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1 .

ESTIMATION OF FERROUS ION BY CERIMETRY



Titration I: Standardisation of Cerium (IV) sulphate solution:


S. No.
Volume of Std FeSO4
(ml)
Burette reading (ml) Volume of CAS
(ml) Initial Final










Calculation :
Volume of FeSO4 =
Normality of FeSO4 =
Volume of CAS =
Normality of CAS =--------------------N.

















1. ESTIMATION OF FERROUS ION BY CERIMETRY

Exp. No: Date:

Aim:
To estimate the amount of ferrous ion present in the whole of the given solution.A standard solution of
0.01N ferrous ammonium sulphate and an approximately 0.01N solution of Ceric ammonium sulphate are
supplied.

Principle:
Ceric ions oxidise ferrous ions in acid medium according to the equation,
3 3 2 4
Fe Ce Fe Ce
The ceric ammonium sulphate solution of approximately known strength is standardized against
standard FAS.
For the above titrations, redox indicator ferroin can be used. Ferroin is a complex formed between
Fe(II) ion and 1,10-phenanthroline, [Fe(Phen)3]
+2
. The reduced form of indicator has an intense red colour,
whereas oxidised iron (III) complex has a blue colour. The indicator reaction may be written as,
c Phen Fe
3
3
] ) ( [
2
3
] ) ( [

Phen Fe
Pale blue Red
When iron (II) is titrated with Ce (IV) in sulphuric acid medium, the ferroin indicator is initially red in
colour in its reduced form.At the end point, Ce (IV) oxidises it to Fe (III) complex. The end point, is a sharp
change from red to pale blue colour.

Titration I: Standardisation of Cerium (IV) sulphate solution:
Pipette out 20ml of Ferrous ammonium sulphate solution in to a clean conical flask. Add about 20ml of
2N sulphuric acid followed by 2 drops of ferroin indicator. Titrate it against Cerium (IV) solution taken in the
burette. The end point is colour change from red to pale blue colour. Repeat the titration to get concordant
value. From the titre value, calculate the strength of cerium (IV) solution.

Titration II: Estimation of Ferrous ion
Make up the given ferrous ion solution to 100ml in a standard flask. Pipette out 20ml of this solution in to
a clean conical flask. Add about 20ml of 2N sulphuric acid solution and 2 drops of ferroin indicator. Titrate it
against standardised cerium (IV) solution taken in the burette. End point is colour change from red to pale blue
colour. Repeat the titration to get concordant value. From the titre value, calculate the strength of ferrous ion
and hence calculate the amount of ferrous ion present in the given solution.


Titration II: Estimation of Ferrous ion


S. No.
Volume of FeSO4
(ml)
Burette reading (ml) Volume of
CAS(ml) Initial Final









Calculation

Volume of CAS =
Normality of CAS =
Volume of FeSO4 =
Normality of FeSO4 = --------------------N.




The amount of Ferrous present in the whole of given solution =(Normality x Eq.Wt)/10

=----------------------g.

Result:
The amount of ferrous ion present in the whole of the given solution = ___________g.





Experiment No.: 2 Date:


Objective: Determine the concentration of KMnO
4
solution Spectrophotometrically
Apparatus Required: UV- Visible spectrophotometer, cuvette, test tubes, pipette
Chemical required: KMnO
4

Principle: When an electromagnetic radiation is passed through a sample, certain characteristic wavelengths are
absorbed by the sample as a result the intensity of the transmitted light is decreased. The measurement of the
decrease in intensity of the radiation is the basis of spectrophotometry.
The
max
of

KMnO
4
solution is calculated by plotting the graph in between the absorbance (A) and
wavelength and the concentration of the KMnO
4
solution is calculated by plotting the graph in between the
absorbance (A) and concentration of the solution.
The relationship between absorbance and transmittance is illustrated in the following diagram:

Fig. 1

Significance:
UV / Visible spectrophotometers are used in the modern life science laboratory for the quantification of
nucleic acids, the determination of protein concentrations and the calculation of enzyme activity in kinetics
studies.
The purity of DNA and RNA extractions from cells can be readily measured using spectrophotometry
Procedure:

1. Switch ON the instrument and allow it to self calibrate.
2. Set the instrument as per the direction given by the instructor.
3. Prepare the solution of different concentrations from the given stock solution.
4. Note down the value of absorbance for different concentration of KMnO
4
solution at 440 nm
wavelength (say 0.5%, 1.0%, 1.5%, 2.0% etc.)

