Final Chemistry Lab Manuals - Word File
Final Chemistry Lab Manuals - Word File
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Beaker
Filter funnel
TITRATION ASSEMBLY
D. FIRE HAZARD
1. In case of fire bring the fact immediately in the notice of concerned laboratory instructor.
2. Do not dry chemicals in a drying oven or heat any materials with an open flame unless specifically
directed to do so by the laboratory instructor.
ACKNOWLEDGEMENT BY STUDENT
I have read and understood the Laboratory Safety Regulations. The details have been called to my
attention by the instructor in charge of my laboratory section. I agree to abide by these regulations in
the interest of my own safety and that of my other batch mates.
Name:
Roll No.:
Section: ____________
EXPERIMENT NO –
REQUIREMENTS:
APPARATUS: Burette, burette stand, conical flask, Funnel, Dropper etc.
CHEMICALS: Standard Nil HCI as an intermediate solution, alkaline water.
INDICATOR: Phenolphthalein and Methyl orange (Internal indicator).
THEORY: The alkalinity in water due to the presence of OH-, HCO3- and CO3-2 ions. These ions can be estimated
by titrating them against standard acid solution using phenolphthalein and methyl orange as indicator.
The possibilities of ions present in water are-
1. OH- Only
2. CO3-2 Only
3. HCO3- Only
4. OH- and HCO3-
5. CO3-2 and HCO3-
The possibility of OH- and HCO3- together is ruled out as they combine to give carbonate Ion
OH- + HCO3- CO3-2 + H2O
On the same basis all the three ions cannot be present at the same time in a water sample.
REACTIONS:
OH- + H+ H2O
[P]
CO3-2 + H+ HCO3- [M]
END POINTS: The end point of reaction one and two is known as phenolphthalein end point [P], here the pink
colour of the solution is just disappearing. The methyl orange end point [M] indicates the completion of all the
three reactions and here colour change from yellow to pink.
PROCEDURE:
4. Note down the reading from the burette, which corresponds to phenolphthalein end point (P).
5. Now add 2-3 drops of methyl orange indicator to the same solution, continue the titration with
standard N\10 HCI.
6. Again note down the total volume of N\10 HCl used from. burette, which corresponds to methyl
orange end point (M).
7. Repeat the experiments till concordant readings are obtained.
OBSERVATIONS TABLE:
3. 10ml 0.0 - -
4. 10ml 0.0 - -
CALCULTIONS:
Now, N1 V2 = N2V2
(Sample)= (N/10 HCl)
N1 × 10 =N/10 × x
N1 = x/100
Strength in terms of CaCO3 = x/100 ×50 gm/litre = x/2 gm / litre
PRECAUTIONS:
(1) The apparatus should be cleaned before the start of experiment.
(2) Phenolphthalein end point and methyl orange end point should be noted carefully.
(3) On adding phenolphthalein, if no pink colour appears, it means that no OH- or CO3-2 are present in the
given water sample. In this case add methyl orange in the beginning.
VIVA-QUESTIONS
Q1. What is the suitable range for methyl orange and phenolphthalein to act as Indicators?
Q2. Why OH- and HCO3- ions can-not exist together?
Q3. Give the reason to find the alkalinity in a given water sample?
Q4. Why do we use two indicators to find alkalinity in given water sample?
EXPERIMENT NO –
OBJECT: To determine the temporary and permanent hardness in the given water sample using EDTA as
standard solution by complexometric titration.
APPARATUS: Conical flask, burette, pipette, beaker, measuring flask.
REAGENTS: 0.1N EDTA solution, buffer solution of pH 10, standard hard water, supplied water sample and
boiled water sample.
INDICATOR: Eriochrome Black-T
PRINCIPLE: Temporary hardness of water is due to the presence of soluble salts of bicarbonates of calcium
and magnesium, while the permanent hardness of water is due to the presence of sulphates, chlorides, nitrates
etc. of calcium, magnesium and other heavy metals. Temporary hardness of water can be removed by boiling
the water sample while permanent hardness cannot be removed by mere boiling.
Estimation of total hardness by EDTA method is based on the complexometric titration employing a metal ion
indicator. In EDTA method, a known volume of given hard water is titrated against EDTA solution using
Eriochrome Black-T indicator.
