APPLIED SCIENCE CHEMISTRY JOURNAL

NAME: SHRUTI MANOJ CHAVAN

DIV: A BATCH: A12 ROLL NO.: 21

INDEX
SR NO. TITLE

1. Exp1: Estimation of copper in brass.

2. Exp2: To determine heat of

neutralization of strong acid by strong
base.

3. Exp 3: Verification of Henderson’s

equation.

4. Exp 4: Determination of the strength of

the given HCl to that of NaOH.

5. Exp 5: Paper chromatographic

separation and identifying the metals.
 CERTIFICATE

CLASS : A YEAR: 2019 – 20

This is to certify that the work entered in this journal is the work of Miss.

SHRUTI MANOJ CHAVAN of FYBTECH( CST ) division A roll no. 21

has satisfactorily completed the required number of practicals and worked for the

both terms of the year 2019 – 2020 in the college laboratory as per laid down by the

university.

Head of the External examiner Internal examiner

department ssubject
[((subject teac

DATE: 04 / 05 / 2020 DEPARTMENT OF APPLIED CHEMISTRY

 EXP 1: ESTIMATION OF COPPER IN BRASS

AIM:

1.9846 gram of sample of brass is dissolved in conc. HNO 3 and the solution
is boiled with urea to destroy the nitrogen oxides. The resulting solution is placed
in a 250 cm3 standard measuring flask. Estimate the amount of copper in the
solution. Your provided with an approximately decinormal solution of sodium
thiosulphate and pure crystals of the potassium dichromate.

PRINCIPLE:

Brass is the alloy of copper and zinc with a little Sn, Pb and Fe. Copper in the
given brass solution is estimated iodimetrically. First sodium thiosulphate is
standardized using standard potassium dichromate solution. A definite volume of
K2Cr2O7 solution is treated with KI solution in the presence of conc. HNO 3. The
liberated iodine is titrated against sodium thiosulphate solution using starch as
indicator towards the end point.

Secondly, the given brass solution is made up to the mark. A known

volume of this solution after being made neutral is treated with KI solution and
the iodine liberated is titrated against standardized sodium thiosulphate solution
using starch as the indicator towards the end.

APPARATUS:

Digital balance, burette, conical flask, measuring flask, funnel, glass rod,
beakers, etc.

REAGENTS:

Bleaching powder, standardized sodium thiosulphate solution (0.1 N), 10%

potassium iodide solution, dilute acetic acid and freshly prepared starch solution
as indicator.
PROCEDURE:

1) Standardization Of Sodium Thiosulphate Solution:

25 ml of the standard K2Cr2O7 solution is pipette out into a clean

conical flask. About 5 ml of concentrated HCl and 20 ml of 10%
KI solution are added and the flask is kept aside for a minute. The
solution is diluted with two test tubes full of distilled water. The
liberated iodine is titrated against sodium thiosulphate solution
from the burette till the reaction mixture becomes greenish-
yellow in color. Now 2 ml of freshly prepared starch is added as
indicator and the addition of Na2S203 solution is continued till
the deep blue color just disappears leaving behind the green
solution of chromic salt. The titration is repeated for concordant
values.

2) Estimation Of Copper :

The given brass solution is made up to the mark in the 250ml

standard clean conical flask. The given ammonium
hydroxide solution added drop wise till a bluish white precipitate
is obtained. The precipitate is then just dissolved by adding
acetic acid drop wise. About 30 ml of 10% of KI solution is
added and the flask is kept aside for a minute. The liberated
iodine is titrated against Na2S203 solution from the burette till the
reaction mixture turns straw yellow. Now starch is added and the
titration is continued till the deep blue color just disappears
leaving behind the white precipitate of cuprous oxide. Then the
titration is repeated for concordant values.