5. Plot the observed values of absorbance against concentration.
6. Find the concentration of given unknown KMnO
4
solution from the plotted graph.




Observation:
Determination of concentration of given KMnO
4
solution



Sr. No. Concentration (C) Absorbance (A)
1.
2.
3.
4.
5.
6.
Unknown












Absorbance




Concentration
Graph in between absorbance and Concentration
Result:
Concentration of given KMnO
4
= mg/l
Precautions:
1.Always use the dilute solution.
2. Cuvette should be cleaned properly and must be wiped with tissue paper.
3.Do not leave any finger marks on the cuvette.

Questions:
1. What is the purpose of this experiment? What is the relation between concentration and absorbance?
2. Mention the role of potassium permanganate in the water treatment.
3. What is the light source for visible region and UV region of the spectrum?
4. What are the advantages of using Quartz or silica cells over Glass and plastic when
measuring absorption of ultraviolet wavelengths by a solution?
5. Why is it important to determine max before determine the concentration of the
unknown?
3. ESTIMATION OF NICKEL IN AN ALLOY BY COMPLEXOMETRY

Exp. No: Date:

Aim:
To estimate the amount of Nickel present in the whole of the given nickel alloy solution. A standard
solution of 0.01N Nickel sulphate and an approximately 0.01N EDTA solution are supplied.

Principle:
Nickel can be estimated by using EDTA as titrant and murexide as indicator. Murexide form complexes
with nickel at pH 11. Murexide is the ammonium salt of Purpuric acid. The colour change in the direct titration of
nickel at pH 10 11 is from yellow to bluish violet.

Procedure:
Titration I: Standardisation of EDTA
Pipette out 20ml of standard nickel sulphate solution into a clean conical flask. Add a pinch of Murexide
indicator , and 10ml of 1M ammonium chloride solution and then add concentrated ammonia solution drop wise
till the pH is about 7 as shown by yellow colour of the solution. Titrate the mixture in conical flask against EDTA
taken in burette until colour changes from yellow to violet. (Nickel complexes rather slowly with EDTA and
consequently the EDTA solution must be added drop wise near the end point). Repeat the titration to get
concordant value. From the strength of Nickel sulphate solution calculate the strength of EDTA.

Titration II: Estimation of Nickel
Transfer the given nickel alloy solution into a clean 100ml standard flask quantitaively and make upto
the mark using distilled water. Pipette out 20ml of made up nickel alloy solution into a clean conical flask. Add a
pinch of Murexide indicator and 10ml of 1M ammonium chloride solution and then add concentrated ammonia
solution drop wise till the pH is about 7 as shown by yellow colour of the solution. Titrate the mixture against
standardised EDTA taken in burette until colour changes from yellow to violet. Repeat the titration to get
concordant value. Calculate the strength of nickel solution by using strength of EDTA and hence the amount of
nickel present in the given solution.











Titration II: Estimation of Nickel

S. No. Volume of Nickel Sulphate
(ml)
Burette reading (ml) Volume of
EDTA(ml) Initial Final









Calculation


Volume of EDTA =
Normality of EDTA =
Volume of NiSO4 =
Normality of NiSO4 =--------------------N



The amount of Nickel present in the whole of given solution =(Normality x Eq.Wt)/10

=----------------------g.






Result:
The amount of nickel present in the whole of the given solution = g.



Experiment No4.. Date:.
Objective: To determine the concentration of iron in water sample by spectrophotometric method.
Requirements: Spectrophotometer. Stock solution of Fe
3+
ions, conc. HCl, Potassium thiocyanate.
Principle: The colorimetric determination of iron using KCNS as colour developing agent is based on the
formation of a red coloured complex between Fe3+ and CNS
-
ions
Fe
3+
+ 3CNS [Fe (CNS)]
2+

Red
In the determination of iron in the water sample, a series of standard solutions having iron is treated with KCNS
to get iron-thiocyanate complex. The absorbance of all the standard solution prepared is noted at max 480 nm
because iron-thiocyanate complex shows maximum absorbance at this wavelength. Now the absorbance for the
unknown solution is also determined. A graph is plotted against the absorbance (OD) against the concentrations
of the known solutions. From the graph the concentration of the unknown solution can be found out.
Procedure:
1. Set the Spectrophotometer and adjust the wavelength to 480 nm.
2. Prepare the stock solution of Fe
3+
ions by dissolving 2.0g of ferric ammonium sulphate in 50 ml of
distilled water and 10 ml. of conc. HC1. HCl is added to suppress the hydrolysis of ferric ammonium
sulphate.
3. Take the stock solution in the burette and prepare 5 solutions of different known concentrations by
diluting the above stock solution in five different flasks.
4. Transfer 1 ml solution of standard stock solution to 50 ml measuring flask and add 10 ml of
thiocyanate solution. Dilute the solution to 50 ml.
5. Repeat the process (step 4) with the solutions of other concentrations prepared above and also with the
unknown sample.
6. Prepare the blank solution by dissolving 10 ml of thiocyanate solution in distilled water and making the
volume to 50 ml.
7. Keep the solution at rest for 5 minutes.