Initially when Eriochrome Black-T indicator is added to the hard water sample, it forms a loose wine red
colored complex with Ca2+ /Mg2+ metal ions present in hard water.
Further when EDTA is added, the loose wine red colored complex completely breaks down and EDTA combines
with Ca2+ /Mg2+ to forms a stable colorless EDTA Metal ion complex and blue Eriochrome Black-T is released, so
the solution now appears blue in color.
PROCEDURE:
1. Take 10ml. of standard hard water in a conical flask. Add 2ml of buffer solution and 3 drops of
Eriochrome Black-T indicator, the colour of the solution turns wine red. Now titrate the solution against
EDTA till the color changes from wine red to blue. Repeat the titration for two concordant readings
2. Take 10 ml of the unknown water sample and titrate it by the same procedure as mentioned above.
3. Take 10 ml of the boiled water sample and titrate it by the same procedure as mentioned above.
OBSERVATIONS:
[A] Titration with standard hard water sample:
S.No. Volume of Water Sample Burette Readings(ml) Volume of EDTA
(ml) used (ml)
Initial Final
1. 10 0.0 -
2. 10 0.0 -
v1 ml
3. 10 0.0 -
4. 10 0.0 -
1. 10 0.0 -
2. 10 0.0 -
v2 ml
3. 10 0.0 -
4. 10 0.0 -
1. 10 0.0 -
2. 10 0.0 -
v3 ml
3. 10 0.0 -
4. 10 0.0 -
CALCULATIONS:-
(A) 1 lit. Solution = 1gm. CaCO3
1000 ml. solution = 1000 mg. of CaCO3
1 ml. solution = 1 mg. of CaCO3
1 ml of standard hard solution = 1 mg CaCO3
v1 ml of EDTA = 10 ml of standard hard water
= l0 mg CaCO3
So 1 ml of EDTA = 10/v1 mg. CaCO3
V2 10
1 ml of given hard water = × mg. CaCO3
V1 10
V2
= mg. CaCO3
V1
V
1000 ml of given hard water = V2 × 1000 mg. CaCO3
1
V2
Total hardness = V1
× 1000 mg. CaCO3
V
= V2 × 1000 mg. CaCO3
1
=…………...ppm
(C) Permanent Hardness :-
10 ml of boiled water = v3 ml EDTA
V3
Permanent hardness = × 1000 mg. CaCO3
V1
=…….…...ppm
(D) Temporary Hardness :-
Temporary hardness = Total hardness - Permanent hardness
=……….....ppm
RESULT: - The given water sample contains.
Total hardness = …..…...ppm
Permanent hardness = ………....ppm
Temporary hardness = ……….ppm.
PRECAUTIONS:-
(1) The glass wares should he properly rinsed with distilled water.
(2) The reaction mixture should be shaken properly.
(3) The amount of indicator should be same in all the titrations.
(4) The pH ( 10+/- 0.1) should be maintained during titration.
VIVA- QUESTIONS
OBJECT: To determine the percentage of available chlorine in the supplied sample of bleaching powder.
(lodo metrically)
REQUIREMENTS:
APPARATUS: Burette, Pipette, Conical flask, Funnel, Mortar and Pestle.
CHEMICALS: Bleaching powder, Potassium iodide, Glacial acetic acid, Sodium thiosulphate as an
intermediate solution (HYPO). Distilled water.
INDICATOR: Freshly prepared starch solution.
THEORY: The bleaching powder in actual is a mixture of calcium hypo chloride Ca(OCl)Cl.3H2O, basic
calcium chloride CaCl2.Ca(OH)2.H2O & some free calcium hydroxide Ca(OH)2. But the active constituent is
calcium hypo chloride, which produce hypo chlorous acid (HOCl) when react with H2O. The HOCl is
responsible for the disinfectant action of bleaching powder.
The amount of Chlorine liberated by the action of dilute mineral acid (H2SO4, HNO3, HCl) on
bleaching powder is known as available chlorine. This available Cl2 is estimated with the help of
iodometric titration. In this method the bleaching powder suspension is treated with dilute mineral acid in
presence of excess of potassium iodide (KI). The Cl2 liberated from CaOCl2 react with KI producing on
equivalent amount of I2. This Iodine get adsorb on the surface of starch (used as indicator) forming a deep
blue coloured starch iodine adsorbed complex. When it is titrated against hypo, the adsorbed iodine reacts
with hypo to form sodium tetra thionate (Na2S4O6).
