CHAPTER 9

INSTRUMENTAL METHODS OF ANALYSIS

Dr Hmwe Nantthar
Professor
Department of Engineering Chemistry
Yangon Technological University
26.12.2022
1
 (1) Colorimetry
are made
• Colorimetric measurements using
a white light source
pass
through a colour filter (or) alternative wavelength selection device

pass
• incident light through a currette containing a coloured
chemical compound in solution
• the loss of light or absorption α to the concentration of
compound

2
colorimetry measure visible region of the electromagnetic
spectrum (e.g. 370-780 nm)

wavelength of the incident light

depend colour
thickness of the solution

determined concentration of a substance to know

concentration of a substance
Beer-Lambert’s Law
A = εcd
A αC

3
 d Thickness

Incident light Transmitted light

I0 Ia It

Concentration of absorbing
C
sample, C moles/dm3

I0 = Ia + It
A = log I0 /It = εcd
4
Beer-Lambert’s Law
A = εcd
A αC
A = absorbance of the coloured solution
C = concentration of the substance in solution (mol/dm3)
ε = molar extinction coefficient
d = path length

Transmittance T = Transmitted light,

It Incident light, I0

A = log 1/T
= log I0 / It
A = absorbance (A) or optical density OD

5
Figure 9.1 Schematic working of a calorimeter

6
7
 do not absorb (or)
In colorimetry coloured solution very low absorbance
visible region

Absorbance (A) against concentration, the graph give a straight

line, which give calibration curve (or) standard curve.

e.g. copper complex solution (blue) → 620 nm

for reddish colour → 480 nm

8
9
10
 2. Potentiometry

measured
potential electrochemical cell (no current flow)
potential α concentration of same component of the
analyte
one is reference electrode
two half cells other indicator electrode

SCE = saturated calomel electrode (0.2422 V)

electrochemical analysis depend on electrode reaction
redox analyte species indicator electrode
platinum electrode indicator electrode
depends redox ionic concentration
11
12
13
14
Determination of the Equivalence Point in
Potentiometry

15
Fig 9.4 Endpoint curves of potentiometric titrations (a) potential Vs
volume of titrant (b) first differential plot (c) second differential plot
16
❖ Direct plot of the potential E against the volume of titrant gives
the fig. 9.4 (a).
The endpoint of the titration is where there is an abrupt change in
the potential value at the indicator electrode.

❖ The first derivative values of the potential and the volume of

titration is taken and plotted against volume of titrant show the
fig. 9.4 (b).
The point at which the maximum value of ΔE is taken as the end
point of titration. ΔV
The values taken as the second derivative for the potential and
volume gives the best result.

❖ The point at which the second derivative cross zero is the

inflection point which is taken as the end point of titration Fig. 9.4
(c).
17
 9.3.5 An Electrochemical Cell with Ion Sensitive Electrode

Determination of pH of a solution
The pH observed through the ion selective electrode (ISE) is
directly proportional to the concentration of the H+ ion concentration
of the analyte solution.

E 0 ̶ E 0
pH = G SCE ̶ E cell
0.0591

18
Other Applications

Reviewed in instrumental analysis and quantitative analysis

(1) Acid –Base titrations

(2) Redox titrations
(3) Precipitation titrations
(4) Complexation titrations

19
 Advantages of Potentiometric Titrations

To determine
• Turbid
• Coloured
• Very dilute solutions

Advantages
• Very sharp end point
• Ease of automation
• A large number of commercial rigs are available
• Accurate methods for many electroanalytical processes

20
(3) Conductometry
application chemical and biochemical studies
conductometer measuring the conductivity of an ionic solution
migrate
anion to the anode
cation to the cathode
source high frequency

Solution Conductance
to measure conductance of ionic solution rather than
its resistance

21
Ohm’s Law
V = IR
V = potential difference (V)
I = electric current (A)
R = resistance (Ω)

R = ρ l/A
ρ = proportionality constant (specific resistance)
Ƙ = 1/ρ
Ƙ = specific conductance

