H2O.
Example: Nylon-66
33 | 5 0
EXPERIMENT No. 7
Aim: Determination of strength of a given hydrochloric acid solution by

titrating it against sodium hydroxide solution conductometrically.
experiment
f. Fundamentals of conductometric titration.

g. Operation of the conductometer.
h. Concept of acidimetry and alkalimetry.
i. Concept of normality and strength of acid.

1. Able to understand the terms like volumetric titration, specific and equivalent conductance and
their units.
2. Able to operate and calibrate the conductometer.

1. Able to acquire the skill to find out end point of the titration by plotting the graph. .

1. Learning about the conductometric titration, specific and equivalent conductance.
2. Practice for fixing and operating of conductometer by each student.
3. Recording of Observations, plotting of graph and calculation of the results by applying
the concept of acidimetry and alkalimetry.
34 | 5 0
Apparatus: Conductometer, burette, pipette.
Requirement: Distilled water, N/100 KCl solution, N/10 NaOH solution and the given HCl
solution (approximately N/10)
Theory: Conductometry can be used to detect the equivalence point (end point) of a titration
without using any indicator. This method is based upon the measurement of conductance during
the course of titration. The conductance varies differently before and after the equivalence point.
This is due to the reason that electrical conductance of a solution depends on the number of ions
present and their ionic mobilities or speeds. When a strong acid like HCl is being titrated with
strong alkali like NaOH, following reaction takes place.
[ H+ + Cl-] + [ Na+ + OH-] [ Na+ + Cl-] + H2O
Initially the solution contains H+ and Cl- ions and have high conductance due to greatest mobility
of H+ ions. During titration, the conductance of the solution decreases as Na + ions possess low
mobility compared to H+ ions. After neutralization point, OH- ions are excess and have second
highest mobility consequently, the conductance of the solution will again increase.
So when conductance values are plotted against volume of titrant added, two straight lines were
obtained; the point of intersection of the lines gives the end point (as shown in Figure A).
Conductance . .
. .
. . End point
volume of NaOH
Fig A
The Calibration of Instrument
1. Switch on the instrument and warm up for half a minute.
2. Take 50 mL N/100 KCl solution in a 100 mL beaker and immerse the cell in the solution so
that the electrodes completely dip in solution.
3. Push the cal./meas switch to cal. position.
35 | 5 0
4. Set the temperature control to 25oC and adjust calibration control to get 1000 on the screen
position.
5. Measure the temperature of the standard solution and set the temperature control to the value
of temperature.
6. Now push the cal./meas switch to meas position.
8. Adjust the calibration control switch to get the desired value of conductivity of N/100 KCl .
9. After the calibration of the instrument remove the cell from KCl solution and wash with
distilled water and do not disturb the calibration control switch till the experiment is complete.
Procedure:
1. Take 50 mL of the given N/10 HCl acid solution in a 100 mL beaker and immerse the
conductivity cell in the solution so that the electrodes completely dip in the solution.\
2. Select the proper conductance range and put the cal/meas. switch to meas, position.
3. Measure the temperature of the sample solution and set the temperature control to the value of
the measured temperature.
4. Note down the conductance of the solution.
5. From the burette add N/10 NaOH solution in 0.5 mL lots. Mix the solution with the help of a
glass rod and note the conductance of the mixed solution till 10-12 mL of solution is added,
6. Plot a graph between observed conductance values along y-axis against the volume of alkali
added along x-axis. The point of intersection gives the amount of alkali required for
neutralization of acid.
Observation and Calculation:
Volume of HCl taken = 50 mL
Normality of NaOH solution = N/10
S. No. Volume of NaOH solution (mL) Observed conductance (mho-1)
36 | 5 0
3
Suppose volume of NaOH used at equivalence point= A mL
Applying normality equation, N1V1= N2 V2 where N1= strength of HCl solution and
N2= strength of NaOH solution = N/10
N1 x 50 = 1/10 x A (N)
N1= A/500 (N)
Result: Normality of the given HCl solution is A/500 (N)
Standard result: The strength of HCl solution will depend on the nature of the supplied HCl
solution. 5% Deviation is accepted from the exact result.
Sources of error: 1. Calibration error in conductometer.
2. Personal errors like taking readings incorrectly.
Precaution:
1. The solution taken in the burette should be ten times stronger than the solution taken in beaker
so that the volume change of the latter solution is negligible on the addition of the former
solution.
2. After every addition of NaOH solution, the solution must be stirred thoroughly.
VIVA-VOCE
1. Define Ohms law.

