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Engg.

Chemistry
Lab Manual

BAS152/BAS252
Experiment No. 1

Object: To understand the Standard laboratory devices for weight and volume measurement and
Caliberation of Analytical Equipment.

The experiment is divided into two parts. The purpose of this experiment is to make the students:
• familiar with commonly used laboratory glassware and equipments,
• learn to take observations,
• analyze data and
• prepare standard solution.
• Learn to Caliberate Analytical Instument.
Learning objectives:
By the end of this experiment the student shall be able to:
• understand the safety measures of laboratory.
• know how to make correct measurements using burette, pipette and graduated cylinder.
• know the mass of compound weighed out and transferred to volumetric flask
• volume of the volumetric flask used to make the standard solution
• know how to use digital analytical balance.
• record experimental observations.
• prepare standard solution.
• Caliberate Equipment

(A) Use of laboratory equipments and understanding the standard units of measurement.

Measurement of Weight:
Units of Weight: e.g. Milligrams (mg), Grams (g)
Analytical Balance: An Instrument used for measurement of weight in laboratory is analytical balance.
It is an accurate and precise instrument to measure weight.
The most commonly used analytical balance is beam balance, precision scales, and moisture analyzers.
An analytical balance measures masses to within 0.0001 g.
The balance is enclosed in a glass case in order to avoid disturbances due to air (fig. 1).

Precautions:
1. Do not exceed capacity.
2. Use tong/forceps to transfer sample and weights.
3. Protect from hot/corrosive substance.
4. Cleaning the balance after every use.
5. Vibration free table. Figure 1: A Beam Balance

Measurement of Volume:

Units of Volume: e.g. Milli liter (mL), liter (L)


For accurate measurement of volume of solutions, volumetric analysis require various types of
apparatus as:
Titration Flask: It is a conical flask made of borosil glass. It is available in different capacities like 100mL, 250mL,
etc.
Pipette: It is a cylindrical glass tube with a bulb in the middle. It is used to measure and transfer definite volume of
the solutions. The capacity of the pipette is marked on the bulb.
Burette: It is laboratory equipment used to dispense and measure volume of a chemical solution. The burette used
in our laboratory is graduated from 0 to 50ml and each ml is further subdivided into 10 equal divisions. Thus the
least count of burette is 0.1ml and with the help of it we can measure volume accurately upto 0.1ml.
Guidelines for reading the burette correctly: The reading should be taken by keeping the eye at the same level as
the meniscus.
For colorless solution: Lower meniscus is read
For colored solution: Higher/upper meniscus is read

Precautions:
1. Clean the burette thoroughly.
2. Rinse the burette with the solution to be taken into it before use.
3. Clamp the burette vertically on the burette stand.
4. Do not blow the last drop from the pipette.
5. Ensure that there are no air bubbles in the burette.
Figure 2: Reading a burette
Measuring Cylinder: A graduated cylinder, measuring cylinder or mixing cylinder is a common piece of laboratory
equipment used to measure the volume of a liquid. Each marked line on the graduated cylinder represents the amount
of liquid that has been measured. Typical capacities of graduated cylinders are from 10 mL to 1000 mL.

Measurement of Concentration:
Strength: Strength of a solution is defined as the amount of the solute in gms, present in one litre of the solution. It
is expressed as gramsLiter-1.
Strength of the solution is expressed in following ways:

Molarity (M): Molarity is the concentration of a solution expressed as the number of moles of solute per liter of
solution
𝒏𝒐 𝒐𝒇 𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆(𝒏) 𝑴𝒂𝒔𝒔 𝒊𝒏 𝒈𝒓𝒂𝒎𝒔
M= where n =
𝒍𝒊𝒕𝒆𝒓𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏(𝑽) 𝑴𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓 𝒘𝒆𝒊𝒈𝒉𝒕

Normality (N): Normality is defined as the number of gram equivalents of solute present per liter of solution.
Normality formula is given by:

𝒈𝒓𝒂𝒎 𝑬𝒒𝒖𝒊𝒗𝒂𝒍𝒆𝒏𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆


N=
𝑳𝒊𝒕𝒆𝒓𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏

Molality (m): Molality of a given solution is def ined as the total number of moles of solute per kilograms
of solvent present in the solution. Molality is represented by m, which is termed as molal. One molal is
the molality of solution where one mole of solute is present in 1000 grams of solvent.
𝒏𝒐.𝒐𝒇 𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆
m=
𝑾𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕 𝒊𝒏 𝑲𝒈

Equivalent Weight: Defined as the number of parts by weight of chemical species combined with or displaced by
one parts of hydrogen or 8 parts of oxygen.
Equivalent Weight of Acid = Molecular Weight/Bascicity
Equivalent Weight of Base = Molecular Weight/Acidity
Equivalent weight of oxidizing or reducing agent = Molecular Weight/Change in oxidation number
Equivalent weight of Ion(cation or anion) = Molecular Weight/Charge on the ion
Types of standard solutions
i) Primary Standard Solution
Primary standard is a reagent that is very pure, representative of the number of moles and can be easily weighed.
Their solutions are used in titration to determine the concentration of unknown solution. Primary standards are often
used to make standard solutions for an experiment.
A good primary standard solution has following properties:
• high level of purity
• low reactivity (high stability)
• high equivalent weight (to reduce error from mass measurements)
• not hygroscopic (to reduce changes in mass in humid versus dry environments)
• non-toxic

ii) Secondary Standard solution:


A secondary standard is a chemical that has been standardized against a primary standard for use in a specific
analysis. Secondary standards are commonly used to calibrate analytical methods and its solution remains stable for
a long time. e.g. Sodium hydroxide, once its concentration has been validated through the use of a primary standard,
is often used as a secondary standard.
A secondary standard is a chemical or reagent which has certain properties:
• Less pure than primary standard.
• Hygroscopic
• High reactivity
• Less stable and more reactive than primary standard.
• Titrated against primary standard to calculate exact concentration.

Procedure of preparation of standard solution

• Step 1: Place a small amount of distilled water into a clean, dry 250mL volumetric flask.
Swirl the water around the whole interior of the flask to rinse it. Discard the water and dry the flask before
use.
• Step 2: Weigh the calculated amount of the salt (the solution of which is to be prepared) onto a clean, dry
watch glass.
• Step 3: Position a clean, dry glass funnel into the neck of the volumetric flask.
Leave a small air gap around the stem of the funnel inside the neck of the volumetric flask.
• Step 4: Place the weighed salt into funnel and wash it into the volumetric flask with a little distilled
water. Repeat this process until all the salt has been transferred to the volumetric flask. Finally, position the
watch glass over the funnel and run a little distilled water over this to transfer any microscopic amounts of it
that might be still adhering to the watch glass to the volumetric flask. Repeat this process. Swirl the
volumetric flask gently to dissolve the salt. Do not shake the flask. Do not invert the flask.
• Step 5: Pour distilled water through the funnel slowly until the water level in the volu metric flask reaches
the base of the neck. Allow any water still remaining in the funnel to run through (there shouldn't be any if
you maintained the air gap, and, if you poured slowly.) Carefully pour distilled water through the funnel very
slowly until the bottom of the meniscus is about 1 cm from the graduation mark on the neck of the volumetric
flask.
• Step 6: Remove the funnel from the volumetric flask.
• Step 7: Use a pipette to transfer distilled water drop by drop to the volumetric flask until the bottom of the
meniscus sits on the graduation mark on the neck of the volumetric flask when viewed at eye level.
• Step 8: Stopper the volumetric flask and invert it several times to ensure thorough mixing and label it with
the name of reagent and date of preparation.