22
 Molar Conductance

The specific electrical conductivity and electrical conductance

are a measured of the ability of a solution to conduct an electrical
current.
Molar conductance of ionic solutions (ΛM) is defined as the
conducting power of all the ions produces by one mole of an
electrolyte in 1 dm3 of water.
decrease
specific conductance Ƙ, concentration decrease
molar conductance increases
The value of К contributed by one mole ions contained in 1
dm3 (1000 cm3) of solvent.
1000 × Ƙ
ΛM = C (Sm2 mol-1)
ΛM = molar conductance
23
Kohlrauch Law
ΛM = λ0+ - λ0-
ΛM = molar conductance

λ0+ = ionic conductance of cation

λ0- = ionic conductance of anion
The mobility of an ion is independent of concentration.

For infinite dilution,

λ0+ = k μ0+ and λ0- = k μ0-

μ0+ and μ0- are the ionic mobilities of cation and anion
Where mobilities are expressed in terms of m/second under
unit potential gradient.
1 Faraday = 96500 Coulomb

u0± = λ0 ± = λ0 ±
F 96500 24
Applications of Conductometry
Conductometry used direct measurement in titration
Uses; (1) monitoring surface water
(2) waterworks
(3) water desalination plants
(4) preparation of ultra pure water
Conductivity detection used precipitation titration
Applications
▪ degree of dissociation of weak electrolyte
▪ Ionic product of water
▪ solubility's and solubility product of sparingly soluble salts and
▪ acid-base and precipitation titrations
electrical conductance depend (i) number of ions
(ii) mobility of ions
25
Conductometric titration curve

Fig. 9.6 Conductometric titration curve for hydrochloric acid

titrated using solution of sodium hydroxide
26
 Consider a solution of a strong acid, hydrochloric acid, HCl for
instance, to which a solution of a strong base, sodium hydroxide NaOH,
is added.
H+ + OH- H2O (unionised water)

For each amount of NaOH added equivalent amount of

hydrogen ions is removed. Effectively, the faster moving H+ cation is
replaced by the slower moving Na+ ion, and the conductivity of the
titrated solution as well as the measured conductance of the cell fall.
This continues until the equivalent point is reached, at which we have a
solution of sodium chloride, NaCl. If more base is added an increase in
conductivity or conductance is observed, since more ions are being
added and the neutralization reaction no longer removes an
appreciable number any of them.

27
Fig. 9.7 Titration of weak acid Vs NaOH

28
 Consider the titration of solution of a weak acid, such as acetic
acid CH3COOH, using a solution of strong base, NaOH. The weak acids,
as well as other weak electrolytes, are dissociated into very small
extent and they exist in solution essentially in form of the neutral acid
molecules. When a solution of NaOH is added the reaction occurs the
undissociated molecules of acetic acid are transformed into dissociated
molecules of potassium acetate. The changes are accompained by
increase in conductivity of the solution.

CH3COOH + NaOH Na+ + CH3COO- + H2O

29
Fig. 9.8 Conductometric titration curve for the hydrochloric acid-
acetic acid mixture titrated using solution of sodium hydroxide
30
 The method of conductometric titration is adapted to
the estimation of mixtures of acids of differing strengths.
When a mixture of strong and weak acid is titrated a plot of
conductance against alkali added takes form as Fig 9.8 (c). The
conductometric titration curve is a combination of the
diagrams obtained during the titration of strong and weak
acid respectively, where the first end point correspond to a
neutralisation of the strong acid present in the sample and
the second one is associated with a neutralisation of the weak
acid in the solution under investigation. The volume of the
alkali consumed by the latter is given by a difference of the
respective volumes.

