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Lab Project-Experiment Procedure

The document outlines a laboratory procedure for estimating the temporary and permanent hardness of water using the EDTA method. It includes the necessary apparatus, chemicals, principles of the reaction, and detailed steps for preparing solutions, standardizing EDTA, and performing titrations. Additionally, it provides calculations for determining hardness levels and includes a section on measuring surface tension of liquids using a stalagmometer.
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0% found this document useful (0 votes)
3 views34 pages

Lab Project-Experiment Procedure

The document outlines a laboratory procedure for estimating the temporary and permanent hardness of water using the EDTA method. It includes the necessary apparatus, chemicals, principles of the reaction, and detailed steps for preparing solutions, standardizing EDTA, and performing titrations. Additionally, it provides calculations for determining hardness levels and includes a section on measuring surface tension of liquids using a stalagmometer.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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ESTIMATION OF TEMPORARY HARDNESS OF WATER BY USING EDTA

AIM: To determine the permanent hardness of water by EDTA method.

APPARATUS: Standard Flask, Pipette, Burette, Conical Flask, Beakers, Weighing Bottle,
Funnel
CHEMICALS REQUIRED: Epsom Salt (MgSO4 .7H2O), EDTA (Ethylene Diamine Tetra
Acetic acid) solution, EBT indicator (Eriochrome black-T), Buffer solution (NH4Cl+ NH4OH)
(pH= 9-10) & Hard water sample.

PRINCIPLE:
The hardness of water is generally due to the presence of calcium and magnesium ions in water.
The chlorides, nitrates and sulphates of calcium & magnesium are responsible for permanent
hardness, while bicarbonates of calcium & magnesium are the cause of temporary hardness.
EDTA forms a stable complex of Ca-EDTA or Mg-EDTA with hardness causing ions of Ca
and Mg present in hard water at pH= 9-10. EBT is used as the indicator to detect the completion
of the reaction. When a small amount of EBT is added to hard water sample, it reacts with Mg2+
or Ca2+ to produce wine red coloured solution due to the formation of a complex. This wine red
coloured solution is titrated with EDTA till the colour of the solution changes blue, as EBT is
released free in the solution and the stable Mg-EDTA or Ca-EDTA complex is formed. End
point is determined by the change in colour from wine red to blue.
pH= 9-10
M2+ + EBT --------→ M-EBT complex (wine red colour)
Hard water Blue (Less stable)

pH= 9-10
M-EBT complex + EDTA --------→ M –EDTA complex + EBT
More stable, (colourless) (blue)

(Here M+2 = Ca+2 or Mg+2)

Permanent hardness of water will be found out after removing temporary hardness causing salts
by boiling followed by filtration. The filtrate water will be estimated using EDTA in presence of
EBT till the end point reaches blue color. The temporary hardness will be calculated from the
following …
Temporary hardness = Total hardness – Permanent hardness

Procedure:
PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weigh out accurately the given Epsom salt (MgSO4.7H2O) and transfer it into clean 100 ml
standard flask using a funnel. Dissolve the substance in minimum quantity of distilled water and
make it up to the mark with distilled water. Shake the solution thoroughly for uniform
concentration.
PART – II: Standardization of EDTA solution using standard Epsom salt solution:
Fill burette with EDTA solution till the mark ‘0’. Next, pipette out 20ml of Epsom salt solution
into a clean conical flask and add 5 ml of buffer solution (mixture of NH4OH + NH4Cl) followed
by 4 to 5 drops of EBT-indicator. Titrate this solution against the EDTA solution taken in the
burette, until the wine red color of the solution turns blue (end point). Repeat the titration for at
least two concurrent titre values.
PART – III: Estimation of Total hardness of water:
Pipette out 20 ml of the given hard water sample into a clean conical flask and add 5 ml of the
buffer solution (NH4OH + NH4Cl) followed by 4 to 5 drops of EBT indicator. Titrate this
solution against the standardized EDTA solution, until the wine red colour changes blue (end
point). Repeat the titration for at least two concurrent titre values.
PART – IV: Estimation of Permanent hardness of water:
Take 100 ml of sample water in 250 mL beaker. Boil it to remove the temporary hardness to
about half of the volume and cool to room temperature. Filter using filter paper to remove the
insoluble CaCO3 and Mg(OH)2 salts. Make up volume to 100 mL using distilled water. Pipette
out 20 ml of the solution into a clean conical flask and add 5 ml of the buffer solution (NH4OH
+ NH4Cl) followed by 4 to 5 drops of EBT indicator. Titrate this solution against the
standardized EDTA solution, until the wine red colour changes blue (end point). Repeat the
titration for at least two concurrent titre values.
PART – V: Estimation of Temporary hardness of water:
The temporary hardness will be calculated from the following …
Temporary hardness = Total hardness – Permanent hardness
CALCULATIONS AND TABLES:
PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weight of the weighing bottle + Epsom salt (W1) = -------------- gms
Weight of the empty weighing bottle (W2) = ------------- gms
Weight of the Epsom salt (W1 – W2) = ----------------- gms
Eqv. wt of Epsom salt =123
Volume of the solution = 100 ml
୛ଵି୛ଶ ଵ଴଴଴
Normality of Epsom salt solution. (N1) = x
ଵଶଷ ଵ଴଴

