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Introduction to Chemistry Lab (the teachers are expected to teach fundamentals like
Primary, Secondary Standard Solutions , Normality, Molarity, Molality etc. and
laboratory ware used, error ,accuracy, precision, Theory of indicators, use of
volumetric titrations.
Every indicator shows colour change at its respective pHrange mentioned above. For instance
methyl orange shows red colour up to pH 3.1 and orange colour beyond pH 4.4. Methyl
orange exists in two structures, one is benzenoid (yellow in basic medium) and another one is
quinonoid (red in acidic medium). These two structures are in equilibrium with each other.
CH3
N N HN SO3H Red (Acid solution)
CH3
Quinonoid
Below pH 3.1, it exists in quinonoid structure and shows red colour and
above pH 4.4, it exists in benzenoid structure with orange colour or yellow colour.
Selection of an acid base indicator depends mainly on two factors.
1. pH range of the indicator.
2. Change in pH of the solution at the end point.
An indicator shows colour change when the above two factors match with each other.
B. Redox Indicators
1. Highly colored substances that may be reversibly oxidized or reduced and change
colors upon oxidation and reduction
Inox + ne- + m H+ Inred
one color another color
2. Each redox indicator changes color over a certain potential range
Hence indicator must have a transition potential corresponding closely to the
equivalence point potential of the titration
Inox + ne- + m H+ Inred
V1N1 = V2N2
V1 : Volume of Hydrochloric acid
N1 : Normality of Hydrochloric acid
V2 : Volume of Sodium Carbonate solution
N2 : Normality of Sodium Carbonate solution
V2 N 2
N1
V1
Titration to pH=4.5with methyl orange or the appearance of pink colour will indicate
total alkalinity.
Formula:
The amount of alkalinity interms of CaCO3 equivalents
V1 0.02 50 1000
Phenolphthalein Alkalinity in terms of CaCO3equivalent = ppm
Vs
= .ppm
Determination of total alkalinity:
V2 0.02 50 1000
Total Alkalinity in terms of CaCO3 equivalents = ppm
Vs
= ..ppm
Result:
Phenolphthalein alkalinity of the given water sample= ------------------- ppm
Aim: To determine the total acidity of the given water sample by using 0.02N NaOH
solution.
Apparatus: Burette, Pipette, Conical Flask, Beakers, Wash Bottle, Burette Stand.
Chemicals required: Standard sodium hydroxide(0.02N), Phenolphthalein indicator, Methyl
orange indicator, sodium thiosulphate, water sample.
Theory: The acidity of a solution is a measure of its capacity to neutralize bases.
Acidity is due to the presence of mineral acids like H2SO4, HCl, HNO3 and dissolved CO2 in
the form of H2CO3. These acids can be estimated by titration against standard sodium
hydroxide using methyl orange and Phenolphthalein indicators.If methyl orange indicator is
used in the titration (at pH=4.5), it gives acidity of mineral acids only. This acidity is called a
partial acidity or methyl orange acidity. If Phenolphthalein indicator is used (at pH=8.3) in
the titration, it gives acidity of all compounds(mineral acidity and CO2). This acidity is called
total acidity or Phenolphthalein acidity. The difference of these two is equal to carbonic
acid acidity. Interference due to the presence of residual Chlorine is removed by adding two
drops of Na2S2O3(hypo) solution to the water sample.
Procedure:
(A)Titration of water sample using Methyl orange indicator (Partial Acidity)
1. The burette is first cleaned with tap water and then with distilled water.
2. Finally, it is rinsed with given NaOH solution. Then it is filled with NaOH Solution.
3. The NaOH is allowed to run out to fill the nozzle portion without any air bubble.
4. The initial reading of the burette is adjusted to 0 mark and fixed vertically in the
stand.
5. First the pipette is rinsed with distilled water.
6. Pipette out 20ml of water sample in to a conical flask.
7. Add 2 drops of hypo and two drops of methyl orange indicator.
8. The color of conical flask solution becomes pink.
V1 0.02 50 1000
= ppm
20
= ppm or mg/litre.
V2 0.02 50 1000
= ppm
20
= . ppm or mg/litre.
(C) Acidity due to carbonic acid=Total acidity-Partial acidity.
= ppm or mg/litre
Result:
Partial acidity of water sample =
Total acidity of water sample =
Carbonic acidity of water sample =
V1N1 = V2N2
Where V1 = Volume of Oxalic acid=10ml
N1 = Normality of Oxalic acid= N
V2 = Volume of KMnO4 solution= ml
N2 = Normality of KMnO4 solution=?
V1 N 1
N2
V2
= ...........N
Estimation of Mohrs salt solution.
