SHREE VENKATESHWARA

HI-TECH ENGINEERING COLLEGE

(AUTONOMOUS)
GOBI

DEPARTMENT OF SCIENCE & HUMANITIES

(CHEMISTRY)

23PCL11 - CHEMISTRY LABORATORY MANUAL

(REGULATION 2023)
(For private circulation only)
(2023 - 2024 BATCH - FIRST SEMESTER)

NAME : ………………...........................................

REG. No.:…………………………………………………………

CLASS : ………………………………………………………..
 23PCL11 CHEMISTRY LABORATORY (Any seven experiments) LTPC
0042

COURSE OBJECTIVES:
 To inculcate experimental skills to test basic understanding of water quality
parameters, such as acidity, alkalinity.
 To acquire the knowledge in total hardness and dissolved oxygen and its
impacts in industries through experiments
 To understand the impacts of chlorine in water sample through volumetric
analysis.
 To induce the students to familiarize with electroanalytical techniques in the
determination of impurities in aqueous solutions.
 To determine the amount of metal ions through spectroscopic techniques.

LIST OF EXPERIMENTS
1. Preparation of Na2CO3 as a primary standard and estimation of acidity of a water sample
using the primary standard.
2. Determination of types and amount of alkalinity in a water sample
3. Determination of total, temporary & permanent hardness of water by EDTA method.
4. Determination of DO content of water sample by Winkler’s method.
5. Determination of chloride content of water sample by Argentometric method.
6. Determination of strength of given hydrochloric acid using pH meter.
7. Determination of strength of acids in a mixture of acids using conductivity meter.
8. Conductometric titration of barium chloride against sodium sulphate (precipitation
titration).
9. Estimation of iron content of the given solution using potentiometer.
10. Estimation of sodium /potassium present in water using a flame photometer.

TOTAL : 30 PERIODS

COURSE OUTCOMES:
CO’s OUTCOMES
Analyse the quality of water samples with respect to their acidity, alkalinity of water
CO1
samples
Examine the water quality parameters like total hardness and DO with volumetric
CO2
analysis.
CO3 Learn the permissible limit of chlorine in the given water sample
CO4 Analyse the impurities in solution by electroanalytical techniques quantitatively
CO5 Determine the amount of metal ions through spectroscopic techniques.

TEXT BOOKS :

1. Vogel‘s Textbook of Quantitative Chemical Analysis (8th edition, 2014).

2. J. Mendham, R. C. Denney, J.D. Barnes, M. Thomas and B. Sivasankar, Vogel’s
Textbook of Quantitative Chemical Analysis (2009).
 LIST OF EXPERIMENTS

S.NO EXPERIMENT NAME

EXPERIMENTS BEYOND THE SYLLABUS

1 ESTIMATION OF IRON CONTENT OF THE WATER SAMPLE USING
SPECTROPHOTOMETER BY THIOCYANATE METHOD
2 CONDUCTOMETRIC TITRATION OF STRONG ACID VS STRONG BASE

EXPERIMENTS IN THE SYLLABUS

1 DETERMINATION OF TYPES AND AMOUNT OF ALKALINITY IN WATER
SAMPLE
2 DETERMINATION OF TOTAL , TEMPORARY & PERMANENT HARDNESS OF
WATER BY EDTA METHOD
3 DETERMINATION OF CHLORIDE CONTENT OF WATER SAMPLE BY
ARGENTOMETRIC METHOD
4 DETERMINATION OF STRENGTH OF GIVEN HYDROCHLORIC ACID USING PH
METER
5 DETERMINATION OF STRENGTH OF ACIDS IN A MIXTURE OF ACIDS USING
CONDUCTIVITY METER
6 CONDUCTOMETRIC TITRATION OF BARIUM CHLORIDE AGAINST SODIUM
SULPHATE (PRECIPITATION TITRATION)
7 ESTIMATION OF IRON CONTENT OF THE GIVEN SOLUTION USING
POTENTIOMETER
S.No. DATE EXPERIMENT NAME MARKS STAFF
(write in capital letters) OBTAINED SIGN
(60 MARKS)

TOTAL MARKS

LAB IN-CHARGE SIGN

 GENERAL INSTRUCTIONS TO STUDENTS
1. STUDENTS ARE INSTRUCTED TO COME TO CHEMISTRY LAB IN TIME. LATE COMERS
ARE NOT ENTERTAINED IN THE LAB

2. STUDENTS SHOULD BE PUNCTUAL TO THE LAB. IF NOT, CONDUCTED EXPERIMENTS

WILL NOT BE REPEATED

3. STUDETNS ARE EXPECTED TO COME PREPARED AT HOME WITH THE EXPERIMENTS

WHICH ARE GOING TO PERFORM

4. STUDENTS ARE INSTRUCTED TO WEAR ID CARD & OVER COAT AT ALL TIMES WHILE
IN THE LAB

5. CLOSED SHOES AND SOCKS MUST BE WORN AT ALL TIMES IN THE LAB

6. STUDENTS ARE INSTRUCTED NOT TO BRING MOBILE PHONES TO THE LAB

7. KEEP YOUR BAGS IN A CORNER OF THE LAB

8. WASH ALL YOUR APPARATUS BEFORE STARTING AND AFTER FINISHING THE
EXPERIMENTS

9. READ THE PROCEDURE THOROUGHLY BEFORE STARTING THE EXPERIMENT

10. HANDLE THE APPARATUS AND CHEMICALS CAREFULLY

11. DO NOT WASTE THE SOLUTIONS/CHEMICALS

12. STUDENTS SHOULD UPDATE THE MANUAL/RECORD REGULARLY.BEFORE LEAVING

THE LAB STUDENTS SHOULD GET HIS LAB MANUAL SIGNED BY THE LAB INCHARGE

13. REPLACE ALL THE BOTTLES BEFORE LEAVING THE LAB IN PROPER PLACE.

14. KEEP YOUR WORKING TABLE NEAT AND CLEAN.

15. KEEP THE TAP CLOSED WHILE NOT IN USE.

16. NEVER POUR WATER INTO ACID.

17. NEVER RETURN THE UNUSED CHEMICALS TO THE ORIGINAL BOTTLE.

18. ANY DAMAGE OF GLASSWARE OR EQUIPMENT IS STUDENT’S RESPONSIBILITY AND

FINE WILL BE COLLECTED FROM THE STUDENT.

19. THOROUGHLY WASH YOUR HANDS WHILE LEAVING THE LAB

20. IN THE CASE OF ANY ACCIDENT LIKE SWALLOWING CHEMICALS, SOLUTIONS OR

SPLASHING OF ACIDS AND OTHER CHEMICALS IN THE EYES OR ON THE BODY,
REPORT TO THE LAB INCHARGE IMMEDIATELY.
 SAFETY PRECAUTIONS
1. WHILE WORKING IN THE LAB SUITABLE PRECAUTIONS SHOULD BE
OBSERVED TO PREVENT ACCIDENTS

2. ALWAYS FOLLOW THE EXPERIMENTAL INSTRUCTIONS STRICTLY.

3. THE LAB COAT SHOULD BE WORN WHILE WORKING IN THE LAB TO

PROTECT CLOTHING FROM THE CHEMICALS

4. USE THE FIRE EXTINGUISHER AVAILABLE IN THE LAB IN CASE OF FIRE.

5. USE FIRST AID BOX IN CASE OF ANY ACCIDENT.

6. NEVER WORK IN THE LAB UNLESS LAB-INCHARGE OR LAB ASSISTANT IS

PRESENT

7. NEVER TASTE ANY CHEMICALS & SOLUTIONS

8. DO NOT ALLOW THE CHEMICALS TO COME IN CONTACT WITH YOUR

SKIN

9. KEEP ALL THE DOORS AND WINDOWS OPEN WHILE WORKING IN THE
LAB

10.DON’T ENTER INTO THE LAB BAREFOOT. ALWAYS WEAR CLOSED

SHOES AND SOCKS INSIDE THE LAB

11.IN CASE OF ANY ACCIDENT DON’T PANIC. INFORM IT TO THE LAB-

INCHARGE OR DO THE FOLLOWING THINGS:

A) IF YOU RECEIVE A CHEMICAL BURN FROM A CAUSTIC MATERIAL, I.E. ACID OR BASE,

IMMEDIATELY WASH THE BURNED AREA WITH LARGE QUANTITIES OF WATER.