31
32
 (4) Flame Photometry
flame photometry atomic emission method
detect metal salts Na, K, Li, Ca and Ba
Instrumentation
consists (1) burner
(2) nebuliser
(3) monochromator
(4) detector
(5) recorder
flame photometry sample and inexpensiveused
for clinical biological environmental
analysis

33
Fig. 9.9 Flow diagram of a flame photometer
34
 Applications
used to determine metals in solution (alkali and
alkaline earth) in the given samples
➢ Like described for atomic absorption.
➢ Qualitative determination is also possible as each element emits its
own characteristic line spectrum.

Disadvantages
➢ very sensitive to change
➢ spectral interference
➢ self-absorption
➢ affect the precision of the measurement

absorbance Vs concentration is not expected to obtain linear.

35
36
 (5) Atomic Absorption Spectroscopy (AAS)
measured absorption of optical radiation by atoms in the
gaseous state
atoms absorb visible and ultraviolet region (excited state)

absorbed
wavelength of light electrons go to excited state

measure
characteristics of the sample

37
Fig 9.10 Component of an atomic absorption spectrophotometer
38
Three basic components for every AA spectrophotometer

( i) Light Source

HCL (hollow cathode lamps)

used
specific lamps
EDL (electrodeless lamp)

39
 (ii) Sample Cell
❖ burner system (flame AAS)
❖ electrically heated furnace or platform
❖ aligned in the optical path of the spectrophotometer

(iii) Specific Light Measurement

disperse
(a) monochromator several wavelength of lights
emitted isolate
from light source a particular line of interest
produce depend
(b) detector electrical current light intensity
(c) readout concentration units

40
Applications
✓ quantitative determination of metals at trance levels (0.1 to 100
ppm)
✓ used to Beer-Lambert’s Law
✓ Standard curve (absorbance Vs concentration)
✓ Plot give the linear range
✓ To know the concentration from the plot

Disadvantages
Sample must be solution at least volatile
needed
individual source lamp and filters for each elements
every metal own characteristic absorption

41
Fig Atomic absorption spectroscopy
42
 (6) Flurometry
measure amount of fluorescent radiation
produced
to monochromatic radiation
Principle
supplied
adequate energy electrons excited to higher energy
levels of the atom fall different lower energy states
back
emission
before reading to the actual ground state
energy

Applications
benzene
limited quantitative
estimations
fused benzene ring system

43
❖ inorganic metals (to form complexes with the ligands)

❖ uses foods for vitamin content (riboflavin, niacin, etc)

Disadvantages
limited only a few substances fluorescence

44
Figure Fluorometry

45
Figure Fluorometry 46
Figure: Fluorometry
47
(7) Ultraviolet Visible Spectroscopy (UV/Vis)

Principles
200- 700 nm
Apply Beer-Lambert Law
A = εbc

48
 (i) Electronic Transitions

Three types of electronic transition

▪ transitions involving p, s and n electrons

▪ transitions involving charge-transfer electrons
▪ transitions involving d and f electrons (not covered in this unit)

Atom or molecule absorbs electron promoted

energy

from ground state to excited state

atoms can rotate and vibrate discrete
energy levels
packed on top of each electronic level
49
Fig 9.11 Rotational and vibrational electronic levels of an
atom or molecule 50
 (ii) Absorbing species containing p,
s and n electrons
• Absorption of UV and Vis radiation in organic molecules is restricted
to certain functional groups (chromophores) that contain valence
electrons of low excitation energy
• The spectrum of a molecule containing these chromophores is
complex
• superposition of rotational and vibrational transitions (overlapping
lines)
• appear continuous absorption band

51
Fig 9.12 Possible electronic transitions in atom or molecule

52
 1. σ σ* Transitions

❖ An electron is a bonding s orbital is excited to the corresponding

antibonding orbital.
❖ The energy required is large.
❖ eg methane, C-H bonds, and can only undergo σ σ* transitions)
shows an absorbance at 125 nm.
❖ Absorption maxima due to σ σ* transitions are not seen in
typical UV/VIS spectra (200-700nm).