Ans: Ohms law states that the ratio of the potential difference (E) applied across the ends of a
conductor to the current (l) flowing through it is always constant at a particular temperature.
Mathematically, E/l = R where R is the resistance of the conductor.
37 | 5 0
1. What is conductance and what are its units?
Ans: The reciprocal of resistance is called conductance. Its units are ohm-1 or mho.
2. What is specific conductance and what are its units?

Ans: Specific conductance is defined as the conductance of 1 cc of the solution. Its unit is
denoted by Kappa () and its units are ohm-1 cm-1 or mho cm-1.
3. What is equivalent conductance and what are its units?

Ans: Equivalent conductance (Eeq) is the conductance of all the ions produced by dissociation by
1 gm equivalent of a solute in solution and its units are ohm-1 cm2 g,eq-1
4. What is the effect of dilution on conductance?

Ans: Conductance increases with dilution because on dilution dissociation increases and hence
the number of ions increases.
5. Why ordinary water is unsuitable for conductivity measurements? What is conductivity

water?
Ans: Ordinary water is unsuitable for conductivity measurements because it possesses large
conductance due to the materials dissolved in the container and due to CO2 and NH3 dissolved
from air. So water is specially purified by distilling it a number of times after addition of little
KMnO4. Such water is called conductivity water and their conductivity should not be more than
2- 3 x 10-8 ohm-1.
38 | 5 0
EXPERIMENT No. 8
Aim: To determine (a) max of a solution of cobalt chloride (b) verify Beers law
and apply it to find the concentration of given unknown solution by
spectrophotometer
experiment
j. Fundamentals of UV spectroscopy.
k. Concept of Lambert Beers Law.
l. Operation of the UV spectrophotometer.
.

3. Able to understand the terms like absorbance, max, optical density etc.
4. Able to operate and calibrate the UV spectrophotometer.

3. Able to acquire the skill to find out max..

5. Learning about the Lambert Beers Law.
6. Practice for fixing and operating the UV spectrophotometer by each student.
7. Recording of Observations, plotting graph and calculation of the results.
39 | 5 0
Apparatus Spectrophotometer, Beaker, Tissue paper
Requirement: Distilled water and cobalt chloride solution of different concentrations
Theory:
When an electromagnetic radiation is passed through a sample, certain characteristic
wavelengths are absorbed by the sample. As a result the intensity of the transmitted light is
decreased. The measurement of the decrease in intensity of radiation is the basis of
spectrophotometry. Thus the spectrophotometer compares the intensity of the transmitted light
with that of incident light.
The absorption of light by a substance is governed by Lambert Beers law. According to
this law when a beam of monochromatic light of intensity (I 0) passes through a medium that
contains an absorbing substance, the intensity of transmitted radiation (I) depends on the length
of the absorbing medium and the concentration of the solution. Mathematically it can be
represented as:
Absorbance = log (I0/I) = cl
Where, I0 = intensity of incident light
I = intensity of transmitted light
A = absorbance
l = length of the absorbing medium
c = concentration of the solution
= molar absorption coefficient or molar extinction coefficient
A plot between absorbance and concentration is expected to be a straight line plot, passing
through the origin, shows that Lambert Beers law is obeyed. This plot can be used to find the
concentration (or strength) of a given solution.
Procedure:
40 | 5 0
Step 1: Initial Setting of Spectrophotometer:
Connect the instrument to the power supply. Set the switch at ON position. Before starting the
experiment ensure that the meter initially reads zero on transmittance scale (T). Adjust the
wavelength knob to the required wave length region on scale. Set the position of gain selector
switch corresponding either to 340-400 nm or 400-960 nm wavelengths. Adjust the set zero knob
so that meter needle reads zero on T - Scale and 100 on OD (optical density) Scale.
Step 2: Final Setting of Spectrophotometer.