B) WASH YOUR HANDS AND FACE QUICKLY AND THOROUGHLY WHENEVER THEY

COME INTO CONTACT WITH A CHEMICAL.

C) ALWAYS WASH YOUR HANDS, BEFORE LEAVING THE LAB SINCE TOXIC CHEMICALS

MAY BE TRANSFERRED TO THE MOUTH AT A LATER TIME.

D) CHEMICALS SPILLED OVER A LARGE PART OF THE BODY REQUIRE IMMEDIATE

ACTION. REMOVE ALL CONTAMINATED CLOTHING AND USE THE SAFETY SHOWER,

FLOODING THE BURNED AREA. GET MEDICAL ATTENTION.

ENGINEERING CHEMISTRY LAB APPARATUS
 ENGINEERING CHEMISTRY LAB INSTRUMENTS

CONDUCTIVITY METER CONDUCTIVITY CELL

POTENTIO METER CALOMEL ELECTRODE &

PLATINUM ELECTRODE

PH METER GLASS ELECTRODE

SCHEMATIC DIAGRAM OF SPECTROPHOTOMETER

 PREPARATION OF VARIOUS CONCENTRATIONS OF Fe3+ SOLUTION

Volume of
Volume of Volume of Volume of distilled Concentration
S. Iron HNO3 NH4SCN H2O (to of Iron ppm
No. solution
(ml) (ml) make equal (or) N
(ml)
volume)

1 1 1 1 7 0.01 N

2 2 1 1 6 0.02 N

3 3 1 1 5 0.03 N

4 4 1 1 4 0.04 N

5 5 1 1 3 0.05 N
 EXPERIMENT BEYOND THE SYLLABUS - 1

EXPT.No. NAME OF THE EXPERIMENT DATE

ESTIMATION OF IRON CONTENT OF THE WATER SAMPLE

USING SPECTROPHOTOMETER (THIOCYANATE METHOD)
AIM:

To estimate the amount of iron content of an unknown solution by

spectrophotometry by thiocyanate method.

CHEMICALS REQUIRED:

1. Ferrous ammonium sulphate

2. HNO3
3. Ammonium thio cyanate
4. Distilled water

MATERIALS REQUIRED:

Spectrophotometer, Cuvette, Beaker & glass rod

PRINCIPLE:

Spectrophotometry is an instrument used to measure the intensity of the

light absorbed by a substance. The relationship between absorbance (A) and the
concentration of the solution (C) is given by Beer-Lambert’s law.

Where

Io = Intensity of incident light

I = Intensity of transmitted light
Ε = Molar absorption co-efficient
x = Thickness of the cell
C = Concentration of the solution

From the equation it is seen that, the absorbance (A) is directly proportional
to the molar concentration and thickness of the cell. In the determination of iron,
ferrous iron solution is acidified with HNO 3 to convert Fe2+ into Fe3+. Fe3+ ion does
not given any colour in solution. But, it gives red colour when it reacts with
potassium thiocyanate (KSCN) or ammonium thiocyanate (NH4SCN) solution.
Fe3+ + 6KSCN [Fe (SCN)6]3- + 6K+
 MODEL GRAPH:

CALIBRATION CURVE (ABSORBANCE Vs CONCENTRATION)

Blank (distilled water): zero absorbance; λmax = 480 nm

S. No. Concentration Absorbance

1 0.01 N

2 0.02 N

3 0.03 N

4 0.04 N

5 0.05 N

6 Unknown

CALCULATION:

Amount of iron present in the given solution = Normality of unknown sample X Eq. wt. of iron

= gms.
 This complex has maximum absorption in the region λ = 480 nm. A
calibration curve is drawn by measuring the absorbance of known solution. Then,
the absorbance of unknown solution is measured, using which the concentration
can be determined from the calibration curve.

PROCEDURE

PREPARATION OF STOCK Fe3+ SOLUTION

A stock solution of 0.1 N Fe 3+ is prepared by dissolving 39.0 gms of ferrous

ammonium sulphate with 1 ml of con. HNO 3 in 1 litre of distilled water. Forms the
stock solution, various concentrations are prepared (0.01, 0.02, 0.03, 0.04, 0.05 &
0.06 N).

DETERMINATION OF IRON CONTENT

The spectrophotometer is switched on and warmed up for 10 minutes. The

monochromater is adjusted for λ =480 nm.

The blank solution (distilled water) is kept in the cell and the absorbance is
measured for which the absorbance is zero and transmittance is 100.

Now the absorbance of all the standard solutions are similarly measured.
Also the absorbance of unknown solution is measured.

The calibration graph is drawn between the concentration and absorbance

from which the concentration of unknown solution is measured.

RESULT

Amount of iron present in the whole of the given solution = gms

 TITRATION OF STRONG ACID VS STRONG BASE

(HCl Vs. NaOH)

Volume of NaOH Conductance

S.No
added (ml) (mho)
 EXPERIMENT BEYOND THE SYLLABUS - 2

EXPT.No. NAME OF THE EXPERIMENT DATE

CONDUCTOMETRIC TITRATION OF STRONG ACID VS STRONG BASE

AIM:

To determine the strength of HCl present in the given solution by

conductometric titration using standard NaOH.

MATERIALS REQUIRED:

1. Conductivity meter
2. Conductivity cell
3. Beaker
4. Standard NaOH
5. Approximately HCl
6. Burette, pipette, glass rod etc.,

PRINCIPLE:

Solution of electrolytes conducts electricity due to the presence of ions. Since

specific conductance of a solution is proportional to the concentration of ions in it,
conductance of the solution is measured during titration.

When the sodium hydroxide is added slowly from the burette to the solution, HCl
(strong acid) gets neutralized first. Since the fast moving H + ions are replaced by
slow moving Na+ ions, decrease in conductance take place until the end point is
reached.

HCl + NaOH  NaCl + H2O (neutralization).

When the end point is reached, addition of NaOH will cause sudden increase
in the conductance. This is due to the presence of fast moving OH – ions.

PROCEDURE:

The burette is washed well with water and rinsed with the given standard
NaOH solution. It is then filled with NaOH solution up to the zero level. 20ml of the
given acid (HCl) is pipetted out into a clean 100ml beaker then diluted to 50ml by
adding conductivity water, so that the electrodes are well immersed in the solution.
The two terminals of the cell are connected with a conductivity bridge.
 Calculation:

Volume of NaOH (V1) = ml

Strength of NaOH (N1) = N

Volume of HCl (V2) = ml

Strength of HCl (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of HCl (N2) = V 1 x N 1 / V2

Strength of HCl (N2) = N

Amount of HCl present in whole of the given solution = Eq.Wt. of HCl X N2

= 36.5 X

= g
Now 1ml of NaOH from the burette is added to the solution, taken in the beaker,
stirred for some time and then conductivity is measured. (The conductivity is going
on decreasing up to the end point.) This process is repeated until at least five
readings are taken after the end point has been reached.

After the end point, sudden increase in conductance is observed on further

addition of NaOH. The reading (conductivity) is continuously measured for each
addition of NaOH and are tabulated. Now the graph is plotted between the volume
of NaOH Vs conductivity. From the graph the end point is noted. From the end point
the amount of HCl present in 1 litre of the solution is calculated.

