EM 4, Sector V, Salt Lake, Kolkata-700091,

West Bengal, India Phone: +91 33 2357 6163, Fax: +91 33 2357 1097

DEPARTMENT OF CHEMISTRY

CHEMISTRY LAB MANUAL

List of Experiments

Experiment 1:Standardization of H2SO4 (Sulphuric acid) with NaOH (Sodium Hydroxide)

Experiment 2:Determination of total hardness of Water by EDTA (Complexometric) titration

Experiment3 : PH – METRIC Titration of monobasic acid and determination of PKa value of that acid.

Experiment4:To determine the relative surface tension of glycerol solution by Stalagmometer

Experiment 5:To determine the relative viscosity of glycerol solution by Ostwald viscometer

Experiment 6:Detection of functional groups(carboxylic acid, ester, carbonyl).

Experiment 7:Conductometric titration

Experiment 8:Standardisation of KMnO4 solution with standard sodium oxalate/oxalic acid Solution
AIM:Standardization of H2SO4 (Sulphuric acid) with NaOH (SodiumHydroxide)

APPARATUS:

Electronic weighing balance, 250 ml conical flask, Measuring cylinder, funnel, glass rods,

Pipettes, Burettes and 100mlbeaker

PRINCIPLE

The principle behind this experiment is an acid-base titration. It is also known as neutralization reaction. This
experiment is a neutralization reaction of a base (NaOH) with acid (H2SO4). An acid solution neutralizes an
alkali solution in equal volumes provided their normal strength is equal. This means that 1 gm equivalent
weight of an acid will completely neutralise 1 gm equivalent weight of a base.In this experiment neutralization
of sodium hydroxide with H2SO4 takes place as:

2NaOH(aq)+H2SO4(aq) = Na2SO4 (aq)+ 2H2O(l)

The indicator used in this experiment is methyl orange. Methyl orange is an acidicindicator and is a weak
base. It ionizes in solution to give Me+ and OH- ions respectively.

MeOH(yellow) ->Me+ (red or pink) + OH-

In presence of alkali (base), the concentration of OH- ions increases in the solution and the equilibrium shifts
to left hand side (due to common ion effect), i.e. the ionization of MeOH is practically negligible. Thus on
addition of methyl orange in the alkali solution the colour remains yellow, which slowly turns to red or light
pink in colour with addition of acid in the medium resulting in the formation of sufficient amount of Me + ions in
the solution.

PREPARATION OF CHEMICALS

Preparation of 250ml (x N) NaOHSolution___ gm of sodium hydroxide pellets are dissolved in 1000 ml of

water. The solution is mixed properly to achieve a homogenous solution. The strength of the resulting
solution is __N.The solutions are freshly prepared.

DIAGRAM OF TITRATION
 PROCEDURE:

• Clean the given burettes with tap water, followed by distilled water, and rinse the same with given
acidsolution.
• Clean all the required glass wares with tap water, followed by distilledwater.
• Fill the burette with the given acid solution up to the 50ml mark.
• Check the marking with lower meniscus touching thelevel.
• Remove any air bubbles present if, by flowing the solution for a period of time till the bubbles are
clearedoff.
• Refill the burette Take 10 ml of the freshly prepared sodium hydroxide solution in a clean 250
mlconicalflask.
• Add 1 drop of methyl orange to the solution using glass rod or glasspipettes.
• The colour of the solution turns to faint yellow.
• More than 1 drop of the indicator is not recommended to avoid erroneousresult.
• Titrate the base with acid by drop by drop addition of acid from the burette till a faint pink colour
appears.
• Stop the titration once the pink colour is developed.
• Record the burette reading taken as the end point of the titration.
• Repeat the same(thrice) to achieve an average titre value.

OBSERVATIONTABLE

Sr.N Volume Of NaOH Initial Burette Final Burette Titre Reading Average (ml)
o. Solution(ml) Reading(ml)
reading (ml) (Final – Initial) (ml)

1. 10

2. 10

3. 10

4. 10

CALCULATION:

The strength of the acid solution is calculated according to the given formulae:
V1 S1 = V2 S2
Where,
V1 = Volume of the H2SO4 consumed
S1 = Strength of the acid solution (H2SO4)
V2 = Volume of the base (NaOH) (10 ml)
S2 = Strength of the base, NaOH (x N)

RESULT & CONCLUSION:

The strength of the given H2SO4 (Hydro Sulphuric acid solution) was foundtobe------------N.

Normality – Normality (N) is defined as the number of mole equivalents per litre of solution, i.e.
normality (N) = (Number of mole equivalents / Volume of solution inlitres).

Molality – Molality (m) is defined as the number of moles of solute per kg of solvent,

i.e. Molality (m) = (Moles of Solute / Weight of solvent inkg)

.Molarity – Molarity (M) is defined as the number of moles per litre of solution, i.e.

Molarity (M) = (Moles of solute / Volume of solution inlitres).

Formality – Formality (F) of a solution is the number of gram formula weight of the ionic solution dissolved
per litre of the solution, i.e.

Formality (F) = (Weight of solute in gram per litre of solution / Formulaweight).

1-Normal solution – 1(N) solution means that the solution contains exactly 1 mole equivalents of the
solute per litre of thesolution.