Open the lid of the sample housing and insert a cuvette containing blank solution (distilled
water). Close the lid so that it fits properly. Adjust the control knob (set 100) in appropriate
direction to bring the needle to 100 on transmittance or zero on optical density. Open the lid and
remove the cuvette. Close the lid tightly. Check zero on the meter and adjust to zero if disturbed.
Repeat the procedure again for zero and 100% Transmittance.
Step 3: Determination of max

Insert the cuvette containing standard solution in the similar fashion as explained in the step
above. Note down the reading of OD at zero wavelength. Change the wavelength with the
increment of 20nm every time and note down the value of corresponding OD. Plot a graph
between wavelength on x-axis and OD on y-axis. The value of max can be determined by
extrapolation of the curve towards x-axis. The maxima in the curve gives the value of max
Step 4: Verification of Beers Law i.e. Determination of Unknown Concentration
Fix the wavelength of max position. Prepare the standard solution as well as having different
concentrations ranging from 20 to 100% of cobalt chloride in distilled water. Note down the
optical density of solutions of different concentrations of cobalt chloride prepared above. Plot a
graph between OD and concentration. It should be a straight line. Take a solution of the unknown
concentration and note down OD. The concentration of the unknown solution can be determined
from the graph corresponding to the OD of the solution.
Observation Table:
Record the observations in the following Table
41 | 5 0
S. No. Wavelength (in nm) Absorbance or Optical Density
1.
2.
The wavelength at which maximum absorption will take place can be depicted by drawing a
graph between Wavelength (on x-axis) and Optical density (on y-axis).
S. No Concentration Absorbance or Optical Density

1 20%
2 40%
3 60%
4 80%
5 100%
6 Unknown (let it be C1) y
Conclusion:
We know that
A= log (I0/I) = cx
It is clear that absorbance A is directly proportional to the concentration of the solution. Plot the
graph between conc. and absorbance (i.e. OD) by taking concentration on X-Axis and
absorbance on Y-Axis.
42 | 5 0
Fig 1
From the above graph, the concentration of the unknown solution can be determined
corresponding to the observed absorbance (y) the Y-axis, the unknown conc. (C 1) on the X-axis
can be noted from the graph.
Result:
The straight line verifies Lambert Beers law and the unknown Concentration as given by the
graph is __________%.
Standard result: The graph (absorbance vs. concentration) should be a straight line (as shown in
Fig 1) which verifies Lambert Beers law and this will give the value of unknown concentration
by knowing its absorbance value via UV spectrophotometer. 5% Deviation from the exact
concentration value is accepted.
Sources of Error: 1.
Precautions:
1) For preparing the standard calibration curve, dilute solution of known concentration should
be used.
2) Ensure that you are handling the cuvette with tissue paper .Never touch it with your hand.
3) Wipe the cuvette with tissue paper before placing it in the spectrophotometer.
4) max value should be carefully observed.
Results and Discussion
Absorption spectroscopy can be used to quantify the absorbing species present in the sample.
The greater the quantity of absorbing species present, the greater will be the extent to which the
incident light will be absorbed. When a beam of monochromatic light falls on a substance, a part
of it is absorbed and the rest is transmitted. The intensity of the transmitted light is decreased. It
happens that a given material will always absorb light in the same way and not equally at all
wavelengths of light- thats why different things are of different colors. Some compounds absorb
light outside of the visible light spectrum, and thats why there are colorless solutions like water.
Because different compounds absorb light at different wavelengths, a spectrophotometer can be
43 | 5 0
used to distinguish compounds. Additionally, the amount of light absorption is directly
proportional to the distance that the light traveled through a sample and the concentration of
absorbing compounds in that sample.
The primary objective of this experiment is to determine the concentration of an