(Part B)
Calibration of Analytical Equipment and Apparatus

Analytical intruments are used for a specific analysis. To ensure the accuracy in performance or validation of the
intrument, calibration is being done. In simple words, Calibration is the demonstration by which, we ensure that an
instrument is suitable for its intended purpose (i.e. its readings are accurate the reference to establish standard).
Calibration is performed using primary reference standards.Instrument need to be calibrated before use.
The specific calibration procedures of few intruments are discussed below:

1. Weighing Balance
Balance or scale calibration is essential to achieve accurate weighing results. To calibrate, you simply need to place
a calibration weight on the pan and record the result. If it is within pre determined limits then no further action is
required. If the result is not within limits then the balance should be adjusted to the value of the calibration weight.

2. pH meter
A pH meter is used to measure the pH of a solution. Depending on the laboratory, this device may be analog or
digital. A pH meter should be calibrated in solutions of known pH before use.
To calibrate and use a pH meter, prepare a neutral buffer with a pH of 7 and a second buffer with a pH of 4 for acidic
samples or 9.2 for base samples. Next, put a clean electrode in the neutral buffer and press the “Measure” or
"Calibrate" button.

3. Colorimeter
A Colorimeter is a device which is used to measure the transmittance and absorbance of light that passes through a
liquid sample. It also measures the intensity or colour concentration that develops upon introducing a perticular
reagent into a solution.
To Calibrate the Colorimeter, slide the lid of the Colorimeter open to reveal the cuvette slot. Insert a cuvette, filled
with distilled water or other solvent used to prepare your solutions, for your calibration blank (100% transmittance
or 0 absorbance).
The result of the calibration is a correction with its uncertainty. This correction is the difference between the reference
standard value and the value measured by your equipment.
Experiment No. 2
CO1 Estimate different impurities present in water sample

OBJECT: To determine the total hardness of given water sample by using (EDTA)Na 2 as standard
solution by complexometry.

REQUIREMENTS: Conical flask, burette, pipette, beaker, measuring flask, M/100 of


(EDTA)Na 2 solution, buffer solution of pH 10, Eriochrome black –T indicator, supplied water
sample.

THEORY: Temporary hardness of water is due to the presence of soluble salts of bicarbonates of
calcium and magnesium, while the permanent hardness of water is due to the presence of sulphates,
chlorides, nitrates etc. of calcium, magnesium and other heavy metals. Temporary hardness of
water can be removed by boiling of water while permanent hardness can not be removed by
boiling.

EDTA( Ethylenediaminetetraceticacid) is a complexing agent, which is widely used due to its


strong complexing agent, which is widely used due to its strong complexing action and commercial
availability.EDTA is a tetraprotic acid,because of its limited solubility, it is not used directly.
(EDTA)Na 2 is used which in auueous solution ionize to give two Na+ ions and a strong chelating
agent. The indicator used is [Sodium-1-(1-hydroxy-2-naphthylazo)-6-nitro-2- naphthol-4-
sulphonate] commonly known as Eriochrome Black-T (EBT). EBT has two ionisable phenolic
hydrogen atoms and for simplicity it is represented as Na+H2In-.
END POINT: Wine red to blue.

PROCEDURE: Take 25ml. of hard water sample in a conical flask. Add 2ml of buffer solution
and 2drops of Eriochrome black-T indicator, the colour of the solution turns wine red. Now titrate
the solution against (EDTA)Na 2. So that the colour changes from wine red to blue. Repeat the
titration for two concordant readings.

OBSERVATION:

S.No. Vol.of unknown solution Burette reading (mL) Vol.of(EDTA)Na2


taken (mL) used
Initial Final

1. 25

2. 25 V2(mL)

3. 25
CALCULATION:

M1V1 = M2V2

(SAMPLE) (EDTA)Na2

M1 X 25 = 1/100 X V2

M1 = 1/100 X V2 / 25

Strength of water simple = M1 X 100 g/L

= 1/100 X V2 / 25 X 100 X 1000 mg/L

= V2 / 25 X 1000 mg/L

RESULT: The total hardness of given water sample is ............................. ppm.

PRECAUTIONS:

1) The glass wares should be properly rinsed with distilled water .

2) The reaction mixture should be shaken properly.

3) The amount of indicator should be same in all titrations.


Experiment No. 3
CO1: Estimate different impurities present in water sample.

Object To determine the constituents and amount of alkalinity of the supplied water
sample.

Require HCl (N/10), Phenolphthalein (Ph), Methyl Orange (MO), Water sample,
ments
Burette, Pipette, Conical Flask, Beaker, Funnel

Principle Alkalinity of water sample is mainly due to the presence of various hydroxides,
carbonates and bicarbonates. Following possibilities may arise with respect to the
constituent’s causing alkalinity in water:

❖ due to OH − only
❖ due to 𝐶𝑂32−only
❖ due to 𝐻𝐶𝑂3− only
❖ due to OH − and 𝐶𝑂32−
❖ due to 𝐶𝑂32−and 𝐻𝐶𝑂3−

Note: OH − and 𝐻𝐶𝑂3− cannot exist together as they react to produce 𝐶𝑂32−
ions.

𝐻𝐶𝑂3− + OH − → 𝐻𝐶𝑂3− + H2O


These can be estimated separately by titration against standardized acid using
phenolphthalein (pH range: 8.2 – 10.0) and methyl orange (pH range: 3.2 – 4.4)as
indicators.

(a) H + + OH − → H 2 O
(b) 𝐶𝑂32− + H + → 𝐻𝐶𝑂3−
(c) 𝐻𝐶𝑂3− + H + → CO 2 + H 2 O

Titration of the water sample against a standardized acid to Ph end point marks
the completion of reactions (a) and (b) only. The amount of acid used thus
corresponds to OH − and one-half of the normal 𝐶𝑂32− present.
3

On the other hand, titration of the water sample against a standardised acid to MO
end point marks the completion of reactions (a), (b) and (c). Hence,
the amount of acid used after the phenolphthalein end point corresponds to one - half
of normal carbonate plus all the bicarbonates while the total amount of acid used
represent the total alkalinity.
End point With Ph as indicator – pink to colourless

With MO as indicator – yellow to reddish

Procedure ▪ Pipette out 25mL of the water sample in a clean titration flask.
▪ Add 2 drops of phenolphthalein indicator and titrate against standardised HCl with
constant shaking until the pink colour just disappears.
▪ Note the burette reading, which corresponds to Ph end point (P).
▪ Then to the same solution, add 2-3 drops of methyl orange indicator and continue
titration until a colour change from yellow to raddish takes place.
▪ Note the burette reading as methyl orange end point (M).
▪ Repeat the procedure for the other samples

Observations

Volume of Burette reading / mL


P (in mL) = M (in mL) =
S.No. water sample
Initial (IR) Final (V1 ) Final (V2 ) V1 – IR V2 –IR
taken ( mL)

1 25

2 25

3 25

Calculations

Depending upon the P and M values, different cases of alkalinity due to individual ions are presented in the table below

CO 2− / ppm HCO −
/ ppm
S.No. Alkalinity −
OH / ppm 3 3

1 P=0 Nil Nil M

2 M=0 P Nil Nil

3 P =1/2 M Nil 2P or 2M Nil

4 P <1/2 M Nil 2P M-2P

5 P >1/2 M 2P-M 2(M-P) Nil


For the case, P < 1/2M so CO3 2− and HCO3− are present.