1-Molal solution – 1(m) solution means that the solution contains exactly 1 mole of solute per kg of the
solvent.

1-Molar solution – 1(M) solution means that the solution contains exactly 1 mole of solute per litre of the
solution.

1-Formal solution – 1(F) solution means that the solution contains 1 gram (in terms of formula weight) of
an ionic solute dissolved per litre of thesolution.

Standard solution – A standard solution is a solution containing a precisely known concentration of an

element or a substance. Its concentration remains constant all thetime.

Primary-standard solution – A primary standard solution is a reagent that is very pure, representative of
the number of moles the substance contains, and easily weighed. These are used in titration to determine
an unknownconcentration.

Secondary-standard solution – A secondary-standard solution is a chemical term that refers to a solution

that has its concentration measured by titration with a primary
standardsolution.
pH – It is the figure expressing the acidity or alkalinity of a solution on a logarithmic scale on which 7 is
neutral, lower values more acidic and higher values more alkaline.

The pH is equal to -log 10 c, where c is the H+ ion concentration in moles perlitre.

pOH – It is a measure of OH- ion concentration. It is used to express the alkalinity of a solution. Higher the
value on a pOH scale, more acidic the solution is, lower values are more alkaline and 7 isneutral.

pKa- pKa is the negative base-10 logarithm of the acid dissociation constant (Ka) of a solution, i.e.

pKa= -log 10 Ka. It is used to determine the strength of an acid or acidic solution.

pKb –pKb is the negative base-10 logarithm of the base dissociation constant (Ka) of a solution, i.e. pKb =
-log 10 Kb.

It is used to determine the strength of a base or alkalinesolution.

pKw - pKw is the product of the concentration of H+ and OH- ions in water, i.e.
pKw = -log 10 Kw = [H+][OH-]. pKw of water at 25◦C is14.

What do you mean by titration?

Ans) Titration is a common laboratory method of quantitative chemical analysis to determine the
concentration of an identified analyte. A reagent, termed as titrant is prepared as a standard solution of
known concentration and volume. The titrant reacts with a solution of analyte to determine its
concentration.Name six indicators and colours in acidic and basic medium.

INDICATOR ACIDIC MEDIUM BASIC MEDIUM

Thymol Blue Red Yellow

Methyl red yellow red

Methyl Orange Red yellow

Chlorophenol Red Yellow Red

Azolitmin Red Blue

Phenolphthalein Colourless Pink

Model questions for viva-voce

1. What do you understand by strength and normality of solution?

2. What is molarity of a solution? Give example.
3. What is the equivalent weight of NaOH?
4. What is the equivalent of aulfuric acid?
5. What is the role of acid –base indicator in acid –base titration?
6. Compare the concentration of 1N sulfuric acid and 1M sulfuric acid.
7. How do PH and PKW depends on temperature?
8. What is molality? Why it is independent of temperature?
9. What is primary standard solution? Give example.
10. What is secondary standard solution ? give example.
11. Define pH.
12. What is pH of pure water?
13. What is the colour of methyl orange indicator in acidic medium?
14. What is the colour of phenolphthalein indicator in basic medium?
15. What is the equivalent weight of oxalic acid?
16. Prepare 500 ml 2(N) NaOH solution.
17. Give examples of two strong acids and two weak acids.
18. Give examples of two weak acids and two weak bases.
19. What are the uses of burette and pipette?
20. How can you measure the accurate strength of a secondary standard solution?
Aim: Determination of total hardness of Water by EDTA (Complexometric) Titration

Purpose: To determine the “hardness” of a sample of water by using EDTA to determine the
concentration of calcium and magnesium ions.

Apparatus: Electronic weighing balance, 250 ml conical flask, Measuring cylinder, funnel, glass rods,
Pipettes, Burettes and 100mlbeaker

Background

Water hardness refers to the presence of calcium and magnesium salts in water, which react with soap to
form an insoluble precipitate:

2Na stearate + CaCl2 -> 2NaCl + Ca stearate (insoluble)

Water hardness affects the effectiveness of your soap and is responsible for the “scum” in your bathtub if
you have hard water. An historical method for determining water hardness was titration with a standard
soap solution. We will use a more modern titrant, ethylenediaminetetraacetic acid (EDTA).EDTA is a
hexadentate metal ion ligand: it has 6 potential sites for binding a metal ion (4 carboxyl groups and 2
amino groups). Describing EDTA as a chelating agent similarly denotes that it can simultaneously bind a
metal ion through more than one binding site. To determine the water hardness, you will determine the
total content of Ca2+ and Mg2+ in the water sample by titrating to form complexes between these metal
ions and EDTA. Deprotonated EDTA, given the symbol Y4-, reacts with these ions in the following way:

Ca2+ + Y4-->CaY2-and

Mg2+ + Y4-->MgY2-

Note that this is 1:1 stoichiometry—the EDTA may be hexadentate, but it is only one EDTA molecule per
complex.

You will fix the solution pH at 10 with a pH 10 buffer to ensure that the EDTA is deprotonated. The reaction
endpoint will be established using an Eriochrome Black T indicator.