53
 2. n σ* Transitions
▪ Saturated compounds containing atoms with lone pairs (non-
bonding electrons) are capable of n σ* transitions.
▪ These transitions usually need less energy than σ σ*
transitions.
▪ Wavelength is in the range 150-250 nm.
▪ The number of organic functional groups with n σ* peaks
in the UV region is small.

54
 3. n π* and π π* Transitions

• Based on transitions of n or p electrons to the excited state.

• Convenient region of the spectrum (200-700nm).
• These transitions need an unsaturated group in the molecule to
provide the p electrons.
• n π* transitions range from 10 to 100 L mo1-1 cm-1
• π π* transitions range between 1000 and 10000 L mol-1cm-1
• n π*transitions shorter wavelength (blue shift)( increased
solvation of the lone pair, which lowers the energy of the n orbital
• π π* transition (red shift) (attractive polarisation forces
between the solvent and the absorber

55
 Charge-Transfer Absorption
❖ Many inorganic species show charge-transfer absorption and are
called charge-transfer complex.
❖ eg., one is electron donating properties and another is electron
acceptor properties
electron from donor
absorption of radiation involves
transfer orbital associated with acceptor

❖ molar absorbtivities from charge-transfer absorption are large

(greater that 10,000 L mol-1 cm-1)

56
Instrumentation
Two types of instruments
(1) single beam
(2) double beam (widely used)

• sources (UV and Visible)

• wavelength selector (monochromator)
• sample containers
• detector
• signal processor and readout
• each of these components will be considered in turn

57
Fig 9.13 A single beam UV/VIS Spectrophotometer

Ratio Output

Fig 9.14 A double beam UV/VIS Spectrophotometer 58

Sources of UV/VIS Radiation

deuterium or hydrogen at low pressure

breaks up to give two atomic species and an ultraviolet photon

D2 + electrical energy D2* D’ + D’’ + hν

both deuterium and hydrogen lamps emit radiation in the range 160-
375 nm.
quartz cuvettes must be used
but glass absorbs radiation of wavelength less than 350 nm

59
Sources of Visible Radiation

tungsten filament lamp is used

wavelength range of 350-2500 nm
The energy emitted by a tungsten filament lamp is proportional to
the fourth power of the operating voltage
electronic voltage regulators or constant-voltage transformers are
used to ensure this stability

60
Wavelength Selector (Monochromator)

All monochromators contain the following component parts

An entrance slit
A collimating lens
A dispersing device (usually a prism or a grating)
A focusing lens
An exit slit

61
Applications

• quantitative trace analysis, apply Beer-Lambert Law

• identification and structural analysis of organic materials
• molecular absorption spectrum
• tell the nature of the compound

Disadvantages
❑ should be in solution
❑ interference sometimes
❑ difficult to analyses (mixture)
❑ disturbances

62
Figure UV/VIS Spectrophotometer
63
(8) Infrared Spectroscopy (IR)
Region wave number range (cm-1)
wave number = 1/ wavelength(cm)
Near 1200-4000
Middle 4000-200
Far 200-10
most useful IR region 4000-670 cm-1
Theory of Infrared Absorption
molecule absorbs electromagnetic radiation in the form of
stretching, bending, etc
(a) Molecular Rotations
Rotational levels quantized
gives line spectra
liquid or solid line broaden (due to molecular
collisions and other interactions)
64
(b) Molecular vibrations
stretching and bending
stretching symmetric
asymmetric

Stretching: Change in inter-atomic distance along bond axis

65
Fig 9.15 Symmetric and aymmetric stretching vibrations
66
Fig 9.15 Symmetric and aymmetric stretching vibrations
67
Bending: Change in angle between two bonds.

