Sathyabama Institute of Science and Technology 1

Department of Chemistry

SCHOOL OF SCIENCE & HUMANITIES

DEPARTMENT OF CHEMISTRY

CHEMISTRY LAB MANUAL

I Semester and II Semester B.E. / B.Tech
(Common to All Branches of Engineering and Technology)

COURSE NAME: CHEMISTRY LAB

COURSE CODE: SCYB 2101

Name :

Year : Branch and Section:

Roll No. :

Reg. No. :

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Department of Chemistry

GENERAL INSTRUCTIONS
• 100% attendance is compulsory for all the laboratory classes.

• Students must bring their lab coat, lab manual, observation book and record note book for
their chemistry practical classes.

• Students should maintain their observation note book and record note book neatly.

• Students should write the date, name of the expt., diagram, tabulation, procedure, etc. in
their observation note book before entering the lab.

• Students should write the completed experiment in the record note book only after getting it
corrected in the observation note.

• In the record, LHS should be used for diagrams, tabular column, calculation and model
graph (if any) and RHS should be used for writing aim, formula, apparatus required,
procedure and the result.

• Diagrams, tabular column and graph should be drawn with pencil and procedure in blue /
black ink and students should paste the graph along with the corresponding experiments
neatly.

• Students who are late for the practical class will not be allowed to do their experiment.

• A place and number will be allotted to each student. Students have to follow this seat
number for regular practical classes for the whole semester.

• Do not place any glass apparatus on the working table. They should be kept only in the
plastic tray. Do not keep the glass ware at the edge or corner of the table so that breakage
of glass ware can be avoided. Always keep your place neat, clean and dry.

• Numbered solution bottles are kept on the side tables in the lab. Students should take the
bottles according to their seat number (for some solutions need not follow the seat number,
consult with staff for more information). After the completion of experiment, these bottles
should be replaced in the same place.

• Each concordant reading should be attested by the staff members before proceeding to the
next part of the experiment. Without getting the readings attested, students should not
proceed with the experiment.

• Students should wash all the glass wares after completing the experiment and should be
replaced in the plastic tray.

• The instruments kept in the lab are already calibrated. These instruments should not be
disturbed or tampered. All the instruments and electrodes should be handled carefully.

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• Any breakage or damage to glass ware or equipment should be informed to the staff
members (do not touch or clean the broken glass wares) immediately. Students should sign
in the breakage register and the breakage amount will be collected.

• Materials like filter paper, glass beads etc. should not be thrown in the sink after their usage.

• Students are requested not to leave the lab without the permission of the staff in-charge.

• Your place will be checked by the assistants for cleanliness and for the replacement of the
glass ware. Students have to leave the lab only after the period gets over.

Digital Conductivity Meter Digital Potentiometer

Digital pH Meter Digital Photocolorimeter

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INDEX

Ex. No. Name of the Experiment Page No.

1. Estimation of Mixture of Acids by Conductometry 5

2. Estimation of Ferrous Ion by Potentiometry 9

3. Determination of pKa Value of Glycine by pH Metry 13

4. Estimation of Iron by Photocolorimetry 17

5. Estimation of Hardness of Water by EDTA method 20

6. Estimation of Copper in Brass 23

7. Determination of Alkalinity of Water 27

8. Determination of High Molecular Weight of a Polymer by 31

Using Ostwald Viscometer

Short Procedure 34

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Ex. No. 1
Date:

ESTIMATION OF MIXTURE OF ACIDS BY CONDUCTOMETRY

AIM:

To estimate the amount of acids present in the whole of the given solution. You are provided
with standard 0.2 N sodium hydroxide solution.

PRINCIPLE:

Initial conductance of acid mixture is due to the presence of fast moving H+ ions. Upon titration
with NaOH, the fast moving H+ ions are replaced by slow moving Na+ ions. This results in
decrease of conductance till the entire HCl is neutralized.

H + Cl − + Na + OH − → NaCl + H 2O

Further addition of NaOH increases the conductance value due to the formation of sodium
acetate.

CH 3COO − H + + Na + OH − → CH 3COONa + H 2 O

After the complete neutralization of acetic acid, any further addition of NaOH increases the
conductance value rapidly.

A plot between volumes of NaOH added versus the conductance of the solution will give two
intersection points. The first point corresponds to the titration between strong acid vs strong base.
The second point corresponds to the titration between weak acid vs strong base.

APPARATUS & REAGENTS:

Conductivity meter, beaker, burette, pipette, glass rod, sodium hydroxide, hydrochloric acid etc.

PROCEDURE:

Makeup the given acid solution into a clean 100 ml standard flask with distilled water. Pipette
out 20 ml of the made up acid solution into a clean 100 ml beaker. Pipette out 20ml of distilled
water into the beaker. Rinse the conductivity cell thoroughly with distilled water and immerse
into the beaker. Stir the solution gently and carefully with a glass rod. Measure the initial
conductance of acid solution.

Now add 1 ml of NaOH from the burette. Stir the solution carefully with the glass rod and note
the conductance.