After first determining the total water hardness (assuming that the two target metal ions are the only ions in
the sample with which EDTA complexes), you will separately determine the amounts of each of the two
metal cations. You will titrate samples to determine the concentration of Ca2+, only, by masking the
interference from Mg2+ by precipitating it from solution. That is, you will add excess strong base to
precipitate Mg2+ as insoluble Mg(OH)2 and then titrate the remaining Ca2+ with EDTA. In your analysis,
you will assume that no precipitate formed during the pH10 titration, and that errors such as coprecipitation
of Ca2+ with Mg2+ did not occur.
Procedures:

• Pipette out 10 ml of the sample water into a 100 ml conicalflask.

• Add NH4Cl – NH3 buffer solution 2-3ml to the watersample.
• Add the EBT indicator to the water sample and the colour of the water will turn to winered.
• Fill up the burette with the supplied EDTA solution of knownstrength.
• Titrate the water sample against the EDTA drop by drop until the wine red colour turns to blue.
• Once the blue colour is developed stop thetitration.
• Record the burette reading and repeat ittwice.

OBSERVATIONTABLE

Sr.N Volume of water Initial burette Final Titre reading Average (ml)
o. sample(ml) reading(ml) burettereadin (Final - Initial) (ml)
g (ml)

1. 10

2. 10

3. 10

Calculation andResults:

1000 ml 1(M) EDTA ≡≡ 100gm of CaCO31000ml

1(M) EDTA ≡≡ 100 x 1000 mg of CaCO3

1 ml (M/100) EDTA ≡ 1 mg of CaCO3

X ml (M/100) EDTA ≡ X mg of CaCO3

10 ml of water sample contains X mg of CaCO3

1000 ml of water sample contains 100X mg of CaCO3

Conclusion:

The hardness of the given sample water is 100 X ppm (ppm = mg / litre)
Model questions for viva-voce:
1. What do you mean by hardness of water?
2. What salts are responsible for temporary and permanent hardness of water?
3. Name the method used to remove temporary hardness from water?
4. Name the methods used for removal of permanent hardness from water.
5. Except complexometric titration, how can you estimate total hardness present in water?
6. Write unit of hardness.
7. What is meant by Complexometric Titration?
8. Draw structure of EDTA.
9. Draw structure of EBT.
10.
Draw Metal-EDTA (1:1) Complex, where M=Ca2+, EDTA4-
11. How many potential donor sites present in EDTA and identify them.
12. Write full form of EDTA.
13. Write full form of EBT.
14. What is meant by Buffer solution?
15. Give examples of acidic and basic buffer solution.
16. Name the buffer solution used in this practical and comment on its role.
17. During this practical at end point of complexometric titration wine- red coloured solution changes to
blue coloured solution- why?
18. Comment on stability of Calcium-EDTA complex and Calcium-EBT complex.
19. What is meant by Chelate effect?
20. How do you prepare 1000 ml (M/100) Na2EDTA solution?
AIM:PH – METRIC Titration of monobasic acid and determination of PK value of that acid.

APPARATUS AND MATERIALS:

Burette, Pipette , beaker , NaOH , Acetic Acid.

PRINCIPLE:

The PH of an aqueous solution can be measured using glass –calomel electrode system in which following
electrochemical cell is formed.

Ag|AgCl (s) |0.1 (M) HCl | Glass|Solution of unknown PH |Saturated Calomel Electrode

The right hand electrode is the saturated calomel electrode (ESC) and the left hand electrode is the glass
electrode which is actually an ion selective membrane electode , reversible with respect to H+ ion. The glass
electrode is the most likely used hydrogen ion responsive electrode and its use depends on the fact that when
a glass membrane is immersed in a solution , a potential is developed which is a linear function of hydrogen
ion concentrationof the solution .the internal HCl solution is maintained at constant concentrations , the
potential of the silver –silver chloride electrode inserted into it will be constant , and so too will the potential
between HCl solution and the iner surface of the glass bulb . hence the only potential which can vary is the
potential between the outer surface of the glass bulb and the test solution in which it is immersed , so the
overall potential of the electrode is governed by the hydrogen ion concentration of the test solution . glass
electrodes are also available as combination electrode which can contain the indicator electrode and a
reference electrode combined in a single unit .the potential (Eg ) of the glass electrode at 250 C may be
expressedas

Eg = Eg0 + 0.059 log aH+= Eg0 –0.059 PH (1)

For actual PHmeasurement , the glass electrode is standardized in buffer solutions of known PHvalues.

Ionization of a weak monobasic acid (HA) in aqueous solution may be represented as,

HA ⇄ H++ A- ------------------------------------------------------------------------------------------------------------(2)

Of which the ionization constant (Ka )is given by the activity quotient of the ionization equilibrium

Ka= (aH+ .aA- )/ aHA --------------------------------------------------------------------------------------------------------(3)

Where , a represents activity for the respective species which is related to the molar concentration , (C)
according to a = c.f ., whwre f = activity coefficient . in dilute aqueous solutions of weak acids , ionic strength
is very low , so the activity coefficient approach unity . hence , the concentration approach activities .
consequently the ionization constant (Ka) may be expressed as

Ka= [H+].[A-]/[HA] --------------------------------------------------------------------------- -------------------------(4)

When a strong base ( NaOH) is added to a weak acid ( Acetic Acid ) in an amount less than the stoichiometric
requirement a buffer solution I formed whose PH is given by the Henderson’s equation.