EQUATIONS:
 1) K2Cr2O7 + 8HCl 2KCl + 2CrCl2 + 4H2O + 3(O)
{2KI + 2HCl + (O) 2KCl + H2O + I2} * 3
---------------------------------------------------------------
K2Cr2O7 + 14HCl + 6KI 8KCl + 2CrCl3 + 7H2O + 3I2
---------------------------------------------------------------

2) 2Cu(NO3)2 + 4KI neutral or faintly acidic

CU2I2 + 4KNO3 + I2
3) I2 + Na2S203 2NaI + Na2S204

OBSERVATIONS AND CALCULATIONS:

1) Standardization Of Solution :
a. Scheme of titration:
i. Burette: Na2S2O3 Solution (to be standardized)
ii. Conical Flask: 10 ml of 0.1 N K2Cr2O7 + 10 ml of dil.
H2SO4 + 10 ml of 10% of KI
iii. Indicator used: 2 ml of freshly prepared starch (near end
point)
iv. End point: Disappearance of deep blue color

b. Titration table:

VOL OF BURETEE READINGS

BRASS (ml) VOL. OF SODIUM
SR NO. IN THIOSULPHATE
CONICAL INITIAL FINAL USED UP (ml)
FLASK
1 10 0 12 ml

2 10 0 12 ml 12 ml

3 10 0 12 ml

i. Vol. of potassium dichromate V1 = 10 ml

ii. Strength of potassium dichromate N 1 = 0.1 N
iii. Vol. of sodium thiosulphate V2 = 11 ml
iv. Strength of sodium thiosulphate N2 = ?
V 1 * N1 = V 2 * N2
N2 = ( V1 * N1 ) / V 2
= ( 10 * 0.1 ) / 11
= 0.091 N

2) Estimation Of Copper :

a. Scheme of titration:
v. Burette: Na2S2O3 solution (standardized)
vi. Conical flask: 10 ml 0f brass solution + ammonium
hydroxide followed by CH3COOH (drop wise) + 10 ml of
10% KI
vii. Indicator: 2 ml of freshly prepared starch towards the
end point.
viii. End point: Disappearance of dark blue color.

b. Titration table:
 VOL OF BURETEE READINGS
BRASS VOL. OF SODIUM
SR NO. (ml) IN THIOSULPHATE
CONICAL INITIAL FINAL USED UP (ml)
FLASK

1 10 0 12 ml

2 10 0 12 ml 12 ml

3 10 0 12 ml

i. Concordant volume of Na2S2O3 solution, v1 = 12 ml

ii. Normality of standard Na2S2O3 solution, N1 = 0.091 N
iii. Volume of brass, V2= 10 ml
iv. Normality of brass, N2 can be calculated by normality
formula i.e. N1 * V1 =N2 * V2
v. Therefore normality of brass, N2 = 0.1092 N
vi. Amount of copper available in brass = N2 * 63.5 = 6.9342
g/Lit
vii. Amount of copper present in 250 ml of solution =
(6.9342 * 250) / 1000
= 1.73355 g
viii. The percentage of copper available in the given
sample of brass
= (1.73355 * 100) / 1.9846
= 87.35 %

RESULT:
 The percentage of copper in the given solution of brass is 87.35 %.

EXP 2: TO DETERMINE THE HEAT OF NEUTRILIZATION OF

STRONG ACID BY STRONG BASE

AIM:-

To determine the heat of neutralization of strong acid by strong base.

THEORY:-

Chemical reactions usually accompany the formation and absorption of energy in the
form of heat. The branch of chemical science dealing with the study of heat and energy
changes is known as thermodynamics. The heat changes within a specific system can be
studied using the device calorimeter. Formation of chemical bonds releases energy in the form
of heat and hence known as an exothermic reaction. The reaction which is accompanied
absorption of heat is known as endothermic reaction. Calorimetry is a scientific term dealing
with the changes in energy of the system by measuring the heat exchanged with the
surroundings. In a broader sense it is defined to determine the heat released or absorbed in a
chemical reaction. A calorimeter is a device designed to measure heat of reaction or physical
changes and heat capacity. The device can be sophisticated and expensive or simple and
cheap.

A calorimeter consists of two vessels, outer vessel and an inner vessel. The space
between these vessels acts as a heat insulator and hence there is very little heat exchange in
between the inner and outer vessels. Thermometer measures the temperature of the liquid in
the inner vessel. The stirrer functions in such a way to stir the liquid to distribute the heat in
the entire vessel. The fibre rings in the calorimeter helps to hold the inner vessel hanging in
the center of the outer vessel. It also has an insulating cover or lid with holes for attaching the
stirring rod and thermometer.

A BRIEF OVERVIEW OF CALORIMETRIC REACTIONS:

A calorimeter contains water or other substances with known heat capacity. The heat,
denoted as Q released by a reaction or process is absorbed by the calorimeter and any
substances in the calorimeter. If the only other substance in the calorimeter is water, the
following energy balance exists:
Q = QCAL + QW
 Where, QCAL = The heat flow for the calorimeter.
QW = The heat flow for the water.