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Continue the titration by adding NaOH (in an aliquot of 1 ml) from the burette. When we add
NaOH the conductance initially decreases to certain volume of NaOH. After that, the
conductance starts increasing slightly for the addition of NaOH. After a particular volume the
conductance increases rapidly. Plot a graph between the conductance values and volume of
NaOH added as shown in the model graph. The first point of intersection of the two lines in the
graph gives the first end point of the titration. Consider this value as V1. Consider the second
point of intersection of the two lines in the graph as V3. V3―V1 gives the second end point of the
titration.

RESULT:

1. Amount of HCl present in the whole of the given solution = ………… g

2. Amount of CH3COOH present in the whole of the given solution = ………… g

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OBSERVATION:

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

1 1
2 2
3 3
4 4
5 5
6 6
7 7
8 8
9 9
10 10
11 11
12 12
13 13
14 14
15 15
16 16
17 17
18 18
19 19
20 20
21 21
22 22
23 23
24 24
25 25
26 26
27 27
28 28
29 29
30 30

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MODEL GRAPH:

CALCULATION

1. Volume of NaOH (V1) = ml

Normality of NaOH (N1) = 0.2 N
Volume of Mixture of acids (V2) = 20 ml
V1  0.2
Normality of HCl = [V1 - Refer graph]
20
The amount of HCl present in one litre = Normality of HCl  Equivalent weight of HCl (36.5)

The amount of HCl present in the whole of the given solution

Normality of HCl  36.5 100
= grams
1000

2. Volume of NaOH (V4) = (V3-V1) ml

Normality of NaOH (N1) = 0.2 N
Volume of mixture of acids (V2) = 20 ml
(V3 − V1 )  0.2
Normality of CH 3 COOH = [V1 and V3 - Refer graph]
20
The amount of CH 3 COOH present in one litre
= Normality of CH 3COOH  Equivalent weight of CH 3COOH (60)
The amount of CH 3 COOH present in the whole of the given solution
Normality of CH 3 COOH  60  100
= grams
1000

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Department of Chemistry

Ex. No. 2
Date:

ESTIMATION OF FERROUS ION BY POTENTIOMETRY

AIM:

To estimate the amount of ferrous ions present in the whole of the given solution. You are
provided with s standard 0.1 N potassium dichromate solution.

PRINCIPLE:

For a ferrous – ferric system: Fe2+  Fe3+ + e −

The electrode potential is determined by combining platinum electrode immersed in F2+ - Fe3+
system with saturated calomel electrode to form a cell and it is measured as emf. The cell is
represented by:
Hg / Hg 2Cl2 , KCl (satd ) // Fe3+ , Fe2+ / Pt

and Ecell is given by:

Ecell = ER.H.S _ EL.H.S
by applying the Nernst equation,

 o 0.0591 Fe3+ 
Ecell =  EFe 3+
/ Fe 2+
+ log  − 0.2422
 n Fe2 + 
o
Where E is the emf of the electrode, E Fe 3+
/ Fe2+
is the standard electrode potential for ferrous-
ferric system, n is the number of electrons involved in the reaction, F is the Faraday’s constant, R
is the gas constant and T is the temperature.

Ferrous ions are oxidized to ferric ions by adding potassium dichromate which simultaneously
increases the emf of the cell with a sharp increase in the emf. at the end point which is due to
complete conversion of ferrous to ferric ions.

APPARATUS & REAGENTS:

Potentiometer, standard calomel electrode, platinum electrode (indicator electrode), beaker,

burette, pipette, glass rod, standard flask, potassium dichromate, ferrous solution and sulphuric
acid

PROCEDURE:

Transfer the given ferrous ion solution into a clean 100 ml standard flask. Make up the solution
with distilled water. Pipette out 20 ml of the made up solution into a 100 ml beaker and add 20

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ml of dil. H2SO4. Immerse the platinum and calomel electrodes in the solution and connect them
to the potentiometer.
Stir the solution and note the initial constant emf of the solution. Then add 0.5 ml aliquots of
K2Cr2O7 solution from the burette and note the emf. Initially the difference in emf will be small
followed by a large difference in the emf values near the end point. After the end point again the
difference in emf values will be small. By calculating ∆E, ∆V and ∆E / ∆V, a graph is plotted by
taking volume of K2Cr2O7 solution (V) on the X-axis and ∆E / ∆V on the Y-axis. From the
graph, the volume of K2Cr2O7 solution consumed is determined.

RESULT:

Amount of ferrous ion present in the whole of the given solution = ________ g.

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OBSERVAION:

Volume of Observed emf, ∆E / ∆V

S. No. ∆E ∆V
K2Cr2O7, V (ml) E (mV) (mV/ml)
1 0
2 0.5
3 1
4 1.5
5 2
6 2.5
7 3
8 3.5
9 4
10 4.5
11 5
12 5.5
13 6
14 6.5
15 7
16 7.5
17 8
18 8.5
19 9
20 9.5
21 10
22 10.5
23 11
24 11.5
25 12
26 12.5
27 13
28 13.5
29 14
30 14.5
31 15

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MODEL GRAPH:

CALCULATION

V1  0.1
Normality of Fe 2+ ion solution = [V1 - Refer graph]
20

The amount of Fe 2+ ion present in one litre

= Normality of Fe 2+ ion  Equivalent weight of Fe 2+ ion (55.85)

The amount of Fe 2+ ion present in the whole of the given solution

Normality of Fe 2+ ion  55.85 100
= grams
1000

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Ex. No. 3
Date:

DETERMINATION OF pKa VALUE OF GLYCINE BY pH METRY

AIM:

To determine the titration curve of the given amino acid, glycine and to use this curve to estimate
its pKa values.