REACTIONS:
CaOCl2 2HCl CaCl2 + H2O + Cl2
Cl2 + H2O HOCl + HCI
CaOCl2 + 2CH3COOH (CH3COO)2Ca + H2O
2KI + Cl2 I2 + 2KCl
Starch + I2 Starch Iodine adsorbed complex (deep blue)
2Na2S2O3 + I2 Na2S4O6 + 2NaI
(Sodium tetra thionate)
PROCEDURE:
1. Pipette out 10ml of given water sample in a conical flask.
2. Add about half test tube KI solution and half test tube of glacial acetic acid to this solution.
3. Titrate the liberated iodine against standard sodium thiosulphate solution with continuous shaking till the
appearance of light yellow colour.
4. Now add about 7-8 drops of freshly prepared starch (C6H10O5)n solution to it blue colour appears.
5. Titrate again the solution with sodium thiosulphate (Hypo) solution till the disappearance of blue colour
(End Point).
6. Note down the volume of Hypo use from the burette.
7. Repeat the experiments till concordant readings are obtained.
8. Weight of Bleaching Powder (W)……………..gm
END POINT : The deep blue colour is disappeared from solution.
OBSERVATION TABLE:
1. 10 0.0 -
2. 10 0.0 -
V2 ml
3. 10 0.0 -
4. 10 0.0 -
CALCULATIONS:
N1 x V1 = N2 x V2
(Sample) (Hypo)
N1 x 10 = N2 x V2
N1 = N2 x V2
10
RESULTS: The % of available chlorine in the given bleaching powder sample is ---------
PRECAUTIONS:
Q1. What is difference between available chlorine and chlorine content in bleaching powder?
Q2. Why is a fresh solution of starch used?
Q3. For what purpose bleaching powder is used and why do we estimate chloride content in given sample?
Q4. Why is starch indicator added near the end point?
Q5. Why blue color disappears at the end point in iodine titration?
EXPERIMENT NO –
OBJECT: Determine the chloride content in given water sample by Mohr’s method.
REQUIREMENTS:
THEORY: The chlorides are generally present in water in the form of NaCl, CaCl2, MgCl2 etc. These chlorides can
be estimated by titrating against standard AgNO3 solution using K2CrO4 as indicator. The AgNO3 first react with
chlorides present in water forming white colour precipitate as AgCl, the excess drop of AgNO3 react with
K2CrO4 forming brick red coloured precipitate of Ag2CrO4. As the Ksp of AgCl is greater than the Ksp of Ag2CrO4,
hence AgCl will first precipitate. If chloride ions are present in excess, they can replace chromate ion from
Ag2CrO4
REACTIONS:
PROCEDURE:
1. Pipette out 10 ml of water sample in a conical flask.
2. Add 3-4 drops of K2CrO4 indicator solution.
3. Titrate it against standard N/30 AgNO3 solution till the brick red colour of Ag2CrO4 persists
4. Note down the volume of AgNO3 solution used from burette.
5. Repeat the process till concordant readings are obtained.
OBSERVATION TABLES:
1. 10 0.0 -
2. 10 0.0 -
X1 ml
3. 10 0.0 -
4. 10 0.0 -
1. 10 0.0 -
2. 10 0.0 -
X2 ml
3. 10 0.0 -
4. 10 0.0 -
CALCULATIONS:
Volume of given water sample taken = 10 ml
N1 ×V1 = N2 ×V2
N1× l0 = N2 × x
N1 = (N2 × x )/10 = (1/30) × x /10
RESULT: The chloride content in the given water sample is ……… mg/litre.
PRECAUTIONS:
Q1. Why does AgNO3 combine first with chloride ions in the water and not with K2CrO4
Q2. Can tap water be used for the preparation of AgNO3 solution and why a bottle containing AgNO3 is dark
brown or always wrapped with carbon paper?