The individual heat flow rate can be directly related to the heat capacity and
temperature change for the substance. This can be denoted by the equation:
QCAL = CCAL * ΔT
QW = CW * ΔT
Where, CCAL = The heat capacity of the calorimeter.
CW = The heat capacity of the water.

Since the water and calorimeter are in thermal equilibrium they exhibit same ΔT value.
The energy change of a reaction that occurs at constant pressure is termed as the
enthalpy change or the heat of reaction.
The heat capacity, which is defined as the amount of heat required to raise the
temperature of a given quantity of a substance by one degree Celsius,( unit is J/ 0 C) of the
entire system, denoted by C, is represented as the sum of the heat capacities for the individual
components involved in the reaction process.
C = CCAL + CW

Note: Since the calorimeter is insulated there is no heat exchange with the surroundings.
This can be shown as:
QREACTION = -QCALORIMETER

It is noted that the calorimeter exists as a fixed unit and thus its heat capacity is also
thought to be having a fixed value. In some cases, where the amount of substance is varying,
an intensive measurement of heat capacity, specific heat capacity is employed to study the
reactions. Specific heat capacity is defined as the heat required for raising unit mass of
substance by one degree of temperature. It has the units J/g0 C.
The relation between the heat capacity and specific heat of a substance is denoted as:
C = ms
m= mass of substance in grams.
C= Heat capacity.
S= specific heat.

PRINCIPLE:
 A known volume of HCl solution of exactly known concentration is allowed to react with
a strong alkali in dilute solution. The temperature change is then noted. With the known
volume of HCl solution, the heat of neutralization can be calculated. It is the amount of heat
evolved when V cm3 of HCl solution of concentration C g/liter equilibrium dcm -1 is neutralized
completely. Thus,
HEAT OF NEUTRALIZATION = (1000 * Q) / (V * C)
Q = (50 + W) * (T3 – T1) + 50(T3 – T2)
Where, Q = The amount of heat gained (cal).
V = The volume of acid (cm3).
C =The concentration of acid (g/L).

 Graph of Heat of Neutalization

MATERIALS REQUIRED:-Calorimeter, Thermometer, and Stirrer

REAGENTS:-HCl, NaOH

PROCEDURE:
(a) Determination Of Water Equivalent Of Calorimeter
1. Take 50 ml cold distilled water in 250 ml beaker keep it inside the thermo flask filled
with two neck corks. Insert a thermometer and glass stirrer in it.
 2. Heat 50 ml of water in a separate beaker to a temperature about 20-25°C, than that
of cold water. Note down temperature of both and note down the temperature of
them at every one minute for 5 minutes.
3. Make a mixture of both cold water and hot water in equal ml to add up 50 ml and
note down initial temperature and temperature at every one minute for 5 minutes.

(b) Estimation Of Heat Of Neutralization Of HCl And NaOH

1. Prepare standard solution of 0.5N HCl and 0.5N NaOH.
2. Note down the initial temperatures of HCl and NaOH, and note down the
temperature of them at every one minute for 5 minutes.
3. Make a mixture of both cold water and hot water in equal ml to add up 50 ml and
note down initial temperature and temperature at every one minute for 5
minutes.

OBERVATIONS AND CALCULATIONS:

A) Water Equivalent Of Calorimeter:

Temperature ( °C)
SR No. Time (min)
Cold water Hot water Mixture
1 1 26.5 38.0 30.6
2 2 26.6 37.0 30.4
3 3 26.6 37.0 30.2
4 4 27.0 36.5 30.0
5 5 27.0 36.0 30.0
Mean 26.74 36.9 30.24

Temperature of cold water, T1 = 26.74 °C.

Temperature of hot water, T2 = 36.9 °C.
Temperature of mixture, T3 = 30.24°C
Mass of cold water = 50g
 Mass of hot water = 47.31g
at = Sw = 1 cal / g
C = (47.31*(36.9-30.24) – 50*(30.24-26.74)) / (30.24-26.74) = 167.3 J / °C

B) Heat Of Neutralization:

Heat of Neutralization
Temperature ( °C)
No Time (min)
HCl NaOH Mixture
1 1 27.5 26.8 27.0
2 2 27.5 26.8 26.8
3 3 27.5 26.8 26.8
4 4 27.5 26.8 26.8
5 5 27.5 26.8 26.6
Mean 27.5 26.8 26.8

Temperature of alkali and calorimeter, T1 = 27.5 °C.