PH = PKa + Log[salt]/[Acid] ------------------------(5)

A PH metric titration curve may be constructed by plotting the PH of the acid solution after each addition of the
strong base and the equivalence point of the titration may be determined graphically . the derivative plot |∆PH /
∆n| vs n shows a maximum at the value of n corresponding to the equivalence point.

PROCEDURE :

• Prepare 100ml of a standard (N/20) solution of Oxalic acid by accurate weighing in a digital balance.
• Prepare 100ml of (N/2) NaOHsolution.
• Prepare 100ml of (N/20) Acetic acid solution.
• Prepare standard buffer solution of PH = 4 & 7 by dissolving the corresponding PH tablets in the
specified volume of distilled water.
• Standardize the PH meter by alternately dipping the glass – calomel electrode assembly in PH = 4 & 7
buffer solutions and adjusting the instrument accordingly at the experimental temperature.
• Take 25ml of (N/20) Acetic acid solution in a 100ml beaker .
• Add sufficient quantity of distilled water so that the combined electrode ( glass – calomel assembly) dip
into it properly.
• Allow the system to attain the equilibrium at the experimental temperature and record thePH.
• Add 2 drops of the (N/2) NaOH solution from a burette / micro burette stir gently to mix uniformly and
record the PH.
• repeat the process until the PH of the solution reads ≈ 4.5 . then add 1 drop each time till the
equivalence point is reached (indicated by sharp rise in PH) .
• Record the PH and the number of drops of the titrant in a tabular form.
• Take a few more readings beyond the endpoint.
• Determine the volume of 50 drops of the titrant solution and calculate the volume of one drop.

NOTE :

The same experiment may be carried out by coupling a quinhydrone electrode ( reversible with respect to H+
ion) with a saturated calomel electrode.

Experimental data:

PH Metric titration of ( N/20) Acetic acid against supplied (N/2) NaOH solution.
 TABLE 1:

Recording of PH agains no of drops of NaOH added.

No of observation No of drops ofNaOH Total No of dropsof PH value

NaOH added

1 0 0

2 2 2

3 2 4

4 2 6

Plotting of graph using the recorded data : PH vs no of drops of NaOH added and hence determine
the PkH value from the graph.
Model questions for viva-voce:

1. What do you mean by pH of solution?

2. What do you mean by pKa of an acid?
3. How do pH of pure water and pKw depend on temperature?
4. Prove that- pH+pOH = 14 for pure water at 298K.
5. Calculate Equivalent weight of Oxalic acid.
6. Calculate Equivalent weight of sodium hydroxide.
7. How do you prepare 100 ml (N/2) sodium hydroxide solution?
8. How do you prepare 100 ml (N/20) oxalic acid solution?
9. How do you prepare 100 ml (N/20) acetic acid solution?
10. Sodium hydroxide solution is standardized by standard oxalic acid solution before using it in pH metric
titration- why?
11. Name the electrode and give the electrochemical cell representation in pH metric titration.
12. Draw labelled diagram of Glass electrode.
13. Give the reaction associated in pH metric titration of acetic acid with sodium hydroxide solution.
14. Mention Henderson’s equation of pH , used in this practical.
15. Discuss the nature of graph pH of solution against volume of alkali added for the following pH metric
titration of Strong acid vs Strong base solution,
16. Discuss the nature of graph pH of solution against volume of alkali added for the following pH metric
titration of Strong acid vs Weak base solution
17. Discuss the nature of graph pH of solution against volume of alkali added for the following pH metric
titration of Weak acid vs Strong base solution.
18. Discuss the nature of graph pH of solution against volume of alkali added for the following pH metric
titration of Weak acid vs Weak base solution.
19. Comment on pH at half-equivalence point in this pH metric titration of acetic acid with sodium
hydroxide solution.
20. Acetic acid is weak monobasic acid- explain.
AIM:To determine the relative surface tension of aqueous glycerol solution by Stalagmometer.

PRINCIPLE:

The measurement of surface tension by stalagmometer is based on the fact thatDrop of a liquid (at the end of
the stalagmometer / capillary tube) falls when the weight of the drop just equal to the surface tension of the
liquid.Thus , the weight of the drop (due to the force of gravity) which pulls the drop downward is equal to vdg
,where g is the gravitational force, v is the volume of the drop and d is the density of the the liquid

(i.e.. mg=vdg)

On the other hand, the force tend to uphold the drop 2πrγ = vdg ; where 2πr is the circumference of a
circular surface , γ is the surface tension of the liquid. Unit of surface tension are dyne/cm (CGS system) and
Newton/ meter (SI system) where 1 dyne/cm= 1 mN/m.At equilibrium,(i.e. when two forces are balanced):

2πrγ = vdg ---------------------------------------------------------------------(i)

If n is the number of drops in volume V of the liquid , the volume of each drop the liquid will be v=V/n .