Note: Alkalinity has to be reported in terms of CaCO3

For HCO3 −

N 𝐻𝐶𝑂3− X V 𝐻𝐶𝑂3−= NHCl X VHCl


N HCO 3− x 25 = 0.1N X (M-2P)
3  50 1000 mg/L (≡ ppm)

Alkalinity due to HCO 3− ions = N 𝐻𝐶𝑂

For CO 32 −
N 𝐶𝑂32− V 𝐶𝑂32− = NHCl VHCl

N CO 32 − X 25 = 0.1N X 2P

Alkalinity due to 𝐶𝑂32−ions = N 𝐶𝑂32−x 50 x 1000 mg/L (≡ ppm)

Total alkalinity = Alkalinity due to HCO −


+ Alkalinity due to 𝐶𝑂32−
3

For the case, P >1/2 M so CO3 2− and OH − are present.



For OH

N OH − X V OH − = NHCl X VHCl N OH -

NOH − X 25 = 0.1N X (2P-M)

Alkalinity due to ions = N OH − x 50 x 1000 mg/L or ppm

The total alkalinity of given water sample is ….. mg/L.


Result

Precautions 1. Add only phenolphthalein indicator initially.


2. If no pink colour is generated with phenolphthalein, add methyl orange at the
start.
3. End point should be noted carefully since two indicators are used
simultaneously.
EXPERIMENT NO. 4

CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and
concentration of solution.

Object: To determine the viscosity of the given liquid at room temperature by Ostwald’s Viscometer.

Apparatus: Ostwald’s Viscometer, beaker, R.D. bottle, Stop watch

Theory: 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,
π𝑟4 Pt
η=
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 = ℎ𝑑𝑔
Where 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 = 𝜋𝑟4hd1gt1 × 8Vl
η 8Vl 𝜋𝑟4hd g t
2 2 2

η1 𝑑1 𝑡1
= ×
η2 𝑑2 𝑡2
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

Procedure:

1) Clean the Ostwald’s viscometer first with chromic acid and then wash thoroughly with distilled
water.
2) 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.
3) Clamp the viscometer in quite vertical position.
4) 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.
5) 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.
6) Take at least three reading for solvent .
7) Now clean the viscometer and dry it.
8) Repeat the whole procedure for the given solution.
9) The density of given solution can be calculated by R.D. bottle.

Observation Table:

Solvent Given Solution


S.No.
Flow time between Mean (t1) Flow time between Mean (t2)
C& D C& D
1.
2.
3.
4.

Room temperature =--------- 0 C


Density measurement of liquid:
Mass of empty R.D. bottle (w1 ) = ------------- gm
Mass of R.D. bottle with solvent(w2 ) = ------------- gm
Mass of R.D. bottle with solution (w3 ) =-------------- gm
Mass of solvent (w2 - w1 ) = --------------gm
Mass of solutions (w3 - w1 ) = --------------gm
Calculation:
Density of solvent at the room temperature = ------------ gm/cm3
The viscosity of solvent at the room temperature = ------------- poise

Mass of solution (w3 − w1)


Density of liquid (d 2) = × d1
Massofsolvent(w2 − w1 )

.
η1 𝑑1 𝑡1
= ×
η2 𝑑2 𝑡2
𝑑2 𝑡2
η2 = 𝑑 𝑡 × η1
1 1
Result: The viscosity of the given solution at the room temperature is ------------- poise.

Precautions:
1. The viscometer must be cleaned and dried properly before use.
2. The viscometer should be kept in a vertical position.
3. The flow time should be noted carefully.
Formation of air bubbles in the viscometer should be avoided.
EXPERIMENT NO.5
CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and
concentration of solution.

Object To determine the surface tension of the given liquid at room temperature by
stalagmometer.

Requirements Stalagmometer, Distilled Water, Unknown liquid, Clamp stand, Specific


gravity bottle etc.

Principle The surface tension of the given liquid is determined at the room temperature
by using stalagmometer. The numbers of drops for the same volume of distilled
water and the given liquid are counted and let these be as n 1 and n 2
respectively. Now if d 1 and d 2 are densities of water and given liquid at the
room temperature as determined separately by using specific gravity bottle,
then the surface-tension y 2 of the given liquid can be calculated by using the
simplified relationship as: ρ 1 / ρ 2 = n 2 /n 1 . d 1 /d 2
Stalagmometer: Stalagmometer is essentially a pipette with a capillary at the
lower end and a bulb in the middle. The end is flattened and grounded carefully so
that there is a large dropping surface. There are two marks A and B above and
below the bulb respectively. These marks define the volume to be delivered for
counting the drops.

The surface tension ‘y’ is the magnitude of ‘F’ of the force exerted parallel to the
surface of a liquid divided by the length ‘L’ of the line over which the force acts.

Procedure 1. Cleaned the stalagmometer and specific gravity bottle thoroughly first with
chromic acid solution and wash finally with distilled Water and then dry.

2. By immersing lower end in a beaker containing distilled water, suck up


water until it rises above the mark C.

3. Now allow the liquid drops to fall and count it.

4. Clean the stalagmometer and dry it. Fill it with liquid it rises above the upper
mark C and count the number of drops as before.

5. Clean and dry the specific gravity bottle and measure the density of liquid.
Observation-

Room Temperature = ------------ 0C.

Density of water at room temp. (d 1) = -------- gm/cm3

Surface tension of water at room temp. (y 1) = 72.14 dynes/cm

S. No. Water Given Liquid

No. of drops Mean (n1) No. of drops Mean (n2)

1.

2.

3.

Calculation :

Measurement of Density of Solution

1. Weight of empty specific gravity bottle = w1 gm


2. Weight of bottle + water = w2 gm
3. Weight of bottle + Some volume of liquid = w3 gm

Density of the given liquid (d 2) = (w3 – w1/ w2 – w1) X d 1

Also, ρ 1/ ρ 2 = n 2/n 1 . d 2/d 1.

ρ 2 = ρ 1 . n 1/n 2 . d 2/d 1.

Where ρ 1 = surface tension of water at room temperature.

Substituting the values of ρ 1, n 1, n 2, d 1 and d 2 the surface- tension of the given liquid at room
temperature thus becomes known.
Result: The surface tension of liquid at room temperature is -------------(dynes/cm).

Precautions: 1. The stalagmometerr and specific gravity bottle should be cleaned properly and
dried before use.

2. Fit the stalagmometer vertically.

3. The rate of the fall of drops should be adjusted in a way of having interval of
at last 2-3 seconds in successive drops. The number of drops per minute must be
in between 15-20.

4. The drops should fall from the tip of the stalagamometer under their own
weight rather than pushing them by force.

5. Wash and dry the stalagmometer after use.


EXPERIMENT NO. 6
CO3 Identify iron concentration and percentage of available chlorine in supplied sample
using titration methods.

Object To determine the iron (II) content in the supplied sample Mohr’s salt solution by
volumetric analysis against standard potassium dichromate solution using
potassium ferricyanide (K3[Fe(CN)6]) as an external indicator.

Requirements Standard potassium dichromate (K2Cr2O7) solution (N/20), potassium


ferricyanide indicator, Mohr’s salt solution, conical flask, glass rod, glazes tile

Principle Ferrous ions are the active constituents of the Mohr’s salt solution. Potassium
dichromate solution in acidic medium is a strong oxidizing agent which converts
ferrous ions into ferric ions. The end point can be determined by using potassium
ferricyanide as an external indicator.