unknown cobalt (II) chloride solution. In this device, light will pass through the solution and
strike a photocell. The CoCl2 solution used in this experiment has a light pink color. A higher
concentration of the colored solution absorbs more light (and transmits less) than a solution of
lower concentration. The spectrophotometer monitors the light received by the photocell as either
an absorbance or a percent transmittance value. The second part of this experiment was looking
for the relationship between absorption and concentration of cobalt chloride solution. In fact, the
absorption would be increased when the concentration rose.
Discussion of errors and limitation of the experiment:
There were two main errors happened in the experiment that may influence or affect this
experiment, which were:
1. The actual concentration of Cobalt (II) ion solution.
2. The spectrophotometer itself.
First, the actual concentration of Cobalt ion solution may be not same as concentration showed
on label. The laboratory-made solution should very accurate and pure. However, during
reserving and moving those solutions into lab, many factors affect the concentration of solution
by environment. Therefore, the error of the solution used may transfer into the experiment and
caused error. Fortunately, this error should be small and will not affect experiment seriously.
Second, the spectrophotometer may have some instrumental errors in this experiment. By
calibrating the instrument and using a blank, we prevented these errors from becoming too big.
This experiment required high accuracy of operation and measurement. Therefore, several
procedures were used in this experiment to avoid error.
What was done further to minimize error?
44 | 5 0
First, the accuracy is so important; the equipment used for measuring should be as accurate as
possible. Also, liquids should be measured carefully.
Second, the cuvettes had to be rinsed with deionized water, and the Cobalt Chloride solution
before they was filled and placed in the spectrophotometer. In addition, the outside of tube was
wiped clean to erase any fingerprint oils on the surface of the cuvettes. Finally, the test tubes
used to dilute the solutions was dried and not rinsed before being used in order to prevent water
droplets from producing an inaccurate result.
Viva Voce:
1. Which region of electromagnetic spectrum is taken into consideration during electronic

transitions?
Ans: UV visible region.
2. State Lambert Beers law.
Ans: According to the Lambert Beers law: When a beam of monochromatic light of intensity I 0
passes through medium that contains an absorbing substance, the intensity of transmitted
radiation I depends on the length of the absorbing medium and the concentration of the
solution.
3. What are electromagnetic radiations?
Ans: Radiations having both electric and magnetic field which oscillate perpendicular to each
other.
4. Which law governs the absorption of light radiations by a sample?
Ans: Lambert Beers Law.
5. What does a spectrophotometer measures?
Ans: A Spectrophotometer compares the intensity of transmitted light to the absorbed light.
6. What is the significance of linear plot between concentration and absorbance?
Ans: Linear plot between Concentration and Absorbance verifies Lambert Beers Law.
7. What is the range of UV Visible radiations?
Ans: Uv radiations: 200-400nm and Visible radiations 400-800nm
8. What are the units of Wavelength?
45 | 5 0
Ans: nanometer.
9. 1 nm corresponds to how many meter?
Ans: 10-9 m.
10. Define transmittance and Absorbance.
Ans: Transmittance: The fraction of incident light at a specific wavelength that passes through a
sample.
Absorbance: The fraction of incident radiation that is absorbed by a sample at a specific
wavelength.
46 | 5 0
EXPERIMENT NO. 9
Aim: To separate and identify the amino acids in a mixture by thin layer
chromatography and find out Rf value of amino acids
experiment
m. Fundamentals of chromatography
n. Concept of thin layer chromatography
o. Concept of elution, mobile phase and stationary phase.
p. Importance of Rf value.
q. Basic idea about amino acids
.

1. Able to run TLC plate.
2. Able to find out the Rf value of organic compounds.
3. Able to measures the tendency of the sample to form a flammable mixture with air under
controlled laboratory conditions. It is only one of a number of properties that must be
considered in assessing the overall flammability hazard of a material.

1. Learning about chromatographic technique especially thin layer chromatography.
2. Practice to run TLC plate.
3. Calculation of Rf value of different amino acids

4. Conclude result with the observed readings.
47 | 5 0
Apparatus: TLC Plate, TLC Chamber, Capillary tubes, Reagent spray bottle, Beakers, Conical
flasks.
Requirement: 2% solution of individual amino acids, Solvent mixture of n- butanol, acetic acid
and water in the ratio 12:3:5 by volume, Ninhydrin reagent
Theory:
Chromatography is the most useful technique available for the separation of

