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LABORATORY MANUAL
CHE102
CHEMISTRY LAB
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LMCHE 102: CHEMISTRY LAB
General Rules:
2. Mobile phones should be switched off and kept in the bag during lab hours.
5. Do not do any undisciplined activity in lab as you are under strict cc-TV
surveillance.
Precautionary Rules:
1. Never pipette out strong acids and bases with your mouth, it can be
dangerous, therefore use measuring cylinders for such chemicals.
3. Cap the bottles after taking chemical as uncovered bottles can be a source of
harmful fumes.
4. In case of any accidental spill over of any chemical on you, report your
teacher or lab technician immediately.
5. Report your lab technician if any breakage of glass apparatus takes place.
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LMCHE 102: CHEMISTRY LAB
Table of Contents
Chemistry)
Other Reading:
th
2. J. B. Yadav, Advance Practical chemistry, Krishna Publications, Merrut 12
Revised Edition
3. Basset J Denny. R. C., Jeffery C. H. and Mendham J., Vogel’s Textbook of
Quantitative Inorganic analysis, ELBS, 1978. (Inorganic)
4. N. K. Vishnoi Advanced Practical Organic Chemistry, Vikas Publications, New
nd
Delhi, 2 edition
5. M.S. Saini, Senior practical chemistry-Vol-III, Modern Publishers-2006
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LMCHE 102: CHEMISTRY LAB
Experiment No. 1
Title: To determine the hardness of the given hard water sample by EDTA method.
Provided Standard Hard Water (1 ml of SHW =1 mg of CaCo3).
Chemicals Used: Standard Hard water, EDTA solution, Eriochrome black-T (EBT),
Buffer Solution, Sample hard water.
Learning Objectives:
ii. To know about use of buffer solution: The buffer being used has composition
NH4Cl and NH4OH. Its pH is the order of 10.5.
iii. How the indicator works: When indicator is added to hard water it combines
with free metal ions present in water.
When all the free metal ions are exhausted, next drop of EDTA removes the metal
ion engaged with indicator and the original blue color is restored.
Procedure:
(a) Standardisation of EDTA solution:
Pipette out 10ml of standard hard water in the titration flask. Add to it 2-3ml of
buffer solution and two drops of Eriochrome Black-T indicator. A wine red
color appears.
Titrate this solution against EDTA solution taken in a burette till wine red
colour changes to blue color.
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LMCHE 102: CHEMISTRY LAB
This is the end point. Recovered the volume of EDTA consumed as A ml.
Repeated the procedure to get at least three concordant readings.
Pipette out 10ml of sample hard water in the titration flask. Add to it 2-3ml of
buffer solution and two drops of Eriochrome Black-T indicator.
A wine red colour appears. Titrate this solution against EDTA solution taken in
a burette till wine red colour changes to blue color.
This is the end point. Recovered the volume of EDTA consumed as B ml.
Repeated the procedure to get at least three concordant readings
Calculations:
(a).Standardisation of EDTA solution:-
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LMCHE 102: CHEMISTRY LAB
A ml of EDTA = 10 mg of CaCO 3
Scope of result: The determination of water hardness is a useful test that provides
a measure of quality of water for households and industrial uses. Originally, water
hardness was defined as the measure of the capacity of the water to precipitate
soap.
Parameters: Volumetric
Error Analysis:
Cautions:
i. The burette, pipette and conical flask should be washed and then rinsed with
distilled water.
ii. Redistilled water should be employed for preparing the EDTA solution.
iii. The colour change near the end point is very slow and thus should be
observed very carefully.
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LMCHE 102: CHEMISTRY LAB
Experiment No. 2
EQUIPMENTS TO BE USED: China dish, water bath, glass rod, Buchner funnel,
glass funnel, weighing machine, filter papers, measuring cylinder, beakers etc.
LEARNING OBJECTIVES:
(i) To know about gravimetric analysis of ions
(ii) The students will learn how the transition complex formation is helpful to
determine amount of particular ion in given salt.
PROCEDURE:
Put some water in a beaker and place it on a hot plate for heating.
Weigh 2g ferrous ammonium sulphate (Mohr’s Salt) (NH4)2SO4•FeSO4•6H2O.
Transfer the ferrous ammonium sulphate to a beaker containing 25 mL of
warm water.