After the reaction is completed, ferrous ions are completely oxidized to ferric
ions. As a result, when checked using an external indicator, no coloration will
be produced.

K2Cr2O7 + 4 H2SO4 → K2SO4 + Cr2 (SO4 )3 + 4 H2O+ 3O

{2 FeSO4 + H2SO4 + O → Fe2 (SO4 )3 + H2O} 3


K2Cr2O7 + 7 H2SO4 + 6 FeSO4 → K2SO4 + Cr2 (SO4 )3 + 3 Fe2 (SO4 )3 + 7 H2O
Reaction between external indicator and FeSO4

K3[Fe(CN)6 ] + 3FeSO 4 → Fe3[Fe(CN)6 ]2 + 3K2SO4


(yellow) Ferrous f erricyanide

End point No change in yellow colour of the indicator.

Procedure 1. 25 mL of the sample solution was pipetted out in a conical flask.


2. 10 drops of indicator (Potassium ferricyanide) was placed on a glazed tile.
3. The initial reading of the burette was noted down (upper meniscus of the
K2Cr2O7 solution).
4. The sample solution was titrated against K 2Cr2O7 solution. After the
addition of 5 drops K2Cr2O7 solution the reaction mixture was mixed well.
5. A drop from the reaction mixture was placed on the drop of indicator. The
blue colour developed.
6. Step 4 & 5 was repeated after adding……mL K2Cr2O7 solution the colour
of indicator remains yellow.
7. The procedure was repeated till concordant readings were obtained.

Results Ferrous content in the sample provided = .......... g/L


Precautions 4. All reagents should be freshly prepared.
5. The glass apparatus should be washed with chromic acid and then with
distilled water.
6. After every titration wash the conical flask with distilled water.
7. Potassium dichromate acts as an oxidizing agent in acidic medium
therefore add dilute H2SO4 in the Mohr’s salt solution.

Observations

Burette reading in mL
Volume of sample Volume of K2Cr2O7
S.No.
taken in mL Initial Final solution used in mL

1 25

2 25

3 25

Calculations N1 V1 = N2 V2

N1 × 10 = N2 V2

Strength of iron in sample solution = N1 × 56 g/L

4.
EXPERIMENT NO. 7

CO3 Identify iron concentration and percentage of available chlorine in supplied sample using titration methods

Object To determine the percentage of available chlorine in the given sample of bleaching
powder (Iodometrically)

Requirements Sodium Thiosulphate (hypo) solution, Potassium Iodide (KI), Bleaching powder,
glacial Acetic acid (CH3 COOH), (N/20) Starch solution (freshly prepared), Burette,
Pipette, Measuring cylinder, Titration flask.

Principle The available chlorine is the amount of chlorine liberated by the action of mineral
acids on bleaching powder. It is generally expressed in terms of % by mass of
bleaching powder.

Commercial bleaching powder is a mixture of calcium hypochlorite (CaOCl 2 ), basic


calcium chloride (CaCl2 .Ca(OH) 2 ) and some free calcium hydroxide. The active
part of the bleaching powder is calcium hypochlorite, responsible for disinfection
and bleaching action.

When a (dilute) mineral acid reacts with bleaching powder then free chlorine is
liberated.

CaOCl2 + 2CH3CO OH → Ca(CH 3 COO )2 + H2O+ Cl2


This liberated Cl2 reacts with KI to release free I 2 .
Cl2 + 2KI → 2KCl+ I2

I 2 + KI(excess)  [KI 3 ]
Free I2 liberated is titrated against a standard hypo solution using freshly prepared
starch solution as indicator.

I2 + 2 Na2S2O 3 → 2 NaI+ Na2S4O 6


Sodium tetrathionate

End point is detected with the help of starch indicator which makes a blue
colour complex with iodine.

I2 + starch → Adduct (starch – iodide complex)


End point Blue to colourless

Procedure • 25 mL of the sample solution was taken in a conical flask.


• Added 1 mL of KI solution and about half a test tube of acetic acid
(glacial) acetic acid.
• The liberated iodine was titrated against hypo solution till a light yellow
colour persist.
• Now 5 drops of freshly prepared starch solution is added, then a blue
colour appears.
• Now the solution is titrated against hypo till colour disappears.
• The titration is repeated to get concordant readings and noted down
the total volume of hypo used.

Observations

Strength of bleaching powder taken (w) = 5 g/L

Burette reading (mL) Volume of hypo


Volume of sample taken
S.No. solution
(mL) Initial Final consumed (mL)

1 25

2 25

3 25

Calculations

1g equivalent of available Chlorine ≈ 1g equivalent of hypo solution

N1 V1 = N2 V2

N1 × 25 = N2 V2
N1 = N2 V2 / 25

Amount of chlorine = N1 × 35.5 g/L

% available chlorine = (Amount of chlorine × 100)/w

Results

The available chlorine in the given sample of bleaching powder = %

Precautions

1. All reagents should be freshly prepared


2. The glass apparatus should be washed with chromic acid and then with distilled water
3. Same amount of starch indicator must be used in all titrations.
4. The end point of titration should be carefully observed.
EXPERIMENT NO. 8

CO1 Estimate different impurities present in water sample

Object To determine the chloride content in supplied water sample by Mohr’s method.

Requirements Burette, Pipette, Conical Flask, Beaker, Funnel AgNO 3 (N/100), Water
sample, Potassium chromate indicator.

Principle Mohr’s method is used to determine chloride content in water sample. In this
method a slightly alkaline solution is titrated against standard silver nitrate
solution using potassium chromate as an indicator. As the titration proceeds,
the chloride ions present react with AgNO 3 forming white precipitate of AgCl.
The extra drop of AgNO 3 reacts with indicator forming red silver chromate. The
change of colour from bright yellow to faint but distinct reddish brown colour
marks the end point.

NaCl + AgNO3 → AgCl + NaNO3

White ppt.

2AgNO3 + K2CrO4 → Ag2CrO4 + 2KNO3

Reddish brown

Reddish colour disappears if solution contains high concentration of chloride


ions.

Ag2CrO4 + 2Cl- → 2AgCl + CrO4 - -

In this method a slightly alkaline solution is used because in acidic medium


Ag2CrO4 gets dissolved where as in basic medium AgOH gets formed.

End point bright yellow colour to reddish brown colour

Procedure ▪ Filled the burette with AgNO3 Solution.


▪ Initial reading of the burette is noted down.
▪ 10mL of the water sample was pipetted out in a clean conical flask.
▪ Added 2 drops of potassium chromate indicator and titrated against standard
AgNO3 with constant shaking until a colour change from yellow to reddish
brown colour marks the end point.
▪ Noted the volume of the AgNO3 from the burette reading.
▪ Repeated the titration for concordant readings.
▪ Repeated the titration for blank correction.

Observations

Table for sample solution

Volume of water Burette reading / mL Volume of AgNO3


S.No.
sample taken / mL Initial Final V2 (mL)

1 10

2 10

3 10

Calculations

Chloride content determination :

N1 V1 = N2 V2

(Sample ) (AgNO3 )
N1 x 25 = N2 x V2

N1 = N2 x V2/ 10

So strength of chloride ions = N1 x 35.5 g/ L

= N1 x 35.5 x 1000 mg/ L

Result The chloride content in given water sample =….. mg/L.

Precautions 1. The apparatus should be washed with distilled water.


2. The reaction mixture should be properly shaken during titration.
3. End point should be noted carefully.
EXPERIMENT NO. 9
CO 2 Determine molecular properties such as surface tension, viscosity, pH, conductance and
concentration of solution

Object: Object: To verify Beer’s law using colorimetric method with KCNS as color
developing agent.