closely related compounds in a mixture. Here the separation is affected by
differences in the equilibrium distribution of the components between two
immiscible phases, viz., the stationary and the mobile phases. The stationary
phase is a porous medium like silica or alumina, through which the sample
mixture percolates under the influence of a moving solvent.
Thin layer chromatography is a technique used to separate and identify compounds of interest. A
TLC plate is made up of a thin layer of silica adhered to glass or aluminium for support. The
silica gel acts as the stationary phase and the solvent mixture acts as the mobile phase.
Procedure:
1. Preparation of thin layer plate:
Dip two clean and dry glass plates held together by crucible tongs into the slurry, slowly in a
continuous movement. Remove the slides slowly and allow them to drain on the edge of the
container. Separate the slides by handling only the top edges. Place them on a sheet of filter with
the films facing upwards and dry them for five minutes. Remove the excess adsorbent from the
edge.
48 | 5 0
2. Applications of the sample (spotting the plate):
Apply two sample drops at least 1 cm apart and about 1 cm above the lower end of the plate. One
of the drops is of the pure amino acid and the other drop is of the mixture of the amino acid.
Allow the drops to dry in the air for some time.
3. Development of the chromatogram:
Prepare the developing solvent by mixing 70 mL of propan-1-ol with 30 mL of concentrated aq.

ammonia. Soak a filter paper strip and stick it to the interior of the jar. Carefully introduce the
developing solvent by means of a pipette so that lower edge of absorbent layer is immersed in
the solvent. Cover the mouth of the jar and allowed chromatogram to develop.
4. Visualization of Components
Remove the chromatogram from the developing jar. Spray it with ninhydrin reagent. Brown
spots appear on the white background.
5. Checking the purity of the sample:
Three spots from the mixture of three amino acids, one above the order will be observed and
their Rf values can be determined as given below:
Rf = Displacement of the compounds (d1)
Displacement of the solvent front (d2)
49 | 5 0
Where d1=distance between centres of the initial spot and the located spot and
d2= distance between centres of initial spot and the solvent front.
Precautions:
1) Bottles containing slurry must be properly stoppered, since the solvents in which slurry is
prepared are highly volatile.
2) The glass plates must be absolutely clean.
3) The chromatographic plate should be handled with care.
4) There should be a thin or uniform film of slurry on the glass plates.
Result & discussion:
Different compounds in the sample mixture travel at different rates due to the differences in their
attraction to the stationary phase and because of differences in solubility of the solvent. By
changing the solvent or perhaps using a mixture, the separation of components (measured by the
Rf value) can be adjusted.
Separation of compounds is based on the competition of the solute and the mobile phase for
binding places on the stationary phase. Silica gel which is used as a stationary phase is
considered polar & out of the two compounds which differ in polarity, the more polar compound
has a strong interaction with silica and is therefore more capable to dispel the mobile phase from
binding places. Consequently, the less polar compound moves higher up the plate resulting in a
higher Rf value & vice versa.
50 | 5 0
VIVA-VOCE
Q.1 Define the term chromatography.
Ans. Chromatography is an analytical technique used for identification of compounds or

separation of mixture of solutes. It is brought about by differential movement of the individual
solutes through a porous medium under the influence of a solvent.
Q.2 What is adsorption chromatography? Name its types.
Ans. The use of solid as a stationary phase with a liquid mobile phase is known as the adsorption
chromatography. It is further subdivided into (i) column chromatography (ii) paper
chromatography and (iii) thin layer chromatography.
Q.3 what are eluents?
Ans. The solvents employed for the adsorbed components from the surface of the adsorbent in
column chromatography are called eluents. The solvents used for developing the chromatogram
in TLC is also an eluent.
Q.4 Give the advantages of TLC over paper chromatography.
Ans. TLC is applied in preferances to paper chromatography on account of the following

advantages.
i) It is far more rapid than paper chromatography and give quick and reliable results.
ii) Sharp spots are obtained as compared to paper chromatography where the spots are diffused.
iii) Acidic or alkaline solution can be used for the location of spots,which is not possible in paper
chromatography.
iv) The chromatoplates can be heated,if requried.This is not possible in paper chromatography.
v) The spots can be scrapped out for further analysis.
51 | 5 0
Q.5 What do you want understand by the term retention factor (Rf)?
Ans. The movement of any substance relative to the solvent front in a given chromatographic
system is constant and characteristic of a substance. The constant is expressed as R f value and is
defined as:
Rf = Distance moved by substance
Distance moved by solvent front
EXPERIMENT NO. 10
Aim: Determination of heat of neutralization of solution of sodium hydroxide

against the solution of hydrochloric acid.
experiment
r. Concept of heat of neutralization..

s. Description of calorimeter.
t. Concept of water equivalent or heat capacity of calorimeter.
u. Mathematical concept to carry out calorimetric calculations
.