PRINCIPLE:

Amino acids have the general formula NH2-CHR-COOH. They can act as both acids and bases.
In water, most amino acids exist as zwitter ions, i.e., a dipolar ion. Thus, they are amphoteric
molecules that can be titrated with both acid and alkali. Glycine, the simplest amino acid, has
one acid and one amine group and is diprotic in nature. Isoelectric point, pI, is the pH of an
amino acid at which the net charge on the molecule is zero. When such an amino acid is titrated
against a base, it acts as an acid, and with an acid, it acts as a base.

The pH of such a weak acid or base can be calculated from the Henderson-Hasselbalch equation

[basic species]
pH = pK a + log
[acidic species]

APPARATUS AND REAGENTS:

0.1 N glycine, 0.1 N HCl, 0.1 N NaOH, pH meter, pH glass electrode, burettes, beaker and buffer
solutions (4, 7 and 9) for calibrating pH meter.

PROCEDURE:

TITRATION I: Glycine vs HCl

10 ml of the given 0.1 N amino acid, glycine is pipetted out into a clean 100 ml beaker followed
by the addition of 20 ml of distilled water. A pH glass electrode is rinsed in de-ionized water and
immersed in the glycine solution. The pH of the mixture is recorded using a calibrated pH meter.
A clean burette is taken and filled with 0.1 N HCl.

Initially, 1 ml of HCl is added to the mixture. The solution is stirred well using a glass rod and
the change in pH is recorded. The acid is added in increments of 1 ml until the pH falls to 3.
Between pH 3 and 2, HCl is added in increments of 0.5 mL. Beyond pH 2, HCl is added in
increments of 1 ml until the pH reaches 1.5. The readings are recorded in a tabular column as
shown in Table 1.

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TITRATION II: Glycine vs NaOH

10 ml of the given 0.1 N amino acid, glycine is pipetted out into a clean 100 mL beaker followed
by the addition of 20 mL of distilled water. A pH glass electrode is rinsed in de-ionized water
and immersed in the glycine solution. The pH of the mixture is recorded using a calibrated pH
meter. A clean burette is taken and filled with 0.1 N NaOH.

Initially, 1 ml of NaOH is added to the mixture. The solution is stirred well using a glass rod and
the change in pH is recorded. The base is added in increments of 1 mL until the pH increases to
9. Between pH 9 and 10, NaOH is added in increments of 0.5 mL. Beyond pH 10, NaOH is
added in increments of 1 mL until the pH reaches 11.5. The readings are recorded in a tabular
column as shown in Table 2.

The titration curve is plotted with Volume of HCl and NaOH on the x axis and pH on the y axis.
The two plateaus on the curve obtained is noted where despite the addition of the acid or base,
the pH of the solution does not vary significantly. The pKa values of glycine are estimated from
the graph. These values are then compared with that reported in literature.

RESULT: The two pKa values of glycine are ________ and __________.

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OBSERVATION:

TABLE 1: Glycine vs. HCl TABLE 2: Glycine Vs. NaOH

Sl. Volume of Sl. Volume of Observed
Observed pH
No. 0.1 N HCl No. 0.1 N NaOH pH
1 1 1 1
2 2 2 2
3 3 3 3
4 4 4 4
5 5 5 5
6 6 6 6
7 7 7 7
8 8 8 8
9 9 9 9
10 10 10 10
11 11 11 11
12 12 12 12
13 13 13 13
14 14 14 14
15 15 15 15
16 16 16 16
17 17 17 17
18 18 18 18
19 19 19 19
20 20 20 20
21 21 21 21
22 22 22 22
23 23 23 23
24 24 24 24
25 25 25 25
26 26 26 26
27 27 27 27
28 28 28 28
26 26 26 26
30 30 30 30

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MODEL GRAPH:

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Ex. No. 4
Date:

ESTIMATION OF IRON BY PHOTOCOLORIMETRY

AIM:

To estimate the amount of Fe3+ ion present in the given water sample using spectrophotometer.

PRINCIPLE:

When a monochromatic light passes through a homogeneous coloured solution, a portion of

incident light is reflected, a portion is absorbed and the remaining is transmitted.

I0 = Ir + Ia + It

Where
I0 = Intensity of light incident before entering the solution
Ir = Intensity of incident light reflected
Ia = Intensity of incident light absorbed
It = Intensity of incident light transmitted

Ir is usually eliminated and hence I0 = Ia + It. The mathematical statement of Lambert- Beer’s
Law is given by
T = I/I0 = 10– kcl

Where
T = Transmittance of solution
I = Intensity of light leaving the solution
I0 = Intensity of light incident on the solution
k = Molar absorption coefficient
c = Concentration of the solution in moles/ litre
l = Length (path thickness) of the absorbing solution

(or) A = log (I0/I) = k c l

where A is the absorbance or optical density of solution i.e when a ray of monochromatic light
passes through an absorbing medium, its density decreases exponentially as the concentration of
absorbing substance and the width or thickness increases independently. Keeping the path length
constant (say l = 1 cm), the variation is only due to concentration, c.