RESULT:

1. The strength of HCl = N

2. The amount of HCl present in whole of the given solution = g

EXPERIMENTS
 TITRATION – I: STANDARDISATION OF HCl
(Std. Na2CO3 vs. HCl)

Volume Burette Readings

Volume
of Concordant
(in ml) of HCl Indicator
S. No. Na2CO3 value
(V2)
(V1)
(in ml)
(in ml)
(in ml) Initial Final

2 phenolphthalein

Calculation:

Volume of standard Na2CO3 Solution (V1) = ml

Strength of standard Na2CO3 Solution (N1) = N

Volume of HCl Solution (V2) = ml

Strength of HCl Solution (N2) = ?

According to the law of volumetric analysis, V1N1 = V 2 N2

Strength of HCl Solution (N2) = V 1 x N 1 / V2

N2 = N
EXPT.No. NAME OF THE EXPERIMENT DATE

DETERMINATION OF TYPES AND AMOUNT OF ALKALINITY IN WATER

SAMPLE

AIM:

To determine the alkalinity present in the given water sample. A standard

solution of sodium carbonate is provided.

CHEMICALS REQUIRED:

Hydrochloric Acid, Sodium carbonate, Water Sample, Phenolphthalein

Indicator & Methyl Orange Indicator

MATERIALS REQUIRED:

Burette, Pipette & Conical Flask

PRINCIPLE:

Alkalinity is caused by the presence of hydroxide, carbonate and

bicarbonate. There are five alkalinity conditions possible in a given sample of water.
They are hydroxide only, carbonate only, bicarbonate only, combination of
carbonate and hydroxide or carbonate and bicarbonate. The various alkalinities can
be estimated by titrating with a standard acid using phenolphthalein and methyl
orange indicators successively.

(i) Phenolphthalein end point:

Hydroxide alkalinity is completely neutralized and carbonate alkalinity is

partially neutralized during phenolphthalein end point.

(ii) Methyl Orange end point:

Bicarbonate neutralization occurs during methyl orange end point.

 TITRATION – II: DETERMINATION OF ALKALINITY
(Std.HCl vs. sample water sample)

Volume Burette Readings (in ml)

of Methyl Concordant
Water Phenolphthalein orange value
sample
end point (in ml)
end point
S. No. (V1) Indicator

(in ml)
Initia Fina Initi
l l al Final (V2) (V3)

1
phenolphthalein

&
2
methyl orange

Calculation:

1. Calculation for Phenolphthalein alkalinity:

Volume of water sample (V1) = ml

Strength of water sample (N1) = ?

Volume of standard HCl Solution (V2) = ml

Strength of standard HCl Solution (N2) = N

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of water sample (N1) = V 2 x N 2 / V1

N1 = N

Phenolphthalein alkalinity [P] = N1 X 50 X 1000

P= ppm
PROCEDURE

TITRATION – I:

STANDARDISATION OF HCl:

The burette is washed well with distilled water and rinsed with the small
amount of HCl solution. It is then filled with the same solution up to the zero mark
without any air bubbles.

The pipette is washed with distilled water and rinsed with the small amount
of standard Na2CO3 solution. 20 ml of this solution is pipetted out into a clean
conical flask. Two drops of phenolphthalein indicator is added and titrated against
HCl solution taken in the burette. The end point is the change of colour from pink to
colourless. The titration is repeated for concordant values.

TITRATION – II:

DETERMINATION OF ALKALINITY:

The burette is washed and rinsed with the given hydrochloric acid. Then the
burette is filled with Std. Hydrochloric acid. 20 ml of water sample is pipette out in a
clean conical flask. A drop of phenolphthalein indicator is added. Pink colour is
observed. This solution is titrated against the standard acid until pink colour is
disappeared. The end point is noted.

Few drops of methyl orange indicator are added to the same solution after
the phenolphthalein end point. The titration is continued until the solution becomes
red orange. The total titre value is noted. The titration is repeated for concordant
values.
2. Calculation for Methyl orange alkalinity:

Volume of water sample (V1) = ml

Strength of water sample (N1) = ?

Volume of standard HCl Solution (V3) = ml

Strength of standard HCl Solution (N3) = N [Here, N3 = N2]

According to the law of volumetric analysis, V1N1 = V3 N3

Strength of water sample N1 = V 3 x N 3 / V1

Strength of water sample = N

Methyl orange alkalinity [M] = N1 X 50 X 1000

M = ppm

CALCULATION FOR ALKALINITY

STEP 1: (based on calculation 1 & 2)
P = ppm

M = ppm

½M= ppm

STEP 2: TICK (√)THE PROPER CONDITION (based on STEP 1)

P=0 P=½M P<½M P>½M P=M

STEP 3:(based on the STEP 2 & reference table)

Results of Nature of
[P] and [M] OH - CO32- HCO3- alkalinity

P=0 0 0 M Only
bicarbonate
P=½M 0 2P 0 Only carbonate
P<½M 0 2P M- 2P Bicarbonate
and carbonate
P>½M 2P –M 2(M-P) 0 hydroxide and
bicarbonate
P=M P or M 0 0 Only hydroxide
HYDROXIDE (OH-) CARBONATE (CO32-) BICARBONATE (HCO3-)
ALKALINITY ALAKALINITY ALAKALINITY
RESULT:

Water sample contains the following alkalinity:

1. Phenolphthalein alkalinity = _________ ppm

2. Methyl orange alkalinity = _________ ppm
3. Hydroxide alkalinity = _________ ppm
4. Carbonate alkalinity = _________ ppm
5. Bicarbonate alkalinity = _________ ppm
TITRATION – I: STANDARDISATION OF EDTA
(Standard Hard Water Vs EDTA)

Volume Burette Readings

of Std.
(in ml) Volume of Concordant Indicator
Hard
EDTA(V2) value
S. No. Water Initial Final
(V1) (in ml) (in ml)

(in ml)

2 EBT

1. Calculation of standardisation of EDTA:

Volume of standard hard water sample (V1) = ml

Strength of standard hard water sample (N1) = N

Volume of EDTA solution (V2) = ml

 Strength of EDTA Solution (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of EDTA Solution (N2) = V1 x N1 / V2

N2 = N

EXPT.No. NAME OF THE EXPERIMENT DATE

DETERMINATION OF TOTAL, TEMPORARY & PERMANENT HARDNESS

OF WATER BY EDTA METHOD

AIM:

To determine the amount of total, temporary and permanent hardness of the

given water sample by EDTA method. Standard hard water will be provided.

CHEMICALS REQUIRED:

EDTA, Ammonia Buffer (NH4Cl + NH4OH), Eriochrome black – T & Calcium

Carbonate

MATERIALS REQUIRED:

Burette, Pipette & Conical Flask

PRINCIPLE:

Disodium salt of EDTA is used to estimate the various hardness of the hard
water containing Ca2+ and Mg2+ ions. When EDTA is added to hard water, it reacts
with calcium and magnesium ions present in it to form a stable complex. The
hardness can be calculated from the volume of EDTA consumed.

Eriochrome Black – T is used as an indicator, which forms a weak [EBT –

metal ion] complex with the metal ions present in the hard water and gives wine
red colour.

Ca2+ + EBT [Ca – EBT] COMPLEX

(WINE RED COLOUR)

When EDTA is added to the hard water, the metal ions form a stable [EDTA-
metal ion] complex with EDTA by leaving the indicator. When all the metal ions
are taken by EDTA from the [EBT - metal ion] complex, the wine red colour changes
into steel blue, which indicates the end point. The metal EDTA complex is stable at
pH 8-10. This pH range can be maintained by adding ammonia buffer.

