EM 4, Sector V, Salt Lake, Kolkata-700091, West Bengal, India

Phone: +91 33 2357 6163, Fax: +91 33 2357 1097

DEPARTMENT OF CHEMISTRY

CHEMISTRY LAB

Lab Safety Do’s & Don’ts

DO’S

The Chemistry laboratory must be a safe place in which to work and learn about
Chemistry. Most of these involve just using common sense

Do keep your lab and office space clean and free of clutter.

Do place one copy of your approved form in the plastic document holder on the door of
the lab you are working in. If you are working in a number of labs, put a note in the
plastic document holder on the door of each lab you are working in stating where your
experimental registration form is located

Do wear appropriate safety attire when in the lab - safety goggles, lab coat, etc.

Do not wear open-toed shoes (sandals) in the lab.

Do use the buddy system when working in the lab alone.

Do not eat or drink in the lab Even if your desk is in the lab!

Do avoid trip hazards

Keep wires and/or

tubing off the floor

Do maintain good lab cleanliness - it’s for your own safety and as well as for others!
We do not want to hear …………...

Do clean up after using any glassware or equipment!

Do leave the lab cleaner than you found it!

If we all DO follow these guidelines, everyone will be happy and safe

Do maintain good lab cleanliness - it’s for your own safety and as well as for others!

Be familiar with your lab assignment before you come to lab. Follow all written and
verbal instructions carefully. Observe the safety alerts in the laboratory directions. If
you do not understand a direction or part of a procedure, ask the teacher before
proceeding.

Wash acid, base, or any chemical spill off of yourself immediately with large amounts of
water. Notify your teacher of the spill.

Clean up spills immediately. If you spill a very reactive substance such as an acid or
base, notify the people in the area and then obtain assistance from your teacher. Acid
spills should be neutralized with baking soda, base spills with vinegar before cleaning
them up.

If chemical substances get in your eye, wash the eye out for 15 minutes. Hold your eye
open with your fingers while washing it out.

Place the reagents in a systematic manner.

If you burn yourself on a hot object, immediately hold the burned area under cold water
for 15 minutes. Inform your teacher.

Observe good housekeeping practices. Work areas should be kept clean and tidy at all
times. Only lab notebooks or lab handouts should be out on the table while performing
an experiment. Books and book bags should not be on the lab table. Passageways need
to be clear at all times.

Always add acid to water and stir the solution while adding the acid. Never add water
to an acid.

DON’T
Work in the laboratory without an instructor present. Work only with your lab
partner(s). Do not venture to other lab stations for any reason.
Wear bulky or dangling clothing.
Eat or drink in the laboratory. Don't chew on the end of a pen which was lying on
the lab bench.

Directly touch any chemical with your hands. Never taste materials in the
laboratory.
Waste the reagents.

When entering the lab/classroom, do not touch any equipment, chemicals, or other
materials without being instructed to do so. Perform only those experiments
authorized by the instructor.
When weighing never place chemicals directly on the balance pan. Never weigh a
hot object.
Smell anything in the laboratory unless your teacher tells you it is safe. Do not
smell a substance by putting your nose directly over the container and inhaling.

Instead, waft the vapors toward your nose by gently fanning the vapors toward yourself.
Absolutely no running, practical jokes, or horseplay is allowed in the laboratory.

Allow the reagent bottles to accumulate on the bench.

 CHEMISTRY LAB EQUIPMENTS:

1. BALANCE: Used for measuring mass.

2. BEAKER: Used to hold , mix and heat liquids.

3. BEAKER TONGS : Used to Pick up beaker.

4. BUNSEN BURNER : Frequently used as a heat source in the absence of
flammable materials.

5. BURETTE : Used for dispensing an accurate volume of a liquid.

6. CLAY TRIANGLE : Used to support a crucible during heating.

7. CRUCIBLE: Used for holding chemicals during heating to very high temperatures.

8. CRUCIBLE TONGS: Used to hold Crucible.

9. ERLENMEYER FLASK : Used to hold and mix chemicals. The small neck is to

facilitate mixing without spilling.

10. EVAPORATING DISH : Used to heat liquids for evaporation.

11. FORCEPS : Used to pick up or hold small objects.

12. FUNNEL : Used to transfer liquids or fine-grained materials into containers with
small openings. Also used for filtration.