Acidify this solution with 1 mL dilute 3M H2SO4.
To this solution add 25 mL of oxalic acid solution (5 g/50mL).
Cautiously heat the solution to boiling on a hot plate, continuously stirring the
solution to avoid bumping.
Remove and then allow the precipitate to settle.
Decant and discard the clear supernatant liquid (avoid loss of precipitate). Stir
the remaining precipitate with 25 mL of hot water.
Again decant and discard the wash liquid. Add 25 mL of hot water to the
precipitate and stir.
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LMCHE 102: CHEMISTRY LAB
Then filter by suction using a small Buchner funnel and wash the precipitate
thoroughly with small portions (10-20 mL) of hot water. Finally rinse with acetone.
Keep these precipitates in oven for drying. Weigh the final product.
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LMCHE 102: CHEMISTRY LAB
Parameters: NA
Relationships to be determined: NA
Graphs/Plots: NA
Error Analysis:
Cautions:
2. 3M H2SO4
3. 30% H2O2
4. alcohol
5. Acetone
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LMCHE 102: CHEMISTRY LAB
Experiment-3
EQUIPMENTS TO BE USED: Test tube, China dish, fusion tubes, glass rod, Bunsen
Burner, tripod stand, funnel, beaker, filter papers, beakers etc.
LEARNING OBJECTIVES:
(i) To know about presence of various elements present in the given compound
(ii) Presence of nitrogen and sulphur in the given compound can be detected.
(iii) Presence of halogens present in the compound can be detected.
THEORY:
Chemical equations:
FeSO4 + 2NaOH Fe(OH) 2 + Na2SO4
PROCEDURE:
Preparation of Lassaigne's extract:
In a dry fusion tube take a small piece of sodium metal, and heat the fusion tube
in the flame so that the sodium metal is melted completely.
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LMCHE 102: CHEMISTRY LAB
To this heated tube add carefully a small amount of given compound, and heat
the fusion tube again in the flame till it gets red hot.
Pour the red hot fusion tube immediately into a china dish containing 20 mL of
distilled water (care should be taken that china dish should not contain any
impurity or chemical which could interfear in the detection)
Repeat the procedure for at least seven times with fusion tube (add the fusion
tube to the same china dish having distilled water)
Crush all the fusion tube in china dish with the help of a clean glass road and boil
the solution in china dish to evaporate so that the volume is reduced nearly half.
Filter the content through filer paper and collect the solution obtained in a clean
beaker, the solution obtained will be Lassaigns extract.
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LMCHE 102: CHEMISTRY LAB
In a clean test tube take about 2 mL of the Lassaignss extract and add one mL
Conc. HNO3 to this solution add 1 mL of tollen’s reagent the formation of
precipitate indicates the presence of halogens in the given compound
Identification of halogen
If the precipitate formed are white in colour which are readily soluble in NH4OH,
these indicates the presence of chloride in the given compound
If the precipitate formed are pale yellow in colour which are partially soluble in
NH4OH, these indicates the presence of bromine in the given compound
If the precipitate formed are yellow in colour which are insoluble in NH4OH, these
indicates the presence of iodine in the given compound
RESULT: ...........................……….
of an element?
Graphs/Plots: NA
Error Analysis:
Cautions:
i. Sodium metal should be handled very carefully
ii. Sodium metal should never be allowed to come in contact with water.
iii. On addition of Fe(OH)2 a dirty green precipitate comes out which are not true
indicator for the presence of nitrogen in the compound, these appear due to the
formation of ferric hydroxide which is soluble in dilute sodium hydroxide.
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LMCHE 102: CHEMISTRY LAB
Experiment No. 4
Learning objectives:
i. Students will learn the basics of pH meter and how to use pH meter.
ii. To monitor the total pH of a solution and to determine equivalence point of
titrations that involve ions.
iii. Students will learn how to use a calibration curve to determine the unknown
strength of a solution.
iv. To calculate the dissociation constant of weak acid.
Glass electrode
To set temperature To set knob at pH
Fig: pH meter
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LMCHE 102: CHEMISTRY LAB
equilibrium constants as the unionized form is present to such a small extent. Hence,
the study of ionic equilibrium and calculation of K is applicable only to weak acids.