[Ca – EBT] COMPLEX + EDTA [Ca – EDTA] COMPLEX

(WINE RED COLOUR) (STEEL BLUE COLOUR)

TITRATION – II: ESTIMATION OF TOTAL HARDNESS

(Hard water sample Vs Std. EDTA)

Volume Burette Readings

of Hard
(in ml) Volume of Concordant
Water
EDTA(V1) value
S. No. sample Initial Final Indicator
(V2) (in ml) (in ml)

(in ml)

2 EBT

2. Calculation of Total Hardness:

Volume of standard EDTA Solution (V1) = ml

Strength of standard EDTA Solution (N1) = N

Volume of hard water Sample (V2) = ml

Strength of hard water Sample (N2) = ?

According to the law of volumetric analysis, V1N1 = V 2 N2

Strength of hard water sample N2 = V 1 x N 1 / V2

Strength of hard water sample N2 = N

Total hardness of water sample = N2 X Eq. wt of CaCO3 X 1000

= _________ N X 50 X 1000

= __________ ppm
PROCEDURE:

TITRATION – I:

STANDARDISATION OF EDTA:

The burette is washed well with the distilled water and then rinsed with a
little amount of the given EDTA solution. It is then filled with the same EDTA
solution up to the zero level without air bubbles. Initial reading of the burette is
noted. 20 ml of standard hard water solution is pipetted out into a clean conical
flask. 5ml of ammonia buffer solution and 2 drops of Eriochrome Black – T
indicator are added. The solution turns wine red in colour and it is then titrated
against EDTA taken in the burette. The change of wine red colour to steel blue
colour is the end point. The final reading in the burette is noted. The difference in
the burette reading gives the volume of the EDTA solution. The titration is repeated
to get concordant values.

TITRATION – II:

ESTIMATION OF TOTAL HARDNESS:

20 ml of the given hard water is pipetted out into a clean conical flask. 5
ml of ammonia buffer solution and 2 drops of Eriochrome Black – T indicator are
added. The solution turns wine red in colour. This solution is titrated against EDTA
solution taken in the burette. The change of wine red colour into steel blue colour
is the end point. The titration is repeated to get concordant values.
 TITRATION – III: ESTIMATION OF PERMANENT HARDNESS
(Boiled water Vs Std. EDTA)

Volume of Burette Readings

Boiled Volume of Concordant
(in ml) Indicator
Water EDTA (V1) value
S. No.
(V2) Initial Final
(in ml) (in ml)
(in ml)

2 EBT

3. Calculation of permanent hardness:

Volume of standard EDTA Solution (V1) = ml

Strength of standard EDTA Solution (N1) = N

Volume of boiled water sample (V2) = ml

Strength of boiled water Sample (N2) = ?

According to the law of volumetric analysis, V1N1 = V 2 N2

Strength of boiled water sample (N2) = V1 x N1 / V2

N2 = N

Permanent hardness of water sample = N2 X Eq. wt of CaCO3 X 1000

= _________N X 50 X 1000

= __________ ppm

4. Calculation of Temporary Hardness:

Temporary hardness = Total hardness – Permanent hardness

= ……………... - ……………………

= ……………… ppm
TITRATION – III:

ESTIMATION OF PERMANENT HARDNESS:

100 ml of the given sample of hard water is taken in a clean 250 ml

beaker and boiled for 10-15 minutes. It is then cooled and filtered. The filtrate is
collected in a 100ml standard flask. 20 ml of this made up solution is pipetted out
into a clean conical flask. 5 ml of ammonia buffer solution and 2 drops of
Eriochrome Black – T indicator are added. The solution turns wine red in colour.
This solution is titrated against EDTA solution taken in the burette. The change of
wine red colour into steel blue colour is the end point. The titration is repeated to
get concordant values.

RESULT:

1. Amount of temporary hardness of the given water sample = ______ ppm

2. Amount of permanent hardness of the given water sample = ______ ppm
3. Amount of total hardness of the given water sample = ______ ppm
 TITRATION – I: STANDARDISATION OF SILVER NITRATE
(Std. NaCl vs. AgNO3)
Burette Readings Volume of
Volume of Concordant
(ml) Silver
NaCl value Indicator
S. No. nitrate
Initial Final
(V1) (ml) (ml)
(V2) (ml)

2 K2CrO4

Calculation:

Volume of sodium chloride (V1) = 20 ml

Strength of sodium chloride (N1) = N

Volume of silver nitrate (V2) = ml

Strength of silver nitrate (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N 2

Strength of Silver nitrate (N2) = V 1 x N1 / V2

N2 = N
EXPT.No. NAME OF THE EXPERIMENT DATE

DETERMINATION OF CHLORIDE CONTENT OF WATER SAMPLE

BY ARGENTOMETRIC METHOD

AIM

To estimate the amount of chloride ion present in the given water sample by
argentometric method being supplied with standard solution of sodium chloride
and silver nitrate solution.
CHEMICALS REQUIRED
1. Sodium chloride
2. Silver nitrate
3. Potassium chromate
4. Water sample

MATERIALS REQUIRED
Burette, Pipette & Conical flask

PRINCIPLE
Generally water contains chloride ions in the form of NaCl, KCl, CaCl 2
and MgCl2. The concentration of chloride ions more than 250 ppm is not desirable
for drinking purpose. The total chloride ions can be determined by argentometric
method (Mohr’s Method). In this method ion solution is directly titrated
against AgNO3 using potassium chromate (K2CrO4) as the indicator.

At the end point, when all the ions are removed, the yellow colour of chromate
changes into reddish brown due to the following reaction.
 TITRATION – II : ESTIMATION OF CHLORIDE ION
(Std. AgNO3 vs. water sample)
Volume of Burette Readings Volume of
Concordant
Water (ml) Silver
S. No. value Indicator
sample nitrate
Initial Final
(V2) (ml) (ml)
(V1) (ml)

2 K2CrO4

Calculation:

Volume of Silver nitrate (V1) = ml

Strength of Silver nitrate (N1) = N

Volume of Water sample (V2) = 20 ml

Strength of Water sample (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of Water sample (N2) = V 1 x N 1 / V2

Strength of Water sample (N2) = N

Amount of Cl- ion in the water sample = Eq.Wt. of chlorine X N2

= 35.45 X

= mg/lit
PROCEDURE
TITRATION – I: STANDARDISATION OF AgNO3

The burette is washed well with distilled water and rinsed with the small
amount of AgNO3 solution. It is then filled with the same solution up to the zero
mark without any air bubbles.

The pipette is washed with distilled water and rinsed with the small amount
of standard NaCl solution. 20 ml of this solution is pipetted out into a clean conical
flask. 1 ml of 2% K2CrO4 indicator solution is added and titrated against AgNO 3
solution taken in the burette. The end point is the change of colour from yellow to
reddish brown. The titration is repeated for concordant values.

TITRATION – II : ESTIMATION OF CHLORIDE ION

20 ml of the given water sample is pipetted out into a clean conical flask and
1 ml of 2% of K2CrO4 indicator solution is added. It is then titrated against
standardized AgNO3 solution taken in the burette. The end point is the change of
colour from yellow to reddish brown.

RESULT:

Amount of chloride ion present in the given water sample = mg/lit

 TITRATION OF HCl Vs. NaOH

Volume of
S.No NaOH pH pH V(ml) pH/V
(ml)
EXPT.No. NAME OF THE EXPERIMENT DATE

DETERMINATION OF STRENGTH OF GIVEN HYDROCHLORIC ACID

USING pH METER

AIM:

To determine the strength of given HCl present in the given sample by pH meter.
A standard solution of NaOH is provided.