13. GRADUATED CYLINDER: Used to measure a precise volume of a liquid.

14. MORTAR AND PESTLE: Used to crush and grind materials.

 List of Experiments

B.Tech

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

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

Experiment3 : Detection of functional groups .

Experiment 4: To determine the relative surface tension of aqueous glycerol solution by

Stalagmometer .

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

Experiment 6: To determine the rate constant of the hydrolysis of ethyl acetate in presence of
an acid catalyst .

Experiment 7: PH – METRIC Titration of monobasic acid and determination of PKa value of that
acid.

Experiment 8: To determine alkalinity of given water sample.

Experiment 9: Standardisation of KMnO4 solution with standard sodium oxalate/oxalic acid

Solution.

Experiment 10: Standardisation of Mohr’s salt solution / estimation of Fe’’ with standard KM nO4
solution.
 EXPERIMENT NO. 1

AIM Standardization of H2SO4 (Sulphuric acid) with NaOH (Sodium Hydroxide)

APPARATUS Electronic weighing balance, 250 ml conical flask, Measuring cylinder, funnel, glass
rods, Pipettes, Burettes and 100ml beaker

PRINCIPLE

The principle behind this experiment is based on a acid-base titration. It is also

known as neutralization reaction. This experiment is a neutralization reaction of a
base (NaOH) with acid (H2SO4). An acid solution neutralizes an alkali solution in
equal volumes provided their normal strength is equal. This means that 1 gm
equivalent weight of an acid will completely neutralise 1 gm equivalent weight of a
base.

In this experiment neutralization of sodium hydroxide with H2SO4 takes place as:

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

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

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

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

PREPARATION OF CHEMICALS

a. Preparation of 250ml (0.1N) NaOH Solution

1.0 gm of sodium hydroxide pellets are dissolved in 250 ml of water. The solution is
mixed properly to achieve a homogenous solution. The strength of the resulting
solution is 0.1N. The solutions were prepared freshly.

b. Preparation of 250 ml (------------N) H2SO4 (Hydro sulphuric acid) Solution

Approximately ------------ml of concentrated H2SO4 (Hydro Sulphuric acid) is diluted with
-------------------- ml of water to get a final volume of 250 ml. The strength of the resulting
solution is -------------------------- N.
 PROCEDURE:

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

DIAGRAM OF TITRATION
 1. OBSERVATION TABLE

Sr. Volume of NaOH Initial burette Final Titre reading Average

No. Solution reading burette (Initial – Final) (ml)
(ml) (ml) reading (ml)
(ml)

1. 10

2. 10

3. 10

4. 10

CALCULATION:

The strength of the acid solution is calculated according to the given formulae:

V1 S1 = V2 S2
Where,

V1 = Volume of the H2SO4 consumed

S1 = Strength of the acid solution (H2SO4)
V2 = Volume of the base (NaOH) (10 ml)
S2 = Strength of the base, NaOH (0.1N)

RESULT & CONCLUSION:

The strength of the given H2SO4 (Hydro Sulphuric acid solution) was found to be ---------------N
 EXPERIMENT NO. 2

Aim: Determination of total hardness of Water by EDTA (Complexometric) Titration

Purpose: To determine the “hardness” of a sample of water by using EDTA to determine

the concentration of calcium and magnesium ions.

APPARATUS Electronic weighing balance, 250 ml conical flask, Measuring cylinder, funnel, glass
rods, Pipettes, Burettes and 100ml beaker

Background

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

Na stearate + CaCl2  2NaCl + Ca stearate (insoluble)

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

Ca2+ + Y4-  CaY2-

and
Mg2+ + Y4-  MgY2-
Note that this is 1:1 stoichiometry—the EDTA may be hexadentate, but it is only one EDTA
molecule per complex.

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

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

i) Pipette out 10 ml of the sample water into a 100 ml conical flask.

ii) Add NH4Cl – NH3 buffer solution 2-3ml to the water sample.

iii) Add the EBT indicator to the water sample and the colour of the water will turn
to wine red.

iv) Fill up the burette with the supplied EDTA solution of known strength.

v) Titrate the water sample against the EDTA drop by drop until the wine red
colour turns to blue. Once the blue colour is developed stop the titration.

vi) Record the burette reading and repeat it twice.

