NATIONAL INSTITUTE OF TECHNOLOGY

राष्ट्रीय प्रौद्योगिकी संस्थान

TIRUCHIRAPPALLI-620 015

NAME

ROLL NO.

BRANCH

SECTION

B. TECH. I YEAR
CHEMISTRY LABORATORY MANUAL
DEPARTMENT OF CHEMISTRY, NITT
Department of Chemistry

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LIST OF EXPERIMENTS

1. Estimation of carbonate, non-carbonate and total hardness in the given water

sample.

2. Estimation of dissolved oxygen in the given water sample.

3. Determination of the percentage of Fe in the given steel sample.

4. Estimation of Fe3+ by spectrophotometer.

5. Corrosion rate by polarization technique

6. Conductometric titration

7. Potentiometric titration

8. pH-metric titration

9. Percentage purity of bleaching powder

10.Determination of molecular weight of the polymer by Viscometry

11.Study of three component system.

12.Demonstration of experiments using Advanced Spectroscopic Techniques

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Titration-1 : Standardization of EDTA

Titrand : Standard 0.1 M ZnSO4 solution

Titrant : EDTA
Indicator : EBT
End Point : Wine red to Blue

Standard EDTA solution vs Water sample

S.No. Volume of ZnSO4 Burette Reading Volume of EDTA

solution (mL) Initial Final Solution (mL)
1
2
3

Calculations

VZnSO4 x M ZnSO4
Molarity of EDTA =
VEDTA

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1. ESTIMATION OF CARBONATE, NON-CARBONATE AND TOTAL HARDNESS

IN THE GIVEN WATER SAMPLE

AIM
To estimate the total hardness, carbonate hardness and non-carbonate hardness of the given
sample of water using standardized EDTA.

PRINCIPLE

EDTA reacts with Ca2+ and Mg2+ forming highly stable metal ion complexes in the pH
range 9‐10.
M2+ + H2Y2‐ MY2‐ + 2H+

where H2Y2‐ is the anion of the disodium salt of EDTA and M2+ = Ca2+ & Mg2+ .

Being a reversible reaction, its extent and hence the titration value will vary slightly with the
concentration of H+. Hence a buffer is used to keep this factor constant. In order to detect the end
point, a metal‐ion indicator, Eriochrome Black‐T (EBT), is used. EBT forms wine‐red coloured
complexes with metal ions like Ca2+, Mg2+, Zn2+ etc. These are, however, less stable than EDTA
complexes. When EDTA solution is added, initially the free M2+ ions react to form M‐EDTA
complex and finally the metal ion from M‐EBT complex reacts to form M‐EDTA releasing free
indicator, which is blue in the pH range 9‐10. The end point is the change of colour from wine‐red
to blue.
-
O O
N+ O

O OH

N OH O
HO N
N S O-

HO O N O Na+
HO
OH
O
EDTA EBT

Direct titration of water using standardized EDTA and EBT indicator gives the total hardness.
Non‐Carbonate hardness can be determined by precipitating the carbonate hardness by boiling,
followed by titration with EDTA solution. The difference between the total hardness and non‐
carbonate hardness corresponds to the carbonate hardness.

Ca(HCO3)2 → CaCO3↓ + H2O + CO2↑

Mg(HCO3)2 → Mg(OH)2↓ + 2CO2↑
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Titration – 2: Estimation of total hardness

Titrand : Water sample

Titrant : EDTA
Indicator : EBT
End Point : Wine red to Blue

Standard EDTA solution vs Water sample

S.No. Volume of Water Burette Reading Volume of EDTA

sample (mL) Initial Final Solution (mL)
1 60
2 60
3 60

Calculations

VEDTA X MEDTA
Molarity of water sample =
Vwater sample

Total Hardness of water sample = Mwater sample X MCaCO3 X 1000 ppm as CaCO3 eq

Total Hardness of water sample = M water sample X 100 X 1000

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PROCEDURE

Standardization of EDTA

The given standard ZnSO4 solution is quantitatively made up to 100 mL by following all
the usual precautions. 20 mL of ZnSO4 solution is pipetted out into a clean conical flask, 1 mL of
buffer (pH = 10; NH4Cl/NH4OH) is added followed by 1‐2 drops of EBT indicator. The contents of

the conical flask are titrated against EDTA taken in the burette, with constant shaking. The end
point is the colour change from wine red to blue. The titration is repeated to get concordant
value.

Estimation of total hardness

60 mL of the given sample of water is pipetted into a clean conical flask. 1 mL of buffer
(pH = 10, NH4Cl/NH4OH) and 1‐2 drops of EBT are added. The solution in the conical flask is

titrated against EDTA until the wine red colour just changes to blue. The titration is repeated
for concordance.

Estimation of carbonate and non‐carbonate Hardness

60 mL of the given sample of water is taken in a clean beaker. The beaker is covered
with a watch glass and its contents gently boiled for 5 min.
Now, the watch glass is removed, after washing its bottom into the beaker with freshly
boiled and cooled distilled water. The solution is filtered into a clean conical flask. The beaker
and the precipitate are washed twice with freshly boiled and cooled water. The washings are also
collected in the same flask. 1.5 mL of the buffer and 2 drops of EBT are added to the filtrate.
The solution is titrated against standard EDTA until the wine red colour changes to blue.
The titration is repeated, adding the buffer towards the end point.
The total hardness, carbonate hardness and non‐carbonate hardness are

calculated.

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Titration – 3: Estimation of carbonate hardness and non‐carbonate hardness

Titrand : Filtrate of boiled Water sample

Titrant : EDTA
Indicator : EBT
End Point : Wine red to Blue

Standard EDTA solution vs Boiled Water sample

S.No. Volume of Water Burette Reading Volume of EDTA

sample (mL) Initial Final Solution (mL)
1 60

Calculations

VEDTA X MEDTA
Molarity of water sample =
V water sample

VEDTA X MEDTA
Non -Carbonate Hardness of water sample =
V water sample X MCaCO3X 1000

Carbonate Hardness of water sample = Total Hardness - Non Carbonate Hardness

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RESULT

Total hardness = ppm as CaCO3 eq.

Carbonate hardness = ppm as CaCO3 eq.

Non – carbonate hardness = ppm as CaCO3 eq.