Fe3+ ion does not give any colour in solution. However, it develops a red colour when it reacts
with potassium thiocyanate solution.

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Fe3+ + 6KSCN → [Fe(SCN)6]3-+ 6K+

Red colour complex
Further, this colour is in the blue region, (λ=480 nm). Spectrophotometer has a wide range of
adaptability that allows selection of monochromatic light of any wavelength in the visible
spectrum.

INSTRUMENTATION:

The light source is an ordinary light bulb and monochromatic light is obtained by using either a
glass prism or a diffraction grating. The monochromatic light then passes through the filter and is
directed through a cell containing the sample. The incident light passes through the solution and
hits the photoelectric cell and the output of this can be seen in the display.

PROCEDURE:

Prepare a series of standard solution containing 2-10 ppm of iron by adding 1 ml of 1:1 HCl and
1 ml of 10% potassium thiocyanate solution. The red solution is made up to 100 ml in a standard
flask. Switch on the photocolorimeter and warm it up for about 10 minutes. Adjust the
monochromator at the wavelength λ = 480 nm. The blank is distilled water with the reagents
used for the experiment. Keep the blank solution in the cuvette and adjust the instrument to
transmittance corresponding to 100 or absorbance is zero. Similarly, place the various standard
concentrations of nickel solutions in the cuvette one by one and measure the corresponding
absorbance. Also, measure the absorbance of the unknown solution. Draw the calibration graph
to determine the concentration of the unknown solution.

RESULT:

Amount of iron present in the given solution = ______________ ppm.

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OBSEERVATION:

Wavelength, λ = 480 nm Distilled water (Blank) = zero absorbance

Sl. No. Concentration (ppm) Absorbance

1 Blank 0
2 2
3 4
4 6
5 8
6 10
7 Unknown

MODEL GRAPH:

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Ex. No. 5
Date:

ESTIMATION OF HARDNESS OF WATER BY EDTA METHOD

AIM:

To estimate the total hardness of the given sample of water by EDTA method

PRINCIPLE:

This estimation is based on complexometric titration. Ethylene diamine tetra acetic acid (EDTA)
forms stable complexes with calcium and magnesium ions present in the hard water.

The hard water is buffered to a pH of about 9-10 and Eriochrome black T indicator is added. The
indicator combines with some of Ca2+ and Mg2+ ions in the hard water to form an unstable
complex of wine red in colour.

When the EDTA is added, the free Ca2+and Mg2+ ions form complex with EDTA. These
complexes are more stable than the indicator metal ion complex. When all the hardness causing
ions are complexed by EDTA the indicator is set free which gives steel blue colour

APPARATUS & REAGENTS:

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Burette, pipette, Conical flask, EDTA, Standard hard water, NH4OH-NH4Cl buffer solution,
EBT indicator

PROCEDURE:

TITRATION I: Standardization of EDTA solution

Pipette out 20 ml of the standard hard water into a clean conical flask. Add about 5ml of (NH4Cl
+ NH4OH) buffer solution and a small quantity of Eriochrome Black T indicator. The solution
turns to wine red in colour. Titrate against EDTA solution taken in the burette until the solution
turns to steel blue colour. Repeat the titration for concordant values. Let V1 be the volume of
EDTA consumed by standard hard water.

TITRATION II: Estimation of total hardness of given water sample

Pipette out 20 ml of sample hard water into a clean conical flask. Add about 5 ml of (NH4Cl +
NH4OH) buffer solution and a small quantity of Eriochrome Black T indicator. The solution
turns to wine red in colour. Titrate against EDTA solution taken in the burette until the solution
turns to steel blue colour. Repeat the titration for concordant values. Let V2 be the volume of
EDTA consumed by the sample hard water.

RESULT: Total hardness of the given sample of water = ………… ppm (parts of CaCO3 per
million parts of water).

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OBSERVATION AND CALCULATION:

Titration I: Standardization of EDTA solution

Burette : EDTA solution
Pipette solution : 20 ml of std. hard water + 5ml buffer solution
Indicator : Eriochrome Black T
End point : Wine red to steel blue

Sl. No. Volume of Std. Burette Reading Volume of Concordant

hard water Initial Final EDTA Value

1 ml of standard hard water = 1 mg of CaCO3 equivalent hardness …..(1)

20 ml of standard hard water = 20 mg of CaCO3 equivalent hardness …..(2)
20 ml of standard hard water consumes = V1 ml of EDTA …..(3)
From equation (1) and (2):
V1 ml of EDTA = 20 mg of CaCO3 equivalent hardness
20
1 ml of EDTA = mg of CaCO3 equivalent hardness
V1

Titration II: Estimation of total hardness of water

Burette : Standardised EDTA solution
Pipette solution : 20ml water sample + 5ml buffer solution
Indicator : Eriochrome Black T
End point : Wine red to steel blue

S. No. Volume of Given Burette Reading Volume of Concordant

Water Sample Initial Final EDTA Value

20 ml of sample hard water consumes = V2 ml of EDTA

20 ml of sample hard water = V2 × 1 ml of EDTA
20
20 ml of sample hard water = V2  mg of CaCO3 equivalent hardness
V1
20 1000
1000 ml of sample hard water = V2   mg of CaCO3 equivalent hardness
V1 20
V
Total hardness of given water sample = 1000  2 ppm.
V1

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Ex. No. 6
Date:

ESTIMATION OF COPPER IN BRASS

AIM:

To estimate the percentage of copper present in the given ore. You are supplied with an
accurately 0.5 N potassium dichromate solution and an approximately 0.05 N sodium thio
sulphate solution.