Calculation and Results:

1000 ml 1(M) EDTA ≡≡ 100gm of CaCO3

1000ml 1(M) EDTA ≡≡ 100 x 1000 mg of CaCO3

1 ml (M/100) EDTA ≡≡ ( 100 x1000)/ (1000/100) mg of CaCO3
X ml (M/100) EDTA ≡≡ X x ( 100 x1000)/ (1000/100) mg of CaCO3
= X mg of CaCO3

10 ml of water sample contains X mg of CaCO3

1000 ml of water sample contains 100X mg of CaCO3

Conclusion:
The hardness of the given sample water is 100 X ppm (ppm = mg / litre )
 EXPERIMENT NO. 3

Detection of functional groups

Test for carboxylic acid group (-COOH)

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

Test for Ester group:

Add a pinch of the substance to a light pink alkaline phenolphthalein solution, prepared by
adding a drop of phenolphthalein to a very dilute NaOH solution with shaking.
(a) If the pink colour is not discharged in the cold, heat the solution to boiling, disappearance of
the pink colour indicates the presence of ester group. Acidify the clear solution with dilute
HCl. Appearance of white precipitate of water-insoluble hydrolysed acid, indicates the
presence of ester group.

(b) If the pink color is discharged in the cold showing the presence of acidic group, then add dilute
NaOH solution dropwise till a permanent pink color is obtained. Now boil the solution for a few
minutes. Discharge of color indicates the presence of ester group.

Test for carbonyl group:

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

AIM: To determine the relative surface tension of aqueous glycerol solution by

Stalagmometer.

PRINCIPLE:

APPARATUS AND MATERIALS: Stalagometer, Distilled Water, Aqueous Glycerol solution,

Pyknometer or Specific gravity bottle for density
measurements, weighing balance.
 OBSERVATION TABLE AND CALCULATION:

Table 1: Recording of LABORATORY temperature

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

Table 2: Counting the number of DROPS for Distilled Water and Supplied Glycerol
Solution and their Relative Surface Tension.
Solution Number of Mean of drops Density of the Surface tension of
in Stalagometer drops solution (g/ml) the solution
(dyne/cm)
i)
Water ii) 0.996 71.97
iii)
i)
5% Glycerol ii) 1.00867
iii)

PRECAUTIONS:
(a) Stalagometer should be cleaned properly before use
(b) Drops should be properly formed
(c) Stalagometer should be kept vertically during measurements
(d) Same Stalagometer should be used for water and aqueous glycerol solution
(e) Observe carefully when liquids are passing the upper and lower marks of the Stalagometer

RESULT AND CONCLUSION

 EXPERIMENT-5

AIM: To determine the relative viscosity of glycerol by Ostwald viscometer and

Determination of concentration of an unknown glycerol solution from the
calibration curve.

PRINCIPLE:

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

Pyknometer or Specific gravity bottle for density
measurements, Stop-watch to note the time, Weighing
balance.
 OBSERVATION TABLE AND CALCULATION:

Table 1: Recording of LABORATORY temperature

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

Table 2: Measurement of Flow Time of Different Percentage of Glycerol Solution and

Evaluate their Relative Viscosity

Solution Flow time Mean flow time Density of the Viscosity of the
in viscometer in ‘Second’ in ‘Second’ solution (g/ml) solution
(milipoise)
Water i) 0.996 8.01
ii)
iii)
5% Glycerol i) 1.00867
ii)
iii)
10% Glycerol i) 1.02092
ii)
iii)
15% Glycerol i) 1.0278
ii)
iii)
UNKNOWN i) 1.003*
Glycerol ii) 1.01012**
solution iii)

 Plot “Viscosity” versus “% of Glycerol solution” to obtain a calibration curve by

plotting the data obtained from water, 5%, 10% and 15% aqueous glycerol
solution.