CHEMICALS REQUIRED:

1. NaOH
2. HCl

MATERIALS REQUIRED:

1. pH meter
2. Glass electrode
3. Beaker
4. Burette, pipette, Glass rod etc.,

PRINCIPLE:

Since the pH of the solution is related to the H + ion concentration by the

following formula,

pH = - log [H+]

Measurement of pH of the solution gives the concentration of H + ions in

the solution. When NaOH is added slowly from the burette to the solution of HCl, the
fast moving H+ ions are progressively replaced by slow moving Na + ions. As a result
pH of the solution increases.

HCl + NaOH  NaCl + H2O

Increase in pH takes place until all the H + ions are completely

neutralized (upto the end point). After the end point, further addition of NaOH
increases pH sharply as there is an excess of fast moving OH – ions.
Calculation:

Volume of NaOH (V1) = ml

Strength of NaOH (N1) = N

Volume of HCl (V2) = ml

Strength of HCl (N2) = ?

According to the law of volumetric analysis, V1N1 = V 2 N2

Strength of HCl (N2) = V1 x N1/ V2

Strength of HCl (N2) = N

Amount of HCl present in whole of the given solution = Eq.Wt. of HCl X N2

= 36.5 X

= g
PROCEDURE:

The burette is filled with std. NaOH solution. Exactly 20 ml of the given HCl
solution is pipetted out into a clean beaker. It is then diluted to 20 ml by adding
distilled water. The glass electrode is dipped in it and connected with a pH meter.

Now NaOH solution is gradually added from the burette to the HCl solution
taken in the beaker and pH of the solution is noted for each addition. This process is
continued until at least 5 readings are taken after the end point. The observed pH
values are plotted against the volume of NaH added. From the graph the end point is
noted.

RESULT:

1. Strength of HCl present in whole of the given solution = _______ N

2. Amount of HCl present in whole of the given solution = _______ g

TITRATION OF MITURE OF ACIDS VS STRONG BASE

(CH3COOH+HCl Vs. NaOH)

Volume of NaOH Conductance

S.No.
added (ml) (mho)
EXPT.No. NAME OF THE EXPERIMENT DATE

DETERMINATION OF STRENGTH OF ACIDS IN A MIXTURE OF ACIDS

USING CONDUCTIVITY METER

AIM

To determine the amount of a strong acid and a weak acid (HCl and CH 3COOH)
present in one litre of the given mixture of acid solution by conductometric titration
using standard NaOH.

CHEMICALS REQUIRED

1. NaOH
2. HCl & CH3COOH

MATERIALS REQUIRED

1. Conductivity meter
2. Conductivity cell
3. Beaker
4. Burette, pipette, glass rod etc.,

PRINCIPLE

Solution of electrolytes conducts electricity due to the presence of ions. Since

specific conductance of a solution is proportional to the concentration of ions in it,
conductance of the solution is measured during titration.

When the sodium hydroxide is added slowly from the burette to the solution,
HCl (strong acid) gets neutralized first. Since the fast moving H + ions are replaced by
slow moving Na+ ions, decrease in conductance take place until the end point is
reached.

HCl + NaOH  NaCl + H2O (First neutralization)

After the complete neutralization of all HCl, the neutralization of CH 3COOH starts,

CH3COOH + NaOH  CH3COONa + H2O (Second neutralization)

Since CH3COONa is stronger electrolyte than CH3COOH, conductivity slowly

increases until all CH3COOH is completely neutralized. When the end point is
reached, addition of NaOH will cause sudden increase in the conductance. This is
due to the presence of fast moving OH– ions.

TITRATION OF MIXTURE OF ACIDS (HCl + CH3COOH) Vs NaOH

Calculation:

(i) HCl:
Volume of NaOH (V1) = ml

Strength of NaOH (N1) = N

Volume of HCl (V2) = ml

Strength of HCl (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of HCl (N2) = V 1 x N 1 / V2

Strength of HCl (N2) = N

Amount of HCl present in whole of the given solution = Eq.Wt. of HCl X N2

= 36.5 X

= g
PROCEDURE

The burette is washed well with water and rinsed with the given
standard NaOH solution. It is then filled with NaOH solution up to the zero level. 20
ml of the given mixture of acids (HCl + CH 3COOH) is pipetted out into a clean 100 ml
beaker.

The conductivity cell is placed in it and then diluted to 50 ml by adding

conductivity water, so that the electrodes are well immersed in the solution. The
two terminals of the cell are connected with a conductivity bridge.

Now 1 ml of NaOH from the burette is added to the solution, taken in

the beaker, stirred for some time and then conductivity is measured. (The
conductivity is going on decreasing up to the end point). This process is repeated
until at least five readings are taken after the end point (A) has been reached.

After the end point, again NaOH is gradually added, which causes
increase in conductance. This increase in conductance is observed until the end
point (B) is reached.

After the second end point, sudden increase in conductance is observed

on further addition of NaOH. The reading (conductivity) is continuously measured
for each addition of NaOH and are tabulated. Now the graph is plotted between the
volume of NaOH Vs conductance. From the graph the first end point (A) and the
second end point (B) are noted. From the end points the amount of HCl and
CH3COOH present in 1 litre of the mixture of solution is calculated.
(ii) CH3COOH:

Volume of NaOH (V1) = ml

Strength of NaOH (N1) = N

Volume of CH3COOH (V2) = ml

Strength of CH3COOH (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of CH3COOH (N2) = V 1 x N 1 / V2

Strength of CH3COOH (N2) = N

Amount of CH3COOH present in the given solution = Eq.Wt. of CH3COOH X N2

= 60 X

= g
RESULT

1. Strength of HCl = N
2. Strength of NaOH = N

3. The amount of HCl present in the given solution = g

4. The amount of CH3COOH present in the given solution = g

TABLE - 1

(BaCl2 Vs. Na2SO4)

Volume of Na2SO4 Conductance

S.No
added (ml) (mho)
EXPT.No. NAME OF THE EXPERIMENT DATE

CONDUCTOMETRIC TITRATION OF BARIUM CHLORIDE AGAINST SODIUM

SULPHATE (PRECIPITATION TITRATION)

AIM:
 To determine the amount of BaCl2 present in the given solution by
conductometric titration using standard Na2SO4 solution.

CHEMICALS REQUIRED

1. Standard Na2SO4 solution

2. BaCl2 solution

MATERIALS REQUIRED:

1. Conductivity meter
2. Conductivity cell
3. Beaker
4. Burette, pipette, glass rod etc.,

PRINCIPLE:

Solution of electrolytes conducts electricity due to the presence of ions. Since

specific conductance of a solution is proportional to the concentration of ions in it,
conductance of the solution is measured during titration.

In the precipitation titration, the ions are converted into insoluble

precipitate, which will not contribute to the conductance. When Na 2SO4 is added
slowly from the burette to the solution of BaCl 2, BaSO4 gets precipitated while the
chloride ions remain unchanged.

BaCl2 + Na2SO4  BaSO4 + 2NaCl

The Ba2+ ions in the solution are replaced by free Na + ions are less than that
of Ba2+ ions, the conductance of the solution decreases. After the end point, when all
the Ba2+ ions are replaced, further addition of Na 2SO4 increases the conductance.
This is due to the increase of Na+ and SO42- ions in the solution.
 Calculation:

Volume of BaCl2 (V1) = ml

Strength of BaCl2 (N1) = ?

Volume of Na2SO4 (V2) = ml

Strength of Na2SO4 (N2) = N

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of BaCl2 (N1) = V 2 x N 2 / V1

Strength of BaCl2 (N1) = N

Amount of BaCl2 present in whole of the given solution = Eq.Wt. of BaCl2 X N1

= 122.14 X

= g
PROCEDURE:

The burette is washed well with water and rinsed with the given standard
Na2SO4 solution. It is then filled with Na 2SO4 solution up to the zero level. 20ml of
the given BaCl2 solution is pipetted out into a clean 100ml beaker then diluted to
40ml by adding conductivity water, so that the electrodes are well immersed in the
solution. The two terminals of the cell are connected with a conductivity bridge.