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Titration – 1: Standardization of thiosulfate solution

Titrand : Standard K2Cr2O7 solution
Titrant : Thiosulfate
Indicator : Starch
End Point : Blue to green
Weight of K2Cr2O7 = 0.25 g

Weight of K2Cr2O7 x 10
Normality of K2Cr2O7 =
Equivalent Weight of K2Cr2O7

Standard K2Cr2O7 solution vs Thiosulfate solution

Sl.No. Volume of K2Cr2O7 Burette reading Volume of thiosulfate

solution (mL) solution (mL)
Initial Final
1. 20

2. 20

3. 20

Calculations

V K2Cr2O 7 x N K2Cr2O 7
Normality of Thio =
VThio

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2. ESTIMATION OF DISSOLVED OXYGEN IN THE GIVEN WATER SAMPLE

AIM
To determine dissolved oxygen in a sample of water.

PRINCIPLE
It is based on oxidation of potassium iodide. The liberated iodine is titrated against standard
hypo solution using starch as a final indicator. Since oxygen in water is in molecular state and not
capable to react with KI, an oxygen carrier manganese hydroxide is used to bring about the reaction
between KI and O2. Manganous hydroxide is produced by the action of potassium hydroxide and
manganous sulphate.
2KOH + MnSO4 → Mn(OH)2 + K2SO4
2Mn (OH) 2 + O2 → 2MnO(OH)2
MnO(OH)2 + H2SO4 → MnSO4+ 2H2O+ [O]
2KI + H2SO4 + [O] → K2SO4 + H2O + I2
I2 + 2Na2S2O3 → 2NaI + Na2S4O6
(Sodium tetrathionate)
Starch + I2 → Starch iodide complex
(Blue in colour)

PROCEDURE
Standardization of sodium thiosulfate solution
The given K2Cr2O7 solution is quantitatively made up to 100 mL by following all the usual
precautions. 20 mL of this solution is pipetted out into a clean conical flask. 5 mL of 10% KI
solution and then 5 mL of dilute HCl are added to the flask. The mouth of the flask is covered and
shakes well for few minutes. The mixture becomes brown due to liberation of iodine. The contents of
the flask are titrated against the given thio solution taken in the burette. The brown colour is started
to fade. The addition of thio is continued until a pale yellow colour is formed. At this point, 1 mL of
freshly prepared starch solution is added and the titration is continued.

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Titration – 2: Estimation of Dissolved Oxygen
Titrand : Water
Titrant : Thiosulfate
Indicator : Starch
End Point : Blue colour disappears

Sl.No. Volume of water (mL) Burette reading Volume of thiosulfate

solution (mL)
Initial Final
1.

2.

3.

Calculation:

1 L of water sample contains = 2V mg of O2 = ppm

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The end point is the change of colour from blue to green. The titration is repeated to get concordant
values.
Estimation of dissolved oxygen
Take 500 mL of water in a D.O bottle. Add 10 mL of alkaline KI and 10 ml of MnSO4 into it.
Close the bottle and shake it well. Keep the bottle in dark and con. H2SO4 till the brown precipitates
are dissolved. Take the 100 mL of this solution in a conical flask and titrate it against standardized
sodium thiosulfate till the colour changes to light yellow. Add 3-4 drops of starch into it and the
colour changes to blue. The blue colour solution is then titrated against sodium thiosulphate solution
till blue colour disappears. The end point is noted and the titration is repeated to get concordant
readings.

RESULT
The amount of oxygen dissolved in water = ppm

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Titration – 1: Standardization of KMnO4

Titrand : Standard Oxalic acid

Titrant : KMnO4
Indicator : Self indicator
End Point : Appearance of permanent pale pink colour

Weight of oxalic acid taken = 6.3 g/L

Weight of oxalic acid

Normality of std. oxalic acid =
Equivalent weight of standard oxalic acid

Standard oxalic acid solution Vs KMnO4

S.No. Volume of std oxalic acid Burette reading Volume of KMnO4
solution (mL) Initial Final solution (mL)

Calculations
Vox. acid X Nox. acid
Normality of KMnO4 =
VKMnO4

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3. DETERMINATION OF THE PERCENTAGE OF IRON IN THE GIVEN

STEEL SAMPLE

AIM
To determine the amount and percentage of iron in the whole of the given steel sample
solution.
PRINCIPLE
Steel is an alloy of iron, which contains certain amount of C, Si, P, S and Mn. For special
purposes other metals such as Cr, V, Mo, W, Ti and Cu are added.
In order to determine the amount of iron in steel when the sample is dissolved in dil. H 2SO4,
Fe dissolved as FeSO4 and H2 gas evolved.
Fe + H2SO4 = FeSO4 + H2

The amount of Fe3+ ion can be determined titration using standard KMnO4 solution. The overall
reaction is a redox process in which oxidizing agent is reduced and reducing agent is oxidized.

MnO4- + 8H+ + 5e- Mn2+ + 4H2O

5Fe2+ 5Fe3+ + 5e-
MnO4- +5Fe2+ + 8H+ Mn2+ + 5Fe3+ + 4H2O

PROCEDURE
1. Standardization of KMnO4 solution
Pipette out 20 mL of standard (N/10) oxalic acid solution into a 100 mL conical flask. Add 10
mL of dilute H2SO4 and heat the solution to about 70 oC using hot plate. Then, titrate this solution
slowly against the KMnO4 solution from the burette until a faint but permanent pink colour persists
in the solution. Repeat the titration until concordant results of titre value are obtained and calculate
the normality of KMnO4 solution.
2. Determination of iron in the steel sample
The given steel sample is quantitatively made up to 100 mL with distilled water. Pipette out
20 mL of solution into a conical flask, add 10 mL of dilute H2SO4 and titrate against KMnO4 solution
taken in the burette. The appearance of a faint but permanent pink colour marks the end point. Repeat
the titration until concordant reading is obtained.
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Titration – 2: Estimation of Fe(II) in the given solution

Titrand : Steel solution

Titrant : KMnO4
Indicator : Self indicator
End Point : Appearance of permanent pale pink colour

Standard KMnO4 vs Steel solution

S.No. Volume of steel solution (mL) Burette reading Volume of KMnO4
Initial Final solution (mL)

Calculations

Weight of the steel sample = 2.7 g

VKMnO4 X NKMnO4
Normality of Fe(II) solution =
VFe(II) solution

Amount of Fe(II) ions present in NFe(II) solution x Equivalent weight of Fe(II)

the whole of the given solution =
10

Amount of Fe(II) ions X 100

Percentage of Fe(II) ions in the steel sample =
Weight of steel sample

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RESULT

The percentage of Fe(II) in the whole of the given steel sample solution = ________