 From the calibration curve determine concentration of unknown glycerol solution

 EXPERIMENT -6

AIM: To determine the rate constant of the hydrolysis of ethyl acetate in presence of an acid
catalyst

APPARATUS AND MATERIALS:

Burette, Pipette, Conical flask, Glass rod, Stopwatch, Ethyl acetate ester, N/2 HCl, N/20 NaOH,
Phenolphthalein
PRINCIPLE:
The hydrolysis of ethyl acetate which is extremely slow in pure water is catalyzed by H+ ions.
When water is present in large, excess i.e change in its concentration is negligible and the
backward reaction is also prevented, the hydrolytic reaction appears to be of first order. The
progress of the reaction can be studied by withdrawing aliquots from the reaction mixture from
time to time and at the end of the reaction and titrating with alkali. The amount of alkali required
at any stage is equivalent to the sum of the acetic acid produced and the acid catalyst which
remains constant throughout the reaction. Let, Vo and V∞ be the volumes of alkali required
initially and finally respectively and Vt be the same after time t. Since the ester hydrolyzed is
directly proportional to the acetic acid formed, a, the initial concentration of the ester is
proportional to V∞-Vo and the concentration (a-x) after time t is proportional to V∞-Vt. Hence, for
the rate constant k for the first order reaction at a particular temperature
k = 2.303 log a/ (a-x) t may be written in terms of volumes of alkali as

k = 2.303 log V∞-Vo

t V∞-Vt

Vo. which is difficult to obtain, as hydrolysis stars as soon as the ester is mixed
with water, can be eliminated by taking the difference Δtn= tn-t1 such that

Δtn= tn-t1= 2.303 log V∞-V1(n=2, 3,…)

k V∞-Vn

where, V1 and Vn are volumes of alkali required after time t1 and tn

respectively. If now log ( V∞ – V1 / V∞-Vn) is plotted, against Δt a straight line,
passing through the origin, is obtained
From the slope k can be determined.
 PROCEDURE:

1. Prepare about 500ml of an approximately N/20 NaOH solution.

2. Prepare 100ml of approximately N/2 HCl solution and take 50ml of the solution and dilute to 100ml
so that the strength of the solution thus prepared is exactly half of the original solution.

3. Take 25ml of N/2 HCl solutions in a 250ml dry conical flask cover it with a watch glass and place
the flask in a water bath and keep it there for 15mins.Note the temp. of the bath.

4. Add 2ml of pure (redistilled) ethyl acetate with a clean dry pipette constantly swirling the flask
during addition and starting the stop watch when the pipette is half emptied. Shake the mixture to
provide thorough mixing.

5. Withdraw 2ml of reaction mixture and pour into a conical flask containing 25-30ml of (if necessary,
chilled) water to slow down the reaction noting the time of half discharge. Titrate the solution with
N/20 NaOH solution using phenolphthalein as indicator as quickly as possible.

6. Repeat the step (5) several times approximately after 5, 10,15,20,30 and 40 minutes after the
initiation of the reaction.

7. Repeat step (3)-(6) with N/4 HCl solution.

8. Keep both the reaction mixtures overnight and then get the titre values for infinity.

9. Plot log {(V∞-V1)/ (V∞-Vn)} against Δtn for both the sets on the same graph paper, determine k 1 and
k2 from the slopes and then find the ratio k1 and k2.
 TABLE 1
Set I with N/2 HCl solution
t1 = --------------min. =………………..sec
V1=…………………………………….ml V∞=…………………………………….ml

Time(min) tn(sec) Δt(sec) Volume of V∞-Vn log {(V∞-V1)/(V∞-Vn)}

alkali(ml)

10

15

20

25

30

40

RESULT AND CONCLUSION

 EXPERIMENT-7

AIM: PH – METRIC Titration of monobaic acid and determination of PKa value of that
acid.
APPARATUS AND MATERIALS:
Burette, Pipette , beaker , NaOH , Acetic Acid.]
PRINCIPLE:
The PH of an aqueous solution can be measured using glass –calomel electrode system in
which following electrochemical cell is formed.
Ag|AgCl (s) |0.1 (M) HCl | Glass|Solution of unknown PH |Saturated Calomel Electrode
The right hand electrode is the saturated calomel electrode (ESC) and the left hand electrode is
the glass electrode which is actually an ion selective membrane electode , reversible with
respect to H+ ion. The glass electrode is the most likely used hydrogen ion responsive electrode
and its use depends on the fact that when a glass membrane is immersed in a solution , a
potential is developed which is a linear function of hydrogen ion concentrationof the solution .the
internal HCl solution is maintained at constant concentrations , the potential of the silver –silver
chloride electrode inserted into it will be constant , and so too will the potential between HCl
solution and the iner surface of the glass bulb . hence the only potential which can vary is the
potential between the outer surface of the glass bulb and the test solution in which it is
immersed , so the overall potential of the electrode is governed by the hydrogen ion
concentration of the test solution . glass electrode s are also available as combination electrode
which can contain the indicator electrode and a reference electrode combined in a single unit .
the potential (Eg ) of the glass electrod at 250 C may be expressed as
Eg = Eg0 + 0.059 log aH+
= Eg0 – 0.059 PH (1)
For actual PH measurement , the glass electrode is standardized in buffer solutions of known PH
values.
Ionization of a weak monobasic acid (HA) in aqueous solution may be represented as,
HA ⇄ H+ + A- (2)
Of which the ionization constant ( Ka ) is given by the activity quotient of the ionization
equilibrium (2),