= ---------
= --------- N

PART – II: Standardization of EDTA solution using standard MgSO4.7H20 solution:

S.No Volume of Epsom Burette readings Volume of EDTA


salt Pipette out (ml) Initial Final required (ml) (Final-Intial)
1 20
2 20
3 20

Epsom salt solution EDTA solution


Normality of Epsom salt sol.(N1) =------ N Normality of EDTA sol.(N2) =----- N
Volume of Epsom salt sol. (V1)= -------ml Volume of EDTA sol. (V2) =------ml

Normality of EDTA solution (N2) = N1V1


V2
= -------------

= ----------- N
PART – III: Estimation of Total hardness of water:

S.No Volume of Hard Water Burette readings Volume of EDTA


Pipette out (ml) Initial Final required (ml) (final-intial)
1 20
2 20
3 20
EDTA Solution
Normality of EDTA solution (N2) = ------ N (from Part-II)
Volume of EDTA solution (V2′) = Burette reading from Part-III (ml);
Hard water
Normality of hard water (N3) =------- N
Volume of hard water (V3) = 20 ml

Normality of hard water (N3) = N2 V2′


V3

= ----------- N

Total hardness of water in terms of CaCO3 equivalents = N3 x 50 x 1000 mg/lit

= ---------------- mg/lit or ppm

PART – IV: Estimation of Permanent hardness of water:

S.No Volume of water Burette readings Volume of EDTA


Pipette out (ml) Initial Final required (ml) (final-intial)
1 20
2 20
3 20

EDTA Solution
Normality of EDTA solution (N2) = ------ N (from Part-II)
Volume of EDTA solution (V2′) = Burette reading from Part-III (ml);

Hard water
Normality of hard water (N3) =------- N
Volume of hard water (V3) = 20 ml

Normality of hard water (N3) = N2 V2′


V3

= ----------- N

Permanent hardness of water in terms of CaCO3 equivalents = N3 x 50 x 1000 mg/lit

= ---------------- mg/lit or ppm


Therefore temporary hardness =Total hardness – Permanent hardness
= ………………………. ppm

RESULT:

1) Normality of EDTA solution (N2) =--------------N


2) Temporary hardness of water in terms of CaCO3 equivalents =---------------- ppm
ESTIMATION OF PERMANENT HARDNESS OF WATER BY USING EDTA

AIM: To determine the permanent hardness of water by EDTA method.

APPARATUS: Standard Flask, Pipette, Burette, Conical Flask, Beakers, Weighing Bottle,
Funnel
CHEMICALS REQUIRED: Epsom Salt (MgSO4 .7H2O), EDTA (Ethylene Diamine Tetra
Acetic acid) solution, EBT indicator (Eriochrome black-T), Buffer solution (NH4Cl+ NH4OH)
(pH= 9-10) & Hard water sample.

