Lab Project-Experiment Procedure
Lab Project-Experiment Procedure
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)
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
ଵିଶ ଵ
Normality of Epsom salt solution. (N1) = x
ଵଶଷ ଵ
= ---------
= --------- N
= ----------- N
PART – III: Estimation of Total hardness of water:
= ----------- N
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
= ----------- N
RESULT:
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)
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.
= ---------
= --------- N
PART – II: Standardization of EDTA solution using standard MgSO4.7H20 solution:
= ----------- N
PART – III: Estimation of Permanent hardness of water:
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
= ----------- N
Permanent hardness of water in terms of CaCO3 equivalents = N3 x 50 x 1000 mg/lit
Therefore γL = nw dL γw / nL dw
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
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
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
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
KMnO4 Fe2+
N2= ---------N N3 =--------N
V2 = -----------Titre Value V3 = 20 ml
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.
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.
ଵିଶ 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
4
= ------------ N
= ----------- 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.
3
NaOH solution H2SO4 Solution
N1 =--------- N (given) N2 =-------- N
V1 = burette reading V2 =20 ml
ேଵଵ
Normality of H2SO4 solution (N2) =
ேଶ
= ---------N
(mL)
(P) (M)
Result:
1. Carbonate alkalinity =-------ppm
2. Bicarbonate alkalinity = ----------- ppm
3. Total alkalinity = --------ppm
ESTIMATION OF CONCENTRATION OF KMnO4 SOLUTION USING
COLORIMETER
1 450
2 470
3 510
4 520
5 540
6 570
7 600
8 670
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
ii) The amount of Mn present in the given solution = -----------grams /100 ml.