Q4. Name the indicator used in this experiment and what is the end point
OBJECT: Prepare N/30 Ferrous ammonium sulphate (FAS) and find out the strength and ferrous content in
supplied sample of iron solution by titrimetric analysis against standard potassium dichromate solution
(K2Cr2O7) using potassium ferricyanideK3[Fe(CN)6] as an external indicator.
REQUIREMENT:
APPARATUS: Burette, Burette Stand, Pipette, Beaker, Conical flask, Funnel, Glass rod, Tile, Test tube,
Measuring flask, Dropper etc.
REACTION:
𝑲𝟐 𝑪𝒓𝟐 𝑶𝟕 + 𝟒𝑯𝟐 𝑺𝑶𝟒 → 𝑲𝟐 𝑺𝑶𝟒 + 𝑪𝒓𝟐 (𝑺𝑶𝟒 )3 + 𝟒𝑯𝟐 𝑶 + 𝟑[𝑶]
𝑲𝟐 𝑪𝒓𝟐 𝑶𝟕 + 𝟔𝑭𝒆𝑺𝑶𝟒 + 𝟕𝑯𝟐 𝑺𝑶𝟒 → 𝑲𝟐 𝑺𝑶𝟒 + 𝑪𝒓𝟐 (𝑺𝑶𝟒 )3 + 𝟑𝑭𝒆𝟐 (𝑺𝑶𝟒 )3 + 𝟕𝑯𝟐 𝑶
PROCEDURE :
1. 10 0.0 -
2. 10 0.0 -
V1 ml
3. 10 0.0 -
4. 10 0.0 -
1. 10 0.0 -
2. 10 0.0 -
V2 ml
3. 10 0.0 -
4. 10 0.0 -
CALCULATION:
Weight of Salt = NEV/ 1000 = gm-
56 x Strength
Amount of ferrous content =
392.12
Ferrous content =………….. gm.
RESULTS: Strength of supplied water solution is ---- gm/litre
Ferrous content in supplied iron solution is………. gm
PRECAUTIONS:
1. In acidic medium K2Cr207 reacts as an oxidising agent therefore, small amount of dilute H2SO4 is added in
Mohr's salt solution.
2. The glass apparatus should be cleaned properly with distilled water.
3. The volume of solution taken out for the checking of end point should be very small.
VIVA QUESTIONS
Q1. Why is ferrous ammonium sulphate solution used in the titration and not direct ferrous sulphate?
Q2. What is the formula of ferrous ammonium sulphate and any other name for it?
Q3. Why is dilute H2SO4 added while preparing standard solution of ferrous ammonium solution?
Q4. Why is K3Fe(CN)6 potassium ferricyanide is used as external indicator in ferrous ammonium sulphate vs
K2Cr2O7 titration?
Q5. Why is dilute H2SO4 and not HCl/HNO3 used in redox titrations?
Experiment-
Object:
To determine the surface tension of a given liquid at room temperature using stalagmometer by drop number
method.
Requirements:
Stalagmometer, specific gravity bottle, a small rubber tube with a screw pinchcock, distilled water,
experimental liquid.
Theory:
In the drop number method, the number of drops formed by equal volumes of two liquids is counted. Let m 1
and m2 are the mass of one drop of each of the liquid having densities d1 and d2, respectively. If n1 and n2 is
the number of drops formed by volume (V) of the two liquids, then their surface tensions are related as:
γ1 d1 n2
= ×
γ2 d2 n1
One of the liquid is water, its surface tension and density are known. Then, the surface tension of the given
liquid can be calculated.
Procedure:
(1)Clean the stalagmometer with chromic acid mixture, wash with water and dry it
(2)Attach a small piece of rubber tube having a screw pinchcock at the upper end of the stalagmometer.
(3) Immerse the lower end of the stalagmometer in distilled water and suck the water 1-2 cm above the mark
‘A’. Adjust the pinchcock so that 10-15 drops fall per minute.
(4)Clamp the stalagmometer.
Allow the water drops to fall and
start counting the number of
drops when the meniscus
crosses the upper mark A and
stop counting when the
meniscus passes mark B.
(5)Repeat the exercise to take three to four readings.
(6)Rinse the stalagmometer with alcohol and dry it.
(7)Suck the given liquid in the stalagmometer and count the number of drops as in case of water.
(8)Take a clean dry weighing bottle. Weigh it with water as well as with liquid.