8. Note down the absorbance of all the solution against blank solution, spectrophotometrically at 480 nm.
9. Prepare a calibration curve by plotting absorbance against concentration.
10. From the calibration curve, the concentration of the unknown solution corresponding to its absorbance
can be found.
Observation:
Observation:
S.No. Concentration Absorbance



Calibration Curve:













Result:
The amount of Fe(III) in water was found to be =g/L.
Questions:
1. What is spectrophotometry?
2. Discuss Lambert's and Beer's law of absorbance.
3. What is colorimetry?
4. What is absorbance, transmittanc/?, extinction coefficient.
5. How you can verify Beer's law?
6. How you can find out the conc. of the given unknown solution spectro. photometrically?
7. What is the significance of spectrophotometry.
8. What is the structure of orthophenanthroline complex with iron (II).
















Abs
Conc.
Absorbance of unknown
solution
Concentration of unknown solution

Experiment No. 5.. Date:


Objective: To prepare Urea Formaldehyde resins.
Apparatus Required: Beaker, Measuring cylinder, Pipette, Glass rod, and Dropper
Chemicals required: (a) Urea Formaldehyde: Urea, Formaldehyde solution (40%), and Sulfuric acid (H
2
SO
4
)
Principle:
Polymers: The term polymer is derived from the Greek words poly meaning many and mer meaning part.
Thus, a polymer means a substance with many parts. Every polymeric substance has a definite identifying unit
of molecular structure, which is called a part or mer (monomer). A polymer is a large molecule made up of
small, simple chemical units held together by covalent bonds. Some polymers are linear in the form of chains
while others are branched or interlinked chains to form three-dimensional networks.
On the basis of reaction to stress and temperature polymers may be:
(i) Thermoplastics (Thermoplasts) which can be repeatedly given shapes by heat and pressure. Hence, once used
for a particular form, they can again be formed into a different shape or form, e.g. polyethylene (PE),
polystyrene (PS).
(ii) Thermosets are the polymers which once subjected to heat and pressure to give a particular form, cannot be
formed again like the thermoplastics, e.g. urea formaldehyde, phenol formaldehyde, nylon-6,6, etc.
(iii) Rubbers, when subjected to heat and pressure, behave at first like the thermoplastics and subsequently
become highly elastic. Their elasticity may be arrested at an intermediate stage and this process is called curing
(vulcanization)
On the basis of method of production, polymers are classified as:
(i) Addition (chain reaction) polymers are produced by addition or chain reaction polymerization in which a
simple, low molecular weight molecule (monomer), which possesses at least one double bond, is induced to
break its double bond resulting in the free valences, which then link up with other similar molecules to give the
polymer. In this polymerization, the monomer retains its identity in the polymer and also, no byproduct is
formed, e.g. polyethylene:

nCH
2
=CH
2
CH
2
CH
2

n

(ii) Condensation polymers are produced by the method of condensation polymerization in which the monomer
need not contain a double bond and the monomer does not retain its characteristic molecular formula in the
polymer. Moreover a small molecule is essentially given out and hence the resulting molecule is condensed in
the process, e.g.








Urea formaldehyde :

O H
+
O

H
2
N- C- NH
2
+ HCHO H
2
N- C-NH- CH
2
OH
Mono methylol urea

HCHO

O

HOH
2
C-HN- C-NH- CH
2
OH
Dimethylol urea



N-CH
2
-N-CH
2
-N-CH
2

O=C

O = C O = C
N-CH
2
-N-CH
2
-N-CH
2

Cross Linked polymer
(Urea- Formaldehyde)
Procedure:
Take 1.5 gm of urea in a 100 ml beaker.
1. Add 3 ml of formaldehyde solution.
2. Stir the mixture till all the crystals of urea dissolve.
3. Now add 2 drops of Conc. H
2
SO
4
when all of a sudden a white mass of urea formaldehyde resin
appears.
4. Wash the resin several times with tap water to remove any trace of acid.
5. Collect the white resin and take the weight.
Result:
The measured weight of the resin formed is ------------gm.
Precautions:
1. Be very careful while adding Sulphuric acid in the mixture.
2. Keep the beaker away from the body during the reaction.
3. Avoid inhaling the fumes coming out from the reaction mixture
Questions:
1. What is polymer?
2. What arte natural polymer?
3. What are thermoplastic and thermoses polymers?
4. What is importance of Urea formaldehyde resin?