Four types of bends

(1) Rocking
(2) Scissoring
(3) Wagging
(4) Twisting

68
Fig 9.16 Bending vibrations of a molecule

69
Fig Bending vibrations of a molecule

70
71
72
 Vibrational Coupling
If the vibrating bonds are joined to a single, central atom
(1) Strong coupling of stretching vibrations occurs when there is a
common atom between the two vibrating bonds
(2) Coupling of bending vibrations occurs when there is a common
bond between the vibrating groups
(3) Coupling between a stretching vibration and a bending vibration
occurs if the stretching bond is one side of an angle varied by
bending vibration
(4) Coupling is greatest when the coupled groups have approximately
equal energies
(5) No coupling is seen between groups separated by two or more
bonds

73
Instrumentation
A double beam IR spectrophotometer consists of the following
IR source
grating monochromator
thermocouple detector
cells made of either sodium, chloride or potassium bromide
materials, etc.

74
 Applications:

• in the identification and structural analysis of organic

compounds, natural products, polymers, etc.
• presence of particular functional group in a given organic
compound
Disadvantages
mixture substances cannot be analysed

75
76
77
78
(9) Microwave Spectroscopy
This technique is an extension to IR spectroscopy.
The microwave region lies at the far infrared region of the
electromagnetic spectrum.
Its absorption by molecules give rise to changes in the rotational
energies of the molecules.
In IR spectroscopy, the molecule are subjected for changes in
vibrational energies; the energy required for making changes at
rotational levels is lesser than for vibrational levels.
Through the principles are same as that of IR, the instrumentation is
slightly different in that it requires samples in gaseous state for the
analysis.

79
Its application are limited to smaller and simpler molecules since,
larger molecules will have interactions between the rotational
energy levels within the molecule through various bonds they
have.
In certain cases this technique can be considered as a good
alternate to IR spectroscopy.
Besides qualitative analysis, this technique can be applied for
conformational analysis of simpler compounds.

80
81
82
83
 (10) Nuclear Magnetic Resonance Spectroscopy (NMR)
Principles
UV, IR and microwave techniques utilise the absorption of light
in electronic states as well as in molecular vibrational and
rotational levels.
In NMR, the absorption by substances occurs in the radio
frequency region of the electromagnetic spectrum resulting in
changes in the orientation of the spinning nuclei by applying a
magnetic field.
The nuclei of the atoms bonded to each other in molecules spin
on an axis like a top.
Since nuclei are positively charged, this spin will create a small
magnetic field around it.

84
If an external magnetic field applied to these nuclei, then the spin
of the nuclei will align to the magnetic field deviating from the
original axis of spin.
If radio waves are applied to the system, the nuclei will absorb this
energy and re-align back to their original axis of spin.
The nature of the compounds and the presence of various
functional groups and their environment will give.
Since this technique mostly measures the spinning of the hydrogen
nuclei (almost all the organic compounds contain hydrogen
atoms).
It is referred as Proton Magnetic Resonance (PMR) spectroscopy.

85
 Instrumentation
• Powerful magnet
• Radiofrequency signal generator
• Amplifier
• Detector, etc,.

86
87
88
89
 Applications

identification and structural analysis of organic compounds and a

tool for qualitative analysis
valuable information (position of the functional groups in a
molecule and provides distinguished spectra for the isomer
much precise information on the structure of the compounds can
be obtained the same technique with other magnetic nuclei like
C13 , O17.
The instrumentation being the same except that the sweep by the
magnetic field is varied.

90
 Disadvantages

Very expensive and the instrumentation is complex and needs

exceptional skills to operate.
Its sensitivity ranges from moderate to poor, however, one can
get clear information using C13 , or O17 NMR.
The usage of the solvents is limited and in most of the situations
deuterated solvents are required.

91
92
Figure; NMR Spectroscopy 93
(11) Electron Spin Resonance Spectroscopy (ESR)
Electrons always have a spin and thus have a magnetic moment.
This technique is of high value when it comes to the compounds
which contain odd electrons.
Which have paramagnetic behaviour, if it is unpaired then it can
align with the applied magnetic field and the feasibility of
getting ESR spectra is higher.
Thus, the principle and the instrumentation are much similar to
that of NMR technique.
It is also referred as Electron Magnetic Resonance.