Now 1ml of Na2SO4 from the burette is added to the solution, taken in the beaker,
stirred for some time and then conductivity is measured. (The conductivity is going
on decreasing up to the end point.) This process is repeated until at least five
readings are taken after the end point has been reached.

After the end point, sudden increase in conductance is observed on further addition
of Na2SO4. The reading (conductivity) is continuously measured for each addition of
Na2SO4 and are tabulated. Now the graph is plotted between the volume of Na 2SO4
Vs conductivity. From the graph, the end point is noted. From the end point the
amount of BaCl2 present in 1 litre of the solution is calculated.

RESULT:

1. The amount of BaCl2 present in whole of the given solution =

g
 TITRATION OF FAS Vs. K2Cr2O7

Volume of
EMF
S.No K2Cr2O7 E V(ml) E/V
(in mho)
(in ml)
EXPT.No. NAME OF THE EXPERIMENT DATE

ESTIMATION OF IRON CONTENT OF THE GIVEN SOLUTION

USING POTENTIOMETER

AIM:
 To estimate the amount of ferrous ion present in the whole of the given
solution poteniometrically. A standard solution of potassium dichromate is
provided.

CHEMICALS REQUIRED:

Potassium dichromate, Ferrous ammonium sulphate & sulphuric acid.

MATERIALS REQUIRED:

Platinum electrode, Saturated calomel electrode, Beaker, Burette, Pipette &

Glass rod.

PRINCIPLE:

Potentiometric titration depends on measurement of emf between reference

electrode and an indicator electrode. When a solution of ferrous iron is titrated with
a solution of potassium dichromate, the following redox reaction takes place.

6Fe2+ + Cr2O + 14H+ 6Fe3+ + 2Cr3+ + 7H2O

During this titration Fe2+ is converted into Fe3+, whose concentration increases.
At the end point, there will be a sharp change due to sudden removal of all Fe 2+ ions.

The cell is set up by connecting this redox electrode with a calomel electrode
as shown below:

A graph between emf measured against the volume of K 2Cr2O7 added is

drawn and the end point is noted from the graph.
Calculation:

Volume of K2Cr2O7 solution (V1) = ml

Strength of K2Cr2O7 solution (N1) = N

Volume of Ferrous ion solution (V2) = ml

Strength of Ferrous ion solution (N2) = ?

According to the law of volumetric analysis, V1N1 = V2 N2

Strength of Ferrous ion solution N2 = V 1 x N 1 / V2

= N

Amount of Ferrous ion present in given solution = Eq.Wt. of Fe x N2

= 55.85 x N

= g
PROCEDURE:

The given ferrous iron solution is made upto 100 ml in a standard flask. 20
ml of this made up solution is pipetted out into a clean 100 ml beaker. About 10 ml
of dil H2SO4 and 20 ml of distilled water are added in it. A platinum electrode is
dipped into the solution. This electrode is then coupled with a saturated calomel
electrode and the cell is introduced into potentiometric circuit. The std. K 2Cr2O7
solution is taken in the burette and is added.

TITRATION – I :

First a preliminary titration is carried out by adding std. K 2Cr2O7 solution in

portions of 1 ml and the emf of the cell is measured after each addition. The
addition of K2Cr2O7 is continued even after the end point and the range at which end
point lies is found out by plotting volume of K2Cr2O7 added against emf (graph-I).

TITRATION – II:

Another titration is carried out by adding std. K 2Cr2O7 solution in portions of

0.1 ml near the end point and the emf of the cell is measured after each addition.
The addition of K2Cr2O7 is continued even after the end point for further 1 ml. The
accurate end point is determined by plotting E/V Vs Volume of K2Cr2O7 added
(graph-2). From the end point, the strength of ferrous iron solution and hence its
amount can be calculated.

RESULT :

Amount of Ferrous ion present in whole of the given solution = g

VIVA QUESTIONS
 VIVA –VOCE QUESTIONS

 COMMON QUESTIONS FOR ALL EXPERIMENTS:

1. What is the aim of your experiment?
2. What are the chemicals used in your experiment?
3. What is the equivalent weight of given chemical?
4. What is the name of the indicator used?
5. What is the unit used in the result of your experiment?
6. What is the principle of your experiment?

DETERMINATION OF ALKALINITY OF WATER SAMPLE

1. What is alaklinity?
 It is a nature of the water.
 Its pH value is greater than 7. ( for acid pH = less than 7, for water pH = 7)
 Definition 1: excess of hydroxide, carbonate & bicarbonate present in water
sample.
 Definition 2: acid neutralising property of water.

2. What are the indicators used & what is the colour change of indicators?
 Phenolphthalein (HpH) – pink to colourless
 Methyl orange (MeoH) – yellow to reddish orange

3. Why two different indicators are used for same experiment?

There are three types of alkalinity. They are: hydroxide alkalinity, carbonate
alkalinity and bicarbonate alkalinity.
Phenolphthalein indicator is used to determine hydroxide alkalinity & one
half of carbonate alkalinity.
Methyl orange indicator is used to determine bicarbonate alkalinity &
another half of carbonate alkalinity.
If one indicator is used, it is difficult to identify the two other alkalinties.
Hence two indicators are used.

4. Questions from reference table (See page No. 18)

For example, what are ions responsible for alkalinity if P = 0?

5. What is the unit of alkalinity?

mg/ litre or ppm

6. What is ideal amount of alkalinity in drinking water?

100 – 150 ppm
 DETERMINATION OF TOTAL, TEMPORARY & PERMANENT HARDNESS OF
WATER SAMPLE BY EDTA METHOD

1. Define hardness

It is a charecteristics of water which does not produce lather with soap.

2. Define temporary hardness

This is due to bicarbonates of calcium and magnesium.

Temporary hardness = total hardness – permanent hardness

3. Define permanent hardness

This is due to presence of chlorides, sulphates of calcium and magnesium.

Permanent hardness = total hardness – temporary hardness

4. Define total hardness

Total hardness = temporary hardness + permanent hardness

5. Define hard water & soft water

Hard water: water which does not produce lather with soap.

Soft water: water produces lather with soap.

6. What is carbonate hardness & non-carbonate hardness?

Carbonate hardness: this is due to bicarbonates of calcium and magnesium.

Non-carbonate hardness: this is due to presence of chlorides, sulphates of calcium

and magnesium.

7. What are the units of hardness?

PPM – Parts Per Million or mg/L – milligrams per litre or degree Clarke or degree
French

8. Draw the structure of EDTA. (See Page No. 18)

9. Abbreviation of EDTA.

Ethylene Diamine Tetra Acetic acid

10. Abbreviation of EBT.

Eriochrome Black –T (here ‘T’ indicates grade)

11. What is the name of the buffer? Why it is used?

Ammonia buffer is used. It is a mixture of ammonium chloride & ammonium

hydroxide.during the reaction complex compound is formed. For getting complex
compund we need to maintain the pH value between 8 and 10. Ammonia buffer is
used to maintain this pH value throughout the reaction. Hence ammonia buffer is
used.

12. Principle of EDTA method

First, EBT indicator reacts with hardness causing ions (calcium and magnesium)
and form an EBT - weak complex compound. Hence wine red colour is formed.

After adding EDTA, EBT indicator separates from the complex and form an EDTA -
strong complex compound. Hence steel blue colour is formed.

From this strong complex we can determine the hardness.

13. Structure of EDTA:

14. Structure of EBT:

 DETERMINATION OF DO CONTENT IN WATER

1. What is dissolved oxygen?

Amount of oxygen dissolved in unit volume of water. It is essential for the
maintenance of healthy lake and river.
2. What is the minimum amount of dissolved oxygen that should be present in
drinking water?
In a healthy water body the DO is about 8 ppm. The minimum DO for survival of
aquatic life is 4 – 5 ppm.