4. ESTIMATION OF ZINC USING POTASSIUM FERROCYANIDE BY PRECIPITATION

Titration I: Standardisation of Potassium ferrocyanide

S. No. Volume of Zinc Sulphate
(ml)
Burette reading (ml) Volume of Potassium
ferrocyanide
(ml)
Initial Final









Calculation:
Volume of ZnSO4 =
Normality of ZnSO4 =
Volume of Potassium ferrocyanide =
Normality of Potassium ferrocyanide =--------------------N.





















4. ESTIMATION OF ZINC USING POTASSIUM FERROCYANIDE BY PRECIPITATION METHOD

Exp. No: 6 Date:

Aim:
To estimate the amount of zinc present in the whole of the given solution using potassium ferrocyanide
by precipitation titration method. You are provided with a standard solution of 0.05 N zinc sulphate and an
approximately 0.05 N potassium ferrocyanide solution.

Principle:
Zinc ions and ferrocyanide ions react in neutral or acid medium as follows
3ZnSO
4
+ 2K
4
[Fe(CN)
6
] K
2
Zn
3
[Fe(CN)
6
]
2
+ 3K
2
SO
4

The zinc ions get precipitated as potassium zinc ferrocyanide.

The end point of the reaction can be detected using internal indicators such as diphenylamine, sodium
diphenylamine sulphonate etc. These substances are oxidation reduction indicators (redox indicators) whose
action depends on the ratio of the concentration of ferricyanide in the solution. Thus in order to make the reaction
an redox reaction, a small quantity of potassium ferricyanide is added to the ferrocyanide solution. When an
excess of zinc ions are present in solution, the concentration of the ferrocyanide is very small and the reduction
potential is large. When all the zinc ions are quantitatively precipitated, the next drop of ferrocyanide that is
added in excess, will cause a sudden increase in [Fe(CN)6]
2-
and hence a sudden decrease in the potential. This
results in the colour change of the redox indicator. The end point is colour change from blue to yellowish green.

During titration, the solution should be thoroughly shaken, also the titration should be carried out very
slowly especially near the end point.

Procedure:
Titration I:
Standardisation of Potassium ferrocyanide
Exactly 20 ml of standard zinc sulphate solution is pipette out in to a clean conical flask. Add 20 ml of 4
N sulphuric acid, and 2 to 4 drops of diphenylamine indicator. Titrate this mixture against potassium ferrocyanide
taken in the burette. The end point is the colour change from blue to yellowish green. Repeat the titration for
concordant titre value. From the titre value calculate the strength of potassium ferrocyanide








Titration II: Estimation of Zinc



S. No.
Volume of Zinc Sulphate
(ml)
Burette reading (ml) Volume of Potassium
ferrocyanide
(ml)
Initial Final










Calculation
Volume of Potassium ferrocyanide =
Normality of Potassium ferrocyanide =
Volume of ZnSO4 =
Normality of ZnSO4 =--------------------N.



The amount of Zinc present in the whole of given solution = (Normality x Eq.Wt)/10



=----------------------g.
Titration II: Estimation of Zinc
Transfer the given Zinc alloy solution into a clean 100ml standard flask quantitatively and make upto
the mark using distilled water. Pipette out 20ml of made up solution in to a clean conical flask. Add 20ml of 4 N
sulphuric acid,and 2 to 4 drops of diphenylamine indicator. Titrate this mixture against potassium ferrocyanide
taken in the burette. The end point is the colour change from blue to yellowish green. Repeat the titration for
concordant titre value. From the titre value calculate the strength of zinc solution and from the strength estimate
the amount of zinc present in the whole of the given solution.


Result:
The amount of Zinc present in the whole of the given solution = g.
