Temperature of acid, T2 = 26.8 °C.
Temperature of mixture, T3 = 26.8 °C
C = 40.024 cal /°C
Heat of neutralization = (1000 * Q) / (V * C)
Q = (50 + W) * (T3 – T2) + 50(T3 – T2)
= -7.87 cal / mol

RESULT:-

Heat of neutralization of HCl with NaOH= -7.87 cal / mol

 EXP 3: VERIFICATION OF HENDERSON’S EQUATION

AIM:
Preparation of buffer solution of sodium acetate and acetic acid. Measure the pH of
buffer solution and compare the values with theoretical values.

APPARATUS:
Measuring cylinder, conical flask, beaker, reissue paper, glass electrode, pH meter, glass
rod, etc.

CHEMICALS:
Solutions of pH 4 and pH7, 0.2M acetic acid and 0.2M sodium acetate.

THEORY:

Buffer solution is defined as ‘a solution which resists any change in its pH by the addition
of small quantities of either an acid (H+ ions) or a base (OH- ions)’ or ‘a solution that maintains a
fairly constant pH value upon addition of a small amount of acid or base.’ It is able to neutralize
small amounts of added acid or base, thus maintaining the pH of the solution relatively stable.
Acidic buffer consists of a weak acid and a salt of that weak acid with strong base, for example,
acetic acid and sodium acetate (CH3COOH + CH3COONa) and Boric acid + Borax.
 Such buffer solutions have pH on the acidic side, i.e. pH is less than 7 at 298 K. The pH of
an acidic buffer is given by the equation:
[salt]
pH = pka +log [acid]

Where ka is the acid dissociation constant of the weak acid.

pka= −log ka

To prepare the buffer of given pH, an acid or base whose pK aor pKbis near the required
pH is taken. Using the Henderson equation the ratio of acid (or base) and its salt is calculated to
get the required pH.

PROCEDURE:

1. Instrument calibration:
Switch on the pH meter. To calibrate the instrument first remove the electrode from the
storage solution and rinse it with distilled water. Dry the electrode with soft tissue paper
and place it in pH 7 buffer solution. Adjust the pH at 7 using calibration knob. Take out
the electrode from pH solution, rinse it with distilled water and place it in a solution of
pH4. Adjust the pH of the solution at 4 using slope knob which is at the back of the
instrument.
2. Take two clean and dry burettes. Rinse and fill one burette with 0.2M acetic acid solution
and other with 0.2M sodium acetate solution.
3. Take out 9 ml of acetic acid from the burette into a clean and dry beaker and add 1 ml of
sodium acetate solution into it. Label this solution as buffer solution 1.
4. Prepare a series of buffer solutions by mixing different volumes of acetic acid sodium
acetate as given in the table below. Calculate the value of pH of all the buffer solutions
using Henderson equation. This will give you the theoretical value of pH.
5. Dip the glass electrode in the prepared buffer solutions and note their experimental
value of pH.

OBSERVATION TABLE:
 Buffer Volume of Volume of Experimental Theoretical value
solution acetic acid sodium acetate value of pH of pH(pH = pka
solution (ml) solution (ml) [salt]
+log [acid])

1 9 1 3.55 3.80

2 8 2 4.01 4.15

3 7 3 4.21 4.38

4 6 4 4.40 4.58

5 5 5 4.63 4.75

6 4 6 4.74 4.92

7 3 7 4.94 5.11

8 2 8 5.26 5.35

9 1 9 5.49 5.60

CALCULATIONS:

Ka (aceticacid) = 1.80 ∗ 10-5

Thus pKa = −logKa = −log(1.80 ∗ 10-5)

Thus pKa = 4.75

Salt= CH3COONa; Acid= CH3COOH

[salt]
Theoretical values: pH = pKa +log [acid]

[1]
pH = 4.75 + log [9] = 3.80

[2]
pH = 4.75 + log [8] = 4.15

[3]
pH = 4.75 + log [7] = 4.38
 [4]
pH = 4.75 + log [6] = 4.58

[5]
pH = 4.75 + log [5] = 4.75

[6]
pH = 4.75 + log [4] = 4.92

[7]
pH = 4.75 + log [3] = 5.11

[8]
pH = 4.75 + log [2] = 5.35

[9]
pH = 4.75 + log [1] = 5.60

RESULT:

Hence, Henderson’s equation is verified.