During the titration of an acid with a base, the pH of the solution rises gradually at
first, then more rapidly and until at the equivalence point, there is a very sharp
increase in pH for a very small quantity of added base. Once past the equivalence
point, the pH increases only slightly on addition of excess base. The titration curve is
obtained by plotting changes in pH at different amounts of the base added and the
equivalence point is determined.
PROCEDURE:
With the help of temperature knob shown in the Fig set the temperature to the
room temperature.
Then wash the electrode and put it in pH 7 solution and set 7 on the screen.
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LMCHE 102: CHEMISTRY LAB
Pipette out 50 mL of the given weak acid into a 100 cm3 beaker. Immerse
electrode assembly into the acid. Measure the pH of the acid.
Add 1 mL of the base from burette to the acid. Stir the solution thoroughly and
measure the pH after addition.
When the pH begins to show a tendency to increase rapidly (e.g. from 6-9),
add only small increments (say 0.1 mL) of the base and measure the pH after
each addition. Continue till there is only a slight increase in pH on the addition
of the base.
Again add 1mL of base for 3-4 time more and note down the change in pH.
(ml.)
1. 0
2. 1.0
3. 2.0
4. 3.0
- -
2) Half equivalence point =............... (take half of the vol. of NaOH at Eq. Pt. in mL)
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LMCHE 102: CHEMISTRY LAB
pKa = - log Ka
Ask for the original value from your instructor for error calculations.
Result: ……
Parameter used: pKa = - log Ka, hence the value of dissociation constant(Ka) can
be calculated
Plot:
Equivalence point
pH
PRECAUTIONS:
2. Switch on the pH meter at least 10 minutes before the start of the measurements.
4. Let the reading stabilize for tome time (15 seconds) before taking the reading.
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LMCHE 102: CHEMISTRY LAB
Experiment No. 5
Learning objectives:
i. Students will learn the basics of Conductometer and how to use Conductometer.
ii. To monitor the total conductance of a solution and to determine the end points of
titrations that involve ions.
iii. Students will learn how to use a calibration curve to determine the unknown
strength of a solution.
iv. Students will get knowledge about conductometric titrations.
Value of Cell Constant
Range
To set temperature
Fig.: Conductometer
THEORY: Conductometry can be used to detect the equivalence point (end point) of
a titration. This method is based upon the measurement of conductance during the
course of titration. The conductance varies differently before and after the
equivalence point. This is due to the reason that electrical conductance of a solution
depends upon the number of icons present and their ionic mobilities i.e. speeds.
When conductance values are plotted against volume of titrant added, two straight
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LMCHE 102: CHEMISTRY LAB
lines are obtained; the point of intersection of the lines gives the end point. For
studying HCl vs NaOH titration, a know volume of HCl is taken in a beaker and
NaOH solution in the burette. The conductance of acid solution is noted initially as
well as after successive additions of small amounts of NaOH solution.Conductance
of acid solution in the beginning is very high due to presence of highly mobile H +
ions. On adding NaOH solution, the H+ ions are replaced by slow moving Na ions,
decreasing the conductance of solution.
PROCEDURE:
Determine the cell constant of the given conductivity cell which is written on the
neck of the cell.
Connect the conductivity cell to the conductometer.
Set the function switch to check position. Display must read 1.000. If it does not,
set it with CAL control at the back panel.
Put the ‘Function Switch’ to ‘Cell Constant’ and set the value of the cell constant
determined in step-1 with the help of cell constant Knob shown in the Fig.
Set the temperature control to the actual temperature of the solution under test.
Rinse the conductivity cell with the solution whose conductivity is to be
measured.
Take 20 ml of the given HCl in a 100 ml beaker.
Wash the conductivity cell with distilled water and then rinse it with it with the
given HCl solution. Dip the cell in the solution taken in the beaker.
Set the range with the help of “range” knob shown in the Fig to 200.
Set the ‘Function Switch’ to ‘Conductivity’ and read the display. This will be the
exact conductivity note it down.
Take alkali (NaOH) in the burette and 0.5 mL of it into the beaker containing HCl.
Stir and determine the conductivity.
Repeat the procedure of addition of 0.5 mL of NaOH and noting down the
conductivity in the observation table.
Take 12-15 readings in the ways. After each addition, stir the solution gently.
Plot a graph between observed conductivity value along Y-axis against the
volume of alkali added along x-axis. The point of intersection gives the amount of
alkali required for neutralization of acid.