3. Suggest a method to improve DO of the water sample.

 Promote photosynthesis
 Expose to pure oxygen environment
 Bubble pure oxygen into the water

4. What is the name of the method?

 Winkler’s method
 Winkler’s reagent is a mixture of potassium bromide and potassium
bromate.

5. What indicator is used & what is the end point?

Starch – disappearance of blue colour.

6. Why iodine flask is used?

During the estimation of DO, iodine gas is liberated. So iodine flask is used. Hence
the titration is called as iodometric method.

7. Why starch is not added at the beginning?

When starch is added at the beginning, it will form a blue coloured precipitate.
Hence iodine gas liberation is difficult.

8. What is the equivalent weight & molecular weight of oxygen?

Equivalent weight = 8
Molecular weight = 16
9. What is the unit of this method?
ppm (parts per million)

10. Explain the ranges & its impacts of DO in water

 0-2 mg/L: not enough oxygen to support life

 2-4 mg/L: only a few kinds of fish and insects can survive

 4-7 mg/L: acceptable for warm water fish

  7-11 mg/L: very good for most stream fish including cold water fish

 Below 60%: poor; water too warm or bacteria using up DO

 60-79%: acceptable for most aquatic organisms

 80-125%: excellent for most aquatic organisms

 112% or more: too high, may be dangerous to fish

DETERMINATION OF CHLORIDE CONTENT IN WATER

1. Forms of chloride ions

NaCl, KCl, CaCl2 & MgCl2
2. What are the effects of chloride?
 It rises the blood pressure
 It corrodes metal
 It may affect the kidney

3. What is the maximum permissible limit of chloride in water?

Maximum permissible limit of chloride in water – 250 mg/l

4. What is the name of the method & why it is mentioned so?

 Argentometric method
 Main chemical of this experiment is Silver Nitrate. Chemical name of Silver is
‘Argentum (Ag)’. Hence this experiment is mentioned as Argentometric
Method.

5. What indicator is used & what is the colour change of it?

Potassium chromate – yellow to reddish brown

6. What is the equivalent weight of chloride ion?

35.46

7. What is the unit of this method?

Grams

pH METER

1. Define pH

pH is the negative logarithm of H+ ion concentration.

2. Name of the electrode used

Glass electrode (or) pH electrode

3. What indicator is used?

No indicator is used. Instead graph is used to identify the end point.

4. Equivalent weight of HCl

For H = 1 & for Cl = 35.45. Hence for HCl = 1+35.45 = 36.45

5. Explain the graph

Initially, low pH value (this is due to HCl). After adding NaOH to the beaker,
pH value slowly increased. At one stage it reaches the end point (this is due to
neutralization of HCl & NaOH). Further addition of NaOH increases pH sharply as
there is fast moving OH- ions.

CONDUCTOMETRIC TITRATION

1. Define conductance

Definition 1: reciprocal of resistance.

Definition 2: ability of a material to conduct electricity.

Definition 3: ability of a material which allow electron to pass through.

Definition 4: ability of an electrolyte to conduct electricity and involves ionization.

2. What is the principle of Conductometric Titration?

Conductance

3. What are the electrodes used?

Here electrodes are not used. Instead, we are using conductivity cell.

4. Advantages of Conductometric titration

 This titration is used for colourless solutions

 Accurate end point is obtained thro’ graph
 Dilute solutions & weak acids are also used
 No need to keen observation

5. Disadvatages of conductometric titration

  Only limited types of titrations can be carried out.
 High concentrated solutions are not used.

6. Why indicator is not used?

It is an electrical experiment. Hence no need of indicator.

7. How to identify the end point without indicator?

Thro’ graph

8. Explain the graph for strong acid vs strong base

Initially, the solution has high conductance. This is due to fast moving H + ions.

After adding sodium hydroxide, the conductance of the solution decreased. This is
due fast moving H+ ions are replaced by slow moving Na+ ions.

After end point, conductance will increase. This is due to excess of adding hydroxide
ions.

9. Explain the graph for mixture of acids

Initially, the solution has high conductance. This is due to fast moving H + ions.

After adding sodium hydroxide, dissociation of HCl will occur. The conductance of
the solution decreased. This is due fast moving H + ions are replaced by slow moving
Na+ ions.

After this, dissociation of CH3COOH will occur. The conductance of the solution
slowly increased. This is due fast moving H + ions are replaced by slow moving
CH3COO- ions.

After end point, conductance will increase. This is due to excess of adding hydroxide
ions.

10. How many end points are obtained?

For strong acid – strong base experiment – one end point

For precipitation experiment – one end point

For mixture of acids experiment – two end points

POTENTIOMETRIC TITRATION

1. Define EMF
EMF – electromotiveforce. It is defined as “difference of potential which causes flow
of current from one electrode of higher potential to the other electrode of lower
potential is known as EMF.”

Ecell = Eright - Eleft

2. What is the principle of potentiometric titration?

Redox reaction (both reduction & oxidation)

3. What are the electrodes used?

Indicator electrode or working electrode is – platinum electrode

Refrence electrode – saturated calomel electrode

4. Advatages of potentiometric titration

 We can use this titration for both colour and colourless solutions
 Accurate end point is obtained thro’ graph.
 Dilute solutions are used
 No need of keen observation

5. Why indicator is not used?

It is an electrical experiment. Hence no need of indicator.

6. Indicator is not used here. Then, how to identify the end point?

Thro’ graph

7. What are the components of calomel electrode?

Mercury, mercurous chloride & saturated KCl

8. Explain the graph - I.

Graph I - ‘S’ graph – initially low potential and during the process potential is
gradually increased and at one stage potential remains constant.

ESTIMATION OF IRON CONTENT OF THE WATER SAMPLE

BY SPECTROPHOTOMETER

1. What is spectroscopy?
 It deals with the study of interaction of electromagnetic radiation with the
matter.
 The instrument used to study spectroscopy is ‘spectrophotometer’.
  Principle of spectrophotometer is Beer – Lambert’s law.
2. State Beer-Lambert’s law
When a beam of monochromatic radiation is passed through a sloution of an
absorbing substance, the ratre of decrease of intensity of radiation ‘dI’ with
thickness of the absorbing solution ‘dx’ is proportional to the intensity of incident
radiation ‘I’ as well as the concentration of the solution ‘C’.
3. Write the mathematical form of Beer-Lambert’s law?
-dI/dx = kIC or A = εCx
4. What is another name of spectrophotometer?
Colorimeter
5. What is the range of wavelength applied in spectrophotometer?
480nm
6. How to reduce iron from the water?
 By adding softener
 By using iron filter
 By ion – exchange method
 SHORT
PROCEDURE
 DETERMINATION OF ALKALINITY OF WATER SAMPLE

TITRATION - I

STANDARDISATION OF HYDROCHLORIC ACID SOLUTION

BURETTE SOLUTION HCl

PIPETTE SOLUTION NaOH
INDICATOR Phenolphthalein
INITIAL COLOUR Pink
END POINT Colourless
FORMULA V1N1 = V2N2

TITRATION - II

ESTIMATION OF ALKALINITY

BURETTE SOLUTION HCl

PIPETTE SOLUTION Water Sample
INDICATOR - I Phenolphthalein
INITIAL COLOUR - I Pink
END POINT - I Colourless
INDICATOR - II Methyl Orange
INITIAL COLOUR - II Yellow
END POINT - II Reddish Orange
FORMULA - I V1N1 = V2N2
FORMULA - II N2 X Eq. wt of CaCO3 X 1000