Principle: Potassium Permanganate oxidizes Ferrous Sulphate present in the Mohrs salt in
the presence of dil.H2SO4 to Ferric Sulahate according to the following chemical reaction.
2KMnO4 + 8H2SO4 + 10FeSO4 K2SO4 + 2 MnSO4 + 5 Fe2(SO4)3 + 8H2O
1. Rinse and fill the burette with the standard KMnO4 solution till the upper meniscus of
the KMnO4 solution touches the zero mark on the burette.
V3N3 = V2N2
Where V3 = Volume of Mohrs salt solution=10ml
N3 = Normality of Mohrs salt solution=?
V2 = Volume of KMnO4 solution=.. ml
N2 = Normality of KMnO4 solution= .. N
V2 N 2
N3
V3
Amount of Ferrous Iron present in the given 250 ml solution =
= N3 x g.equ. wt. of Iron x 250 / 1000
=. X 56 X 250 / 1000
Result: 1) The normality of the given Mohrs salt solution (N3) = .N
2) Amount of Ferrous Iron present in given 250 ml solution = g
N1V1 =N2V2
N2 =N1V1/V2
= ..N
Amount of Fe3+ present in the given 100 ml solution =
Gram euivalent wt. X Normality X Volume(ml)
1000
= = -----------g
V1N1 = V2N2
V1= Volume of standard hard water =20ml
N1= Normality of standard hard water =0.02N
V2= Volume of given EDTA solution=ml
N2= Normality of given EDTA solution=?
V1 N1
N2=
V2
=
2. Determination of Total Hardness of the given water sample
1. Fill the burette with the EDTA solution.
2. Transfer 20ml of the given water sample into a clean conical flask.
3. Add 1ml of pH=10 buffer solution and 1 or 2 drops of EBT indicator. Solution
turns to wine red colour
4. Titrate with EDTA solution till wine red colour changes to sky blue. This is
the end point.
5. Repeat the titration until two consecutive readings coincide.
V3 N3 = V2 N2
V3= Volume of given water sample =20ml
N3= Normality of given water sample =?
V2= Volume of EDTA solution run down=ml
N2= Normality of given EDTA solution=.N
V2 N 2
N3=
V3
=
Result:
Total degree of hardness of the given water sample is .mg /l(or) ppm
Aim: To determine the concentration of unknown HCl by using 0.1N NaOH solution pH
metrically.
Apparatus: pH meter, electrode, beaker, pipette, burette.
Chemicals required: Hydrochloric acid (HCl), 0.1N sodium hydroxide (NaOH). Buffer
solutions of pH = 4 and 7.
Theory: All acids dissociate in aqueous solution to yield H+ ions. Some acids like HCl,
H2SO4, 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 014. 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 stages of acidbase 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.
Procedure: Switch on the instrument and wait for 1015 minutes so that machine gets
warmed up. Prepare the buffer solution by adding buffer tablets of pH = 4 and pH = 7 in 100
mL of water separately. Wash the electrode with distilled water and calibrate the pH meter as
per the instruction manual.
P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 25
Clean the electrode with distilled water and wipe it with a tissue paper or filter paper. Take
20 mL of HCl solution in a 100 mL beaker and immerse the electrode in it. 0.1N NaOH
solution is filled in the burette . The reading shown on the scale of pH meter is pH value of
the HCl solution. Add NaOH solution drop wise from the burette (maximum 1mL at a time),
shake the solution well and note the corresponding pH values. Near the end point, the acid is
neutralized and there will a sharp increase in pH values. Further addition of even 0.01 mL of
NaOH, increase the pH value to about 910.
Plot a graph between pH and volume of NaOH added and find out the volume of NaOH
required (V2 mL) for complete neutralization of HCl from the graph.
V1N1=V2N2
Normality of HCl (N1) = (V2N2/20) (N)
Result: The concentration of the unknown HCl is ________(N)
Precautions: i) Electrodes must be immersed in the solution properly and sufficient time
to be allowed for the electrodes to obtain the temperature of the solution.
i) pH meter should be calibrated before the experiment.
i) Magnetic stirrer may be used or the solution be stirred mechanically from time to
time during pH metric titration.
Aim: To determine the conductivity of the given water sample by using conductivity meter.
Apparatus: Conductivity meter.
Reagent: Standard electrical conductivity solution.
Standard solution is prepared by dissolving 0.7456grams of KCl in 1 litre distilled
water. It will have 1413 mhos/cm as conductance.
Theory: Conductivity is the capacity of the water to carry an electrical current.
Conductivity is proportional to the concentration of dissolved solids(ions) in the
solution.
Procedure:
Calibration of electrical conductivity meter:
(i) Adjust cal till the display reads 1000.