𝐕𝐝𝐠
Then from equation (i) we have 𝟐𝛑𝐫𝛄 = --------------------------------------------------------------------(ii)
𝐧

If n1 and n2 are the number of drops counted for the same volume of two liquids (1 and 2) of densities d1 and
d2, using the same stalagmometer , then

2πrγ1=Vd1g/n1 ----------------------------------------------------------------(iii)

2πrγ2=Vd2g/n2---------------------------------------------------------------(iv)

𝜸𝟏 𝒏𝟐𝒅𝟏
Dividing equation (iii) by (iv) ; 𝜸𝟐 = 𝒏𝟏𝒅𝟐
Therefore, surface tension of liquid (1)γ1 with respect to liquid (2) γ2 can be expressed as :

γ1= γ2 n2d1/ n1d2

incase, the second liquid is pure water (W), then surface tension of the liquid(L) with respect to water can be
expressed as :

γL=γWnWdL/nLdW

APPARATUS AND MATERIALS:

Stalagometer, Distilled Water, Aqueous Glycerol solution,Pyknometer or Specific gravity bottle for density
measurements, weighing balance.
 OBSERVATION TABLE AND CALCULATION:

Table 1: Recording of LABORATORY temperature

Initial ( 0C) Final ( 0C) Average ( 0C)

Table2:

Counting the number of DROPS for Distilled Water and Supplied Glycerol Solution and their Relative
Surface Tension.

Solution Number of Mean of drops Density of the Surface tension of the

drops solution (g/ml) solution (dyne/cm)
in Stalagometer

Water i) 0.996 71.97

ii)

iii)

5% Glycerol i) 1.00867

ii)

iii)

PRECAUTIONS:

Stalagmometer should be cleaned properly before use

Drops should be properly formed

Stalagmometer should be kept vertically during measurements

Same Stalagmometer should be used for water and aqueous glycerol solution

Observe carefully when liquids are passing the upper and lower marks of the Stalagmometer

RESULT AND CONCLUSION

Probable set of questions for viva-voce
1. Define surface tension.
2. What is the C.G.S and S.I unitsand dimension of surface tension?
3. What are applications of surface tension?
4. What is the effect of temperature on surface tension?
5. Name the apparatus used to determine the surface tension of liquid.
6. What are the forces responsible for surface tension?
7. Write the equation to determine surface tension by liquid drop method.
8. Compare the surface tension of the followings- Pure water and water mixed with detergent.
9. Difference between Cohesive and adhesive force.
10. Why the free surface of water is concave but that of mercury is convex?
11. During this experiment why the stalagmometer is kept vertically?
12. Define angle of contact.
13. Give some practical applications of surface tension.
14. Why do we use hot water to clean dirty clothes?
15. Why do hot soups tastes better than cold one?
16. What is reason behind the fact that flying insects can walk on water surface?
17. Why the drop of a falling liquid is always spherical in shape?
18. Why it is called relative surface tension?
19. Draw the labelled diagram of stalagmometer.
20. How to prepare 5% glycerol solution.
AIM: To determine the relative viscosity of glycerol by Ostwald viscometer and Determination of
concentration of an unknown glycerol solution from the calibration curve.

APPARATUS AND MATERIALS: Ostwald viscometer, Distilled Water, Glycerol solution,Pyknometer or

Specific gravity bottle for density measurements, Stop-watch to note the time, Weighing balance.

PRINCIPLE:

The property of resistance to flow when a stress is applied to a liquid is called “Viscosity”. It is produced by the
shearing effect of moving one layer of the fluid past another. When a liquid is in the laminar flow through a
tube the layer close to the surface of the tube is almost stationary and the layer at the axis of the tube moves
faster than any other layer. A slow moving layer exerts a friction on its nearest layer. The measurement of the
viscosity coefficient (η) of the given liquid by Ostwald’s Viscometer is based on Poiseuille’s equation,

η= Pr4πt/8vl

Where V is the volume of the liquid of viscosity coefficient η which flows in time t through a capillary tube of
radius 𝑟 and length l under a pressure head of P.𝑃 = ℎ𝑑𝑔Where h = height, d= density and g = acceleration
due to gravity.

If equal volume of two liquids are allowed to flow through the same capillary under the identical conditions,

η1=𝜋𝑟4hd1g t1/ 8Vl

η 2=𝜋𝑟4hd g t2 /8Vl

where ,

d1 = density of Solvent

d2 = density of given solution

η1 = viscosity of solvent

η2 = viscosity of given solution

t1 = time flow of solvent

t2 = time flow of given solution

η1= (η 2 d1 t1)/( d2 t2)

Procedure:

• Clean the Ostwald’s viscometer first with chromic acid and then wash thoroughly withdistilled water.
• A sufficient volume of solvent is introduced in bulb B so that the bent portion of tube and half or a little
more than a half of bulb B is filled up.
• Clamp the viscometer in quite vertical position.
• Through upper arm of bulb A, suck up solvent until it rises above the upper mark C and allow it to flow
under its own weight.
• The time of flow of solvent from C to D is continued by starting the stop watch as the Meniscus just
reaches upper mark C and stopping the watch as the meniscus just passes the lower mark D.
• Take at least three reading for solvent .
• Now clean the viscometer and dry it.
 • Repeat the whole procedure for the given solution.
• The density of given solution can be calculated by R.D. bottle.