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Volume of FAS Solution Absorbance Conc. of Fe(II) solution

Calculations

The concentration of stock FAS (Ferric ammonium sulphate) solution = 2.387 x 10-3 M

25 x 2.387 x 10-3
Concentration of made up FAS (250 mL) solution = ------------------------ = 2.387 x 10-4 M
250

Equivalent weight of Iron = 55.85

Conc. of unknown soln x equivalent weight of

iron
The amount of iron present in given sample = -------------------------------------------------------------
10

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4. ESTIMATION OF Fe3+ BY SPECTROPHOTOMETER

AIM
Estimate the amount of iron present in the given solution using spectro-colorimeter
I
PRINCIPLE
According to Beer Lambert’s law the optical density of absorbance ‘A’ of a solution of
concentration ‘c’ moles/litre, placed in a cell of ‘l’ cm width is given by

A = log Io = cl
I

Where Io and I represent the intensities of incident and transmitted radiations and  is molar
extinction coefficient. Since optical density (OD) is proportional to the concentration of the
solution, a linear plot is expected for absorbance vs concentration of the solution.
Iron forms a red coloured complex with potassium thiocyanate and therefore absorbs the
complementary colour bluish green of wavelength maxima (λmax) 480nm.

Fe3+ + 4KSCN ↔ [Fe(SCN)4] ‐ + 4K+

The absorbance of the complex can be measured in a spectro colorimeter, fixing λmax at 480
nm. A calibration line is plotted by measuring the OD of standard solutions of different concentrations.
The concentration of the unknown is determined by matching its OD in the calibration line.

PROCEDURE
0.08 g of Ferric ammonium sulphate is weighed in a chemical balance and transferred into a
100 mL standard flask acidified with 2 mL conc. HNO3 to prevent precipitation of Fe(III) as Fe(OH)3
and made upto 100 mL with distilled water. 20 mL of this made up solution is withdrawn and
transferred to another 100 mL standard flask and made up to mark with distilled water. 1 mL of
this solution is taken in a 25 mL standard flask. 1 mL of concentrated HNO3 and 5mL of KSCN are
added and made up to 25 mL and shaken well for homogeneity.
OD of this solution is measured using a spectrocolorimeter, fixing λmax at 480 nm. Similar

measurements are made with 2,3,4,5 and 6 mL of standard solution and the calibration line is
obtained.

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The given unknown is transferred into a 25 mL standard flask. 1 mL of concentrated HNO3

and 5 mL of KSCN are added and made upto 5 mL and OD is measured as before. From the
calibration line, the amount of Fe in the given solution is determined.

RESULT:

The amount of iron present in the whole of the given solution is given to be _____________

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Tabulation

Cathodic polarization of the steel plate

Active area of the specimen =______ cm2

S.No. Current (mA) Current density (mA/cm2) Log(current density) Voltage (V)

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5. DETERMINATION OF CORROSION RATE BY POLARIZATION TECHNIQUE

AIM
To determine the corrosion rate of mild steel specimen in 3.5% NaCl solution.

PRINCIPLE

Metal under wet conditions experiences electrochemical corrosion. Tafel polarization method is an
accelerated electrochemical corrosion technique which can be used to determine the corrosion rate of the
metal under service conditions. The instantaneous corrosion rate of metal dissolution (anodic) process can
be assessed from the slopes of the Tafel plot.
a  c
B=
2.303(  a +  c )

Where,
βa = slope of the anodic Tafel equation, when plotted on base 10 logarithmic paper in V/decade.
βc = slope of the cathodic Tafel equation, when plotted on base 10 logarithmic paper in
V/decade.
B = Stern-Geary constant, V.

Corrosion current (icorr) is deduced from the Tafel plot.

The corrosion rate (CR) in mm/yr is determined from,
icorr
CR = K  EW

Where,
icorr is in μA/cm2, ρ is density the steel 304 (8.03 g/cm3), K= 3.27 x 10-3 mm g/μA cm yr, EW is
the equivalent weight of steel (304) = 25.12.
The steel specimen of known area is galvanostatically polarized and the potential is measured. A
plot is made between E Vs i. The corrosion current and corrosion voltage are determined from the Tafel
plot.

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Anodic polarization of the steel plate

Active area of the specimen =______ cm2

S.No. Current (mA) Current density (mA/cm2) Log(current density) Voltage (V)

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PROCEDURE

Steel specimen of 10 x 1 cm is polished using emery paper and washed well with distilled water. 1
cm2 area of the specimen is immersed in 100 ml of 3.5% NaCl solution taken in a beaker after masking rest
of the area. Electrochemical connections are made with a galvanostat using calomel reference electrode,
platinum counter electrode and the steel as the cathode. For various values of the imposed current, the
potential is measured. Likewise, the steel specimen is anodically polarized and the current and voltage
values are measured and tabulated. A plot is made between voltage and log current density. From the
intersection of the tangents to the anodic and cathodic polarization curves at linear regions, i corr and Ecorr
values are obtained and the corrosion rate is calculated.

RESULT

(i) Corrosion rate of the given steel specimen in 3.5% NaCl solution is =.............mm/year
(ii) Stern-Geary constant for the steel specimen in 3.5% NaCl solution is =.........V
(iii) Corrosion voltage (Ecorr) =.........V

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S. No. Volume of HCl added Conductance Corrected

(mL) conductance

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6. CONDUCTOMETRIC TITRATION

AIM
To estimate the amount of HCl present in the given whole solution by conductometric titration
using NaOH.

PRINCIPLE
An immersion type of conductivity cell and a Kohlrausch’s bridge enable the measurement of the
conductance of an electrolyte. The conductivity of a solution depends on the number, mobility and charge
of the ions present in the solution. When a fast moving ion is replaced by a slow moving ion of the same
charge leads to decreases the conductance of the solution. This happens when a solution of HCl is added to
a solution of NaOH, the hydroxyl ions being replaced by chloride ions.

Na+ + OH- + Cl- + H+ H2O + Na+ + Cl-

At the neutralization point all the hydroxyl ions have been removed, further addition of HCl leads to
increases the conductance of the solution due to the high mobility hydrogen ions. Thus, a plot of
conductance against volume of HCl added would give two linear regions. Their intersection would
correspond to the end point.