PRINCIPLE:
The hardness of water is generally due to the presence of calcium and magnesium ions in water.
The chlorides, nitrates and sulphates of calcium & magnesium are responsible for permanent
hardness, while bicarbonates of calcium & magnesium are the cause of temporary hardness.
EDTA forms a stable complex of Ca-EDTA or Mg-EDTA with hardness causing ions of Ca
and Mg present in hard water at pH= 9-10. EBT is used as the indicator to detect the completion
of the reaction. When a small amount of EBT is added to hard water sample, it reacts with Mg2+
or Ca2+ to produce wine red coloured solution due to the formation of a complex. This wine red
coloured solution is titrated with EDTA till the colour of the solution changes blue, as EBT is
released free in the solution and the stable Mg-EDTA or Ca-EDTA complex is formed. End
point is determined by the change in colour from wine red to blue.
pH= 9-10
M2+ + EBT --------→ M-EBT complex (wine red colour)
Hard water Blue (Less stable)

pH= 9-10
M-EBT complex + EDTA --------→ M –EDTA complex + EBT
More stable, (colourless) (blue)

(Here M+2 = Ca+2 or Mg+2)

Permanent hardness of water can be estimated after removing temporary hardness causing salts
by boiling followed by filtration. The filtrate water will be estimated using EDTA in presence of
EBT till the end point reaches blue color.
Procedure:
PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weigh out accurately the given Epsom salt (MgSO4.7H2O) and transfer it into clean 100 ml
standard flask using a funnel. Dissolve the substance in minimum quantity of distilled water and
make it up to the mark with distilled water. Shake the solution thoroughly for uniform
concentration.
PART – II: Standardization of EDTA solution using standard Epsom salt solution:
Fill burette with EDTA solution till the mark ‘0’. Next, pipette out 20ml of Epsom salt solution
into a clean conical flask and add 5 ml of buffer solution (mixture of NH4OH + NH4Cl) followed
by 4 to 5 drops of EBT-indicator. Titrate this solution against the EDTA solution taken in the
burette, until the wine red color of the solution turns blue (end point). Repeat the titration for at
least two concurrent titre values.
PART – III: Estimation of Permanent hardness of water:
Take 100 ml of sampel water in 250 mL beaker. Boil it to remove the temporary hardness to
about half of the volume and cool to room temperature. Filter using filter paper to remove the
insoluble CaCO3 and Mg(OH)2 salts. Make up volume to 100 mL using distilled water. Pipette
out 20 ml of the solution into a clean conical flask and add 5 ml of the buffer solution (NH4OH
+ NH4Cl) followed by 4 to 5 drops of EBT indicator. Titrate this solution against the
standardized EDTA solution, until the wine red colour changes blue (end point). Repeat the
titration for at least two concurrent titre values.

CALCULATIONS AND TABLES:


PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weight of the weighing bottle + Epsom salt (W1) = -------------- gms
Weight of the empty weighing bottle (W2) = ------------- gms
Weight of the Epsom salt (W1 – W2) = ----------------- gms
Eqv. wt of Epsom salt =123
Volume of the solution = 100 ml
୛ଵି୛ଶ ଵ଴଴଴
Normality of Epsom salt solution. (N1) = x
ଵଶଷ ଵ଴଴

= ---------
= --------- N
PART – II: Standardization of EDTA solution using standard MgSO4.7H20 solution:

S.No Volume of Epsom Burette readings Volume of EDTA


salt Pipette out (ml) Initial Final required (ml) (Final-Intial)
1 20
2 20
3 20

Epsom salt solution EDTA solution


Normality of Epsom salt sol.(N1) =------ N Normality of EDTA sol.(N2) =----- N
Volume of Epsom salt sol. (V1)= -------ml Volume of EDTA sol. (V2) =------ml

Normality of EDTA solution (N2) = N1V1


V2
= -------------

= ----------- N
PART – III: Estimation of Permanent hardness of water:

S.No Volume of water Burette readings Volume of EDTA


Pipette out (ml) Initial Final required (ml) (final-intial)
1 20
2 20
3 20

EDTA Solution
Normality of EDTA solution (N2) = ------ N (from Part-II)
Volume of EDTA solution (V2′) = Burette reading from Part-III (ml);

Hard water
Normality of hard water (N3) =------- N
Volume of hard water (V3) = 20 ml

Normality of hard water (N3) = N2 V2′


V3

= ----------- N
Permanent hardness of water in terms of CaCO3 equivalents = N3 x 50 x 1000 mg/lit

= ---------------- mg/lit or ppm


RESULT:

1) Normality of EDTA solution (N2) =--------------N


2) Normality of Hard Water (N3) = ------------- N
3) Permanent hardness of water in terms of CaCO3 equivalents =---------------- ppm
DETERMINATION OF SURFACE TENSION OF A LIQUID
Aim: To determine the surface tension of a given liquid using stalagmometer.
Chemicals: Water, Test liquid (liquids like benzaldehyde, aniline, acetophenone, soap solution
etc.)
Apparatus: Stalagmometer, beaker.
Principle: The force in dynes acting along the surface of the liquid at right angles to any line
1cm in length is known as surface tension. The units of surface tension are dynes cm-1. Surface
tension of a liquid can be determined using a stalagmometer by drop counting method. The
number of drops formed by constant volume of a liquid at the flat end of the stalagmometer
depends on the surface tension of the liquid. One can determine the relative surface tension of
liquid to water by counting the number of drops formed by the liquid and water of the same
volume.
Let γL be the surface tension of the liquid
Let γw be the surface tension of the water ( γw = 72 dynes/cm)
Let nL be the number of drops formed by liquid
Let nw be the number of drops formed by water
Let dL be the density of liquid
Let dw be the density of water

These are related by:


γL/ γw = nw dL/ nL dw

Therefore γL = nw dL γw / nL dw

Fig. Surface tension determination using a stalagmometer


Procedure: Clean the stalagmometer and fill it with distilled water by sucking it while
immersing the lower end into the distilled water. Bring the level of water to upper mark. Open
the pinch cock; adjust it so that the rate of flow of liquid is about 12-15 drops per minute. Allow
the drops to fall into a weighing bottle (whose weight has already been taken) till water level
reaches the lower mark. Count the number of drops and take the weight of bottle along with
water. Repeat the same with the given liquid.

Calculations:
Weight of empty weighing bottle (W1) = ------------- g
Weight of weighing bottle + Dist. Water (W2) = ------------ g
Weight of empty weighing bottle + liquid (W3) = ----------- g
mL = W3- W1= --------- g
mW = W2-W1= --------- g
dL = mL/mW X dW
Density of distilled water i.e dW = 1 gr/ml

Surface tension of sample liquid (γL) is given by


γL= nw dL γw / nL dw

S.No. Volume of solution No. of Drops Density of Surface Tension


solution (gm/cc)
1 50ml Distilled water nw = dW = 0.99 gm/cc υw = 72 dynes/cm

2 50 ml Soap Solution ns = ds =

3 25 ml Soap Solution + ns = ds =
25 ml Distilled Water
4 25ml above Soap Solution + ns = ds =
25 ml Distilled Water

Result: The surface tension of sample liquid is = -------------------- dynes/cm


PREPARATION OF ASPIRIN
Aim: To prepare a pure sample of Acetyl Salicylic Acid i.e. Aspirin.
Apparatus: Conical Flask, Beaker, Glass Rod, Water bath and Funnel.
Chemicals required: Salicylic Acid (2 gms), Acetic Anhydride (8 ml), Conc.H2SO4,

Procedure: Take 2 gms of Salicylic Acid in a clean and dry 250ml conical flask and add 8ml of
Acetic Anhydride followed by 2 drops of Conc.H2SO4. Stir well and warm it on a water bath at
50oC to 60oC with occasional stirring for about 30 minutes. Pour the reaction mixture into a
beaker containing 30ml of cold water and stir it with glass rod. Filter and wash the crude Aspirin
with cold water.
Recrystallization: The crude aspirin is purified by dissolving in 30ml of hot boiling water with
charcoal and then filter it; white needles of aspirin will be obtained in the filtrate.
Report: Weight of the aspirin sample…………………..gm

Melting Point: 128oC -135oC


ESTIMATION OF FERROUS IRON (Fe+2) BY PERMANGANOMETRY

AIM: To estimate the amount of Fe2+ present in given solution using standard solution of
Mohr’s salt and KMnO4 solution.
APPARATUS: beaker, glass rod, conical flask, burette, standard flask, weighing bottle, funnel,
pipette.etc...
CHEMICALS: Mohr’s salt (Ferrous ammonium sulphate), Conc. H2SO4, 6N H2SO4, KMnO4,
and distilled water.
PRINCIPLE: KMnO4 is a common oxidizing agent which oxidizes Fe2+ in (sulphuric acid) acid
medium to Fe2+ and gets (itself) reduced to Mn2+, Thus this reaction is a redox reaction.
Oxidation: 5Fe2+ → 5Fe3+ + 5e- ------- (1)
Reduction: MnO-4 + 8H+ +5e- → Mn2+ + 4H2O ------- (2)
Overall: 5Fe2+ + MnO-4 + 8H+ → 5Fe3+ + Mn2+ + 4H2O