PRINCIPLE:

The estimation is based on iodometry titration. In iodometry, a strong oxidizing agent such as
potassium dichromate is treated in neutral or acid solution with a large excess or iodide ions the
latter reacts as a reducing agent and the oxidant will be quantitatively reduced .in such cases an
equivalent amount of iodine is liberated and the titrated with a solution of a reducing agent,
which is usually sodium thiosulphate freshly prepared starch solution is used as an indicator
which given intense blue colour with iodine due to the formation of an adsorption complex. The
end point is the disappearance of the blue colour.

A solution of potassium dichromate acidified with dilute sulphuric acid is treated with excess of
10% KI solution. The liberated iodine is treated against sodium thiosulphate using starch
indicator until the blue colour disappears.

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

6KI +3H2SO4 +3[O] 3K2SO4 + 3H2O + 3I2
2Na2S2O3 + I2 2NaI + Na2S4O6

On adding potassium iodine to a finely ground ore dissolved in perchloric acid, copper reacts to
liberate iodine
2Cu2+ + 4 KI 4K+ + Cu2I2 + I2

The liberated Iodine is titrated against sodium thiosulphate using starch indicator. The
disappearance of blue colour is the end point.

PROCEDURE:

The given copper ion solution is made upto 100ml in a standard flask and is prepared in the
following manner.0.5gm of the ore is accurately weighed and dissolved in 15ml of 75%
perchloric acid in an iodine flask. The mixture is refluxed without allowing the various to escape.
The contents are cooled and 15ml of water is added and again boiled for 5 mintues. After cooling
1:1 ammonium hydroxide solution is added to precipitate ion hydroxide.

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TITRATION I: Standardization of sodium thiosulphate

Pipette out 20ml of standard potassium dichromate into clean conical flask. Add one test tube of
dilute sulphuric acid and 10ml of 10% KI solution. Titrate the liberated iodine immediately
against sodium thiosulphate taken in the burette. When the solution turns pale yellow, add 1ml of
starch indicator and continue the titration. The end point is the disappearance of blue colour.
Repeat the titration for concordant titre value and calculate the strength the sodium thiosulphate
solution.

TITRATION II: Estimation of copper

Pipette out 20ml of the made up copper solution into a clean conical flask. Add liquor ammonia
drop by drop until a deep blue precipitate is formed. Dissolve the precipitate with slight excess of
dilute acetic acid and add 10ml of 10% KI solution. Titrate the liberated iodine against sodium
thiosulphate taken in the burette. When the solution becomes straw yellow, add 1ml starch
indicator and continue the titration. The end point is the disappearance of blue color. Repeat the
titration for concordant titre value and calculate the strength of copper in the solution. From this,
the amount of copper is estimated.

RESULT:

The percentage of copper present in the given ore =_______%

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OBSERVATION AND CALCULATION:

TITRATION I: Standardization of sodium thiosulphate

Burette Solution : Sodium thiosulphate
Pipette solution : Std. potassium dichromate + 20ml dil.H2SO4 +10ml of 10% KI
Indicator : Starch
End Point : Disappearance of blue colour (Appearance of pale green colour)
Volume of Burette Reading Volume of Concordant
S. No.
K2Cr2O7 (ml) Initial Final thiosulphate (ml) value

Volume of potassium dichromate, V1 = ml

Normality of potassium dichromate, N1 = N
Volume of Sodium thiosulphate, V2 = ml
Normality of sodium thiosulphate, N2 = ?

V1N1 = V2N2

V1  N1
N2 =
V2

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TITRATION II: Estimation of copper

Burette Solution : Std. sodium thiosulphate
Pipette solution : 20ml of copper ion solution +10ml of 10% KI
Indicator : Starch
End Point : Disappearance of blue color (Appearance of white percipitate)
S. No Volume of Burette Reading Volume of Concordant
copper ion solution (ml) Initial Final thiosulphate (ml) value

CALCULATION:

Volume of sodium thiosulphate V1 = ml

Normality of sodium thiosulphate N1 = N
Volume of copper ion solution V2 = ml
Normality of copper ion solution N2 = ?
V1N1 = V2N2

V1  N1
N2 =
V2

The amount of copper present in one liter of the solution = Normality × 63.54
= x g/lit.

x  100
The amount of copper present in the whole of the given solution =
1000
=yg

y  100
The percentage of copper in the given ore =
0. 5

= ________%

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Ex. No. 7
Date:
DETERMINATION OF ALKALINITY OF WATER

AIM:

To determine the types and amount of alkalinity present in the given sample of water. You are
provided with a solution of Na2CO3 of strength 0.01N and a link solution of HCl solution are
provided.

PRINCIPLE:

Alkalinity in water is due to the presence of soluble hydroxides, bicarbonates and carbonates.
Determination of the various types and amounts of alkalinity is easily carried out by titration
with standard HCl employing the indicators like phenolphthalein and methyl orange
independently or successively.