(9)Note the temperature of water taken in a beaker.
Observations:
2
3
Calculations:
w2 − w1
Density of water (d1 ) =
Vol. of R. D. bottle
w3 − w1
Density of water (d2 ) =
Vol. of R. D. bottle
d1 n2
Surface tension of liquid (γ1 ) = × × γ2
d2 n1
Q1. Name the instrument used to determine the surface tension of a given liquid at room temperature.
η = ……..(1)
where, P= hydrostatic pressure of the liquid, V= volume of the liquid of viscosity ‘η’ flowing in time ‘t’, through the
capillary tube of radius ‘r’ and length ‘l’. If t1 and t2 are times required to flow for equal volumes of two liquids
through the same length of the capillary tube, then from equation (1) , we have
= ………..(2)
= ………(3)
Where, and are the densities of two liquids and η1 and η2 are their
viscosities.
Procedure:
1. Thoroughly clean the Ostwald’s viscometer with chromic acid and wash
finally with distilled water.
2. A known volume of water is introduced into the bulb-C of the viscometer.
3. The water is then gently sucked into the bulb-A.
4. Allow the water to flow back and note the time (t2) required for the water to
flow through the capillary from the mark A to B.
5. Repeat it for three times.
6. Similarly note down the time of flow of the given liquid (t1)
7. Again take three concordant readings.
8. Density of water and the liquid is determined by R.D. bottle.
OSTWALD’S VISCOMETER
Observations –
1. Viscosity of water (η2) = 0.01 poise.
2. Time of flow between A & B.
Given liquid Water
S.No.
Time of flow Mean (t1 ) Time of flow Mean (t2 )
1
Calculations –
VIVA QUESTIONS
Q1. What do you mean by viscosity?
Q3. How many types of viscometers are there and what is the difference between them?
EXPERIMENT NO.
OBJECT: To determine the pH of the given soft drink with the help of pH meter. And the strength of
the given hydrochloric acid solution by titrating it pH metrically against sodium hydroxide with the
help of pH meter.
REQUIREMENTS:
APPARATUS: Digital pH meter with combined electrode (Glass electrode, reference electrode), Beaker, Burette,
Burette stand, funnel, Stirring road etc.
CHEMICALS: Buffer solution of pH 4.0 and 9.0 (acidic and basic), unknown solution of Hydrochloric acid, sodium
hydroxide solution.
THEORY: The pH of solution is defined as negative of the logarithm of hydrogen ions concentration.
pH = -log [H+]
When an alkali is added to an acid solution the pH of the acid solution increase slowly but near the equivalence
point, it changes very sharply. When volume of alkali added is plotted against the pH of acid, a sigmoid curve is
obtained. From this curve, volume of alkali can be determined up to the equivalence point.
PROCEDURE:
1. Standardize the pH meter against a buffer solution of known pH.
2. Wash the electrode properly with distilled water.
3. Take about 50 ml of HCl in a beaker and dip the electrode completely into it.
4. Note down the pH of the pure acid solution.
5. Now added 1.0 ml of NaOH solution from the burette to this acid solution, after proper mixing note the pH
of the solution.
6. In the similar way, go on adding NaOH solution from the burette up to say 11-12 ml and note the pH of the
solution at every addition.
7. pH of the solution changes rapidly near the equivalence point.
8. Now add alkali in fraction of 0.2 ml.
OBSERVATION TABLE:
Volume of 0.0 1.0 2.0 3.0 4.0 4.5 5.0 5.5 6.0 6.5 - - - - -
NaOH added
(ml)
pH Value
CALCULATIONS: A curve is plotted with pH values as ordinate and the volume of NaOH added (ml) as abscissa.
Find out equivalence point, suppose
Volume of NaOH used at the equivalence point = V2 ml.
Volume of HCl taken = 50ml
N1V1 = N2V2
(Acid) = (Alkali)
N1 × 50 = 1/10 × V2
N1 = (1 × V2)/ (50 × 10)
Strength of HCl solution = (V2 × 36.5) / 10 × 50 = ……………………… gm. / liter.
RESULT:
The strength of the given Hydrochloric acid is ………………………. gm / liter.