In this Redox reaction KMnO4 (pink) also acts as a self indicator, which undergoes
decolourisation due to formation of Mn2+ (colourless) and after completion of redox reaction at
end point) the pink colour of KMnO4 persists.
PROCEDURE: It consists of 3 parts
PART –I: Preparation of standard solution of Mohr’s salt:
Weigh accurately a sample of Mohr’s salt (FeSO4.(NH4)2SO4.6H2O.) and transfer it into
a clean 100ml standard (volumetric) flask using a funnel. Add about 50ml of distilled water
followed by 8 drops of conc.H2SO4 and shake the flask to dissolve the substance. Make the
solution up to the mark with distilled water and shake well for uniform concentration.
Weight of weighing bottle + Mohr’s salt (W1) =--------- gm
Weight of empty weighing bottle (W2) = -------- gm
Weight of Mohr’s salt taken (W1-W2) = --------- gm

ௐଵିௐଶ ଵ଴଴଴
Normality of Mohr’s salt (N1) = x = ----------N
ଷଽଶ ଵ଴଴

PART- II: Standardization of KMnO4 solution:


Pipette out 20ml of standard Mohr’s salt solution into a clean conical flask and add about
20ml of 6N H2SO4 solution. Titrate the contents of the conical flask against the KMnO4 solution
taken in the burette until a permanent pale pink colour (end point) is obtained. Repeat the
titration for at least two concurrent titre values.
S.No. Volume of Mohr’s Burette readings Volume of KMnO4
salt ml) Initial Final (ml)
1
2
3
Mohr’s salt KMnO4
N1 = ----------N N2 =----?----N
V1 = 20 ml V2 = titre value-- ml

Normality of KMnO4 solution: N2 = N1V1 =-----------------N


V2

PART-III: Estimate the amount of Fe2+ in the given solution


Make the given Fe2+ solution up to the mark with distilled water and shake the solution
thoroughly. Pipette out 20ml of Fe2+ solution into a clean beaker and add a 20ml 6N H2SO4 to it.
Titrate the solution against the standard KMnO4 until a light permanent pink colour persists.
Repeat the titration to get atleast two consecutive concordant titre values.

S.No. Volume of Fe+2 Burette Readings Volume of


Solution Initial Final K2Cr2O7 Solution
1
2
3

KMnO4 Fe2+
N2= ---------N N3 =--------N
V2 = -----------Titre Value V3 = 20 ml

Normality of Fe2+solution = N3 = N2V2= -------------N


V2
Amount of Fe2+ present in the given 100ml solution = N3 x55.85 gm
(GEW Fe2+ = 55.85 gm ) 10

Result:
1. Normality of KMnO4 solution: N2 = -----------------N
2. Normality of Fe2+solution: N3 = -------------N
3. Amount of Fe2+ present in the given 100ml solution = ----------- gm
Estimation of the amount of ferrous ammonium sulphate by Potentiometry using
Potassium Dichrometry
AIM : To estimate the amount of Fe2+ present in given solution, using K2Cr2O7 solution by
Potentiometric titration.
APPARATUS: Potentiometer, saturated calomel electrode, platinum electrode, salt bridge,
beakers, glass rod, conical flask, burette, standard flask, weighing bottle, funnel, pipette.etc...
CHEMICALS: Ferrous ammonium sulphate, 6N H2SO4, K2Cr2O7, saturated KCl solution and
distilled water.

1
PROCEDURE: It consists of 2 parts
STEP-1: Preparation of standard Potassium dichromate solution:
Weigh accurately the given pure sample of potassium dichromate and transfer it into 100 ml
standard flask with a funnel. Dissolve it in small quantity of distilled water and make up the
solution up to the mark using distilled water. Shake well for uniform concentration. Calculate the
normality of potassium dichromate solution.