1. Able to perform calorimetric experiments.
52 | 5 0
2. Able to observe correct readings, plot graphs and carry out calorimetric calculations..
3. Able to analyze the results of the experiments and can explain the reason for deviation from exact
result.

1 Learning about the water equivalent of calorimeter.
2 Recording of observations using calorimeter and plotting of graph.
3 Practice of calorimetric calculations by each student

4 Conclude result with the observed readings.
5 Viva voce examination during experimentations.
Apparatus: Calorimeter, thermometer, stirrer.
Theory: The heat of neutralization is the quantity of heat evolved when one
gram equivalent of an acid is neutralized by one gram equivalent of a base.
When strong acids in dilute solutions are neutralized by strong bases in
solutions of about the same concentration, it is found that the heat evolved
is practically a constant quantity for all strong acids and bases, viz., 13,700
cal.
If the changes occurring when such solutions react are examined, the
reason for this constant quantity becomes clear. Strong acids and strong
bases in dilute solution are almost completely ionized and the same may be
said of the salt formed by their union, so that the only change may be said to
the formation of water by the union of hydrogen and hydroxyl ion, as shown
by the following equation:
NaOH + HCl NaCl + H2O + 13,700 cal
53 | 5 0
H+ + OH- H2O + 13,700 cal
Therefore, heat of neutralization of strong acids by strong bases represents

the heat of combination of one gram equivalent of hydrogen ions with one
gram equivalent of hydroxyl ions to form water.
The water equivalent of calorimeter or heat capacity of the calorimeter

is defined as the mass of water which will be heated through 1 0C by the
same amount of heat required to raise the temperature of the calorimeter
through 10C.
Q= ms where, Q= quantity of the heat gain or lose by the substance
S= specific heat of the substance
= temperature difference
ms (=W) is the water equivalent of the calorimeter.

Measurement of W (i.e, water equivalent of the calorimeter) is necessary
because during the heat exchange, the calorimeter also takes some amount
of heat evolved (due to the reaction) and hence should be taken into
account.
Procedure and Calculation:

Part 1: Determination of water equivalent of the calorimeter:
1. First determine the water equivalent of calorimeter.
2. Take 25 mL of distilled water in the calorimeter and record its temperature after every
half minutes.
3. Now take 25 mL hot water (higher than room temperature) in a beaker and note the
temperature after every half minutes.
4. Add this hot water quickly to the cold water in the calorimeter and stir the contents well
with a stirrer and note the temperature after every half minutes.
54 | 5 0
5. Plot the temperature vs time curve (Fig 1) for all three set of readings.
6. Draw a vertical line at the time of mixing (when half of the water has been poured in )
and extrapolate the temperature-time curve of the hot water and the mixture at the time of
mixing. The point of intersection will give you the desired temperature.
..
.. Mixing time
t2
t3
..
Temp
..
.Cold. water
. . t1
Time (minutes)
Fig 1
Calculation:
Volume of cold water taken = M1 mL
Initial temperature of cold water = t1oC
Volume of hot water mixed = M2 mL
Initial temperature of hot water = t2oC
Temperature of the mixed solution = t3oC
Heat taken by the calorimeter and water= (W + M1) (t3 - t1) Cal
Where, W is the water equivalent of calorimeter.
The specific gravity of water is taken as unity.
Heat given out by hot water = M2 (t2 t3) Cal
Now, heat taken up = Heat given out
(W + M1) (t3 - t1) = M2 (t2 t3)
W = M2 (t2 t3) M1 (t3 t1) (t3 t1)
55 | 5 0
Part 2: Determination of the heat of neutralization of sodium hydroxide and hydrochloric
acid
1. Take 100 mL of 1N HCl in the calorimeter and note the temperature reading after every
half minutes for five minutes.
2. Similarly take 100 mL of NaOH in the calorimeter and note the temperature reading after
every half minutes for five minutes.
3. Draw temperature- time curve for both acid and alkali solutions.
4. Now pour NaOH into the calorimeter containing HCl quickly (take care to avoid
splashing).
5. Stir and note the exact time of mixing.
6. Note the temperature readings after every half minutes for five minutes.
7. After the completion of the experiment, add a drop of phenolphthalein to ascertain the
completion of the neutralization reaction.
8. Plot a graph between temperature and time (Fig 2) for all three set of readings.
9. Draw a vertical line at the time of mixing (when half of the NaOH has been added in) and
extrapolate the temperature-time curves at the time of mixing. The point of intersection
will give you the final temperature of mixing.
Mixing time
t
. .
. .
. . ..
Temp
t5
... .
t4
Time (minutes)
Fig 2
56 | 5 0
Calculation:
Volume of 1M HCl = M3 mL
Volume of 1M NaOH = M4 mL
Initial temperature of either HCl or NaOH before mixing = t6 oC = (t4 + t5 ) /2 oC
Final temperature after addition of HCl and NaOH) = toC
Rise of temperature= (t t6) oC
Heat given out by the solution = (M3 + M4 + W) (t t6)
= Q cal (say)
Therefore, Q cal of heat is given out when 0.1 mole of HCl reacts with 0.1 mole of
NaOH.
Hence, molar heat of neutralization = 10 x Q cal
Result:
The heat of neutralization of hydrochloric acid and sodium hydroxide = . Cal
Standard result: 13,700 cal.
6 % deviation is accepted from the above result.
Sources of Error:
1. Calorimeter wasn't a perfect insulator. This is because once