 EXP 4: DETEMINATION OF THE STRENGTH OF THE GIVEN
HYDROCHROLIC ACID SOLUTION AGAINST SODIUM
HYDROXIDE SOLUTION.

AIM:-

To determine the strength of hydrochloric acid by pH meter.

THEORY:-

Most of the chemical and biochemical processes are profoundly affected by the
acidity or alkalinity of the medium in which the reaction takes place. All acidsdissociate
in aqueous solution to yield H+ ions. Some acids like HCl, H 2SO4, and HNO3 etc. are
completely ionized in aqueous medium where as CH3COOH, HCOOH etc. ionize to a
small extent only. The former is known as strong and the later as weak acid. pH of any
solution is defined as (–log H+) and has values between 0–14. pH < 7 indicate acidic
solution, pH > 7 indicate basic solution and pH = 7 means neutral solution.
 The pH of a solution can be measured accurately with the help of a pH meter.
Measurement of pH is employed to monitor the cause of acid-base titration. The pH
values of the solution at different stage of acid–base neutralization are determined and
plotted against the volume of alkali added. on adding a base to an acid, the pH rises
slowly in the initial stages as the concentration of H + ion decreases gradually. But, at
the equivalence point, it increases rapidly as at the equivalent point H + ion
concentration is very small. Then it flattens out after the end point. The end point of
the titration can be detected where the pH value changes most rapidly. However, the
shape of the curve depends upon the ionizability of the acid and the base used and
also on the acidity of base and basicity of the acid.

pH = -log10 [H+]

HCl+ NaOH = NaCl + H2O

APPARATUS:

pH meter, electrode, beaker, pipette, burette.

CHEMICALS:

Hydrochloric acid (HCl), sodium hydroxide (NaOH). buffer of pH = 4 and 9.2.

PROCEDURE:

1. 0.1N NaOH solution is provided.

2. HCl solution of unknown strength is provided.

3. Switch on the instrument and wait for 10–15 minutes so that machine gets
warmed up. Prepare the buffer solution by adding buffer tablets of pH = 4 and
 pH = 9.2 in 100 mL of water separately. Wash the electrode with distilled water.
Then, dip the electrode in the buffer solution (pH = 4) taken in a beaker, so that
the electrode immersed to the solution properly. adjust the pH to 4. Wash the
electrode with distilled water and standardize the pH meter using basic buffer
solution pH = 9.2.

4. Standardization of pH meter can also be done with the help of electronic and
buffer which are integral part of the instrument. Output of the electronic buffer
7.00 is joined to the input of pH meter and the asymmetric knob is adjusted till
display reads 7.00. Output of the electronic buffer 4.00 and 9.2 are then joined to
the input of pH meter and the asymmetric knob and slope knob are adjusted till
display reads 4.00 and 9.2 respectively.

5. pH-metric Titration: Clean the electrode with distilled water and wipe them
with tissue paper or filter paper. Take 20 mL of HCl solution in a 100 ml beaker
and add small amount of conductivity water so that the electrode is immersed in
it. note down the reading on the pH meter which is the pH of the HCl solution.

6. Set the burette with NaOH solution. Add 1ml NaOH solution from the burette,
shake the solution well and note the corresponding pH values. Near the end
point, there will be a sharp increase in the pH value. Process is continued until at
least five readings are taken after the end point.

7. Repeat the experiment to obtain the fine titration value by recording the
change in pH for each 0.1 ml of NaOH near the end point or equivalence point.
Plot a graph of ΔpH/ΔV versus volume of NaOH.

OBSERVATIONS:

A) Rough Titration=

Volume of NaOH pH ΔpH/ΔV

 0 1.49 0.03

1 1.52 0.02

2 1.54 0.04

3 1.58 0.06

4 1.64 0.06

5 1.70 0.08

6 1.72 0.14

7 1.92 0.23

8 2.15 0.70

9 2.85 3.35

10 6.20 3.35

11 9.55 0.87

12 10.42 0.63

13 11.05 0.25

14 11.30 0.16

15 11.46 0.11

B) Fair Titration=

Volume of NaOH pH ΔpH/ΔV

9.1 2.61 0.009

9.2 2.70 0.010

9.3 2.80 0.019

9.4 2.99 0.039

9.5 3.38 0.060

9.6 3.98 0.062

9.7 4.60 0.046

9.8 5.06 0.030

9.9 5.36 0.039

10.0 5.75 0.013

10.1 5.88 0.024

10.2 6.12 0.009

10.3 6.21 0.016

10.4 6.37 0.020

10.5 6.57 0.059

10.6 7.16 0.025

10.7 7.41 0.079

10.8 8.20 0.040

10.9 8.60 0.031

 11.0 8.91 0.025

GRAPH:

Volume of NaOH vs ΔpH/ΔV

0.09

0.08

0.07

0.06
ΔpH/ΔV

0.05

0.04
ΔpH/ΔV
0.03

0.02

0.01

0
0 2 4 6 8 10 12
Volume of NaOH (in ml)

CALCULATION:

N1V1=N2V2

N2 = 0.1*10.7 / 20

N2 = 0.0535 N

W = 0.0535*36.461*20 / 1000

W = 0.0390 g = 39 g
RESULT:-

1) Volume of NaOH required for the neutralization of 20 ml of diluted HCl

solution = 10.7 ml

2) Normality of diluted acid solution = 0.0535 N

3) Amount of HCl present in given 20 ml of solution = 0.0390 g = 39 mg

EXP 5: PAPER CHROMATOGRAPHIC SEPARATION AND

IDENTIFICATION OF METAL IONS

AIM:
Identification of metal cations Na+, K+, Li+ through paper chromatography
technique and calculation of Rf values
REQUIREMENTS:
Beakers, Boiling tubes, Measuring cylinder, Spotting capillaries or toothpicks,
Small test tubes, Whatman No. 1. Filter paper sheets.

CHEMICALS:
Sodium Chloride, Lithium Chloride, Potassium Chloride, Methanol or ethanol,
silver nitrate solution, fluoroscene dye solution

PRINCIPLE:
Chromatography is essentially a separation process which affects a separation by
distributing the sample into two phases. One phase is stationary and second is mobile
and flows through the stationary phase(a solid, gel, or polymer). During the process of
movement of mobile phase, small differences in adsorption-desorption or partitioning
or ion-exchange behavior of each component of a mixture are multiplied many folds
and these parameters distinguish between the different solutes. The ability of
chromatography to separate two solutes depends on the selectivity of the process and
the degree to which the system can distinguish between the two solutes. The
magnitude of the distribution is determined by the physic chemical nature of the solute
and that of the mobile and stationary phases, beside various physical interaction (such
as: hydrogen bonding, dipole moment etc.) of the solute with stationary-and mobile
phases. Some common steps used in different chromatographic techniques are:
application of the sample onto a stationary phase, percolating a mobile phase over the
stationary phase, obtaining the separation of components, collection of the different
components for qualitative or quantitative purposes. Therefore, the principle of
chromatography can be understood by taking any one kind of chromatography. In PC,
the mixture is spotted onto a sheet of paper. Paper chromatography works because of
the capillary action of aqueous solution or organic solvent, in the paper. Capillary
actionist defined as the movement of liquid within the spaces of a porous material due
to the forces of adhesion, cohesion, and surface tension. The liquid is able to move up
the filter paper because its attraction to itself is stronger than the force of gravity.
Compounds that are not soluble in the solvent or are very attracted to the stationary
phase stay in place. Compounds that is very soluble and less attracted to the stationary
phase travel up the stationary phase with the solvent. Some compounds are somewhat
soluble and somewhat attracted to the stationary phase. They travel up the paper, but
at a slower rate.
a. Mobile phase: This is the solvent. It may be a single compound or a
mixture of solvents, often with different polarities.
b. Stationary phase: This is the chromatographic medium – in our
experiment, the paper.
c. Origin: This is where you put the samples of compounds on the
chromatography paper. Generally, you will make pencil line to show you
where you put the samples. The baseline must be above the liquid level, so
that the solvent does not dissolve the compounds into the liquid phase in
the chamber.
d. Solvent front: This is the highest point that the solvent travelled during
“developing”.
Note: You need to mark where the solvent front reaches before the solvent
evaporates.
e. Retention factor (Rf): This is the ratio of how far the solute (metal ions)
travels on the chromatograph vs. how farther solvent front travels. In other
words, the fraction of the distance each solute travels, relative to the
distance the solvent travels. The Rf is a property characteristic of a
substance (intensive property) and will be the same if the solvent and
stationary phase are the same. In order for this technique to be effective,
the paper and the mobile phase must be chosen such that each compound
in the mixture has a different Rf.