PROCEDURE
Standardization of NaOH and estimation of the given HCl
20 mL of the standard 0.1 N NaOH solution is pipetted into a clean 250 mL beaker and diluted to
100 mL with conductivity water. The conductivity cell is dipped into the solution and connections are
made to the salt-bridge measuring the conductance (or resistance) of the solution. Then, 2 mL portions of
the given standard 1N HCl is added from the burette to the beaker and stirred well. The conductance of the
solution is measured for each and every addition of HCl. When the rate of decrease of conductance is
small, the volume of HCl added is reduced to 0.5 mL per step until the rate of increase of the conductance
is large. The volume of HCl added is now increased to 2 mL per step and measurement is made to about
double the volume of HCl needed for neutralization.

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From Graph,

VNaOH x NNaOH
Normality of given HCl solution =
VHCl

NHCl x Equivalent weight (HCl)

Amount of HCl present in whole of the given solution =
10

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A plot of corrected conductance against volume of HCl is drawn and the end point is determined by
the intersection of the two straight lines passing through these points and the amount of HCl in one litre of
the given solution is calculated. From this volume, strength of NaOH is calculated. The above procedure is
repeated using the standardized NaOH solution and unknown HCl to find out its strength.

Equivalent weight of HCl = 36.45

Graph

RESULT
The amount of HCl in whole of the given solution is g/L

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Volume of ΔE/ ΔV
K2Cr2O7 EMF (mV) ΔE (mV) ΔV (mL) (mL/mV) Vmean
(mL)

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7. ESTIMATION OF Fe(II) USING POTENTIOMETER

AIM
To estimate the amount of Fe(II) present in the whole of the given solution potentiometrically.

PRINCIPLE
Potentiometric titration is the titration in which potentiometric measurements are carried out in
order to fix the end point. In this method, the interest is with the change in electrode potential, rather than
with an accurate value for the electrode potential in a given solution. In a potentiometric titration, the
change in cell e.m.f. occurs most rapidly in the neighbourhood of the end point. The Fe(II) –K2Cr2O7
redox system is represented as
Fe2+ + 4H2SO4 + K2Cr2O7 → Fe3+ + K2SO4 + Cr2(SO4)3 + 4H2O + 3 (O)
The determining factor is the ratio of the concentrations of the oxidised and the reduced forms of
the iron species. For the reaction,
Oxidised form + ne- → Reduced form

The potential E acquired by the indicator electrode at 25°C is given by,

where E° is the standard Reduction Potential of the system. Thus the potential of the immersed
electrode is controlled by the ration of these concentrations. During redox reactions, the potential changes
more rapidly at the vicinity of the end point. The indicator electrode is usually a bright platinum wire or
foil, the oxidising agent is taken in the burette. The cell can be represented as,

Here Pt is the indicator electrode and calomel is the reference electrode.

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PROCEDURE
PREPARATION OF 0.1 N K2Cr2O7:
0.1 N K2Cr2O7 is prepared by dissolving 0.49 g of analar crystals in distilled water in a 100 ml
SMF. The solution is made up to the mark.
CALIBRATION OF THE POTENTIOMETER:
A standard cell of known emf is connected to the instrument and its emf is set in the voltage scale.
The galvanometer key is pressed to complete the circuit and the deflection of the galvanometer needle is
noted. If there is any deflection, the current passing through the rheostat is adjusted for null deflection. This
procedure makes sure that the value of emf which is read on the scale is the true potential of the cell
considered. The potentiometer is calibrated using the Weston standard cell of potential 1.018 V.
ESTIMATION OF Fe(II)
The given Fe(II) solution is made upto 100 ml in SMF. 20 ml of the solution is pipetted out into a
clean beaker. To this, 25 ml of 2.5 M H2SO4 and 50 ml of distilled water are added. A platinum electrode is
dipped into this solution, and it is coupled with a calomel electrode through a salt bridge. The resulting cell
is connected to the potentiometer. Standard K2Cr2O7 solution is added from the burette, to this solution,
insteps of 1 ml and the emf is recorded after each addition. At the end point, there is a jump in emf due to
the absence of Fe2+. The approximate range of the end point is determined. The experiment is repeated by
adding the titrant in steps of 0.1 ml near the end point. A graph is plotted between emf, E and the volume
of dichromate added. The inflexion point gives the volume of titrant at the end point. The first derivative
(∆E/∆V vs. Volume of titrant) and the second derivative (∆E2/∆2V vs. Volume of titrant) curves give the
exact volume of dichromate required for the reaction. From the plot of E vs. Volume of titrant, potential at
the equivalent point is obtained. Atomic weight of Fe is 55.85

RESULT:
The amount of iron present in the whole of the given solution is __________ g.

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Titration - 1: Measurement of pH
Titrand : NaOH
Titrant : HCl

Sl. No. Volume of NaOH (mL) pH

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8. pH METRIC TITRATION
AIM
To determine the pH of given sample of water and acetic acid‐acetate buffer using pH meter. To
estimate the amount of HCl in the given solution by pH meter using standard NaOH.

PRINCIPLE
The pH meter employs a glass electrode combined with a salt bridge and a reference electrode
(calomel or Ag/Ag+), together called the combination electrode. The e.m.f. of the combination electrode
can be measured when immersed in a solution. The potential of the glass electrode varies linearly with the
pH of the solution. The standard can be a buffer solution prepared from acetic acid and NaOH of known
strengths. The pH of weak acid‐salt buffer is given by the Henderson‐Hasselbauch equation:
[salt]
pH = pKa + log
[acid]

Ka for acetic acid at 25°C is 1.75 x 10‐5 and pKa = 4.75

In the pH titration, a known volume of the acid is titrated against standardized NaOH. The pH of the
solution increases with the addition of NaOH. At the end point there is a rapid jump in pH. The endpoint
can be obtained accurately from the plot of ΔpH/ΔV vs volume of the added base.

Equivalent weight of HCl = 36.45

PROCEDURE

(a) Calibration of the pH meter

To 20 mL of the 0.1 N acetic acid, exactly half the amount of 0.1 N NaOH required for complete
neutralization is added and stirred well. In this solution [salt] = [acid] and pH = 4.75. The pH meter is
switched on and calibrated. The glass reference electrode is immersed in the standard buffer (pH =4.75) to
the proper level. The reading of the meter is brought to the correct value by the ‘set’ buffer control.