PART-III: Estimate the amount of FAS in the given solution:


Take the given FAS solution into clean 100 ml standard flask, make the solution up to the mark
with distilled water and shake the solution thoroughly. Next, Pipette out 20 ml of FAS solution
into a clean 100 ml beaker and add a 20ml 6N H2SO4 to it. Dip the platinum electrode into the
same solution and connect it to the potentiometer. Dip the calomel electrode into saturated KCl
solution provided in another 100 ml beaker. Connect these two electrodes with a salt bridge and

2
measure the initial EMF. Now titrate the solution by adding 0.5 mL of K2Cr2O7 each time from
burette and note down the corresponding EMF. Take about 21 readings in the following tabular
column. (Note the volume of KMnO4 where there is a steep change in EMF. This volume is the
approximate volume of KMnO4 required for oxidation of Fe2+.

MODEL GRAPHS: Plot a graph (differential graph) between volume of K2Cr2O7 on X-axis and
corresponding ∆E/∆V on Y-axis. From the inflexion point the exact titre value can be known.

OBSERVATIONS AND CALCULATIONS


PART –I: Preparation of standard solution of potassium dichromate
Weight of weighing bottle + K2Cr2O7 (W1) =--------- gm
Weight of empty weighing bottle (W2) = -------- gm
Weight of K2Cr2O7 taken (W1-W2) = --------- gm

୛ଵି୛ଶ ଵ଴଴଴
Normality of K2Cr2O7 (N1) = x
ସଽ ଵ଴଴

= ----------N

3
PART-II: Estimation of the amount of FAS in the given solution using potentiometer:
S.No. Volume of EMF(mV) ∆E=E1-E2 ∆V=V2-V1 ∆E/∆V
K2Cr2O7 (ml)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21

K2Cr2O7Solution FAS Solution


N1 = -------- N N2 = --------- N

V1= -------- ml (from graph) V2 = vol of FAS taken

Normality of FAS solution (N2) = N1V1


V2
= ----------

4
= ------------ N

Amount of FAS in given solution = N3 X 392/10 gms/100ml

= ----------- gm/100ml

RESULT:
1) End point for FAS solution (from graph)=---------- ml
2) Normality of FAS solution(N2) = --------- N
3) Amount of FASin given solution = --------- g/100ml

5
Determine the alkalinity in a given water sample

AIM: To estimate the amount of alkalinity present in a given water sample using H2SO4
solution.
APPARATUS: conical flask, burette, standard flask, funnel, pipette, etc.
CHEMICALS: NaOH solution, H2SO4 solution, phenolphthalein indicator, methyl orange
indicator and distilled water.

Thus, phenolphthalein measures the hydroxides and half the carbonates in between pH range
8.3-10 by showing color change from pink to colorless (end point), whereas, methyl orange
measures total alkalinity due to all carbonate, bicarbonate, and hydroxide in the range of pH
3.4-4.5 showing color change of solution from light yellow to light red at end pint.

PROCEDURE: It consists of 3 parts


PART –I: Standardisation of H2SO4 solution using standard NaOH solution
Pipette out 20ml of the given H2SO4 solution into a clean conical flask and add 1-2
drops of phenolphthalein indicator. Titrate the contents of the conical flask against the NaOH
solution taken in the burette until a pale pink colour (end point) is obtained. Repeat the titration
for least two concurrent titre values.

S.No Vol. of H2SO4 (ml) Burette readings Vol. of NaOH required


taken IBR FBR (FBR – IBR) (ml)
1

3
NaOH solution H2SO4 Solution
N1 =--------- N (given) N2 =-------- N
V1 = burette reading V2 =20 ml
ேଵ௏ଵ
Normality of H2SO4 solution (N2) =
ேଶ
= ---------N

PART-II: Determination of alkalinity of water sample.

(mL)
(P) (M)

Normality of H2SO4 solution = N2

Strength in terms of CaCO3 equivalent..,.