OBSERVATIONS AND CALCULATIONS:
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LMCHE 102: CHEMISTRY LAB
OBSERVATION TABLE
(ml.) (mmoh/cm)
1. 0.5
2. 1.0
3. 1.5
4. 2.0
- -
- -
22. 11.0
23. 11.5
24. 12.0
N1V1 = N2V2
(HCl) (NaOH)
N1 x 20 = 0.1 x A
N1 = a N
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LMCHE 102: CHEMISTRY LAB
% error: Ask your instructor for the actual value and the calculate error in your
result.
PLOT: When a graph is potted between volume of the alkali added and conductance
then a V – shaped graph is obtained. The point of intersection will give the end point.
X z
Conductance (ohm)
Conductance
Conductance
Y end point
PRECAUTIONS:
1. The solution taken in the burette should be about ten times stronger than that
taken in the beaker so that the volume change of latter solution is negligible on the
addition of the former solution.
2. After every addition of NaOH solution, the solution must be stirred thoroughly.
1. 0.1 N NaOH.
2. 0.01 N HCl
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LMCHE 102: CHEMISTRY LAB
Experiment No. 6
AIM: To test the validity of Beer-Lambert’s law using colorimeter and to determine
unknown concentration of solution.
Learning Objectives:
1. Students will learn the basics of colorimetry and how to use colorimeters
2. Students will gain practice in preparing solutions through dilution and in
calculating solution concentrations
3. Students will use algebraic representations to describe data
4. Students will learn how to use a calibration curve to determine the unknown
concentration of a solution
Fig: PhotoColorimeter
According to Beers Lambert’s law the intensity of the incident light is proportional to
the length of thickness of the absorbing medium and the concentration of the
solution.
(1)
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LMCHE 102: CHEMISTRY LAB
(2)
A = ƐCl
PROCEDURE:
Connect the instrument to the mains and put on the power switch.
Open the lid on the cell compartment and insert a cuvette containing the
distilled water. Close the lid.
Adjust the reading on the digital screen to zero optical density with the
knob shown in the Fig.
Remove the cuvette and close the lid tightly again. Empty the cuvette and
rinse it with standard solution of KMnO4 (0.001 IM) [which will be
provided to you by lab technician]. Fill the cuvette this solution and note
the optical density.
Change the wave length to the next high value using set wavelength knob
every time and note down corresponding optical density. Make table with
wavelength on LHS and OD at RHS.
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LMCHE 102: CHEMISTRY LAB
Table 1:
S.No. Wavelength (λ) in nm O.D.
1.
2.
3.
Plot a graph between wavelength on the x-axis and O.D. on the y-axis. Find
the value of λmax ( O.D is maximum)
O.D
λmax
Wavelength (nm)
Now set the λmax value in the colorimeter with the help of the knob used for
setting wavelength and place the cuvette containing Distilled water in the cell
compartment. Set O.D to zero again.
Table 2:
S.No. Composition (%) O.D.
1. 10
2. 20
3. 30
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LMCHE 102: CHEMISTRY LAB
Note down the absorbance (OD) of series of solution of KMnO 4 prepared
above (from 10% to 100%) by the method described above. Do not change
wavelength now.
Plot a graph between O.D against composition. (If a straight line is obtained
Lambert - Beer’s a law is verified)
Now take a solution of a unknown concentration and note down optical
density. Find out the concentration of the unknown solution from graph.
Table 3:
Scope of result: This experiment is used to study the absorbance power of different
solutions and also to find the unknown concentration of solution
Plot: A plot between absorbance and concentration is expected to the linear. Such a
straight line plot, passing through the origin, shows that Beer- Lambert’s law is
obeyed. This plot, known as calibration curve can also be also employed in finding
the concentration of a given solution.
O.D
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LMCHE 102: CHEMISTRY LAB
% error: Ask your instructor for the actual value and the calculate error in your
result.
PRECAUTIONS:
4. Let the reading stabilize for tome time (15 seconds) before taking the reading.
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LMCHE 102: CHEMISTRY LAB
Experiment No. 7
Learning objectives:
(ii) The students will learn how the transition complex formation is helpful to
determine amount of particular ion in given salt.