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Titration - 2: Estimation of HCl

Titrand : HCl
Titrant : NaOH

Volume of NaOH (mL) pH ΔpH ΔV ΔpH/ΔV Vmean

Calculations
VNaOH x NNaOH
Normality of HCl =
VHCl

Amount of HCl = NHCl x Equivalent weight (HCl)

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(b) Measurement of pH
The electrode is washed with deionized water and immersed in the test solution and the pH was
measured. A series of buffer solutions (2 or 3) are prepared by mixing appropriate amounts of acetic acid
and NaOH and their pH values are measured. The calculated and measured pH values are compared to
verify Henderson – Hasselbauch equation.

(c) Estimation of HCl

20 mL of the given 0.2 N HCl is pipetted into a clean 100 mL beaker and diluted to 40 mL by
adding distilled water. The glass electrode is immersed and the pH measured with the calibrated pH meter.
NaOH is added to the beaker from the burette in known quantities of 0.5 mL at a time, the solution stirred
magnetically and the corresponding pH is measured after each addition. When the rise in pH is rapid, the
amount of NaOH added is reduced to 1 drop at a time and the readings are observed. When the rate of
increase in pH is not much, the readings are taken at 1 mL intervals of NaOH added. Slope of this curve,
when plotted, against volume gives the endpoint as a sharp peak. The amount of HCl in l litre of the
solution is calculated.

Graph

RESULT
The amount of HCl in one litre of the given solution is

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Titration – 1: Standardization of thiosulfate solution
Titrand : Standard K2Cr2O7 solution
Titrant : Thiosulfate
Indicator : Starch
End Point : Blue to green
Weight of K2Cr2O7 = 0.25 g

Weight of K2Cr2O7 x 10
Normality of K2Cr2O7 =
Equivalent Weight of K2Cr2O7

Standard K2Cr2O7 solution vs Thiosulfate solution

S.No. Volume of K2Cr2O7 Burette reading Volume of thiosulfate

solution (mL) solution (mL)
Initial Final
1. 20

2. 20

3. 20

Calculations

V K2Cr2O 7 x N K2Cr2O 7
Normality of Thio =
VThio

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9. PERCENTAGE PURITY OF BLEACHING POWDER

AIM
To estimate the amount of percentage of available chlorine in a given bleaching powder sample.

PRINCIPLE
Bleaching powder essentially consists of a mixture of calcium hypochlorite, basic chloride, calcium
hydroxide, water and slaked lime. The active component is the hypochlorite, which is responsible for the
bleaching action. When a dilute mineral acid (HCl, H2SO4) reacts with bleaching powder, chlorine is
liberated, as per the equation

Ca(OCl)Cl + 2HCl → CaCl2 + H2O + Cl2 ↑ (liberated or available chlorine)

The liberated chlorine is known as the available chlorine and is expressed as weight percentage of
bleaching powder. In the iodometric method for estimation of available chlorine, the bleaching powder
solution or suspension is treated with an excess of KI solution. The liberated chlorine from bleaching
powder is equivalent amount of I2 from KI which is titrated against standard sodium thiosulfate (thio)
solution.

Cl2 + 2KI → 2KCl + I2

I2 + 2Na2S2O3 → Na2S4O6 + 2NaI

Therefore, 1 g equivalent of thiosulfate = 1 g equivalent of chlorine

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Titration – 2: Estimation of available chlorine

Titrand : Bleaching powder solution (BPS)

Titrant : Thiosulfate
Indicator : Starch
End Point : Blue to colourless

Bleaching powder solution vs Thiosulfate

S.No. Volume of bleaching Burette reading Volume of thiosulfate

powder solution (mL) Initial Final solution (mL)
1. 20

2. 20

3. 20

Calculations
VThio X NThio
Normality of Bleaching Powder solution (BPS) =
VBPS

Amount of Cl2 available in BPS = NBPS x Equivalent weight (Cl2)

Percentage of Cl2 available in BPS = Amount of Chlorine (g)

x 100
Initial Weight of Bleaching Powder (g)

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PROCEDURE
Standardization of sodium thiosulfate solution
The given K2Cr2O7 solution is quantitatively made up to 100 mL by following all the usual
precautions. 20 mL of this solution is pipetted out into a clean conical flask. 5 mL of 10% KI solution and
then 5 mL of dilute HCl are added to the flask. The mouth of the flask is covered and shakes well for few
minutes. The mixture becomes brown due to liberation of iodine. The contents of the flask are titrated
against the given thio solution taken in the burette. The brown colour is started to fade. The addition of thio
is continued until a pale yellow colour is formed. At this point, 1 mL of freshly prepared starch solution is
added and the titration is continued. The end point is the change of colour from blue to green. The titration
is repeated to get concordant values.

Estimation of available chlorine

20 mL of the given bleaching powder solution is transferred to a clean conical flask. Immediately,
20 mL of distilled water is added followed by addition of 5 mL of 10% KI solution and 5 mL of glacial
acetic acid. The flask is covered with stopper and the solution is mixed by shaking the flask. The resultant
solution is titrated against the standardized sodium thiosulfate solution taken in the burette. The addition is
continued until a pale yellow colour is formed. At this point, 1 mL of freshly prepared starch solution is
added and the titration is continued. The end point is the change of colour from blue to colourless.
Equivalent weight of Chlorine = 35.45
Equivalent weight of K2Cr2O7 = 49

RESULT:

The percentage of available chlorine in the given bleaching powder sample is

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Tabulation

Flow time of the solvent t0 = sec

Concentration Flow time ‘t’

ηo/η=t/to=ηrel
C (g/100ml) sec
0.5
1.0
1.5
2.0
2.5

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10. DETERMINATION OF MOLECULAR WEIGHT OF POLYMER BY

VISCOMETRY

AIM
To determine the molecular weight of polyvinyl alcohol using the Oswald’s Viscometer.

PRINCIPLE:
Molecular weight of a polymer is nothing but the average molecular weight. This can be
determined by measuring the intrinsic viscosity (i) of a dilute polymer solution. This intrinsic
viscosity is related to the molecular weight by following relationship
(Mark-Howink equation)

where i = Intrinsic viscosity

K & a = constants for a given polymer-solvent combination at a given temperature.
M = average molecular weight.
PROCEDURE
(i) Preparation of polymer solutions of different concentrations

Polymer solutions of different concentrations say 0.5%, 1.0%,1.5%, 2.0%, 2.5%, are prepared from
the given polymer stock solution.
(ii) Determination of molecular weight of polymer.