calorimeter is opened for addition of cold water, the heat was lost not
only to the cold water but to the surrounding environment.
Unaccounted heat loss may lead to erroneous result.
2. Manual error or handling error may occur. Student may have waited
long enough for the thermometer to read, so the temperature of the
hot water was lower than it really was, or the temperature of the cold
water was warmer than it really was.
3. Another possible source of error is the increase in heat by stirring due

to increased kinetic energy.
57 | 5 0
Precautions:
1. When the experiment is complete, add a drop of phenolphthalein to the mixture of HCl
and NaOH. If a pink color is seen, then neutralization is not complete and the experiment
should be repeated.
2. Both the volume of strength of acid and base should be the same.
3. Final temperature should be recorded after thoroughly mixing the contents.
VIVA-VOCE
1. When atoms combine to form a stable bond, the energy is lowered. Where does the
energy go?
Ans: It is given out as heat into the surroundings. This heat is also called enthalpy and the heat
required to break 1 mol (6x1023) of these bonds is defined to be the bond enthalpy.
2. What is enthalpy?
Ans: Enthalpy (H): is one of the most important thermodynamic functions in chemistry.
Enthalpy is defined to be the heat exchanged at constant pressure. For a chemical reaction at
constant pressure (say, 1atm), the enthalpy of the reaction, Hrxn is defined to be the heat given
out or taken in.
When, Hrxn < 0, the reaction gives out heat to the surroundings so this is an exothermic
reaction
When, Hrxn > 0, the reaction takes in heat from the surroundings so it is an endothermic
reaction
3. What is calorimetry?
Ans: Generally the reactions taking place in the chemical sciences are breaking and making of
chemical bonds. This is accompanied by some heat effects. Formation of chemical bonds
releases energy in the form of heat and hence known as an exothermic reaction. The reaction
which is accompanied absorption of heat is known as endothermic reaction. Calorimetry is a
scientific term dealing with the changes in energy of the system by measuring the heat
exchanged with the surroundings. In a broader sense it is defined to determine the heat released
or absorbed in a chemical reaction.
58 | 5 0
4. What is calorimeter?
Ans: A calorimeter is a device designed to measure heat of reaction or physical changes and heat
capacity. The device can be sophisticated and expensive or simple and cheap.
5. Describe the main structure of a calorimeter.