𝒂𝑯+ . 𝒂𝑨−
Ka = (3)
𝒂𝑯𝑨
Where , a represents activity for the respective species which is related to the molar
concentration , (C) according to a = c.f ., whwre f = activity coefficient . in dilute aqueous
solutions of weak acids , ionic strength is very low , so the activity coefficient approach unity .
hence , the concentration approach activities . consequently the ionization constant (Ka) may be
expressed as
[𝑯+][𝑨−]
Ka = (4)
[𝑯𝑨]
When a strong base ( NaOH) is added to a weak acid ( Acetic Acid ) in an amount less than the
stoichiometric requirement a buffer solution I formed whose PH is given by the Henderson’s
equation.
[𝑆𝑎𝑙𝑡]
PH = PKa + log (5)
[𝐴𝑐𝑖𝑑]
A PH metric titration curve may be constructed by plotting the PH of the acid solution after each
addition of the strong base and the equivalence point of the titration may be determined
graphically . the derivative plot |∆PH / ∆n| vs n shows a maximum at the value of n
corresponding to the equivalence point.
 PROCEDURE :
1. Prepare 100ml of a standard (N/20) solution of Oxalic acid by accurate weighing in a digital
balance.
2. Prepare 100ml of (N/2) NaOH solution.
3. Prepare 100ml of (N/20) Acetic acid solution.
4. Prepare standard buffer solution of PH = 4 & 7 by dissolving the corresponding PH tablets in
the specified volume of distilled water.
5. Standardize the PH meter by alternately dipping the glass – calomel electrode assembly in
PH = 4 & 7 buffer solutions and adjusting the instrument accordingly at the experimental
temperature.
6. Take 25ml of (N/20) Acetic acid solution in a 100ml beaker . Add sufficient quantity of
distilled water so that the combined electrode ( glass – calomel assembly) dip into it
properly. Allow the system to attain the equilibrium at the experimental temperature and
record the PH.
7. Add 2 drops of the (N/2) NaOH solution from a burette / micro burette stir gently to mix
uniformly and record the PH. repeat the process until the PH of the solution reads ≈ 4.5 . then
add 1 drop each time till the equivalence point is reached (indicated by sharp rise in PH) .
Record the PH and the number of drops of the titrant in a tabular form. Take a few more
readings beyond the end point.
8. Determine the volume of 50 drops of the titrant solution and calculate the volume of one
drop.

NOTE : The same experiment may be carried out by coupling a

quinhydrone electrode ( reversible with respect to H+ ion) with a
saturated calomel electrode.
 Experimental data:
PH Metric titration of ( N/20) Acetic acid against supplied (N/2) NaOH solution.

TABLE 1: Recording of PH agains no of drops of NaOH added.

No of observation No of drops of Total No of drops PH value

NaOH of NaOH added
1 0 0
2 2 2
3 2 4
4 2 6

Plotting of graph using the recorded data : PH vs no of drops of NaOH added and hence
determine the PkH value from the graph.
 Experiment no-8

Aim: To determine alkalinity of given water sample.