1) OH- + H+ H2O Phenolphthalein

2) CO3 2- + H+ HCO3- Methyl orange
3) HCO3- +H+ H2O + CO2 end point
end point
The titration of water sample against a standard acid up to phenolphthalein end point shows the
completion of hydroxide alkalinity and one half of carbonate alkalinity present.

On the other hand titration of the sample against a standard acid using methyl orange end point
makes the completion of reactions 1 to 3. Total amount of the acid consumed is used to measure
the total alkalinity.

The possible combination of ions is OH- only,HCO3-only,CO3 2-only , OH- andCO3 2- together
and CO3 2-and HCO3- together.

OH- andHCO3-ions cannot exist together since both the ions combine instantaneously to form
CO3 2-.
OH- + HCO3- CO3 2- + H2O

Similarly CO3 2- , OH- and HCO3- cannot exist together.

PROCEDURE

TITRATION I: Standardization of HCl

Pipette out 20 ml of standard sodium carbonate solution into a clean conical flask. Add 3 drops
of methyl orange indicator. The solution turns yellow in colour. Titrate the solution against the
HCl solution taken in the burette. The end point is the colour change from yellow to pale pink.
Repeat the titration for concordant titre value.

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TITRATION II: Estimation of alkalinity of water sample

Pipette out exactly 20 ml of the given water sample into a conical flask. Add few drops of
phenolphthalein indicator and titrated against the standard hydrochloric acid taken in the burette.
The end point is the disappearance of pink colour (P ml). Into the same solution add few drops
of methyl orange indicator. The solution changes to yellow in colour. Continue the titration till
pale pink colour reappears by adding the same HCl without break (M ml). Titration is repeated
till you get concordant titre values.

RESULT:
The individual amounts of alkalinity in the water sample

(a) Hydroxide (OH-) alkalinity = ………………… ppm

(b) Carbonate (CO32-) alkalinity = ……………….. ppm
(c) Bicarbonate alkalinity (HCO3-) = ……………….. ppm
(d) Total Alkalinity = ……………….. ppm

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OBSERVATION AND CALCULATION:

TITRATION I: Standardization of HCl

Burette solution: HCl
Pipette solution: 20 ml of std. Na2CO3
Indicator: 2-3 drops of methyl orange
End point: Yellow to pale pink
Burette Reading (ml) Concordant
Volume of Volume of
S. No value (ml)
Na2CO3 (ml) Initial Final HCl (ml)

Volume of Na2CO3 solution (V1) = 20 ml

Normality of Na2CO3 solution (N1) = 0.01 N
Volume of HCl solution (V2) = ……………. ml
Normality of HCl solution (N2) = ?

V1 × N1 = V2 × N2

= ………………. N

TITRATION II: Estimation of alkalinity of water sample

Burette solution: HCl
Pipette solution: 20 ml of water sample
Indicator 1: 2-3 drops of phenolphthalein
End point 1: Disappearance of pale pink colour (Phenolphthalein End Point: P)
Indicator 2: 2-3 drops of methyl orange
End point 2: Reapperance of pale pink colour (Methyl orange End Point: M)
Volume of Concordant
Volume of Burette Std. HCl (ml) Value (ml)
S. No. water sample Reading (ml)
(ml)
Final
Initial [P] [M] [P] [M] [P] [M]

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(i) If P >1/2 M, Water sample contains OH-+ CO32- alkalinity.

OH − =
(2 P − M )  Normality of HCl  50  1000
20
= ------------------ppm

2(M − P )  Normality of HCl  50  1000

CO32− =
20
= ------------------ppm

(i) If P <1/2 M, Water sample contains CO32- + HCO3- alkalinity.

2 P  Normality of HCl  50  1000

CO32− =
20
= ------------------ppm

HCO3− =
(M − 2 P )  Normality of HCl  50  1000
20
= ------------------ ppm

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Ex. No. 8
Date:

DETERMINATION OF HIGH MOLECULAR WEIGHT OF A POLYMER BY USING

OSTWALD VISCOMETER

AIM:

To determine the average molecular weight of given polymer by U-tube viscometer method and
you are provided with a 2.5 wt% of polyvinyl alcohol solution.

PRINCIPLE:

The viscosity of a polymer solution is high compared to that of the pure solvent. The molecular
weight of a polymer is proportional to the intrinsic viscosity of its solution (ηi) when the polymer
molecular chain is extended to its full contour length. The value of intrinsic viscosity is
proportional to the square root of the molecular weight M, when the polymer is in a solvent.

The relationship between intrinsic viscosity and molecular weight is given by Mark-Kuhn-
Hownik’s empirical equation as,

where α is a measure of the shape of the polymer molecular chain (coiled or extended form) and
the value is usually from 0.5 to 0.8. The value of the constant K depends on the polymer and the
solvent involved.

For a liquid flowing through a capillary tube, the time required to pass through the capillary tube
is related to the absolute viscosity according to the equation:

where V is the volume of the liquid which pass through the capillary, r is the radius of the
capillary, l is the length of the capillary and P is the pressure head under which the liquid flow
takes place.

If η and ηo are the absolute viscosities of the polymer solution and the pure solvent respectively
and t and to are their corresponding flow times and if the same capillary tube is used. Therefore,
the relative viscosity of polymer solution is given by:

For each concentration, calculate the value of η/η0 and ηsp (specific viscosity)

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From the plot of ηsp/C vs concentration of the polymer, intrinsic viscosity can be calculated.

