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1 | Page
EXPERIMENT No. 1
Aim: Determination of temporary and permanent hardness of given hard water sample by
volumetric analysis
Apparatus:
Requirement:
Standard Hard water, Hard water sample, N/50 EDTA solution, Buffer
solution (pH~10)
Indicator:
End Point:
Chemical Reaction:
M+2
(from hard water)
+ In2blue colour
[M-In] + EDTA
Wine red
Colour
[M-In]
Wine red colour
[M-EDTA]
Colour less
In-
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.
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
indicator combines with Mg2+ and Ca2+ ions to produce wine red colored complex which is less
2 | Page
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
1
2
3
Concordant Reading = V1 ml
Titration 2:
Sample Hard water v/s EDTA:
Volume of sample hard water taken for each titration =10ml
Solution in burette = N/50 EDTA Approx.
Sr. No.
Initial Reading
Final Reading
1
2
3
Concordant Reading = V2 ml
Titration 3:
Boiled water v/s EDTA:
Volume of boiled water taken for each titration =10ml
Solution in burette = N/50 EDTA Approx.
Sr. No.
Initial Reading
Final Reading
3 | Page
1
2
3
Concordant Reading = V3 ml
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:
= 10ml
= V1
4 | Page
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
V2 ml
V2 ml of EDTA
10 ml 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
=10 ml
= V3ml
10 ml boiled water
= V3 ml EDTA
= V3*10/ V1mg of CaCO3
1 ml boiled water
= V3*1000/ V1 ppm
Temporary hardness of hard water sample = Total hardness- Permanent hardness =X ppm
Total of hard water sample
= X1 ppm
= X2 ppm
= X3 ppm.
5 | Page
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
If hardness 150-300ppm
: 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
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
6 | Page
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
(Soluble in water)
Mg(HCO3)2
CaCO3
+
H2O
Calcium Carbonate
CO2
(insoluble in water)
Magnesium bicarbonate
Mg(OH)2
+
Magnesium Hydroxide
(Soluble in water)
(insoluble in water)
2CO2
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
+
Sodium
stearate
Ca2+
(C17H35COO)2Ca
ppts. of calcium stearate
(Soap)
+ 2Na+
(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
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.
8 | Page
9 | Page
EXPERIMENT No.2
Aim: To determine the amount of residual chlorine present in given water
sample
Apparatus: Burette, Burette stand, Titration flask, Measuring Cylinder, Beakers, Dropper.
Requirement: 10% KI Solution, Hypo solution (N/10), Chlorinated water sample
Indicator: Freshly prepared starch solution.
End Point: Disappearance of blue colour.
Chemical Reaction:
2 KCl+ I
Cl2
2KI
I2
2Na2S2O3
I2
Starch Solution
Na
S O6
2 4
2NaI
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
[O]
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
10 | 5 0
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:
Sr.No.
Initial Reading
Final Reading
1
2
3
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
N2 x 20
1/10 x V1/20
11 | 5 0
Precautions:
Shake the solution vigorously so that KI solution is thoroughly mixed with water sample.
Use only freshly prepared starch solution.
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.
12 | 5 0
I2
Free iodine is titrated against a standard reducing agent usually with sodium thiosulphate.
13 | 5 0
EXPERIMENT NO. 3
Aim:-To find out the viscosity of a given liquid using Ostwalds Viscometer
Apparatus: Ostwalds viscometer, Stop watch, Clamp stand, Rubber tubing
Requirement: Distilled water, Unknown liquid
Diagram:
Or
Where
= r4t1P1 /8Vl
= r4t2P2 /8Vl
1/2
= t1P1/t2P2 2
hdg 3
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.
15 | 5 0
Repeat the same procedure to take 3 readings for noting down the flow time of the given
liquid.
Observations:S.No
1
2
3
Mean Time =sec
= 17.26 poise
= 0.99 g/ml
= 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.
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.
16 | 5 0
VIVA-VOCE
Q.1: What is the CGS unit of coefficient of viscosity?
17 | 5 0
EXPERIMENT No. 4
Aim: Calibration of the digital pH meter. Determination of the pH of the
buffer solutions and an unknown solution
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.
2.
3.
4.
Switch on the instrument; wait for 10-15 minutes so that it gets warmed up.
Prepare the buffer solution of pH 4 and 9 using buffer tablets
Function key was set to stand by position.
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).
18 | 5 0
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
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.
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 viceversa.
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.
19 | 5 0
EXPERIMENT No. 5
Aim: To study the synthesis of Aspirin (acetylsalicylic acid) using different
acid and base catalysts
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,
20 | 5 0
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
OH
Salicylic acid
O
+
H3C
Acid
Cl
or base catalyst
Acetyl chloride
OH
O
CH3
O
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
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.
21 | 5 0
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 g Salicylic Acid
2 ml Acetic Anhydride
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.
0.0072 mol Salicylic Acid
Limiting Reactant
Salicylic Acid
Theoretical Yield
1.3 g
22 | 5 0
136C
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.
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:
23 | 5 0
OH
O
OH
OH
H2O
HO
CH3
CH3
Aspirin
Water
Salicylic Acid
Acetic Acid
24 | 5 0
EXPERIMENT No. 6
Aim: Preparation of polymer (making of plastic) from potato starch,
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 straightchained 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.
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
25 | 5 0
properties, thus acting as a plasticizer. This can be explained to students that the propane-1, 2, 3triol acts as a plasticizer.
Apparatus: 2 beakers (250 ml),
26 | 5 0
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.
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
27 | 5 0
EXPERIMENT No. 7
Aim: Determination of strength of a given hydrochloric acid solution by
titrating it against sodium hydroxide solution conductometrically.
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-]
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
28 | 5 0
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.
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
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S. No.
1
2
3
4
5
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.
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.
1. What is conductance and what are its units?
Ans: The reciprocal of resistance is called conductance. Its units are ohm-1 or mho.
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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
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
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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:
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
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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
S. No.
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
1
2
3
4
5
6
Concentration
20%
40%
60%
80%
100%
Unknown (let it be C1)
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.
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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.
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.
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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
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
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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?
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.
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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
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:
the films facing upwards and dry them for five minutes. Remove the excess adsorbent from the
edge.
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.
4. Visualization of Components
Remove the chromatogram from the developing jar. Spray it with ninhydrin reagent. Brown
spots appear on the white background.
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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.
VIVA-VOCE
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.
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
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44 | 5 0
EXPERIMENT NO. 10
Aim: Determination of heat of neutralization of solution of sodium hydroxide
against the solution of hydrochloric acid.
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
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.
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The heat capacity or water equivalent of a calorimeter is defined as the number of calories
required to heat the calorimeter by 1oC . If M is the mass of the calorimeter and S is the specific
heat, then, Water equivalent = M S
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.
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 water = t1oC
Volume of hot water mixed = M2 mL
Temperature of water = t2oC
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47 | 5 0
Mixing time
. .
. .
Temp
. . ..
... .
t5
t4
Time (minutes)
Fig 2
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.
5 % deviation is accepted from the above result.
Precautions:
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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.
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.
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2.
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.
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.
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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.
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