PROCEDURE:
1. i) Preparation of Solutions: Prepare 100 cm3of aqueous solutions containing
1 mg/ml of (I) Sodium chloride (ii) Lithium chloride (iii) Potassium chloride Add
1-2 drops of hydrochloric acid to prevent hydrolysis. For the preparation of the
mixture of three cations, add few drops of each cation solutions into a test
tube.
ii) Preparation of Developer/Mobile phase/ Fluent: Any one off the following
can be used as the mobile phase
(i) Pure Methanol
(ii) Methanol + Ethanol (1:1 ratio)
(iii) Ethanol + Water (3:1 ratio)
 iii) Preparation of visualizing agent: (i) 1% aqueous solution of Silver nitrate
(ii) Fluoresce in dye solution in ethanol.
2. Cut whatman No. 1 filter strip of about 15x2 cm to be placed in usual boiling
tubes (or chromatographic jars) or beakers.
3. On the strip draw a line with pencil at about 1 cm from one end which can be
considered as origin line. Place one very light pencil dot about 2.0 cm in from
both the left and right edges of the chromatography paper. Place two additional
dots evenly spaced along the origin line. Do not use pen, as the various dyes in
the ink will separate as you elute the paper. These points are the points of
application of the solute/sample solution. Label these points lightly as Na, K, Li
and mixture for identification.
4) Obtain a spot plate and place a few drops each of theknown three metal ion
samples and a mixture of three samples assigned to you into separate, labeled
wells on the plate. Alternatively, you can take the samples in 4 different labeled
beakers or test tubes.
5) Using different toothpicks or capillaries for each solution, place a small amount
of each sample on its corresponding dot mark. Allow the solution to dry for 3-5
minutes and spot again. Repeat this 2-4 more times. The goal is to get enough
material on the paper that the developed spots will be visible, but not so much
that the spot will be too large to get a reasonable measure of the retention
factor.

Part B: Prepare the Eluting Chamber

6) Pour enough of the prepared eluting solution (Methanol/ Ethanol/mixture) into
the bottom of a large beaker or boiling tube to create a pool of the solvent not
more than 0.5 cm above the bottom of the beaker. This will allow enough
solution for eluting the paper, but not so much that the origin line will be below
the initial solvent level.
7) Immediately cover the beaker with plastic wrap and rubber band. Covering the
chamber will prevent the volatile component of the solution (acetone) from
evaporating, changing the concentration of the solution and its eluting
properties.

Part C: Eluting the Chromatography Paper, Visualizing Spots and Calculating

the Retention Factor (Rf)
 8) After the chromatography spots are dry, remove the plastic wrap, carefully
place the chromatography paper inside, and reapply the plastic wrap. Do not
disturb the chamber as elution continues, as it may cause the solution to splash
onto the paper and/or move unevenly up the paper.
9) Allow the solvent to move up the paper until it is approximately 1.5-1.0 cm
from the top of the paper. At that point, carefully remove the plastic wrap and
take out the chromatography paper. Using a pencil, mark the solvent front lightly.
10) After the paper is dry, Spray the paper (or dip in) with silver nitrate solution
followed by a solution containing fluoresce in dye. Wash off the excess solutions
with water.
11) Encircle the colored zones and mark the centre of each zone.
12) Measure the distance travelled by the solvent i.e. solvents front for the paper.
13) Measure the distance travelled by the solute or each metal ions i.e. dspot for
each spot on the paper (dspot always measurefrom the center of the
spot).Calculate the Rf (retention factor) for each spot.
14) Based on spot color and Rf values, identify the metal cations in the unknown
mixtures.

QBSERVATIONS AND CALCULATIONS:

Measure the distance travelled by the centre of the solute zone (ds) and the
distance travelled by the solvent front (dm) on the paper chromatogram.
Calculate the Rf values of each solute by the relation.
Rf = ds/ dm.
Observation Table
Metal ions ds dm Rf
Lithium 4.5 4.7 0.950
Sodium 3.5 4.7 0.744
Potassium 2.6 4.7 0.550
Sample:

RESULT:
Rf value of Lithium = 0.95
Rf value of Sodium = 0.744
Rf value of Potassium = 0.55