Chemical Reaction:
Red ppts
H
O O
H3C H3C CH3
N OH C N N C
2 NiSO4 2NH4OH Ni (NH4)2SO4 2H2O
C N N C
N OH H3C CH3
H3C
O O
H
Theory:
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LMCHE 102: CHEMISTRY LAB
Calculation:
288.69 58.69
Error Analysis:
% error: Calculate the actual amount of Ni in starting Nickel chloride taken for the
preparation and calculate the % error.
Parameters: NA
Plots/Graphs: NA
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LMCHE 102: CHEMISTRY LAB
Experiment No. 8
Chemical required: 0.1 NaOH, methyl acetate, 0.5 N HCl, Stop watch, Water bath,
Phenolphthalein.
(3) Student will learn how to find the order of reaction with the help of rate constant at
different time intervals.
(4) To prove that order of reaction is experimental concept.
During the hydrolysis of ester, acetic acid is produced. Therefore, the progress of
reaction is followed by determining the amount of acetic acid formed at different time
intervals.
H
CH3COOC2H5 + H2O CH3COOH + C2H5OH
A definite quantity of the reaction mixture is withdrawn after different time intervals
and is titrated against a standard solution of alkali. The amount of alkali used is
equivalent to the total amount of HCl present initially and the amount of acetic acid
formed. The volume of alkali used at the start of reaction is equivalent to amount of
HCl alone. Hence, the amount of acetic acid formed (x) after different intervals of time
can be calculated. The amount of acetic acid formed at the end of reaction is
equivalent of initial concentration of ester (a). Suppose the volumes of alkali used
required for the reaction, at the start, after time t and the end of reaction are V 0,Vt,Vα
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LMCHE 102: CHEMISTRY LAB
K = 2.303 log V∞ - V0
t V∞- Vt
If the value of K comes out constant during different intervals of time, then order of
reaction will first order.
Procedure:
Take 50ml of 0.5 N HCl in a clean dry 250mL conical flask and about 10mL
of pure ethyl acetate in a test tube, cork both of them and place them in a
thermostat or water bath at or near room temperature. (Take water in a big
beaker and put conical flask and test tube in it).
Keep the 0.5N HCl and ethyl acetate in the thermostat or water bath for about
10 min to allow them to acquire the temperature of the bath.
In the mean time, fit the burette properly and fill it with 0.1N NaOH solution.
At about 9 minutes add 25mL of ice cold water in a separate conical flask.
After 10 minutes pipette out 5mL of the ethyl acetate from the test tube and
add it to the flask containing 50 mL of 0.5 N HCl. Start stop watch at this
moment from zero again.
Shake the contents for 2-3 seconds and immediately pipette out 5 mL of
reaction mixture and transfer it at once to first conical flask containing ice cold
water.
Keep the flask containing reaction mixture in the water bath again, it should
be noted that reaction mixture will be kept in the water bath at constant
temperate throughout the experiment.
Titrate the solution in conical flask containing 25 mL ice cold water and 5 mL
of reaction mixture against 0.1 N NaOH taken in burette by using
phenolphthalein as indicator. Appearance of pink colour is end point. The
volume of 0.1 N NaOH used against the withdrawn sample of the ester and
dil. HCl mixture is taken as V0.
After about 9 minutes add 25mL of ice cold water in a separate conical flask.
Pipette out 5 mL of mixture and add it to the conical flask containing ice cold
water after 10 min. Titrate it against 0.1 N NaOH . This gives V t after 10 min.
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LMCHE 102: CHEMISTRY LAB
Repeat the above procedure after every 10 min for taking readings upto 40
minutes.
Place the remaining reaction mixture in the separate water bath at 60-70oC for
about half to one hour time. Pipette out 5 mL of mixture and titrate it against
alkali solution. This gives V∞.
1. 0 V0
2. 10 V10 V∞ - V10
3. 20 V20 V∞ - V20
4. 30 V30 V∞ - V30
5. 40 V40 V∞ - V40
6. ∞ V∞
Calculations: Calculation of K at time 10, 20, 30 and 40 min will be done by the
following formula:
t V∞- Vt
Parameter used: Rate constant (K): The value of K comes out constant during
different intervals of time,then order of reaction will first order.
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LMCHE 102: CHEMISTRY LAB
Error Analysis:
Plot:
be calculated.
t (min)
Precations:
1. 0.1 N NaOH
2. 0.5 N HCl
3. Ehtylacetale
4. Icecold water
5. Phenolphthalein indicator
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LMCHE 102: CHEMISTRY LAB
Experiment No. 9
Title: Determine the strength of given solution of ferrous ammonium sulphate
(Mohr’s salt) by titrating against potassium dichromate solution.