Reagents/Apparatus: Stock solution of Ammonium Fe(III) sulphate, KCNS, conc.HNO3,


distilled water, test tubes, beaker, pipette, burette, spectrophotometer etc.

Theory: Colorimetric method represents the simplest form of absorption analysis. It is based on the
change in intensity of color of a solution with variations in concentration. According to Lambert’s-Beer
law “The decrease in intensity of the incident light isproportional to the length of thickness
of the absorbing medium and the concentration of solution.”

log I0/I = A= εCl

I0 = intensity of light, I = intensity of transmitted light,

A = Absorbance, l = thickness of medium,

C = Concentration of the solution, and ε = molar absorption coefficient.

For a particular substance, ε and l are constants, therefore absorbance is directly


proportional to the concentration.

A α C

Now a graph is plotted between absorbance and different concentration of a number of


solutions of known iron concentrations. From this graph the concentration of iron in unknown
solution can be determined by drawing a perpendicular on X-axis with respect to its absorbance
shown on Y-axis.

Fe(III) reacts with thiocyanate to give intense red colored compounds, depending upon the
concentration of thiocyanate solution. Fe(II) does not give this reaction. At high concentrations
of thiocyanate, generally [Fe(SCN) 6]3-complex is formed, which increases the intensity and the
stability of color. So, in colorimetric method, a large excess of thiocyanate sh ould be used. Also,
strong acids(HCl or HNO3) should be used to prevent the hydrolysis of Fe(III) ions.

Fe(III) + nCNS- → [Fe(SCN)n]3-

Where n = 1,2…..... 6.
The maximum absorption of the complex lies at wavelength, max = 480nm.
Fe(II) does not give this reaction.

Procedure:

1. Take different volumes (between 0 to 2.5mL) of the stock solution of iron (III) provided
in six different test tubes. (As listed in table below)
2. Add 1mL conc.HNO3 and 0.5mL KCNS to each test tube.
3. Make the volume upto 10 mL by adding distilled water and mix properly.

Test tube No. 1 2 3 4 5 6

Fe(III)solution (mL) 0 0.5 1.0 1.5 2.0 2.5

Conc. HNO3 (mL) 1 1 1 1 1 1

KCNS (mL) 0.5 0.5 0.5 0.5 0.5 0.5

Distilled water (mL) 8.5 8.0 7.5 7.0 6.5 6.0

4. Make the separate test tube of unknown concentration of iron (III) in

the same manner.

5. Note the absorbance of all the solutions by spectrometer at 480 nm.

Observation Table: 1mL = 0.05 mg/L

Solution No. 1 2 3 4 5 6 unknown

concentration (mg/L) 0

Absorbance 0

Now a graph is plotted between absorbance and different concentration of a number of solutions
of known iron concentrations. From this graph the concentration of iron in unknown solution can
be determined by drawing a perpendicular on X-axis with respect to its absorbance shown on Y-
axis.
Absorbance

0 0.025 0.05 0.075 0.1 0.125 0.15


Concentration (mg/L)

Result: The concentration of iron (III) in the given sample is ....... mg/L.

Precautions:

1. Always use dilute solutions for obtaining calibration curve.


2. Cuvette should be cleaned and wiped properly.
3. Leave no finger marks on cuvette.
Experiment No. 10
CO 2 Determine molecular properties such as surface tension, viscosity, pH,
conductance and concentration of solution

Object To determine the strength of given solutions pH-metrically.

Requirements pH meter, glass electrode, stirrer, beaker, burette

Principle pH of a solution is defined as the negative logarithm of


hydrogen ion concentration

pH = - log[ H+ ]

When an alkali is added to an acid solution, pH of the solution increases slowly


but at the vicinity of equivalence point
the rate of change of pH is very rapid.
From the sharp change in the curve we
can find the Equivalence point which is
defined as the point at which the
amount of titrant added is just enough
to completely neutralise the analyte
solution. Hence, at equivalence point
the below chemical reaction occurs:
HCl + NaOH → NaCl + H2O

The equivalence point can be used to


determine the strength of solution that
is calculated by normality equation:

Nacid  Vacid = Nalkali  Valkali

Neutralization point pH = 7
Procedure

▪ The pH meter was calibrated against buffer solutions of known pH (4, 7 and
9.2).
▪ The glass electrode was washed with distilled water and dried.
▪ 25 mL of HCl solution was taken in a 100 mL beaker and pH of the solution
was noted.
▪ Now 0.5mL of given NaOH from the burette was added to the beaker, stirred
well and pH noted.

NaOH solution from the burette was added in installments till pH of solution
reached ~12.

▪ A graph was plotted between pH value (on Y-axis) and volume of NaOH
added (in mL) on x-axis. With the help of it, the volume of alkali used to
neutralize the given acid solution (at pH=7) was determined.
Observations

Volume of HCl taken = 25 mL

Vol. of NaOH added (mL)

pH
Calculations

For acid pH=-log[H] +

[H+]=1/antilog(pH)

[H+] mol/L which is equivalent to normality of acid(HCl)

For base

Nacid  Vacid = Nalkali  Valkali

Nalkali =Nacid x Vacid /Valkali

Strength of HCl solution = Nacid  36.5 g/L

Strength of NaOH solution = Nalkali x 40 g/L

Result The strength of given acid solution is ……… g/L

The strength of given basic solution is ........ g/L

Precautions
1. Temperature knob of pH meter should be adjusted to the room temperature.
2. After addition of acid, solution should be properly stirred
3. The pH should be first standardized by taking the buffer of a known pH
4. The activation of electrode should be done before 24 h.
EXPERIMENT NO.11
CO 2 Determine molecular properties such as surface tension, viscosity, pH, conductance and
concentration of solution

Object To determine cell constant and conductance of a solution.

Requirements KCl(solid),0.1N acetic acid solution,conductivity cell,conductometre, Wash


bottle 1 Thermometer .

Principle Measurement of conductance is one of the best ways for checking and monitoring
the purity of water. The conductance G is defined as the reciprocal of resistance
R, i.e., Resistance is measured in ohm (a) and conductance in siemens (S). The
conductivity meter in fact measures the conductance, and displays the reading
converted into conductivity.

Cell constant This is the ratio of the distance (d) between the electrodes to the
area (a) of the electrodes.

K = d/a K = cell constant (cm-1)

a = effective area of the electrodes (cm2)

d = distance between the electrodes (cm)

Conductance (G) is defined as the reciprocal of the electrical resistance (R) of a


solution between two electrodes. G = 1/R (S) The conductivity meter in fact
measures the conductance, and displays the reading converted into
conductivity.
Procedure:

Part 1 Determination of cell constant of the conductivity cell

1. Prepare 0.1NKCl by dissolving 0.745 g of it in 100mL of solution.

2.Rinse the conductivity cell and a beaker first with distilled water and then with a small

quantity of 0.1NKCl solution.

3. Place the conductivity cell(clamped vertical) in the beaker and fill it with sufficient

quantity of 0.1NKCl solution.

4. Standardize the conductometre using built in standard conductance.

5. Connect the terminals of the conductivity cell to the conductometre and determine the

conductance of the KCl solution,using this value obtain the cell constant of the

conductivity cell.

Calculation:

Conductance of 0.1N KCl solution =_ S

Specific Conductance of 0.1N KCl = S cm-1 (given


by examiner}

Cell Constant = Specific conductance = …… cm-1

Measured conductance

Part II Determine the strength of hydrochloric acid solutions by titrating it


against standard sodium hydroxide solution conductometrically.