Equivalent weight of calcium carbonate = 50

 DETERMINATION OF TOTAL, TEMPORARY & PERMANENT HARDNESS

OF WATER SAMPLE BY EDTA METHOD

TITRATION I
STANDARDISATION OF EDTA SOLUTION

BURETTE SOLUTION EDTA

PIPETTE SOLUTION Std. Hard Water
ADDITIONAL SOLUTION Ammonia Buffer
INDICATOR EBT
INITIAL COLOUR Wine Red
END POINT Steel Blue
FORMULA V1N1 = V2N2

TITRATION II

ESTIMATION OF TOTAL HARDNESS

BURETTE SOLUTION EDTA
PIPETTE SOLUTION Hard Water sample
ADDITIONAL SOLUTION Ammonia Buffer
INDICATOR EBT
INITIAL COLOUR Wine Red
END POINT Steel Blue
FORMULA - I V1N1 = V2N2
FORMULA - II N2 X Eq. wt of CaCO3 X 1000

TITRATION III

ESTIMATION OF PERMANENT HARDNESS

BURETTE SOLUTION EDTA
PIPETTE SOLUTION Boiled Water sample
ADDITIONAL SOLUTION Ammonia Buffer
INDICATOR EBT
INITIAL COLOUR Wine Red
END POINT Steel Blue
FORMULA – I V1N1 = V2N2
FORMULA - II Temporary hardness =
Total hardness – permanent hardness

Equivalent weight of calcium carbonate = 50

DETERMINATION OF DO CONTENT OF WATER BY WINKLER’S METHOD

TITRATION I – STANDARDISATION OF SODIUM THIOSULPHATE

BURETTE SOLUTION sodium thiosulphate solution

PIPETTE SOLUTION 20 ml of potassium dichromate solution
ADDITIONAL SOLUTION 5 ml H2SO4 + 15 ml of 5% KI
INDICATOR Starch
INITIAL COLOUR Blue
END POINT Disappearance of blue colour
FORMULA V1N1 = V2N2

TITRATION II – DETERMINATION OF CHLORIDE IONS

BURETTE SOLUTION sodium thiosulphate solution

PIPETTE SOLUTION 20 ml Sample Water Sample
ADDITIONAL SOLUTION 2 ml manganous sulphate + 2 ml alkali
iodide + 2ml of conc. H2SO4
INDICATOR Starch
INITIAL COLOUR Blue
END POINT Disappearance of blue colour
FORMULA 1 V1N1 = V2N2
FORMULA 2 Normality X Equivalent Weight of O2

EQUIVALENT WEGHT OF OXYGEN = 8

 DETERMINATION OF CHLORIDE CONTENT IN WATER
BY ARGENTOMETRIC METHOD

TITRATION I – STANDARDISATION OF SILVER NITRATE

BURETTE SOLUTION Unknown silver nitrate solution

PIPETTE SOLUTION 20 ml of standard sodium chloride solution
INDICATOR 1 ml of 2% K2CrO4 solution
INITIAL COLOUR Yellow
END POINT Reddish Brown
FORMULA V1N1 = V2N2

TITRATION II – DETERMINATION OF CHLORIDE IONS

BURETTE SOLUTION Standard Silver Nitrate Solution

PIPETTE SOLUTION 20 ml Sample Water
INDICATOR 1 ml of 2% K2Cr2O4 Solution
INITIAL COLOUR Yellow
END POINT Reddish Brown
FORMULA 1 V1N1 = V2N2
FORMULA 2 Normality X Equivalent Weight of Chloride ion

EQUIVALENT WEGHT OF CHLORIDE ION = 35.45

 DETERMINATION OF STRENGTH OF HCl BY NaOH BY pH METHOD

BURETTE SOLUTION Standard Sodium Hydroxide Solution

PIPETTE SOLUTION 20 mL OF Hydrochloric Acid Solution
ADDITIONAL SOLUTION 20 mL Distilled Water
REACTION HCl + NaOH NaCl + H2O
GRAPH – I (‘S’ GRAPH) Volume of NaOH (X-axis) vs. pH (Y-axis)
GRAPH – II (INVERTED ‘V’ GRAPH) Volume of NaOH (X- axis) vs. Δ pH/ΔV(Y-axis)
FORMULA 1 V1N1 = V2N2
FORMULA 2 Normality X Equivalent Weight of HCl

 MODEL GRAPH – I :

 MODEL GRAPH – II :
 EQUIVALENT WEGHT OF HYDROCHLORIC ACID = 36.45

CONDUCTOMETRIC TITRATION – MIXTURE OF ACIDS VS STRONG BASE

BURETTE SOLUTION NaOH

PIPETTE SOLUTION 10 ml Acetic Acid + 10 ml HCl + 20 mL of
Distilled Water
STEP 1 Conductivity cell is placed in the beaker &
connected it with a conductivity meter
STEP 2 Add 1 ml of NaOH from the burette to the
beaker solution & stirred
STEP 3 Conductance for each addition is noted
REACTION 1 HCl + NaOH NaCl + H2O
REACTION 2 CH3COOH + NaOH CH3COONa + H2O
GRAPH Volume of NaOH (X-axis) vs. Conductance
(Y-axis)
FORMULA 1 V1N1 = V2N2
FORMULA 2 Normality X Equivalent weight of HCl
FORMULA 3 Normality X Equivalent weight of Acetic Acid

MODEL GRAPH:

Equivalent weight of HCL=36.45

 Equivalent weight of CH3COOH=60

ESTIMATION OF IRON CONTENT OF THE GIVEN SOLUTION USING POTENTIOMETER

BURETTE SOLUTION K2Cr2O7

PIPETTE SOLUTION FAS
ADDITIONAL SOLUTION dil.H2SO4 + distilled water
ELECTRODE - I Calomel Electrode
ELECTRODE - II Platinum Electrode
GRAPH - I Volume of K2Cr2O7 (X-axis)
&
EMF (Y-axis)
GRAPH - II Volume of K2Cr2O7 (X-axis)
&
ΔE / ΔV (Y-axis)
FORMULA - I V1N1 = V2N2
FORMULA - II N2 X Eq. wt of Ferrous

MODEL GRAPH - I

MODEL GRAPH - II
 Equivalent weight of iron = 55.85

ESTIMATION OF IRON CONTENT OF WATER BY SPECTROPHOTOMETRY

 The spectrophotometer is switched on and warmed up for 10 minutes.

 Prepare 0.01 N, 0.02 N, 0.03 N, 0.04 N & 0.05 N solutions.

 Fix the wave length ( λ ) = 480 nm

 Set absorbance = 0 & transmittance = 100 with distilled water

 Now absorbance of all solutions is measured in the similar way.

 Finally, absorbance of unknown solution is measured

 Graph - Concentration (X-Axis) Vs. Absorbance (Y-Axis)

 FORMULA – Normality Unkown Solution X Equivalent Weight of iron X 1000

MODEL GRAPH:
 Equivalent weight of iron = 55.45

CONDUCTOMETRIC TITRATION – PRECIPITATION TITRATION

BURETTE SOLUTION Na2SO4

PIPETTE SOLUTION 10 ml of BaCl2 + 20 ml of Distilled Water
STEP 1 Conductivity cell is placed in the beaker &
connected it with a conductivity meter
STEP 2 Add 1 ml of Na2SO4 from the burette to the
beaker solution & stirred
STEP 3 Conductance for each addition is noted
REACTION BaCl2 + Na2SO4  BaSO4 + 2NaCl

GRAPH Volume of Na2SO4 added (X-axis) vs.

Conductance (Y-axis)
FORMULA 1 V1N1 = V2N2
FORMULA 2 Amount of BaCl2 present in whole of the
given solution = Eq.Wt. of BaCl2 X N1

MODEL GRAPH:
Equivalent weight of BaCl2 = 122.14