Equipment Required: Volumetric flask, 250 mL Beakers, 50 mL Burette, pipette,
funnel etc.
Material Required:
Potassium dichromate K2Cr2O7 reagent grade, Ferrous ammonium sulphate,
Sulphuric Acid (concentrated).
Learning Objectives:
i. Student will learn how to calculate the exact normality of Ferrous ammonium
sulphate (Mohr’s salt) by titrating with potassium dichromate solution.
ii. To gain knowledge about redox titration.
Theory: This experiment is an example of redox titration. The loss of electrons is
oxidation; the gain of electrons is reduction. Reduction/oxidation (redox) processes
occur when electrons are transferred from a donor species (the reducing agent
2FeSO4(NH4)2SO4) to another acceptor species (the oxidizing agent K2Cr2O7).
Reactions: The reaction between Potassium dichromate and Mohr’s salt can be
represented as:
Molecular equations:
K2Cr2O7 + 4H2SO4 → K2SO4 + Cr2(SO4)3 + 3[O]
Ionic Equations:
2Cr2O72– + 14H+ + 6e– → 2Cr3+ + 7H2O
Fe2+ → Fe3+ + e-
Procedure:
Titration of K2Cr2O7 soln. with Mohr’s salt solution
Pipette out 10 mL of Mohr’s salt solution in the conical flask.
Add approximately 4 mL of Conc. H2SO4 to the same flask.
Add 2-4 drops of the Ferroin indicator.
Titrate the reaction mixture with potassium dichromate solution taken in burette
till a colour change from Wine red - green is obtained.
Repeat the titration for three concordant readings.
Observations and Calculations
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LMCHE 102: CHEMISTRY LAB
Table.
Precautions:
(i) Always take Potassium dichromate solution in burette.
(ii) Potassium dichromate acts as oxidizing agent in acidic medium. Therefore
always add dil. H2SO4 in the reducing agent.
(iii) Read the upper meniscus while taking burette readings because K 2Cr2O7 is
coloured.
Requirements for Lab Technician:
1. N/20 Mohr’s salt solution.
2. N/20 potassium dichromate solution.
3. Cons. H2SO4.
4. Ferroin indicator.
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LMCHE 102: CHEMISTRY LAB
Experiment No. 10
Title: Separation of amino acids by thin layer chromatography.
Equipments Required: Glass plates, beaker, Glass rod,
Chemicals Required: Silica gel (for TLC), Glycine, Leucine, acetic acid, n-butanol,
water, alcoholic solution of ninhydrin
Learning Objectives:
i. Students will learn the basis of TLC and how to prepare the TLC plates.
ii. To calculate retention factor (Rf).
iii. Students will learn how to separate the mixture of organic compounds on the
basis of Rf value
Theory: Thin Layer Chromatography (TLC) is used extensively for qualitative
analysis (tentative identification of mixture of two or more organic compounds). In
this technique a small amount of the material (to be separated), dissolved in an
appropriate solvent, is spotted near one edge of the plate covered with thin layer of
adsorbent.
The adsorbent is usually a thin layer of alumina or silica gel. After the sample
has been deposited on the adsorbent, the coated plate is placed in a beaker
containing small amount of solvent in such a manner that the lower end of plate dips
1-2 cm below the surface of solvent. The solvent rises through the adsorbent by
capillary action and the various components of the mixture ascends at different rates,
depending on their different affinities to the adsorbent.
This results in the separation from one another. When the solvent front has
almost reached the top of the adsorbent layer or three-fourth of it, the plate is
removed from the beaker, dried and examined.
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LMCHE 102: CHEMISTRY LAB
Rf value =
= b/a
Procedure:
Take small amount of silica gel in a beaker and dissolve it in distilled water
with constant stirring by a glass rod. Continue to stir until a uniform paste free
from air bubbles is formed. Add some more water to obtain slurry of suitable
consistency. (OR this slurry may be provided to you by the lab
technician).
Mark the base line on the glass plate about 1 cm from the bottom edge of the
glass plate. (Mark only at edges with pencil). This line is just to take an idea
that where is 1 cm distance lies from the bottom where sample mixture is to
be applied.