Carbonate alkalinity = 2P ×N2 ×50×1000


Vol of water sample

=-------- mg/L or ppm


Bicarbonate alkalinity = (M-2P) ×N2 ×50×1000
Vol of water sample

=-------- mg/L or ppm

Total alkalinity = M×N2 ×50×1000


Vol of water sample

=-------- mg/L or ppm

Result:
1. Carbonate alkalinity =-------ppm
2. Bicarbonate alkalinity = ----------- ppm
3. Total alkalinity = --------ppm
ESTIMATION OF CONCENTRATION OF KMnO4 SOLUTION USING
COLORIMETER

Aim: To estimate the concentration of given KMnO4 solution using colorimeter.


Apparatus: Colorimeter, beaker, standard flask, Cuvettes and test tubes.
Chemicals: 0.01M KMnO4 solution, distilled water
Principle: It is based on the two principles of photometry Lambert’s law and Beer’s law. i.e. It is
based on the absorption of light by the substances.
Lamberts law: It states that “when a beam of monochromatic light passes through absorbing
medium, the rate of decrease in intensity with the thickness of medium is proportional to the
intensity of incident radiation”. Mathematically, law can be written as

2.303 log (Io/It ) = kt

Where, Io = Intensity of light incident It = Intensity of light transmitted


k = constant t = thickness of the medium
Beer’s law: It states that “when a beam of monochromatic light passes through absorbing
medium, the rate of decrease in the intensity of monochromatic light with the thickness of
medium is directly proportional to the intensity of incident radiation and the concentration of the
solution. (The intensity of a monochromatic light decreases exponentially as the concentration of
absorbing substance increases arithmetically). Mathematically, law can be written as

It = I0.10-ЄCt (or) Log [I0/It] = ЄCt

Where , Є= Molar extinction coefficient. C = Conc. of the solution


t = Thickness of the medium Log I0/It is optical density
Theory:
Colorimeters are used to find the absorption of radiation (i.e, Optical density (O.D.) of the
substances) in the visible region. i.e, it is mainly used for colored solutions. In colorimeters
radiation of different wavelength can be obtained within the visible region by changing the
filters. The instrument consists of a light source (which gives normal light), monochromator or
filter (which gives monochromatic radiation from normal light), is allowed to fall on the solution
placed in sample holder, recorder will record the optical density of the substance , which will be
displayed on the monitor.
Procedure: I) Fixing of λ max:
It is the maximum absorption at a particular wavelength. Sample should be placed in the
sample holder and by passing radiation of different wavelengths, the optical density of substance
should be measured (wavelength range can be selected in colorimeter light of different
wavelengths can be obtained by changing the filters). The wavelength at which maximum
absorption is found should be selected. Each time while measuring the optical density of the
substance, the solvent absorption (which is used to make the solution) should be made zero by
keeping a blank solvent.
S.No. Wavelength Optical density /
(nm) Absorbance

1 450
2 470
3 510
4 520
5 540
6 570
7 600
8 670

II) Calibration Curve:


10 ml of 0.01M KMnO4 solution is taken into a standard flask and is diluted to 100 ml.
Its concentration is gradually changed to 0.001N. From this solution take separately 1, 2,
3,4,5,6,7,8,9 ml in various test tubes add 9, 8, 7,6,5,4,3,2,1 ml of H2O to them respectively.
Optical density of all the samples should be determined and a graph is plotted by taking
concentration of KMnO4 on x-axis and optical density on y-axis. The curve so obtained is called
calibration curve.
S.No Vol. of Vol. of KMnO4 Conc. of KMnO4 Optical density /
Water Solution Absorbance

1 1 9 0.0001
2 2 8 0.0002

3 3 7 0.0003
4 4 6 0.0004
5 5 5 0.0005
6 6 4 0.0006
7 7 3 0.0007
8 8 2 0.0008
9 9 1 0.0009
10 10 0 0.001
11 Unknown concentration

III) Estimation of Conc. of given KMnO4 solution (unknown):


KMnO4 solution whose concentration to be determined is taken in a 100ml flask and
diluted up to the mark with distilled water. Shake well before use for uniform conc. measure its
optical density and find out the concentration of diluted KMnO4 from the calibration curve so
obtained. From the concentration of dilute solution, the concentration of originally given solution
can be calculated using the principle.
Graph:

Result: i) Concentrtion of given KMnO4 solution is _______________M.

ii) The amount of Mn present in the given solution = -----------grams /100 ml.

iii) The molar absorbance coefficient ( ɛ) = ---------- litre / mole/cm

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