APPARATUS & REAGENTS:

Ostwald’s Viscometer, Stop Watch, 100ml Beaker, 25ml Standard Measuring Flask, 10ml
Graduated Pipette; 10ml Ordinary Pipette.

PROCEDURE:

25 ml of 0.25%, 0.5%, 0.75%, 1%, and 1.25% polymer solutions are prepared as follows. Pipette
out 2.5, 5, 7.5, 10, and 12.5 ml of 2.5% polymer solution in a 25 ml standard flask. Then make
up the polymer solution with distilled water and shake the solution thoroughly.

Wash the viscometer with distilled water and dry it. Fix the viscometer vertically in a stand.
Pipette out 10ml of the solvent into the lower bulb of the viscometer and suck the liquid carefully
into the upper bulb, so that the liquid level is above the mark. Allow the liquid to flow freely.
When the liquid level crosses the upper mark, start a stopwatch. When the liquid level crosses
the lower mark, stop the stopwatch. Repeat it for two times. The average value is the flow time
of water.

Similarly determine the flow time of given polymer solutions of different concentrations.
Tabulate the results.

From the flow time we can calculate the specific viscosity.

From the plot of ηsp/c versus concentration, the intrinsic viscosity (Y-intercept) ηi can be
determined. Using ηi, α and K values, the molecular weight of the polymer can be determined.

For polyvinyl alcohol-water system, the ‘α’ and ‘K’ values are 45.3×10‒5 dl/g and 0.64
respectively.

RESULT:

The molecular weight of the given polymer sample =

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OBSERVATION:

Concentration of
S. No. Time of flow (t) η/η0 = t/t0 ηsp = (t/t0)– 1 ηSP / c
the polymer solution, (c)
1. Distilled water (to)
2. 0.25%
3. 0.5%
4. 0.75%
5. 1.0%
6. 1.25%

MODEL GRAPH:

CALCULATION

 i = KM 

logi = log K +  log M

log i − log K
log M =


log i − log( 45.3  10 −5 )

log M = [ηi - Refer graph]
0.64

log i − (−3.3437)
log M =
0.64

 log i − (−3.3437) 
M = anti log of  
 0.64 

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SHORT
PROCEDURE

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Ex. No. 1: ESTIMATION OF MIXTURE OF ACIDS BY CONDUCTOMETRY

Aim: To estimate the amount of acids present in the whole of the given solution. You are
provided with standard 0.2 N sodium hydroxide solution.

Procedure:

Burette Solution : Standard NaOH

Pipette Solution : 20ml of made up HCl solution + 20ml of distilled water
End point : Obtained from graph

Model Table: Model Graph:

Volume of Conductance
NaOH (ml) (mMhos)

Equivalent weight of HCl = 36.5

Equivalent weight of CH3COOH = 60

Result:

1.
The amount of HCl present in the whole of the given solution
Normality of HCl  36.5 100
= grams
1000
2.
The amount of CH 3 COOH present in the whole of the given solution
Normality of CH 3 COOH  60  100
= grams
1000

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Ex. No. 2: ESTIMATION OF FERROUS ION BY POTENTIOMETRY

Aim: To estimate the amount of ferrous ions present in the whole of the given solution. You are
provided with s standard 0.1 N potassium dichromate solution.

Procedure:

Burette Solution : Standard K2Cr2O7

Pipette Solution : 20ml of made up ferrous solution + 20ml dil. H2SO4
End Point : Obtained from the graph

Model Table:
Model Graph:
Volume
of Observed
Sl. ∆E ∆V ∆E / ∆V
K2Cr2O7, emf, E
No (mV) (ml) (mV/ml)
V (ml) (mV)

ΔE/ΔV

Volume of K2Cr 2O7

Result:

Strength of Fe2+ solution (N2) = V1 (Obtained from graph)  0.1

20
Amount of Fe2+ ions present in 1000 ml of the = Normality of Fe2+ solution ×
solution (Y) Equivalent weight
= N2 × 55.85
2+
Amount of Fe ions present in 100 ml of the = Y
solution 10
= _________ g
Amount of Fe2+ present in the whole of the
given solution = _________g.

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Ex. No. 3: DETERMINATION OF pKa VALUE OF GLYCINE BY pH METRY

Aim: To determine the titration curve of the given amino acid, glycine and to use this curve to
estimate its pKa values.

Procedure:

Titration I: Glycine vs. HCl

Burette solution: 0.1N HCl
Pipette solution: 10 ml of 0.1 N glycine + 20 ml distilled water
pKa value obtained from the graph.

Titration II: Glycine vs. NaOH

Burette solution: 0.1N NaOH
Pipette solution: 10 ml of 0.1 N glycine + 20 ml distilled water
pKa value obtained from the graph.

Model Tables:

Glycine Vs HCl Glycine Vs NaOH

Volume of Observed Volume of Observed
S. No. S. No.
0.1 N HCl pH 0.1 N NaOH pH
1 0 1 0
2 1 2 1
3 2 3 2

Model Graph:

Result: The two pKa values of glycine are ________ and __________.

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Ex. No. 4: ESTIMATION OF IRON BY PHOTOCOLORIMETRY

Aim: To estimate the amount of Fe3+ ion present in the given water sample using
spectrophotometer.