PRECAUTIONS:
1. The pH meter should be standardized first by using a buffer of known pH.
2. The electrodes must be washed properly and dried before dipping in the acid solution.
3. The temperature control knob of the pH meter should be adjusted to the room temperature.
4. After each addition of NaOH, the solution should stir thoroughly.
VIVA QUESTIONS
Q3. Which method is more accurate to find the end point volumetric or Ph method and why?
Procedure -:
(1) Place 5 ml glacial acetic acid in 100ml beaker
(4) Warp a cloth or a towel loosely round the beaker and add few ml of conc. HCl into
the mixture carefully. Within 5 minutes a large mass of pink plastic is formed
(5) The residue obtained is washed several times with distilled water and filtered
product is dried and yield is calculated.
VIVA QUESTIONS
It is water soluble and hence is used as sizing agents and textile finishing resin. It is also used in the paper industry
to improve the wet strength of paper. In the plywood industry used as adhesive.
Procedure -:
(1) Place 5 ml of 40% Formaldehyde solution in 100ml beaker
(2) Add about 3 gms of urea while stirring until a saturated solution is obtained.
(3) Add a few drops of conc. Sulphuric acid with stirring continuously during the addition.
(4) All of a sudden a voluminous white solid mass appears in the beaker.
(5) When the reaction is complete wash the residue with water and dry the product and calculate the yield of
the product formed.
OBJECT: Determination of iron concentration in sample of water by colorimetry using KCNS as colour developing
agent.
APPARATUS: Colorimeter, Burette, Pipette, Measuring Cylinder and Beaker, test tubes, Cuvette
CHEMICALS: 0.1% Fe3+ -ion solution (with excess HCl), 20% KCNS in distilled water.
THEORY: Spectroscopy is that branch of science which deals with the interaction of matter with electromagnetic
radiations, which are different waves of energy. It covers a wide range of wavelengths or energies and visible light
is part of electromagnetic radiations. When monochromatic visible light falls on the homogeneous medium, the
intensity of transmitted light is less than that of incident light. A part of incident light has been absorbed.
Io=Ia +It
Io- intensity of incident light, Ia- intensity of absorbed light, It- intensity of transmitted light
A Spectrometer is a device which detects the percentage transmittance of light radiation, when the light of certain
intensity and frequency range is passed through the sample. It is based on Lambert Beer Law which states that
“when a monochromatic light is passed through the sample medium, the intensity of that light decreases
exponentially with the increase in concentration and thickness of absorbing medium.”
It=Io e-ct
A- Absorbance
T- Thickness of medium
If the same sample cell i.e. T is constant is used for measurement of absorbance of solution having different
concentrations then extent of absorbance (A) is directly proportional to the concentration (C) of the medium.
Thus, if a graph is plotted between A and C, we get a straight line in compliance with Lambert Beer Law. This is
known as calibration curve.
For measuring the concentration of given solute, the calibration curve is obtained by measuring the absorbance of
standard solution of different concentration. This calibration curve is then used to measure the conc., of unknown
solution.
PROCEDURE:
a) Setting of colorimeter:
Insert a cuvette containing distilled water in the sample holder adjust the control knob to get zero absorbance
b) Determination of λmax:
Insert the cuvette containing given colored solution and note the absorbance reading at different wavelengths or
filters. At a specific wavelength maximum absorbance will be observed with given coloured solution
c) Determination of concentration of sample solution:
Once λ max is fixed. Prepare the following solution from given sample solution and distilled water using a
measuring cylinder
I 10
II 20
III 30
IV 40
V 50
VI 60
VII 70
VIII 80
IX 90
X 100
Unknown solution
Note down the value of absorbance of above prepared solutions in series. Plot a graph of values of absorbance so
obtained and respective concentration should be a straight line. Now note down the absorbance of unknown
concentration solution.
OBSERVATION TABLE:
% concentration 10 20 30 40 50 60 70 80 90 100
GRAPH:
= (56xA×1000)/392mgm/litre
RESULT: The concentration of Fe (III) in the given sample is obtained from the graph & calculated to be ……….ppm.
PRECAUTIONS:
1) For the preparation of calibration curve, dilute solutions of unknown concentration should be used
Q1. Explain the law on which this experiment is based and how do we prove it.
Q3. What is visible spectrum? What happens when visible spectrum is made to fall upon a colored solution?