94
Figure: Electron Spin Resonance Spectroscopy (ESR) 95
 (12) Chromatography

• The chemical components present in a mixture are separated,

identified and determined using a efficient technique known as
chromatography.
Uses
- For analytical purposes
- Preparative methods
➢ Compounds of high-grade purity can be obtained by this way
Chromatography Technique
The components of a mixture are separated based upon the
rates at which they are carried or moved through a stationary phase
by a gaseous or liquid mobile phase.

96
Based on the mobile phase,

❖ Liquid Chromatography (LC / HPLC)

❖ Gas Liquid Chromatography (GLC)

Liquid Chromatography (LC / HPLC)

long glass columns with wide diameter (150-200 μ range)
The flow rates (eluent time) of the mobile phase with the analyte
were very slow and separation times were long-often several hours.
The speed of the flow rates were improved by applying high
pressure to the column using pumps and hence the performance
was improved.
These are called as ‘High-Performance Liquid Chromatography’ or
‘High-Pressure Liquid Chromatography’ (HPLC).

97
98
Figure : HPLC
99
Figure : HPLC 100
 Gas Liquid Chromatography (GLC)
In gas-liquid chromatography, it is the interaction between the
gaseous sample (mobile phase) and standard liquid (stationary
phase), which causes the separation of different molecular
constituents.
The stationary phase is either polar or non-polar liquid.

The basic components are

inert carrier gas (mostly commonly He, N2, H2)
GC column packed or coated with an appropriate stationary
phase
An oven that that allows for precise temperature control of the
column
Some type of detector capable of detecting the sample as it
exits or elutes from the column
101
102
103
104
 Gas-liquid chromatography works;
The molecules in the samples are carried along the column in the
carrier gas, but partition between the gas phase and the liquid phase.
This partitioning is critically dependent on the solubility of the sample
in the liquid phase, different molecular species travel along the
column and elute at different times
Those molecules that have a greater solubility in the liquid phase take
longer to elute and thus are measured at a longer interval.
Solubility is dependent on the physical and chemical properties of the
solute.
Separation between different components of the sample occurs based
on molecular properties such as relative polarity (like ethylene glycol
vs base oil) and boiling point (like, fuel vs diesel engine base oil).
Using a polar stationary phase, with a mixture of polar and non-polar
compound will generally result in longer elution times for the polar
compounds, because they will have greater solubility in the polar
stationary phase.
105
 Disadvantages of Gas Chromatography

Samples must be volatile and thermally stable below about

4000 ˚C.
No signal universal detector is available and the most commonly
use detectors are non-selective.
One should take much care in the analytical steps starting from
the selection of the column, the detector and must define the
temperatures of all the three ports, viz., injection port, column
oven and detector.
An improper calculation on these will lead to sensitive results.

106
107
Figure; GC chromatography 108
109
 (13) Differential Thermal Analysis (DTA)
measure temperature difference between a sample and a
reference material as a function of temperature as
they are heated or cooled or kept at a constant
temperature (isothermal).

▪ It provides their endothermic and exothermic behaviour at high

temperatures.
▪ It apply in analysing and characterising clay materials, ceramic,
ores, etc.

110
Figure; DTA
111
112
Figure; DTA 113
114
115
 (14) Differential Scanning Calorimeter (DSC)
• This technique is more or less similar to DTA except that it
measures the amount of heat absorbed or released by a sample as
it is heated or cooled or kept at constant temperature (isothermal).
• It is the detection of liquid crystal.
• This technique is applied to detect the heat of melting and melting
point of thermoplastic polymers.
• It provides information regarding the molecular weight and
structural differences between very similar materials.
• The instrumentation is exactly similar to that of DTA except for the
different in the manipulation of the results.