Requirement: Conductometer, conductivity cell, beaker, burette, pipette, funnel, 0.1N NaOH, unknown
HCl solution, KCl solution.
Theory: Conductometric titration is the volumetric analysis based upon the measurement of the
conductance during the course of the titration. Conductance of an aqueous solution containing an
electrolyte depends upon the
• Number of free ions
• Charge on the free ions
• Mobility of the ions

When the solution of one electrolyte is added to another, a change in the conductance will result due to the
change in the number of free ions or substitution of ions.

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


Before NaOH solution is added from the burette, the acid solution has high conductivity due to highly mobile H+
ions. When NaOH is added to the acid, the highly mobile H+ ions are neutralized by combination with OH - ions to
form freely ionized water and hence are replaced by less mobile sodium ions.

HCl + NaOH → NaCl + H2O

Hence, the conductance of solution will decrease and continuous decreasing with the addition of NaOH until the
equivalence point is reached. On further addition of NaOH, the conductivity of the solution will increase due to
addition of Na+ ions and highly mobile OH- ions
If we plot the graph of conductance of the solution (along y axis) against the volume of alkali NaOH added (X -
axis), two straight lines intersecting at a point will be obtained (shown in below figure). This point of intersection
corresponds to the equivalence point since at this point (E in figure), there is no excess of either acid or base.

PROCEDURE:
1. Determine the cell constant as per the above procedure.
2. Rinse the conductivity cell with the solution whose conductivity is to be measured.
3. Take 20 ml of the given HCl solution in a 100ml beaker.
4. Wash the conductivity cell with distilled water and then rinse it with given HCl solution. Dip the cell
in the solution taken in the beaker.
5. Connect the conductivity cell to the conductometer.
6. Set the function switch to check position. Display must read 1.000. If it does not, set it with CAL
Control at the back panel.
7. Put the ‘Function Switch’ to ‘cell constant’ and set the value of cell constant determined in step 1 with
the help of knob.
8. Set the temperature control to the actual temperature of the solution under test.
9. Set the ‘Function Switch’ to ‘conductivity’ and read the display. Note the reading.
10. Take NaOH in the burette and add 0.5 ml of it into the beaker containing HCl. Stir and determine the
conductivity.
11. Repeat the procedure of addition of 0.5 ml of NaOH and noting down the conductivity in the
observation table. Take 12-15 reading in this way. After each addition, stir the solution gently.

Observation:

Volume of unknown solution V1 = 20.0 cm -1

S. No Volume of NaOH added (ml) Conductance C0(S)

1. 0.0

2. 0.5

3. 1.0

4. 1.5

5. 2.0

6. …

7 … And so on…

CALCULATIONS

1. Plot a graph between specific conductance (along y axis) and volume of NaOH added (along x axis)
2. The point of intersection will give the amount of alkali required for neutralization of the acid.
3. Suppose the volume of the alkali used = V2 ml
Applying normality equation

N1V1 (HCl) = N2V2 (NaOH)


N1 = (0.1 X V2)/20

Strength of HCl solution = Eq. weight X Normality


= 36.5 X N1 g/L

Result : 1) The Cell Constant of the given cell is …………cm-1

2) The strength of given HCl solution determined by conductometer.


ENGGCHEMISTRY
LAB VIVA
QUESTIONS
Standard laboratory devices for weight and volume measurement and Caliberation of Analytical Equipment.
CO 1 Estimate different impurities present in water sample.

CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and concentration of
solution.

CO3: Identify Iron concentration and percentage of available chlorine in supplied sample using titration methods .

Viva Questions

1. Define titration. Name the different types of titrations.


Ans. Titrimetry or titration is the quantitative analysis. In this analysis concentration of a solution is determined by allowing a
known volume of the given solution to react quantitatively with another suitable solution of known concentration. Different
types of titrations are:
i) Acid-base Titration ii) Redox Titration iii) Complexometric Tritration iv) Iodometric Titration

2. What is equivalent weight? Find the equivalent weight of K 2 Cr2 O7 and KMnO4 .
Ans. Equivalent weight is the mass of one equivalent that is the mass of a given substance which will
Combine with or displace a fixed quantity of another substance.
Equivalent weight = Molecular weight/ Valancy (No. of electrons gained or loose)
Mol. Wt. of K2 Cr2 O7 = (2×39)+(2×52)+(7×16)(2×39)+(2×52)+(7×16) = 294 g/mol
Number of electrons gained in acidic medium= 6
Now, putting these values in above formula of equivalent weight:
Equivalent weight=294/6 = 49g/eq
Mol. Wt. of KMnO4 = (1x39)+(1x55)+(4x16) = 158
In acidic medium, no. of electron gained = 5 (Oxdn no changes from Mn +7 to Mn+2 )
Now, putting these values in above formula of equivalent weight:
Equivalent weight = 158/5 = 31.61 g/eq

3. Define Indicator. Give examples of different types of Indicator.


Ans.The chemical substance which indicates the end point of a titration by changing its colour is called
indicator. Different types of indicators are: Methy Orange, Phenophthalein, Eriochrome black T,
Potassium ferricynide etc.

4. Define Normality. Also give its mathematical expression.


Ans. Normality of a solution is the number of gram equivalents of a solute dissolved in 1 litre of the
solution. Normaility = No. of gram equivalents/Vol of the solution in liters.

5. What is a standard solution? What are the differences between primary and secondary standards?
Ans.The solution of known concentration is called standard solution.
Primary Standard: Primary standard is a reagent that is very pure, representative of the number of moles and can be
easily weighed.
Seconday Standard: A secondary standard can’t be weighed accurately as they are hygroscopic andit is a chemical that has been
standardized against a primary standard for use in a specific analysis .

6. Why can’t we use NaOH as a primary standard?


NaOH is hygroscopic in nature. It absorbs moisture and carbon dioxide from the atmosphere,
therefore not suitable as a primary standard solution.

7. Why we need to calibrate analytical instruments?


We need to calibrate the analytical instruments as calibration helps in determining the accuracy and
Ensuring the consistency of measurements and limit errors and uncertainties.
HARDNESS BY Na 2(EDTA)
Viva Questions

CO 1 Estimate different impurities present in water sample.

1. Define the term "hardness" of water. What are the different units of hardness?

Ans. Hardness is the property of water which prevents the formation of lather or foam. The different units to express
hardness are parts per million (ppm), milligrams per liter (mg/L), French degree (°fH or °f) and Clark degree

2. Distinguish between temporary and permanent hardness. Identify the substances that cause.

Ans .Temporary hardness is mainly caused by the bicarbonates of calcium and magnesium [( Ca(HCO3)2 and Mg(HCO3)2
]where as Permanent hardness is due to presence of sulfates and chlorides of calcium and magnesium
[CaCl2, CaSO4, MgCl2, and MgSO4] in water. Temporary hardness can be removed easily by boiling it, but permanent
hardness can not be removed easily

3. What are the methods for removing temporary and permanent hardness of water ?

Ans. Temporary hardness in water can be easily removed by boiling while Zeolite process, Lime soda process and Calgon
Process and other method can be used to eliminate permanent hardness.

4. What are the drawbacks of hard water?

Ans. Hard water is unsuitable for washing because it is difficult to create a lather with soap. In boilers, hard water causes
caustic embrittlement, scale, and sludge formation.