OBSERVATION TABLE AND CALCULATION:

Table 1: Recording of LABORATORY temperature

Initial ( 0C) Final ( 0C) Average ( 0C)

Table 2: Measurement of Flow Time of Different Percentage of Glycerol Solution and Evaluate their
Relative Viscosity

Solutionin Flow time in Mean flow time in Density of the Viscosity of

viscometer ‘Second’ ‘Second’ solution (g/ml) thesolution
(milipoise)

Water i) 0.996 8.01

ii)

iii)

5% Glycerol i) 1.00867

ii)

iii)

10% Glycerol i) 1.02092

ii)

iii)

15% Glycerol i) 1.0278

ii)

iii)

UNKNOWNGlycerol i) 1.003*
solution
ii) 1.01012**

iii)

Plot “Viscosity” versus “% of Glycerol solution” to obtain a calibration curve by plotting the data obtained from water, 5%,
10% and 15% aqueous glycerol solution.From the calibration curve determine concentration of unknown glycerol

Result:The viscosity of the given solution at the room temperature is……………milipoise.

Precautions:

• The viscometer must be cleaned and dried properly before use.

• The viscometer should be kept in a vertical position.
• The flow time should be noted carefully.
• Formation of air bubbles in the viscometer should be avoid

Probable set of questions for viva-voce:

1. What do you understand by viscosity?

2. How is viscosity related to temperature?
3. What is the significance of viscosity?
4. What is Poiseuille’s equation?
5. What are the units of viscosity?
6. Write the name of the apparatus required for viscosity measurement.
7. How is viscosity related to density?
8. Give examples of viscous liquid.
9. Give one limitation of Poiseuille’s law.
10. Compare the Viscosity of the following solutions-Pure water, 5 % aq glycerol, 10% aq glycerol, 15% aq
glycerol
11. Give C.G.S and S.I units of viscosity.Give dimension of viscosity.
12. Why glycerol is more viscous than water?
13. What do you mean by streamline motion and turbulent motion of fluids?
14. Give practical applications of viscosity.
15. Comment on nature of graph of Viscosity coefficient vs concentration of glycerol solution.
16. How does viscosity of gas depend on temperature?
17. What do you mean by laminar flow of a fluid?
18. What do you mean by turbulent flow of a fluid?
19. Draw the labelled diagram of Ostwald viscometer.
20. Why very thin capirallry is used in Ostwald’s viscometer?
 Detection of functional groups
Test for carboxylic acid group (-COOH):

Sodium bicarbonate test

Carboxylic acids being stronger acid than phenol react with NaHCO3 in aqueous solution with the
effervescence of CO2 and become soluble due to the formation of sodium salt of the acids while the phenols,
except nitro-substituted phenols, remain insoluble.Add a pinch of the compound to a saturated aqueous
solution of NaHCO3in a test tube.Effervescence from the surface of the added solid due to the evolution of
CO2, indicates the presence of –COOH group.

Test for Ester group:

Add a pinch of the substance to a light pink alkaline phenolphthalein solution, prepared by adding a drop of
phenolphthalein to a very dilute NaOH solution with shaking.If the pink colour is not discharged in the cold,
heat the solution to boiling, disappearanceof the pink colour indicates the presence of ester group. Acidify the
clear solution withdiluteHCl. Appearance of white precipitate of water-insoluble hydrolysed acid, indicates the
presence of ester group.If the pink color is discharged in the cold showing the presence of acidic group, then
add dilute NaOH solution dropwise till a permanent pink color is obtained. Now boil the solution for
afewminutes. Discharge of color indicates the presence of ester group.

Esterification Test:

0.5 g of organic sample and 1 ml of ethanol is taken in dry test tube, 2 to 3 drops of conc H 2SO4 is added,
heated for 5 minutes in a hot water bath. The mixture is then poured into a beaker containing large volume of
Na2CO3 solution.

Characteristic sweet fruity smell of ester is obtained.

C2H5OH(aq)+CH3COOH(aq)=CH3COOC2H5(aq)+H2O(1)
Test for carbonyl group:

2,4-Dinitrophenyl hydrazine Test:Dinitrophenyl hydrazine reagent (Brady’s reagent) and heat the reaction
mixture on stream bath.An orange or red colored precipitate indicates the presence of carbonyl group.

TestFor Aldehyde (-CHO)

Fehling’s Test:

2 ml of Fehling’s solution (equal volume of Fehling A + Fehling B solution) is added to 0.1 g of organic sample
and heated in a water bath for 5 to 10 minute.Yellow or rust red ppt is formed.
 Probablesetofquestionsforviva-voce:

1. Write down the Preliminary test for detection of carboxylic acid.

2. Write down the confirmatory test for carboxylic acid.
3. Write down thechemicalformulaofmethylacetateandethylacetate.
4. Write down the chemical formula of formic acid,acetic acid,oxalic acid.
5. Write down the test for detection of ester functional group.
6. What is the colour of alkaline phenolphthalein solution?
7. Draw the structure of Braddy’s reagent.
8. What is fehling A Solution?
9. What is fehlingB solution?
10. How do you prepare fehling’s solution?
11. Identify the product when glucose is mixed and heated with fehling’s solution?
12. How do you distinguish between ketone and aldehyde by a chemical test?
13. Can fehling’s solution detect the presence of an aromatic aldehyde?
14. Does fehling’s solution reacts with benzaldehyde?
15. What is the oxidation state of cu in copper sulfate and cuprus oxide?
16. What is the chemical name of the product formed when braddy’s reagent reacts with an ketone?
17. Name an aromatic ketone.
18. Which one is more reactive towards nucleophilic addition reaction between acetaldehyde and acetone?
19. What are the products of basic hydrolysis of an ester?
20. What are the products of esterification reaction?
AIM :Conductometric titrations
Introduction: When an electrolytic solution (titrant solution) is added from a burette to another
electrolytic solution, the conductivity of the solution changes when an ionic reaction occurs between these
solutions.When one ion replaces another, the conductivity of the solution changes. If high-mobility ions like
hydrogen ions are replaced by lower-mobility ions like sodium ions, the conductance of the solution
decreases as we know the conductance of a solution depends on the number of ions and mobility of ions.

Similarly, if low-mobility ions are replaced by high-mobility ions in the solution during the course of the
reaction, the conductance of the solution increases. The basic principle of conductometry or conductivity
titration is based on the fact that ions of one mobility are replaced by ions of another mobility, thus the
conductance of the solution changes during the course of the reaction.

The conductometric titration curve is obtained by plotting graphically the conductance against the volume of
solution(titrant) added from the burette. The point of break or intersection point in the conductometric titration
curve gives the endpoint of the titration.

Conductometric titrations used to investigate neutralization titrations by observing the change in electrical
conductivity. The principle of conductometric titration is based on the fact that during the titration, one of the ions is
replaced by the other and invariably the set of ions differ in the ionic conductivity with the result that conductivity of
the solution varies during the course of titration. The titration reaction involve the addition the reagent to a solution
that contains a substance with unknown molarity. Just before and after the equivalence point, there is a marked
difference in the rate of change of conductivity with addition of reagent. The curve of titration involve plotting
conductivity of the solution against the volume of standard reagent. The use of an excess of the standard reagent
establishes the correct location of the equivalence point therefore it is then possible to find the volume of reagent
equivalent to the solution titrated by measuring the conductivity.

There are some advantages of conductometric titration:

• No need to indicator.
• The end point identified graphically with minimum error.
• Used with colored liquids for which ordinary indicators cannot work.
• Used for dilute solutions as well as for very weak acids.
Types of conductometric titrations:

Titration of strong acid (HCl) with strong base(NaOH)

Infirst,the solution of HCl is unknown molarity;it is possible to find the concentration of HCl by titration with
NaOH(knownconcentration)and using the titration curve. Before the addition of the base, the acid
solution has a high conductivity (due to completely ionized in aqueous medium furthermore
as H+ ion has very large ionic mobility). As base added, the H+ ion has react with OH- ion
to form water and being each H+ ion replaced by Na+ ion (where the conductivity of Na+ less
than conductivity of H+).Consequently, the conductivity of the solution decreases and keeps on falling
with addition of the base until reached to the equivalent point. At the equivalence point, the
solution contains only NaCl

HCl+ NaOH->H2O + Na+ + Cl –

Titrationofweakacid(CH3COOH)withstrongbase(NaOH).
Since the acid is weak, its conductivity is relatively low. On the addition of base, there is decrease in
conductance not only due to the replacement of H+ by Na+ but also suppresses the dissociation of acetic acid
due to common ion acetate. But very soon, the conductance increases on adding NaOH as NaOH neutralizes
the un-dissociated CH3COOH to CH3COONa which is the strong electrolyte.

This increase in conductance continues raise up to the equivalence point. The graph near the equivalence
point is curved due the hydrolysis of salt CH3COONa. Beyond the equivalence point, conductance increases
more rapidly with the addition of NaOH due to the highly conducting OH− ions.

CH3COOH + NaOH H2O + CH3COONa

Conductometric titration of strong acid and weak base( HCl vs NH4OH)
In the beginning, the conductance of the HCl solution is very high due to the liberation of fast-moving H+ ions.
But, when a weak base such as NH4OH is added from the burette, the fast-moving H+ ions are replaced by
slow-moving NH4+ ions. Therefore, the conductance decreases until the endpoint is reached.

Conductometric titration of weak acid and weak base( CH3COOH vs NH4OH)

In the beginning, the conductance of weak acid solution is very low due to low ionization. But when NH4OH is
added gradually to the acid solution, the conductance slightly decreases due to the substitution of H+ ions by
slow-moving NH4+ions. On further addition of NH4OH solution, the conductance of solution increases til the
endpoint due to the formation of highly ionized salt.
in case of titration HCl with NaOH B represents the equivalent point or the neutralization point. In this point, moles
number of H+ ions is equal to the moles number of OH- ions, hence mole balance at the neutralization points yields:

.............................................................................
n H+ = nOH- (1)

M acid × V acid =M base ×Vbase (2)

Procedure:
Titration HCl with NaOH:
(95mL) of distilled water added to (5mL) of HCl (unknown concentration) and its conductivity is measured, then it is
measured after addition of (1mL) from solution (0.1M) of NaOH. This is repeated until (10mL) of NaOH is added.

Observation table

No. Of Drops Volume of NaOH Conductance of

observation of added (ml) the solution
NaOH
added

10

Calculations:

draw the conductivity (k) versus the volume of NaOH added.