Procedure:
Preparation of standard iron solutions: 2 ppm, 4 ppm, 6 ppm, 8 ppm and 10 ppm
Standard iron solution + 1 ml of 1:1 HCl + 1 ml of potassium thiocynate made up to 25 ml.

Model Table:

λ= 480 nm.
Distilled water Blank = zero absorbance

S.No Concentration Absorbance

1 2 ppm
2 4 ppm
3 6 ppm
4 8 ppm
5 10 ppm
6 Unknown

Model Graph:

Result: The amount of iron present in the given solution = ________ ppm.

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Ex. No. 5: ESTIMATION OF HARDNESS OF WATER BY EDTA METHOD

Aim: To estimate the total hardness of the given sample of water by EDTA method

Titration I: Standardization of EDTA solution

Burette : EDTA solution

Pipette solution : 20 ml of std. hard water + 5ml buffer solution
Indicator : Eriochrome Black T
End point : Colour change from wine red to steel blue

20
1 ml of EDTA = mg of CaCO3 equivalent hardness
V1

Titration II: Estimation of total hardness of water

Burette : Standardised EDTA solution

Pipette solution : 20ml water sample + 5ml buffer solution
Indicator : Eriochrome Black T
End point : Colour change from wine red to steel blue

V
Total hardness of given water sample = 1000  2 ppm.
V1
Result:

Total hardness of the given sample of water = ………… ppm (parts of CaCO3 per million parts
of water).

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Ex. No. 6: ESTIMATION OF COPPER IN BRASS

Aim: To estimate the percentage of copper in the given ore. You are provided with a standard
0.5 N potassium dichromate solution and an approximately 0.05 N sodium thio sulphate solution.

Procedure:

Titration I: Standardization of sodium thiosulphate

Burette Solution : Sodium thiosulphate
Pipette solution : Std. potassium dichromate + 20ml dil.H2SO4 +10ml of 10% KI
Indicator : Starch
End Point : Disappearance of blue colour (Appearance of pale green colour)

Titration II: Estimation of copper

Burette Solution : Std. Sodium thiosulphate
Pipette solution : Copper ion solution +10ml of 10% KI
Indicator : Starch
End Point : Disappearance of blue color (Appearance of creamy white precipitate)

Result:

The amount of copper present in one liter of the solution = Normality × 63.54
= x g/lit.
x  100
The amount of copper present in the whole of the given solution =
1000
=yg
y  100
The percentage of copper in the given ore =
0. 5

= ________%

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Ex. No. 7: DETERMINATION OF ALKALINITY OF WATER

Aim: To determine the types and amount of alkalinity in the given sample of water. You are
provided with a solution of Na2CO3 of strength 0.01N and a link solution of HCl solution are
provided.

Procedure:

Titration I: Standardization of HCl

Burette solution: HCl
Pipette solution: 20 ml of std. Na2CO3
Indicator: 2-3 drops of methyl orange
End point: Yellow to pale pink

Titration II: Estimation of alkalinity of water sample

Burette solution: HCl
Pipette solution: 20 ml of water sample
Indicator 1: 2-3 drops of phenolphthalein
End point 1: Disappearance of pale pink colour (Phenolphthalein End Point: P)
Indicator 2: 2-3 drops of methyl orange
End point 2: Reapperance of pale pink colour (Methyl orange End Point: M)

Equivalent weight of CaCO3 = 50

Result: The individual amounts of alkalinity present in the given water sample can be calculated
by using following expressions:

(i) If P >1/2 M, Water sample contains OH-+ CO32- alkalinity.

OH − =
(2 P − M )  Normality of HCl  50  1000 = ------------------ppm
20

2(M − P )  Normality of HCl  50  1000

CO32− = = ------------------ppm
20

(ii) If P <1/2 M, Water sample contains CO32- + HCO3- alkalinity.

2 P  Normality of HCl  50  1000

CO32− = = ------------------ppm
20

HCO3− =
(M − 2 P )  Normality of HCl  50  1000 = ------------------ppm
20

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Ex. No. 8: DETERMINATION OF HIGH MOLECULAR WEIGHT OF A POLYMER BY

USING OSTWALD VISCOMETER

Aim: To determine the average molecular weight of given polymer by U-tube viscometer
method and you are provided with a 5 wt% of polyvinyl alcohol solution.

Procedure: The flow time (t0) for the pure solvent, distilled water is measured by pipetting out
10 ml into the u-tube viscometer. Prepare 0.25%, 0.5%, 0.75%, 1% and 1.25% solutions from the
given polymer solution by using graduated pipette and 25 ml standard flask. 10 ml of each
concentration is pipetted out into the u-viscometer and the flow time (t) for different
concentration is noted.
Model table:
S. Concentration of
Time of flow (t) η/η0 = t/t0 ηsp = (t/t0)– 1 ηSP / c
No. the polymer solution, (c)
1. Distilled water (to)
2. 0.25%
3. 0.5%
4. 0.75%
5. 1.0%
6. 1.25%

Model Graph:

Calculation:
The molecular weight of the given polymer is calculated by using expression:  i = KM 
 i = KM 
 log i − (−3.3437) 
M = anti log of  
 0.64 

Result:

The molecular weight of the given polymer sample = …………

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