Pour the slurry on to the clean and dry plate and prepare a uniform thin layer
by glass rod.
Allow the layer to dry for 5-10 minutes and then heat the plates in an electric
oven at 100-120oC for about 20 min.
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LMCHE 102: CHEMISTRY LAB
At base line and apply small sample of the mixture with the help of thin
capillary tube in the centreu. Take care the spots must be as small as
possible.
Allow the spot to dry. Place the glass plate in a beaker containing solvent to a
depth of about 1 cm or less than that and allow the solvent to flow up until it
nearly reaches the top of the plate. ( take due care that spot must not
touch the solvent)
Remove the plate from the beaker, mark the position of the solvent front (on
edge of the plate with pencil) and allow the solvent to evaporate.
Spray with alcoholic ninhydrin and dry TLC plate in the oven for 2 min.
Spots will develop on the plate. Take measurements of the distance moved by
solvents and each component from the 1 cm mark.
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LMCHE 102: CHEMISTRY LAB
Result:
Rf value of Leucine= …
Plot/Graph: Draw slide with observed lengths of solvent and two components
Error Analysis: To obtain the error bars on the value of the CD
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LMCHE 102: CHEMISTRY LAB
Experiment No. 11
Equipment Required: Conical flasks with corks, beakers, pipette, funnel, filter
paper, glazed paper.
Learning Objectives:
1. Students will learn about the adsorption phenomenon.
2. Students will gain practice of preparing volumetric solutions.
3. Students will learn how to verify Freundlich isotherm.
4. Students will get knowledge about volumetric titrations.
Theory: Adsorption is phenomenon of higher concentration in the surface as
compared to bulk. The substance which adsorbs is called the adsorbent while the
one which gets adsorbed is called adsorbate.
A graph between the amount of substance adsorbed (adsorbate) per gram of
the adsorbent versus equilibrium concentration at the particular temperature is
known as adsorption isotherm. According to Freundlich isotherm:
x = k C1/n where x = weight of the adsorbed substance
m m = weight of the adsorbent
C = equilibrium concentration of the solute
The value of k and n depends upon the nature of solute, solvent and adsorbent.
Taking the log of the above equation:
log x/m = log k+ 1/n log C. It is an equation of the straight line between logx/m
vs. logC with slope 1/n and intercept log k.
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LMCHE 102: CHEMISTRY LAB
Slope = 1/n
Intercept= log k
Procedure:
Take six clean and dry stoppered conical flasks and label them 1 to 6.
(ml)
1 --- 50
2 10 40
3 20 30
4 30 20
Stopper the flaks and shake the solutions thoroughly.
5 40 10
Weigh 2g of activated charcoal each on six different glazed papers. Transfer
6 contents of one paper
the 50 each, to each of the conical ---
flasks without much
loss of time.
Cork the flasks, shake them well and keep them at room temperature for 30-
40 minutes. As far possible, each flask should be shaken for equal time.
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LMCHE 102: CHEMISTRY LAB
Filter the solutions in flasks separately but simultaneously. Reject the first 4-5
ml of the filtrate in each case and receive the rest in six other clean and
numbered flasks (or beakers).
Now titrate 10ml of each filtered solution against 0.1 M NaOH using
phenolphthalein as indicator. Repeat the experiment to get a set of
concordant readings.
Observations:
1 (i) V1
(ii)
2 (i) V2
(ii)
3 (i) V3
(ii)
4 (i) V4
(ii)
5 (i) V5
(ii)
6 (i) V6
(ii)
N1 V1 = N2 V2
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LMCHE 102: CHEMISTRY LAB
N1 X 10 = 0.1 V2
N1 = V2/100
1 0.5 N 0.01V1
2 0.5x40/50 0.02 V2
=0.4N
3 0.5x30/50 0.03 V3
=0.3N
4 0.5x20/50 0.04 V4
=0.2N
5 0.5x10/50 0.05 V5
=0.1N
6 0.5x0/50 0.06 V6
=0
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LMCHE 102: CHEMISTRY LAB
Required Results:
Relationships to be determined:
Graphs/Plots: Applicable
Cautions:
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LMCHE 102: CHEMISTRY LAB
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LMCHE 102: CHEMISTRY LAB
Droppers Beakers
Waterbath
Spatula
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