20 mL of the solvent is measured out into a clean viscometer using a measuring cylinder. The
solution is sucked up to the mark and released. The time of flow between the two marks is noted.
Now fill the viscometer with 20 mL of the polymer solution (say 1) into the viscometer and
determine the flow time of the polymer solution to flow from the upper mark to lower mark. Using the
same procedure, determine the flow time of the various concentrations of the polymer solution.
From the flow times, reduced viscosity (ηsp/C) can be calculated. Graph is plotted between ηred vs.
concentration, a straight line is obtained with an intercept called intrinsic viscosity (ηi).

RESULT

The molecular weight of the given PVA is .

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Tabulation

Vol. Vol. of Vol. Weight Weight of Weight Total Weight % Weight Weight %
of CH3COOH of of H2O CH3COOH of weight of % of of CHCl3
H2O (mL) CHCl3 (g) (g) CHCl3 (g) CH3COOH H2O
(mL) (mL) (g)

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11. STUDY OF THREE COMPONENT SYSTEM

AIM
To construct a miscibility curve of the three component system and to determine the composition of
the given mixture of chloroform and acetic acid.

PRINCIPLE
Information regarding phase equilibria can be predicted by a simple rule (“Gibbs phase rule”):
f=c−p+2
where c is the number of components and p is the number of phases present in the system. The degrees of
freedom f, or variance, gives the number of variables (e.g., pressure, temperature, composition, etc.) that
must be given to completely describe the system, or to locate the state of the system on the phase diagram.
For ternary systems (i.e., consisting of three components), we have c = 3 and f = 5 − p. If the system
consists of only one phase, f = 4. The required four variables for describing such system are: two for
describing the relative composition (mass fractions) and one of the pairs (P, V ), (P, T), or (T, V ). Note
that if only two mass fractions x1 and x2, are given, the third can be obtained by x3 = 1 − x2 − x1. Also in
practice, (P, T) pair is chosen. If the system separates into two different phases, only f = 5 − 2 = 3 variables
are needed (one mass fraction and (P, T)).

Fig.1

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Vol. Vol. of Vol. Weight Weight Weight Total Weight % Weight Weight %
of CH3COOH of of H2O of of weigh of % of of CHCl3
CHCl3 (mL) H2O (g) CH3COOH CHCl3 t CH3COOH H2O
(mL) (mL) (g) (g) (g)

Unknown

Calculation
Unknown concentration determination
Weight of empty bottle =
Weight of bottle + mixture =
Weight of mixture =
Weight of water =

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Phase diagrams for ternary systems are usually represented using a triangle shown in Fig.1. This
graph accounts for the fact that only two variables are required. Along the phase boundary only one
variable is required. Regions where one or two phases appear have also been indicated in Fig.1. Note that
the line drawn is hypothetical, the real curve will be determined in this experiment. When the solution is
stirred, the transition from one region to another can be observed by appearance (or disappearance) of
cloudiness or turbidity in the solution. The turbidity results from scattering of light by the large number of
very small “oily” droplets of the second phase that are produced when the system is stirred. Sometimes it is
easier to see this when stopping the stirring briefly.
If the three components are mixed to give an overall system composition that falls in the 2-phase
region, the system will separate into two phases: a phase rich in water and another rich in CHCl3. The
compositions of the phases that form are given by the intersections of a tie line with the phase boundary.
The tie line must also contain the point describing the overall system composition. A graphical
representation of tie line is shown in Fig.2.

Fig.2.

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Weight percentage of water =

Weight percentage of acetic acid =
Weight percentage of chloroform =

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Note that in the case of fig.2. only the mass fraction of CHCl3 must be given when the system
remains on the phase boundary line. This determines the mass fractions for water and acetic acid. Hence
the phase rule holds with f = 5 − p = 3 (i.e., mass fraction for CHCl3, temperature and pressure). If the
system was initially in the two-phase region, the tie line uniquely connects the points along the phase
separating line. Given the point ’A’ in fig. 2 (depending on the 1-butanol mass fraction in phase 1), the
points ’B’ and ’C’ are uniquely determined. Thus, only the CHCl3 mass fraction in phase 1, temperature
and pressure are required for complete description of the system, which had separated into two phases. This
is again in accordance with the phase rule.

PROCEDURE
Step 1
In the first part of this experiment CHCl3, CH3COOH and H2O are taken in three burettes. 10 mL of
H2O is taken from burette and is added to 100 mL conical flask. To this 2 mL of acetic acid is added. These
two liquids form a miscible single layered clear solution. To this CHCl3 is added dropwise and the flask is
shaken well. At a certain point a turbidity appears. The volume is noted. Again 2 mL of acetic acid is added
to this mixture followed by dropwise addition of CHCl3 until turbidity appears. The procedure is repeated
until the volume of acetic acid is 16 mL. The volume of CHCl3 required to produce turbidity is noted in
each addition.
Step 2
In the second part of the experiment, 10 mL of CHCl3 is taken in a100 mL beaker and 2 mL acetic
acid is added. To this mixture water is added dropwise until turbidity appears and the volume is noted.
Then 2 mL of acetic acid is added to the mixture, followed by dropwise addition of water until turbidity
appears. This procedure is repeated until the volume of acetic acid is 16 mL. The volume of H 2O required
to produce turbidity is noted in every addition.
Density of H2O = 0.997 g/cm3
Density of CH3COOH = 1.049 g/cm3
Density of CHCl3 = 1.499 g/cm3

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Determination of the composition of a given CHCl3 and CH3COOH mixture.

To the given mixture water is added until turbidity appears. The volume of water is noted. Weight
of water is calculated from the volume of water. The point on the miscibility curve corresponding to the
percentage of water is found out and a straight line is drawn from the vertex of the triangle represents water
and the straight line should pass through the point. The line is extrapolated to the opposite side and the
percentage composition of the unknown is determined from the point.

RESULT
1. The miscibility curve for the system
2. The composition of the given mixture =

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12. DEMONSTRATION EXPERIMENTS USING ADVANCED SPECTROSCOPIC
TECHNIQUES
a) IR SPECTROSCOPY
AIM
This experiment will demonstrate the use of infrared (IR) spectroscopy (also known as vibrational
spectroscopy) to elucidate the identity of an unknown compound by identifying the functional group(s)
present.

PRINCIPLE

A covalent bond between two atoms can be thought of as two objects with masses m1 and m2 that
are connected with a spring. Naturally, this bond stretches and compresses with a certain vibrational
frequency. This frequency is given by Equation 1, where k is the force constant of the spring, c is the
speed of light, and µ is the reduced mass (Equation 2). The frequency is typically measured in
wavenumbers, which are expressed in inverse centimeters (cm-1).