Ans: A calorimeter consists of two vessels, outer vessel and an inner vessel. The space between
these vessels acts as a heat insulator and hence there is very little heat exchange in between the
inner and outer vessels. Thermometer measures the temperature of the liquid in the inner vessel.
The stirrer functions in such a way to stir the liquid to distribute the heat in the entire vessel. The
fibre rings in the calorimeter helps to hold the inner vessel hanging in the center of the outer
vessel. It also has an insulating cover or lid with holes for attaching the stirring rod and
thermometer.
6. Name two different types of calorimeter.
A. Bomb Calorimeter
The heat of combustion of a compound is measured by placing a known mass of a
compound in a steel container called a constant-volume bomb calorimeter, which is filled
with oxygen at about 30 atm pressure. This closed bomb is immersed in a known amount of
water. Sample is added in the sample cup and it is electrically ignited. The heat produced by
the combustion reaction is calculated by recording the rise in temperature of the water.
2. Coffee cup calorimeter
59 | 5 0
A constant- pressure calorimeter measures the heat effects of variety of reactions such as
neutralisation reactions, heat of solution and heat of dilutions. A coffee cup calorimeter is
basically constructed from a polystyrene (Styrofoam) cup with a lid, in which, the cup is filled
with a known amount of water and a thermometer inserted measures the heat changes associated
with the reaction.
60 | 5 0
EXPERIMENT NO. 11
Project:
Aim: Along with the prescribed practical syllabus, every student is required to pursue one
project during the semester.
Guidelines for the project:
Allocation of project and collection of samples will be done by the students in unit 1.
The experimentation part of project will be executed in unit 2.
The analysis & conclusions of the project will be drawn and the final report will be
submitted in unit 3.
Each students should prepare power point presentations on his/her project by taking help
from the concerned chemistry teacher and will present his/her work which will be
followed by viva voce examination.
The evaluation of the Project will be done as one of the experiments.
61 | 5 0

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Applied Chemistry Lab Manual (for IT students)

2. To determine the amount of residual chlorine present in given water sample. 11

6. Preparation of polymer (making of plastic) from potato starch. 30

Signature of Subject Coordinator: Signature of HOD (Applied Science):

Applicable to: 1 st year Engineering students (IT group)

Aim: Determination of temporary and permanent hardness of given hard

Fundamentals of hardness of water.

Concept of temporary and permanent hardness of water and their calculation

Concept of complexometric titration.

Effect of buffer solution on the pH of a solution.

Outcomes of this Experiment

Teaching Learning Activities

[M-In] + EDTA [M-EDTA] + In

Determination of total hardness of hard water sample:

Determination of Permanent Hardness

Vol. of hard water taken after boiling and filtering =10 ml

Sources of error: 1. Personal error like taking burette reading incorrectly.

Results and Discussion

Mg(HCO3)2 Mg(OH)2 + 2CO2

Aim: To determine the amount of residual chlorine present in given water

Concept of specification of drinking water

Concept of chlorination technique for purification of drinking water.

Idea of Iodometric titration.

Effect of residual chlorine in drinking water.

Outcomes of this Experiment

1. Able to understand the specification of drinking water and chlorination technique.

Teaching Learning Activities

Indicator: Freshly prepared starch solution.

End Point: Disappearance of blue colour.

Cl2 + 2KI 2 KCl+ I 2

CaOCl2 + H2O Ca (OH) 2 + Cl2

[O] + germs germs are killed by oxidation

2. Strength of free chlorine present in water sample

Sources of error: 1. Personal error like taking burette reading incorrectly.

Result and Discussion:

VIVA VOCE QUESTIONS

Q1: Why freshly prepared starch solution is used as indicator?

Q3: Why is boiled water not 100% safe for drinking?

Q4: What is the significance of break point chlorination?

Q5: What is iodometric titration?

Ans: In iodometric titrations, an oxidizing agent is allowed to react in neutral medium or in

Factors affecting viscosity

Concept viscosity coefficient

Description of Ostwald's viscometer

Outcomes of this Experiment

Teaching Learning Activities

Apparatus: Ostwalds viscometer, Stop watch, Clamp stand, Rubber tubing

Where, V = Volume of the liquid

t = Time of Flow of liquid

r = Radius of Capillary Tube and l = length

P = Hydrostatic pressure of the liquid

Where H = height of the liquid column

g = acceleration due to gravity

d = density of the liquid

Mean Time =sec Mean Time =.sec

Coefficient of viscosity of water 1 = 17.26 poise

Q.1: What is the CGS unit of coefficient of viscosity?

6. What is viscosity index?

Aim: Calibration of the digital pH meter. Determination of the pH of the

Fundamentals of pH of the solutions.

Concept of acidic and basic nature of a solution

Concept of buffer solution.