Find the concentration Of HCl.

Model questions for viva-voce

1. Define the term conductance.

2. What is the effect of temperature on conductivity of electrolytic solution.
3. Define cell constant.
4. What is the unit of conductance.
5. What is the difference between metallic conduction and Electrolytic conduction.
6. Define Specific conductance?
7. What is the unit of specific conductance?
8. What is meant by equivalent conductance?
9. What is the unit of equivalent conductance?
10. What is molar conducitivity?
11. How does molar conductivity depends of dilution for strong and weak electrolytes?
12. What is the nature of graph of conductometric titration of a weak acid vs weak base?
13. What is the nature of graph of conductometric titration of a weak acid vs strong base?
14. What is the nature of graph of conductometric titration of a strong acid vs weak base?
15. What is the nature of graph of conductometric titration of a strong acid vs strong base?
16. What is the effect of dilution on conductance ?
17. What is the relation between resistance and conductance?
18. How to prepare 100 ml (M/20) acetic acid solution.
19. How to prepare 100 ml (M/2) NaOH solution.
20. How to prepare 100 ml (M/10) Oxalic solution.
Redox Titrimetric Estimations Based on Permanganometry

AIM:Standardisation of KMnO4 solution with standard sodium oxalate/oxalic acid solution

Principle:

In dilute H2SO4 acid medium MnO4- quantitatively

4 oxidises C2O 2-to 4CO2and itself is reduced to Mn2+
4 4
2 MnO4- + 16H+ + 5 C2O42- = 2Mn2+ + 8H2O+ 10 CO2

Therefore, MnO4-/5 = C 2O42-/2 4= 1 Equivalent

1000 ml of (N) oxalate = 1000 ml of (N) permanganate

It is an example of autocatalytic reaction, in which Mn2, a product of reaction, acts as the catalyst. Use of
sodium oxalate as the primary standard substance is advantageous over oxalic acid, because the former has
no water of crystallisation and can be easily purified by recrystallisation. Further, its strength does not change
on standing.

KMnO4 solution may be standardised against standard oxalic acid/sodium oxalate solution in 2 (N) H2SO4
medium at 70-80 oC. Purple coloured KMnO4 serves as a self-indicator. Its strength may be calculated using
the relation:

VMnO4-x SMnO4-= VC2O42-x SC2O42-

Chemical Required:

Standard (N/20) oxalic acid, H2C2O4.2H2O (F.W. =126.048)

or Sodium Oxalate, Na2C2O4 (F.W. = 134) to be prepared by accurate weighting.

Strength =(w/0.7879)(N/20) for oxalic acid=(w’/0.8375)(N/20)

for sodium oxalateWhere, w and w’ are the weights of H2C2O4.2H2O or Na2C2O4 respectively per 250 ml of
the solution.

1. (-N/20)KMnO4 solution: -0.4 -0.5g of KMnO4 per 250ml.

2. 4(N) H2SO4 : (1 : 9) H2SO4solution

Procedure:
• Pipette out an aliquot of 25 ml of (N/20) standard oxalic acid or sodium oxalate in a 250 ml conical flask
• add 25 ml of 4 (N) H2SO4 and heat to 70 – 80 oC
• titrate the hot solution with the (-N/20) KMnO4 solution until the solution turns light pink colour that is
stable for -30seconds.
• Repeat the titration twice to have a concordant reading. Calculate the strength of KM nO4solution.
 OBSERVATION TABLE

Sr.N Volume of oxalic Initial burette Final Titre reading (Initial Average (ml)
o. acid Solution (ml) reading(ml) burettereadin – Final) (ml)
g (ml)

1. 10

2. 10

3. 10

4. 10

CALCULATION:

VMnO4- x S MnO4- = VC2O42-x S C2O42-

CONCLUSION

The strength of unknown KMnO4 solution is = ……….(N).

Model questions for viva-voce:

1. Calculate equivalent weight of KMnO4 in acid medium.

2. Calculate equivalent weight of KMnO4 in basic medium.
3. Calculate equivalent weight of KMnO4 in neutral medium.
4. How do you prepare 250 ml (N/20) oxalic acid solution?
5. Comment on the structure of KMnO4.
6. KMnO4 crystals are deep purple coloured- why?
7. KMnO4 is secondary standard- why?
8. Oxalic Acid is primary standard- why?
9. In acidic medium KMnO4is strong oxidising agent- why?
10. Standardisation of KMnO4 solution with standard oxalic acid solution is a redox titration- why?
11. What is oxidation state of Mn in KMnO4?
12. What is oxidation state of carbon in oxalic acid?
13. Name self indicator in this redox titration.
14. The reaction between oxalic acid and KMnO4 solution in acid medium is also example of auto catalysis
reaction – why? Which ion acts as auto catalyst here?
15. Before this redox titration oxalic acid solution is needed to heat 70-80 oC. – why?
16. Give balanced ionic chemical equation associated in this redox titration.
17. Standardisation of KMnO4 solution with standard oxalic acid solution is carried out in acid medium-
why?
18. KMnO4 solution is required to preserve in dark place-why?
19. What is basicity of oxalic acid?
20. How do you calculate strength of given KMnO4 solution in this redox titration?