Apparatus/reagent required: Burette, pipette, conical flask, measuring flask, N/10 H2SO4
Indicator: Phenolphthalein and methyl orange indicator

End point: (i) Pink to colourless with Phenolphthalein

(ii) colour change from light yellow to reddish orange with methyl orange

Alkalinity

It is the total amount of those substances present in water which tend to increase the concentration of
OH- ions either due to dissociation of water or due to hydrolysis. Water becomes alkaline due to
presence of HCO3-, HCO3-, CO 2- ions of salts of weak organic acids which consume H+ ions of water
leading to increase in concentration of OH- ions.
Types

Alkalinity of water in due to presence of

(i) Hydroxide ions (OH- ions)

(ii) Carbonates ions (CO32-)
(iii) Bicarbonates ions (CO32-)
These may be present alone or in combination e.g. OH- + CO32- and CO32- + HCO3-. The possibility
of OH- + HCO3- is ruled out due to following reaction.

OH- + HCO3- → CO32- + H2O

Hence, all three cannot be present together.
Theory :
The type and amount of alkalinity in water can be determined by titrating a known volume of it
against standard acid using two indicator namely phenolphthalein and methyl orange in the same
order.

(i) Volume of acid used up to phenolphthalein end point (A mL) neutralizes all OH-
ions and converts CO32- ions into HCO32- ions (i.e. half neutralization of CO32-).
The end point is disappearance of pink colour at a pH around 8.3. The acid
used in further titration using methyl orange as an indicator neutralizes all
HCO3- ions whether present originally or obtained from CO32- ions. The end
point is colour change from light yellow to reddish orange and comes at a pH
range of 3-4.5. The total acid used in titration (A+B mL) gives total alkalinity of
water. The reactions involved are:

(ii) OH- + H+ →H2O P

(iii) CO32- + H+ →HCO3- M
→ CO
(iv) HCO3- + H+ 2 + H2O

P = Phenolphthalein alkalinity = OH- + ½ CO32-

M = Total or methyl orange alkalinity = OH- + CO32- + HCO3- (due to all

ions) M-P = Alkalinity due to HCO3- ions

From the calculated values of P and M, following alkalinity correlations can be

made using following table:

Alkalinity (ppm)
Case
OH- CO32- HCO3-
P=0 0 0 M
P=M P or M 0 0
P = ½M 0 2P or M 0
P >1/2M 2P-M 2(M-P) 0
P < ½M 0 2P M-2P
Procedure

1. Rinse and fill the burette with standard acid and note down its initial reading.
2. Pipette out 20 mL of water sample in a conical flask and ad 1-2 drops of phenolphthalein
indicator and pink colour will appear.
3. Titrate pink solution against acid till colour disappears and note down the final reading.
4. Now add 1-2 drops of methyl orange indicator to this and colour of solution becomes
light yellow.
5. Titrate it further against acid till colour changes to light orange. Note the final burette
reading again. Repeat for making concordant reading.

Observations

Table: Titration of water vs acid

Final Vol. of
Initial Final burette burette Vol. of acid acid used
Sr. no. burette reading with readin used (mL) up to (mL) up to
readin phenolphthalei g with phenolphthalei methyl
g (x) n (y) methyl n end point (y- orange
orange (z) x) (z-x)
1.
2.
3.

Concordant reading of acid used upto phenolphthalein end point = y-x mL = A mL

Vol. of acid used up to methyl orange = Total volume consumed = z-x mL = B mL

General calculations

For finding the phenolphthalein alkalinity (P)

Concordant volume of acid used = A mL

Applying Normality equation

N1V1 = N2V2

(water) (acid)
 N1× 20 = ×A

N1 =

Strength in terms of CaCO3 = Normality × Eq. wt. of CaCO3

= ×50 gL-1

So, phenolphthalein alkalinity (P) =(A/200)×50 × 1000 mgL-1 =(A/200)× 50 × 1000 ppm

= 250 × A ppm

For finding the methyl orange alkalinity (M)

Concordant volume of acid used = T mL

Applying Normality equation

N3V3 = N4V4

(water) (acid)

N3× 20 = (1/10)×T

N3 = A/200

Strength in terms of CaCO3 = Normality × Eq. wt. of CaCO3

= (T/200) ×50 gL-1

So, methyl orange alkalinity (P) = (T/200) ×50 × 1000 mgL-1 =(T/200) ×50 × 1000 ppm

= 250 × A ppm

Since, P is related to M as ……., the water samples contains following alkalinity:

(i) Alkalinity due to OH- = ……..ppm

(ii) Alkalinity due to CO32- = ……ppm
(iii) Alkalinity due to HCO3- = ……ppm

Results

Phenolphthalein alkalinity = ….. ppm

Methyl orange alkalinity = ……..ppm
Alkalinity due to OH- = ………..ppm
Alkalinity due to CO32- = ………ppm
Alkalinity due to HCO3- = ……...ppm
Redox Titrimetric Estimations Based on Permanganometry
Experiment No. 9: Standardisation of KMnO4 solution with standard sodium oxalate/oxalic acid
solution

Principle:
In dilute H2SO4 acid medium MnO4- quantitatively oxidises C2O42-to CO2and itself is reduced to Mn2+
2 MnO4- + 16 H+ + 5 C2O42- = 2 Mn2+ + 8 H2O + 10 CO3
Therefore, MnO4/5 = C2O42-/2 = 1 Equivalent

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

It is an example of autocatalytic reaction, in which Mn2, a product of reaction, acts as the catalyst. Use
of sodium oxalate as the primary standard substance is advantageous over oxalic acid, because the
former has no water of crystallisation and can be easily purified by recrystallisation. Further, its strength
does not change on standing.
KMnO4 solution may be standardised against standard oxalic acid/sodium oxalate solution in 2 (N)
H2SO4 medium at 70-80 oC. Purple coloured KMnO4 serves as a self-indicator. Its strength may be
calculated using the relation:
VMnO4- x S MnO4- = VC2O42-x S C2O42-
Chemical Required:
i) Standard (N/20) oxalic acid, H2C2O4.2H2O (F.W. = 126.048)
or Sodium Oxalate, Na2C2O4 (F.W. = 134) to be prepared by accurate weighting.
Strength = (w/0.7879) (N/20) for oxalic acid
= (w’/0.8375) (N/20) for sodium oxalate
Where, w and w’ are the weights of H2C2O4.2H2O or Na2C2O4 respectively per 250 ml of the
solution.
ii) (-N/20)KMnO4 solution: -0.4 -0.5g of KMnO4 per 250 ml.
iii) 4(N) H2SO4 : (1 : 9) H2SO4 solution

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

Sr. Volume of oxalic Initial burette Final Titre reading Average

No. acid Solution reading burette (Initial – Final) (ml)
(ml) (ml) reading (ml)
(ml)

1. 10

2. 10

3. 10

4. 10

CALCULATION:

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

CONCLUSION

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

Experiment No.10: Standardisation of Mohr’s salt solution / estimation of Fe’’ with standard
KMnO4 solution.

Principle:
In dilute H2SO4 acid medium, KMnO4 quantitatively oxidises Fe2+ to Fe3+:
MnO4- + 5Fe2+ + 8H+ = Mn2+ + 5Fe3+ + 4H2O
MnO4- = 5Fe2+
MnO4-/5 = (NH4)2SO4.FeSO4.6H2O
Mohr’s salt (Fe ) solution may be estimated by titrating it, in 2(N) H2SO4 medium with a standard
2+

solution if KMnO4 at room temperature in presence of H3PO4.

Calculation:
1000 ml of (N) KMnO4 = 55.847g of Fe = 392.143g of Mohr’s salt
Or, 1000 ml (N) KMnO4 = 1000 ml Mohr’s salt
I.e. V (KMnO4) x S (KMnO4) = V (Mohr) x S (Mohr)

Chemical Required:
1) Standard (M/20) oxalic acid or sodium oxalate solution: To be prepared by accurate weighting.
2) 4(N) H2SO4
3) Syrupy phosphoric acid
4) (N/20) Mohr’s salt solution: 5g of Mohr’s salt per 250 ml in 2(N) H2SO4.

Procedure:
Pipette outan aliquot of 25 ml of Mohr’ salt solution in a 250 ml conical flask, add 25 ml of
4 (N) H2SO4 and 3 ml H3PO4 and titrate the hot solution with the (-N/20) KMnO4 solution until the
solution turns light pink colour that is stable for -30 seconds. Repeat the titration twice to have a
concordant reading. Calculate the strength of Mohr’ salt solution normality and in g/lit .
 OBSERVATION TABLE

Sr. Volume of Mohr’ Initial burette Final Titre reading Average

No. salt Solution reading burette (Initial – Final) (ml)
(ml) (ml) reading (ml)
(ml)

1. 10

2. 10

3. 10

4. 10

CALCULATION:

V (KMnO4) x S (KMnO4) = V (Mohr) x S (Mohr)

CONCLUSION

The strength of mohr’ salt solution is = g/lit.