(ii) Set the Range switch to the proper range for the standard solution.
(iii) Change the cond/cell constant switch position to cell constant position.
(iv)Wash the electrode with distilled water and dry with tissue paper. Immerse the electrode
in standard solution.
(v) Adjust the cell constant present control on the rear panel till the instrument reads 1. The
conductivity of the solution is1413s/cm.
Measurement of conductivity:
(i) Wash the electrode with distilled water and dry with tissue paper.
(ii) Dip the electrode in 50ml sample for which conductivity is to be measured.
The reading indicated on the meter is the conductivity of the sample.
(iv) Rinse the electrode before and after measurement of conductivity of each sample.
Significance: Conductivity increases as the dissolved ionic species in water increases.
According to Indian standards, the conductivity should be inbetween 5-50mS/m.
Report: The conductivity of the given water sample is
Aim: To determine the amount of the given HCl present in the given one litre solution by
using 0.1N NaOH solution conductometrically.
Apparatus required: Conductometer, Conductivity cell, Magnetic stirrer/ Glass stirrer,
beaker, burette and pipette.
Chemicals required: NaOH solution, HCl solution and distilled water
Principle: According to Kohlrauschs law, the electrical conductance of a solution depends
upon the number and mobility of ions.For the titration of a strong acid like HCl against a
strong base like NaOH, before the NaOH solution is added, the acid solution has a high
conductance due to the highly mobile hydrogen ion. As alkali solution is added the hydrogen
ions are removed due to combination with the hydroxyl ions forming feebly ionized water
(H2O) molecules and their place is taken by the much slower moving Na+ ions.
+ + ( )
Consequently the conductance of the solution decreases and continues to decrease on adding
sodium hydroxide solution until equivalence point is reached. Any further addition of alkali
means increase of Na+ and fast moving hydroxyl ions and thus the conductance begins to
increase. If we plot the conductance measured against the volume of NaOH added, the point
of intersection will give the neutralization point.
Significance:
Titrations involving coloured liquids are difficult to be performed using ordinary indicators.
But these can be easily carried out by conductometric titration method. Moreover,
conductometric titration can be performed accurately even with dilute solutions
Procedure:
1. Wash the conductivity cell thoroughly with distilled water and calibrate the
instrument to its cell constant vaue.
2. Take 20 ml of the given HCl solution whose strength is to be determined in a 100 ml
beaker.
N1V1 = N2V2
Volume of unknown HCl solution taken (V1) = 20ml
Normality of HCl(N1)=?
Volume of NaOH at end point (from graph) =.V2 ml
Normality of NaOH(N2)=0.1N
N1= 0.1V2/20
Amount of HCl present in given one litre solution = Normality X gram equivalent wt. of HCl
= N1X 36.5
= g/L
Result:
The amount of HCl present in the given one litre solution = . g.
P.Haritha, Asst. Professor, Dept. of BS&H; Gudlavalleru Engg. College 32
Expt.No:11
Date:
DETERMINATION OF TURBIDITY OF WATER SAMPLE
Aim: To determine the Turbidity of the given water sample using Turbidity meter.
Apparatus: Nephelometer.
Reagents:
Solution-1: Dissolve 1g of Hydrazine sulphate in 100ml distilled water.
Solution-2: Dissolve 10g of Hexamethylene tetramine in 100ml of distilled water.
Solution-3: Mix 5ml of solution-1 and 5ml of solution-2 in a 100ml volumetric flask. Allow
to stand for 24hrs. Dilute it to 100ml. Now the solution has a known turbidity of 400NTU.
From this stock solution, dilution is carried out to obtain lower
concentrations of 100, 40, 20 and 10 NTU.
Theory: Turbidity is a measure of cloudiness. Turbidity is the property of water because of
which it offers resistance to passage of light. It is caused by suspended solids, living or dead
micro-organisms etc.
The turbidity is measured from the amount of light scattered by the sample taking a
reference with standard turbidity suspension.
Procedure: Calibration of Nephelometer:
i) Select the appropriate range
ii) Insert the test tube( cuvette) with distilled water into cell holder and cover with light
shield.
iii) Adjust zero button to get zero an the display
iv) Take the standard solution of 100 NTU in the test tube and adjust calibration as 100
Measurement of Turbidity:
i) Rinse the test tube before and after measurement of each sample with distilled water and
dry it with a tissue paper.
ii) Take unknown sample of water in the test tube upto the mark indicated on it and place it
in the holder. The display directly gives the turbidity in NTU.
Significance: As per WHO standards, the turbidity of drinking water should be less than 5
NTU.
Report: The turbidity of the given water sample is .NTU