5. What is the purpose of adding buffer solution to the titrating mixture?

Ans. Buffer solution is used in EDTA titration because it resists the change in pH. This is because all the reactions between
the metal ions and EDTA are pH dependent.

6. Why it is more convenient to express hardness in term of CaCO 3 ?

Ans. The hardness of water is expressed in terms of CaCO3 because the molecular weight of calcium carbonate is
100gm/mol so it is easy to calculate and it is the most insoluble salt obtained in water treatment.
7. Give the full name and structure of EDTA.
Ethylenediaminetetraacetic acid
Constituents and Alkalinity of Water Samples

Viva Questions

CO 1 Estimate different impurities present in water sample.

Q.1 What is alkalinity?

Ans. Alkalinity is the ability of water to neutralize the acid.

Q2. Which indicator(s) is used in this titration?

Ans. Phenolphthalein and Methyl orange

Q3. Why do we use different types of indicators in acid base titration?

Ans. Indicators are pH sensitive. In this titration phenolphthalein indicator have pH range of 8.0 -9.6 will give end p
when carbonate ions are neutralized to bicarbonate ions. While methyl orange having pH range of 3.1 -4.4 will give
end point when carbonate and bicarbonate are completely neutralized.

Q4. Name the chemical species which are responsible for alkalinity in water.

Ans. Carbonate, bicarbonate and hydroxide ions are responsible for alkalinity.

Q5. Why hydroxide and bicarbonate alkalinity cannot be present together?

Ans. OH - and 𝐻𝐶𝑂3− cannot exist together as they react to produce 𝐶𝑂32− ions

𝐻𝐶𝑂3− + OH − → 𝐻𝐶𝑂3− + H2O

Q6. What colour does phenolphthalein gives with hydroxides and carbonates in the solution?

Ans: Pink colour,

Q7. What colour does methyl orange gives with alkali and bicarbonates?

Ans: Yellow colour


Surface tension of Liquid

Viva Questions
CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and concentration of
solution.

Q.1 Define surface tension.

Ans.Surface tension is the magnitude of F of the force exerted parallel to the surface of a L liquid divided by the

length Lof the line over which the force acts.

Q.2 What is the unit of surface tension?

Ans N/m or dynes/cm

Q.3 What are the applications of surface tension?

Ans. Surface tension has a huge role in daily life, health and many industrial processes.

Industrial applications:

Surface tension is an important factor in industrial processes. In all the industrial plants the R&D departments use the
surface tension phenomena to improve the quality of the products. Many operations are used to improve the quality of
the product such as detergent formulations. By the use of detergent formulations, we can improve the cleaning properties
with more biological surfactants at a lower temperature.
Daily Life:.

a) Disinfectants are mainly the solution of low surface tension so that when we use them in the field they can float on
the water and spread out on the cells to destroy them.

b) Soaps and detergents also work on the basis of surface tension. They lower the surface tension of the water so that
the soaps and detergents easily soak into the pores and holes.

c) The water bubbles are round because the surface tension of water provides the tension to form the bubble with the
water and the surface tension minimizes the bubble into spherical shapes.
Q.4 What is the effect of temperature on surface tension?

As temperature increases, molecules of liquid become more active and they move more rapidly; therefore, the
intermolecular forces are more instable. Surface tension decreases with increasing temperature.
Q.5 Name the apparatus used to determine the surface tension of liquid.

Ans. Stalagmometer.

Q.6 What are the forces responsible for surface tension?

Ans. There are two types of forces – adhesive force and cohesive force. The intermolecular force which acts in between
the molecules is known as a cohesive force and when a liquid is in contact with a surface then there is an attraction
between molecules of the liquid and the surface, these forces are called adhesive forces.
Q.7 Write the equation to determine surface tension by liquid drop method.

y 1/ y 2 = n 2/n 1 . d 1/d 2

d 1 and d 2 are densities of water and given liquid at the room temperature

n 2 and n 1 are number of drops of water and given liquid


Viscosity of the given liquid by Ostwald’s Viscometer

Viva Questions

CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and concentration of
solution.

Q1. What do you understand by viscosity?

Ans. Viscosity is the resistance that one part of a liquid flowing with one velocity offers to another part of the
liquid flowing with different velocity.

Q2. How is viscosity related to temperature?

Ans.The viscosity of a liquid decreases with increase of temperature.

Q3. What is the significance of viscosity.

Ans.Viscosity measurements are useful in predicting the behaviour of lubricants and oils in hot and cold
conditions and it is also used for determination of molar masses of polymer.

Q4. What is Poiseuille ’s equation?.

π𝑟4 Pt
η=
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.

Q5. What are the units of viscosity?

Ans. dynes cm -2 s or Pascal sec or Poise

Q6. Write the name of the apparatus required for viscosity measurement.
Ostwald Viscometre

Q7. What is the effect of pressure on viscosity of a liquid?

Ans.The viscosity of liquid increases with increase in pressure.


Ferrous Content in Water Sample

(External Indicator method)

Viva Questions

CO3: Identify Iron concentration and percentage of available chlorine in supplied sample using titration
methods.

1. What is the formula of F.A.S.?

A: Ferrous Ammonium Sulphate = FeSO4(NH4)2SO4.6H2O

2. Why sulphuric acid is added while preparing standard F.A.S.?

A: Ferrous sulphate reacts with water and undergo hydrolysis to form ferrous hydroxide. The reaction is as

follows:

FeSO4 + 2H2O → Fe(OH)2 + H2SO4

Dilute sulphuric acid is therefore added to prevent the hydrolysis of ferrous sulphate.

3. What is the equivalent weight of F.A.S.?

A: The equivalent weight of F.A.S will be equal to its molecular weight = 392.13 g/mol.

4. Why Mohr’s salt is considered a primary standard?

A: Mohr’s salt is considered a primary standard because Mohr’s salt is stable, pure and is of low cost. It is

available and highly soluble in water. It is not hygroscopic or deliquescent.

5. What is the oxidation state of Cr in K 2Cr2O7?

A: Oxidation state of Cr in K 2Cr2O7 is +6.


6. What is the oxidation state of Fe in K 4 [Fe (CN)6]?

A: The oxidation state of Fe in K 4 [Fe (CN)6] is +2.

7. Why you are using potassium Ferricyanide indicator externally?

A: If we use indicator internally in this experiment, that is if we add potassium ferricyanide directly into the

ferrous ion solution (Mohr’s salt solution) in the conical flask, the entire solution will change into blue colour

(whose colour will not change) . There will be no ferrous ion left in solution to be oxidized with dichromate

during titration and there will be no change in colour at the end point due to which the end point would not

be detected.
Available Cl2 in Bleaching Powder

Viva Questions

CO3 Identify iron concentration and percentage of available chlorine in supplied sample using titration
methods.

Q 1. What do you understand by available chlorine? Write equation.

Ans. The available chlorine is the amount of chlorine liberated by the action of mineral acids on bleaching powder. It is
generally expressed in terms of % by mass of bleaching powder.

CaOCl 2 + 2CH3 COOH → Ca(CH 3 CO O)2 + H2O+ Cl2

Q 2. Which indicator is used for the titration?

Ans. Starch solution

Q 3. What is hypo solution? Write its reaction with iodine.

Ans. Hypo is Sodium Thiosulphate.

I2 + 2 Na2S2 O3 → 2 NaI+ Na2S4O 6

Q 4. What is function of KI in the experiment?

Ans. KI is used as a source of iodine . It reacts with available chlorine to liberate iodine gas.

Q 5. What is the importance to measure the available chlorine?