From Equation 1, the frequency is proportional to the strength of the spring and inversely
proportional to the masses of the objects. Thus, C-H, N-H, and O-H bonds have higher stretching
frequencies than C-C and C-O bonds, as hydrogen is a light atom. Double and triple bonds can be
considered as stronger springs, so a C-O double bond has a higher stretching frequency than a C-O single
bond. Infrared light is electromagnetic radiation with wavelengths ranging from 700 nm to 1 mm, which is
consistent with the relative bond strengths. When a molecule absorbs infrared light with a frequency that
equals the natural vibrational frequency of a covalent bond, the energy from the radiation produces an
increase in the amplitude of the bond vibration. If the electronegativities (the tendency to attract electrons)
of the two atoms in a covalent bond are very different, a charge separation occurs that results in a dipole
moment. For example, in a C-O double bond (a carbonyl group), the electrons spend more time around the

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oxygen atom than the carbon atom because oxygen is more electronegative than carbon. Hence, there is a
net dipole moment resulting in a partial negative charge on oxygen and a partial positive charge on carbon.
On the other hand, a symmetrical alkyne does not have a net dipole moment because the two individual
dipole moments on each side cancel each other. The intensity of the infrared absorption is proportional to
the change in the dipole moment when the bond stretches or compresses. Hence, a carbonyl group stretch
will show an intense band in the IR, and a symmetrical internal alkyne will show a small, if not invisible,
band for stretching of the C-C triple bond. Table. 1. shows some characteristic absorption frequencies.

Table.1.
An IR instrument consists of an IR light source, a sample holder, a means of selecting individual
wavelengths or frequencies of the light, some means of detecting the amount of incident light that the
sample absorbs, and a device for plotting the amount of light absorbed as a function of wavelength or
frequency. This plot is referred to as the 'IR Spectrum.' Since IR light is absorbed by most materials, the
optics of an IR Spectrophotometer requires special materials. Most frequently they are built of NaCl or
KBr — water soluble salts.

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PROCEDURE
Sampling
IR spectra can be determined for solids, liquids, or gases.IR gas analysis is a common analytical
tool for those involved in studies of atmospheric pollution. The only draw-back is that it is very expensive
and delicate cells are needed.IR spectra of solids and liquids are usually obtained by dissolving the sample
in a relatively IR transparent solvent such as CCl4 and using simple liquid cells.. Solid spectra may also be
obtained by mixing the solid with dry KBr, grinding to a fine, well mixed powder, and then forming a disk
of the mixture by applying high pressure in a specially designed device. The resulting 'KBr Disk' will
produce a spectrum free of almost all extraneous peaks. Keep the KBr disk in the sample holder and record
the IR spectrum.

RESULT
Given sample have characteristics peaks at

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b) UV- Vis SPECTROSCOPY

AIM
To record the absorption spectra of given compound.

PRINCIPLE

UV-Vis is often called a general technique because most molecules will absorb in the UV-Vis wavelength
range. The UV extends from 100–400 nm and the visible spectrum from 400–700 nm. The 100–200 nm
range is called the deep UV. Light sources are more difficult to find for this range, so it is not routinely
used for UV-Vis measurements. Typical UV-Vis spectrometers use a deuterium lamp for the UV that
produces light from 170–375 nm and a tungsten filament lamp for visible, which produces light from 350–
2,500 nm.

When a photon hits a molecule and is absorbed, the molecule is promoted into a more excited
energetic state. UV-visible light has enough energy to promote electrons to a higher electronic state, from
the highest occupied molecular orbital (HOMO) to the lowest unoccupied molecular orbital (LUMO). The
energy difference between the HOMO and the LUMO is called the band gap. Typically, these orbitals are
called bonding and anti-bonding. The energy of the photon must exactly match the band gap for the photon
to be absorbed. Thus, molecules with different chemical structures have different energy band gaps and
different absorption spectra. The most common transitions that fall in the UV-Vis range are π-π* and n- π*.
Pi orbitals arise due to double bonds, and n orbitals are for non-bonding electrons. Pi star are anti-bonding
pi orbitals. Thus, the best UV-Vis absorption is by molecules that contain double bonds. Pi orbitals
adjacent to each other that are connected, called conjugation, typically increases absorption. Sigma-σ*
transitions, associated with single bonds, are higher energy and fall in the deep UV, so they are less useful
for routine use. The appearance of broad bands or shoulders on the UV-Vis structure is due to the
numerous vibrational and rotational states of a molecule, which lead to separate energy band gaps of
slightly different energies.

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For molecules with absorption in the visible region, the compounds will often appear coloured.
However, a common misconception is that the wavelength of peak absorption (λmax) for a compound is the
colour it appears. A compound that appears red does not have much absorption in the red region of the
spectrum. Instead, the λmax for a compound that looks red is green. The colour of a compound arises
because those wavelengths of light are selectively transmitted through the sample, and thus they are not
absorbed. A colour wheel is helpful in determining what colour a compound will absorb and what range the
λmax will be, as the colour directly across the wheel from the observed colour is the colour that is most
absorbed.

Absorption follows Beer's Law, A= εbC where ε is the molar attenuation coefficient, b is path
length, and C is concentration. The molar attenuation coefficient is the characteristic of an individual
compound to absorb at a given wavelength and this property is due to functional groups, conjugation, etc.
If a compound does not have a high attenuation coefficient, it could be tagged with an appropriate group to
increase its absorbance. Path length is generally related to the size of the cuvette and is 1 cm in standard
spectrophotometers.

UV-Vis is performed on a variety of instruments, from traditional spectrophotometers to more

modern-day plate readers. The absorbance wavelength must be chosen, either using a filter or a
monochromator. A monochromator is a device that separates the wavelengths of light spatially and then
places an exit slit where the desired wavelength of light is. Monochromators can be scanned to provide a
whole absorbance spectrum. Alternatively, a diode-array instrument allows all colours of light to be
transmitted through the sample, then the light is separated into different wavelengths spatially and detected
using photodiodes. Diode-array instruments collect full spectra faster, but are more complicated and more
expensive

PROCEDURE

1. Calibrate the Spectrometer

a) .Turn on the UV-Vis spectrometer and allow the lamps to warm up for an appropriate period of
time (around 20 min) to stabilize them.