Experiment No.: 7 Date:


Objective: Synthesis & Characterization of Silver Nanoparticles


Apparatus Required: UV- Visible spectrophotometer, cuvette, Beakers,Magnetic stirrer

Chemical required: AgNO
3,
NaBH
4
, PVA

Theory: The formation of silver nanoparticles can be observed by a change in color
since small nanoparticles of silver are yellow. Sodium borohydride is used as a reducing
agent and a layer of absorbed borohydride anions on the surface of the nanoparticles
keep the nanoparticles separated. PVA acts as stabilizing agent. The scattering of light
caused by spherically shaped colloidal silver nanoparticals shows golden yellow colour.
When sodium cholride (NaCl) is added the nanoparticles aggregate and the suspension turns
cloudy gray. The addition of a small amount of polyvinyl pyrrolidone will prevent
aggregation.

Nanotechnology deals with processes that take place on the nanometer scale, that is, from
approximately 1 to 100 nm. Properties of metal nanoparticles are different from those of bulk
materials made from the same atoms. For example, silver metal is grayish,but colloidal silver
from this synthesis is a clear yellow. The striking effect of nanoparticles on color has been
known since antiquity when tiny metal particles were used to color glass in church windows.
Silver particles stained the glass yellow, while gold particles were used to produce ruby glass.

Synthesis of Colloidal Ag

Colloidal silver is made by adding an excess of the reducing agent sodium borohydride,
NaBH
4
to silver nitrate, AgNO
3
. Particle size can also be determined using visible
spectroscopy.

AgNO
3
+ NaBH
4
Ag + 1/2H
2
+ 1/2B
2
H
6
+ NaNO
3

Characterization of Colloidal Ag

Sample has to be characterized by UV spectroscopy. The presence of metal in the solution is
related to a broad absorbance peak at 410 nm.The height of peak gives information about
the metallic compound concentration in the medium. For the 12 nm Ag nanoparticles, the
maximum wavelength is near 400 nm. In general, as the particles become larger the
absorption maximum shifts to longer wavelengths.

When an electromagnetic radiation is passed through a sample, certain characteristic
wavelengths are absorbed by the sample as a result the intensity of the transmitted light is
decreased. The measurement of the decrease in intensity of the radiation is the basis of
spectrophotometry.

The
max
of

solution is calculated by plotting the graph in between the absorbance (A) and
wavelength and the concentration of the solution is calculated by plotting the graph in
between the absorbance (A) and concentration of the solution.

Size and shape dependent colors of Au & Ag nanoparticles are shown in the table.
5
Size
increase
Size
increase
Red
Green
Orange
Yellow
Blue
Brown
Fig 1. Size and
shape
dependent
colors of Au &
Ag nanoparticles


Procedure:
1.Take 1mL of 0.001M silver nitrate (AgNO
3
) and make it up to 10 mL.

2.Add 1mL of polyvinyl alcohol (PVA) 1% solution to the beaker slowly with constant
stirring.
3.Add a magnetic stir bar and place the flask on a stir plate and further add 40 mL of
0.0001M sodium borohydride (NaBH
4
) to above solution slowly with constant stirring.and
and cool the liquid for about 20 minutes.
4.Switch on the spectrophotometer and allow it to self calibrate.
5.Take spectra to find a broad absorbance peak at 410 nm.


Result:
Colour of silver nanoparticals:
Shape of silver nanoparticals:
Size of silver nanoparticals:


Precautions:
1. Costant stirring should be done.
2. Cuvette should be cleaned properly and must be wiped with tissue paper.
3.Do not leave any finger marks on the cuvette.
Safety and Waste Disposal: Safety glasses are always required in the laboratory.
Gloves must be worn throughout this experiment. Silver nitrate is caustic and stains the
skin. A container will be made available for any waste solutions.


CAUTION: Stop the stirring as soon as the silver nitrate solution is added and remove
the stir bar. If the stirring is continued once all the silver nitrate has been added,aggregation
is likely to occur; the yellow darkens, turns violet, then grayish as the particles settle out.

The product should be clear yellow once the reaction is completed and should remain
yellow, although it may darken somewhat. Record the appearance of your product as
soon as the stirring is stopped and after waiting for about 5 minutes. If your product has
aggregated and turned gray---repeat the synthesis if possible.

Questions:
1. What is the purpose of this experiment? What is the relation between concentration and
absorbance?
2. Mention the colour, size and shape of nanoparticals of silver and gold.
3. What are the main applications of silver and gold nanoparticals.
3. What is the light source for visible region and UV region of the spectrum?
4. What are the advantages of using Quartz or silica cells over Glass and plastic when
measuring absorption of ultraviolet wavelengths by a solution?
5. Why is it important to determine max before determine the concentration of the
unknown?