Ans. To check the commercial value of bleaching powder, as it depends on the percentage of av ailable Chlorine.

More the percentage of Available chlorine,better the disinfectant and bleaching action ogf bleaching powder.

Q 6. What is the reason for the appearance of blue colour when starch is added to iodine solution?

Ans It is due to the formation of starch iodine complex

Q 7. Why always freshly prepared starch should be used in the titration?

Ans. It is because starch becomes hydrolyzed to produce monosaccharides.


Chloride Ion Determination by Mohr’s Method

Viva Questions

CO 1 Estimate different impurities present in water sample

Q.1 Why we prepare fresh silver nitrate solution?

Ans. The chemical silver nitrate has a high reactivity. It hydrolyzes when exposed to light, producing silver oxide, a

brownish black material, and nitric acid. As a result, we always make fresh silver nitrate.

Q.2 WhyAgNO3 solution is kept in brown bottle.

Ans. Silver nitrate is a chemical with a strong reactivity. When exposed to light, it hydrolyzes to produce silver oxide, a
brownish black substance, and nitric acid. This implies that silver nitrate is light-sensitive. Brown bottles inhibit the

passage of light through it.

Q.3 How you detect the endpoint in this titration?

Ans. When reddish brown precipitate of Silver Chromate is formed, end point obtained.

Q.4 Which indicator is used in this titration?

Potassium chromate indicator K2 CrO4

Q.5 Why is necessary to maintain the pH near 7-8?

Ans. Because in an acidic medium, Ag2CrO4 dissolves, whereas in a basic medium, AgOH forms. That is why we keep t

pH between 7-8.

Q.6 What is the significance of Cl- ion determination?


Ans. One of the most common inorganic anions in water and wastewater is chloride (Cl -) ion. The salty taste produced by

chloride concentration in potable water is variable and depends on the chemical composition of the water. Furthermore, high

chloride levels can harm metallic pipes and structures, as well as growing plants. The chloride ions measured can be used to

determine the salinity of various water sources.

Q.7 Which method is used in this titration?


Ans. Mohr’s method.
COLORIMETER

Viva Questions

CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and conce ntration
of solution.

Q1. Define Beer-Lambert’s law.

A1. Beer-Lambert’s law states that the decrease in intensity of the incident light is proportional to the length of
thickness of the absorbing medium and the concentration of solution.”

log I0 / I = A= ε C l

I0 = intensity of light I = intensity of transmitted light,


A = Absorbance l = thickness of medium,
C = Concentration of the solution ε = molar absorption coefficient.

Q2. What do you understand by colorimetry?

A2. Colorimetric method represents the simplest form of absorption analysis. It is based on the change in intensity of
color of a solution with variations in concentration.

Q3. Give the reaction involved in the blood red coloured complex formation?

A3. Fe(III) + nCNS- → [Fe(SCN)n] 3-

where n = 1,2… 6.

Q4. What is transmittance?

A4. Transmittance is defined as the ratio of the light passing through to the light incident on the sample.
Q5. How is a filter selected in a colorimeter?

A5. Filter in the colorimeter is used to select the color of light which the solute absorbs the most to maximize the
accuracy of the experiment.

Q6. What is the calibration curve?

A6. Calibration curve is a general method to determine the concentration of a substance in an unknown sample by
comparing it to a set of standard samples with known concentration.

Q7. Define λmax and give the wavelength at which measurements are carried out?

A7. It refers to the wavelength along the absorption spectrum at which a substance shows its strongest absorption.
pH metric titration

Viva Questions

CO2 Determine molecular properties such as surface tension, viscosity, pH, conductance and concentration of
solution.

Q1. Define pH.

A1. pH is the measure of the hydrogen ion concentration in solution and is also referred to as the degree of acidity
or alkalinity. It is the negative logarithm of hydrogen ion concentration given by:

pH = - log[ H+ ]

Q2. What is pH of pure water?

A2. Pure water has a pH of 7.

Q3. Define reference electrode?

A3. Reference electrode is the electrode that has a stable and well-defined electrochemical potential against which
the potential of other electrodes in the system can be controlled and measured.

Q4. What is the effect of temperature on pH?

A4. An increase in temperature of the water decreases the pH level.

Q5. What do you understand by buffer solution?

A5. Buffer solutions are those solutions that resist a change in pH upon dilution or upon the addition of small amounts
of acid/alkali to them.

Q6. Which electrodes are used in pH-metric titration?

A6. A pH meter consists of two electrodes: a glass electrode and a reference electrode.
Q7. What is the effect of dilution on pH of an acidic solution?

A7. The dilution of an acidic solution with water decreases the concentration of H+ and hence the pH of solution
increases.
Cell Constant and Conductance of Solution

Viva Questions

CO2: Determine molecular properties such as surface tension, viscosity, pH, conductance and concentration
of solution.

Q.1 Define the term conductance.


A: The reciprocal of electrical resistance is called the conductance. It is usually represented by C . C = 1/R
Q.2.What is the effect of temperature on conductivity of electrolytic solution?
A: Electrolytic conductivity increases with increase in temperature because as the temperature increases, ionization
increases due to which movement of ions increases, hence the conductivity.
Q.3 Define cell constant.
A: Cell constant for a given cell is defined as ratio of the distance between the electrodes and the cross sectional
area of the electrodes. Cell constant = l/a . The unit of cell constant = /cm.
Cell constant = Specific conductance / Measured conductance
Q.4 Write the unit of conductance.
A: The unit of conductance is siemens (S) or reciprocal Ohm
Q.5 What is the difference between metallic conduction and Electrolytic conduction?
A:
Metallic conduction Electrolytic conduction

1. Flow of electricity takes place 1. Flow of electricity takes place


without the decomposition of the accompanied by the decomposition of
substance. the substance (electrolyte).

2. Flow of electricity is due to the flow 2. Flow of electricity is due to the


of electrons only. movement of ions.

3. There is no flow of matter. 3. There is flow of matter.

Q.6. Define Specific conductance?


A: Specific conductance is also called conductivity which is defined as the ability of a substance to conduct
electricity. It is the reciprocal of specific resistance or resistivity. The unit is siemens per meter.
Q.7. What is the effect of dilution on conductance?
A: Conductance of solution decreases on dilution as the number of ions per unit volume decreases on dilution.
Bakelite and Urea Formaldehyde Preparation

Viva Questions

Q.1What are thermosetting polymers?

Ans.Polymer which do not soften on heating are thermosetting polymer.e.g Bakelite

Q.2 What are thermoplastic polymers?

Ans.Polymer which soften on heating are thermoplastic polymer.e.g Polythene

Q.3 Write the monomers of Bakelite and Urea.

Ans. Phenol and formaldehyde

Q.4 Write few uses of Bakelite and Urea Formaldehyde resin.

Ans.Bakelite is used to make switches,switch board,television and automobile parts.

UF Resin is used to make moulded articles like vaccum flask cup,bottles cap.It is also used as adhesives,electrical
switches etc.

Q.5 What is the difference between additional and condensation polymers

Ans.Addition polymers are those polymer in which self addition of the monomer molecules toeach other,without
loss of any material.

Condensation polymers are those polymers in which monomers containing two or more reactive functional groups
with the elimination of small molecules like H2O,HCl.

Q.6 Why can not thermosetting resins be reused and reshaped?

Ans .Thermosetting polymers are crosslinked polymers and bonded by strong covalent bond and so that they cant
be reused andv reshaped.

Q.7 Bakelite is an example of thermoplastic polymer.(T/F)

Ans False

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