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b) Fill a cuvette with the solvent for the sample and make sure the outside is clean. This will serve
as a blank and help account for light losses due to scattering or absorption by the solvent.

c) Place the cuvette in the spectrometer. Make sure to align the cuvette properly, as often the
cuvette has two sides, which are meant for handling (may be grooved) and are not meant to
shine light through.

d) Take a reading for the blank. The absorbance should be minimal, but any absorbance should be
subtracted out from future samples. Some instruments might store the blank data and perform
the subtraction automatically.

2. Perform an Absorbance Spectrum

a) Fill the cuvette with the sample. To make sure the transfer is quantitative, rinse the cuvette
twice with the sample and then fill it about ¾ full. Make sure the outside is clean of any
fingerprints, etc.

b) Place the cuvette in the spectrometer in the correct direction.

c) Cover the cuvette to prevent any ambient light.

d) Collect an absorbance spectrum by allowing the instrument to scan through different

wavelengths and collect the absorbance. The wavelength range can be set with information
about the specific sample, but a range of 200–800 nm is standard. A diode-array instrument is
able to collect an entire absorbance spectrum in one run.

e) From the collected absorbance spectrum, determine the absorbance maximum (λmax). Repeat the
collection of spectra to get an estimate of error in λmax.

f) To make a calibration curve, collect the UV-Vis spectrum of a variety of different concentration
samples. Spectrometers are often limited in linear range and will not be able to measure an
absorbance value greater than 1.5. If the absorbance values for the sample are outside the
instrument's linear range, dilute the sample to get the values within the linear range.

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RESULT

Absorbance maximum of the given sample =

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Tabulation

Wavelength of Raman Wave number of the Exiting line wave Raman shift
line (nm) peaks number (cm-1)
(cm-1) (cm-1)

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c) RAMAN SPECTROSCOPY

AIM
To record the Raman spectra of Sulphur

PRINCIPLE
The Raman effect arises when a photon is incident on a molecule and interacts with the electric
dipole of the molecule. In quantum mechanics the scattering is described as an excitation to a virtual
state lower in energy than a real electronic transition with nearly coincident de-excitation and a change
in vibrational energy. The scattering event occurs in 10-14 seconds or less. The virtual state description
of the scattering is shown in Figure 1. The energy difference between the incident and scattered
photons is represented by the arrows of different lengths in Figure 1. Numerically, the Raman shift in
wave numbers (cm-1), is calculated through Eq.1 ,
ṽ = 1/λincident – 1/λscattered (1)
in which the λ’s are the wavelengths (in cm) of the incident and Raman scattered photons, respectively.
At room temperature the thermal population of vibrational excited states is low, although not zero.
Therefore, the initial state is the ground state, and the scattered photon will have lower energy (longer
wavelength) than the exciting photon. This Stokes shifted scatter is what is usually observed in Raman
spectroscopy. A small fraction of the molecules are in vibrationally excited states. Raman scattering
from vibrationally excited molecules leaves the molecule in the ground state. The scattered photon
appears at higher energy. This anti-Stokes-shifted Raman spectrum is always weaker than the Stokes-
shifted spectrum, but at room temperature it is strong enough to be useful for vibrational frequencies
less than about 1500 cm-1 . The Stokes and anti-Stokes spectra contain the same frequency information.
The anti-Stokes spectrum can be used when the Stokes spectrum is not directly observable, for
example, because of poor detector response at lower frequencies.

PROCEDURE
The new setup is based on an air-cooled, frequency-doubled Nd:YAG laser at a wavelength of 532
nm and a small Czerny-Turner USB spectrometer. All the components fit on one half of an air-damped

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optical breadboard (1 m x 1.5 m) shared with another experiment (wide field and confocal fluorescence
microscopy).
The laser beam is reflected by two mirrors for beam walking and by 90◦ at a prism mirror and runs
parallel to the optical axis of the Raman setup. An achromatic lens with a diameter and a focal length of 50
mm focuses the laser light onto the sample in the focal plane. Directly reflected excitation light hits a
second prism mirror and is deflected off the optical axis into a beam dump. The solid or liquid samples are
filled into NMR glass tubes with 5 mm diameter. These tubes can be fused at the top, so that volatile or
hazardous substances are safely sealed within the vials. Around 1 mL of the sample substance is filled into
the tube and temporarily frozen with liquid nitrogen. Then the top of the tube is melted with a Bunsen
burner and the tube is sealed. The sample holder is an aluminium block with a vertical hole perpendicular
to the optical axis for the NMR tube and a window for the laser excitation as well as the backwards
scattered light. There is a threaded hole along the optical axis that allows for easy calibration with external
lamps and which is blocked by a screw during Raman measurements. The Raman light is emitted in all
directions and part of it is collimated by the same lens which focuses the laser onto the sample. A second
achromatic lens with a diameter of 50 mm and a focal length of 200 mm focuses the Raman light onto the
end face of an optical fibre. Before hitting the fibre the converging light passes through a polariser and a
notch filter. Usually these filters are placed in a section of the optical train with a collimated beam, because
then all light from the focal spot hits the filter without inclination. This is relevant for interference filters,
since their spectral characteristics depend on the angle of incidence. The notch filter in this setup has a
diameter of 25 mm to save costs. It tolerates angles of incidence of up to +5◦1 and is therefore placed at a
position in the optical path with a smaller beam diameter. The filter blocks light at (532 + 9) nm with an
optical density of 6. It is rotatable around a vertical axis so the angle of incidence and by that the blocked
spectral region of the filter can be tuned. The polariser can be rotated around the optical axis to adjust for
parallel or perpendicular polarisation relative to the vertically polarised excitation light. The position of the
fibre end face can be adjusted in three dimension to optimize the coupling of the Raman light into the 50
μm optical fibre. All the optical components are mounted in a cage system for 50 mm and 25 mm optics.
The fibre end face serves as input slit for the slitless USB spectrometer. The spectrometer was especially
configured for the use in this Raman setup. The grating with 1800 lines/mm allows for a spectral range of
175 nm, the start wavelength range was customized to start at 480 nm, ranging up to 655 nm. With an
excitation wavelength of 532 nm this results in Raman shifts in the anti-Stokes region down below -2000
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adequate while anti-Stokes lines below -1000 cm-1 were difficult to observe due to their small intensity.
The CCD detector for the acquisition of the spectrum consists of 3648 elements. The sensitivity of the
spectrometer was further enhanced by highly reflective mirrors and a collecting lens in front of the CCD
detector array. The spectral data is send via USB interface to a personal computer and the spectrum can be
viewed immediately on the monitor. This supports high quality spectra with optimized parameters, since
the effect of changes can be observed and evaluated directly.

RESULT

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