 CHEMISTRY LAB
ANSWERS

1. Normality – Normality (N) is defined as the number of mole equivalents per litre of solution, i.e.
normality (N) = (Number of mole equivalents / Volume of solution in litres).
2. Molality – Molality (m) is defined as the number of moles of solute per kg of solvent, i.e. Molality (m) =
(Moles of Solute / Weight of solvent in kg).
3. Molarity – Molarity (M) is defined as the number of moles per litre of solution, i.e. Molarity (M) = (Moles
of solute / Volume of solution in litres).
4. Formality – Formality (F) of a solution is the number of gram formula weight of the ionic solution
dissolved per litre of the solution, i.e. Formality (F) = (Weight of solute in gram per litre of solution /
Formula weight).
5. 1-Normal solution – 1(N) solution means that the solution contains exactly 1 mole equivalents of the
solute per litre of the solution.
6. 1-Molal solution – 1(m) solution means that the solution contains exactly 1 mole of solute per kg of the
solvent.
7. 1-Molar solution – 1(M) solution means that the solution contains exactly 1 mole of solute per litre of the
solution.
8. 1-Formal solution – 1(F) solution means that the solution contains 1 gram (in terms of formula weight)
of an ionic solute dissolved per litre of the solution.
9. Standard solution – A standard solution is a solution containing a precisely known concentration of an
element or a substance. Its concentration remains constant all the time.
10. Primary-standard solution – A primary standard solution is a reagent that is very pure, representative of
the number of moles the substance contains, and easily weighed. These are used in titration to
determine an unknown concentration.
11. Secondary-standard solution – A secondary-standard solution is a chemical term that refers to a
solution that has its concentration measured by titration with a primary standard solution.

12. pH – It is the figure expressing the acidity or alkalinity of a solution on a logarithmic scale on which 7 is
neutral, lower values more acidic and higher values more alkaline. The pH is equal to -log 10 c, where c
is the H+ ion concentration in moles per litre.
13. pOH – It is a measure of OH- ion concentration. It is used to express the alkalinity of a solution. Higher
the value on a pOH scale, more acidic the solution is, lower values are more alkaline and 7 is neutral.
14. pKa - pKa is the negative base-10 logarithm of the acid dissociation constant (Ka) of a solution, i.e. pKa
= -log 10 Ka. It is used to determine the strength of an acid or acidic solution.
15. pKb – pKb is the negative base-10 logarithm of the base dissociation constant (Ka) of a solution, i.e.
pKb = -log 10 Kb. It is used to determine the strength of a base or alkaline solution.
16. pKw - pKw is the product of the concentration of H+ and OH- ions in water, i.e. pKw = -log 10 Kw =
[H+][OH-]. pKw of water at 25◦C is 14.
 CHEMISTRY LAB
ANSWERS

17. Surface tension – It is the tension of the surface of a liquid caused by the attraction of the particles in
the surface layer by the bulk of the liquid, which tends to minimize the surface area.
18. Viscosity – It is the quantity expressing the magnitude of internal friction in a liquid, as measured by the
force per unit area resisting uniform flow.
19. Viscosity co-efficient – Viscosity is calculated in terms of the co-efficient of viscosity. It is constant for a
liquid and depends on its liquid nature.
20. Viscous liquid – A liquid which offers resistance to the flow is called viscous liquid. Examples are honey
and petrol.
21. Adhesive force – Adhesive forces are the attractive forces that act between unlike molecules. They are
caused by force acting between 2 substances, such as mechanical forces and electrostatic forces.
22. Cohesive force – These are attractive forces that act between molecules of the same substance. This
force tends to unite molecules of a liquid, gathering them into relatively large clusters due to the
molecules’ dislike for its surroundings.
 CHEMISTRY LAB
ANSWERS

What do you mean by titration?

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

Name six indicators and colours in acidic and basic medium.

INDICATOR ACIDIC MEDIUM BASIC MEDIUM

Thymol Blue Red Yellow
Methyl red yellow red
Methyl Orange Red yellow
Chlorophenol Red Yellow Red
Azolitmin Red Blue
Phenolphthalein Colourless Pink