116
➢It Physical properties include mass, temperature, enthalpy,
dimension, dynamic characteristics and others.
➢ Its application is finding the purity, integrity, crystallinity, thermal
stability of the chemical substances under study.
➢It is used to determine the composition of complex mixtures.
➢It is applied in wide fields, including polymer, glass, ceramics,
metals, explosives, semiconductor, medicine, etc.

117
 Applications:
• characteristic temperature identification
• melting and crystallisation behaviour
• purity
• polymorphism
• specific heat capacity
• heat of reaction
• oxidative stability
• glass transitions
• heat of melting and crystallisations
• compatibility
• solid liquid ratio
• Reaction behaviour
• Reaction kinetics
• Thermal stability 118
9.6.11 Thermogravimetric Analysis (TGA)
• The change in sample weight is measured while the sample is
heated or cooled at a constant rate and so, the technique is
known as thermogravimetric analysis (TGA).
• This technique is effective for quantitative analysis of thermal
reactions that are accompanied by mass change such as
evaporation, decomposition, gas absorption, desorption and
dehydration under normal as well under different gaseous
environment as desired.

119
Figure; TGA 120
Figure; TGA 121
Figure; TGA 122
123
124
125
Figure; TGA 126
Figure; TGA 127
 9.6.12 Cyclic Voltametry

Cyclic voltammetry is the most widely used technique for

qualitative information about electrochemical reactions.

Ability
(1) Information on the thermodynamics of redox processes
(2) Kinetics of heterogeneous electron-transfer reactions
(3) On coupled chemical reactions or adsorption processes

128
129
130
131
In cyclic voltametry have always three electrode functions.

The first of the three electrodes is the indicating electrode also

known as the test or working electrodes.
The second functional electrodes is the reference electrode.
The final functional electrode is the counter or auxiliary electrode
so that current can be passed from the external circuit through the
cell.

(1) Indicator electrodes (platinum metal indicator electrodes)

(2) Carbon Indicator Electrodes
(3) Reference Electrodes

132
133
134
135
136
(1) Absorbance of light by a solution of substance depends on
i. path length ii. concentration of solution
iii. wavelength of incident light iv. all of these

(2) Conductometric estimation is based on

i. Beer-Lambert’s law ii. Henderson-Hesselbalch equation
iii. Nernst equation iv. Ohm’s law

(3) The melting point of thermoplastic polymers can be determined by

i. DTA ii. DSC iii. TGA iv. ESR

(4) The most widely used method for endpoint determination in titrimetric
analysis is
i. Spectrophotometry ii. Potentiometry iii. Amperometry
iv. conductometry

137
(5) In microwave spectrocsopy, samples must be in
i. liquid state ii. Solid state iii. Gaseous state iv. Solution

(6) In nuclear magnetic resonance spectroscopy, the absorption of

substances occurs in
i. the visible region ii. the IR region
iii. the radio frequency region iv. none of these

(7) A mixture of HCl and ethanoic acid can be titrated satisfactorily by

i. conductometry ii. potentiometry
iii. spectrophotometry iv. none of these

(8) Which is the preferred continuous source in visible region?

i. Hollow cathode lamp ii. Tungsten filament lamp
iii. Deuterium lamp iv. None of these

138
(9) In vltraviolet visible spectroscopy, the concentration of an analyte in
solution can be determined by applying
i. Nernst equation ii. Ohm’s law iii. Beer-Lambert’ law
iv. none of these

(10) Organic compound have C-H bonds, that absorption in the

2850-3000 cm-1 is due to
i. sp3 C-H stretching ii. sp2 C-H stretching
iii. sp C-H stretching iv. none of these

(11) Microwave spectroscopy is an extension to ------- spectroscopy.

i. UV/Vis ii. IR iii. NMR iv. None of these

(12) In HPLC method, the mobile phase is -------.

i. liquid ii. solid iii. gas iv. gas and liquid

139
(13) Which method(s) can be used for the end point determination of
acid and base reaction?
i. potentiometry ii. conductometry
iii. spectrophotometry iv. all of these

(14) The hollow cathode lamps are used as the light source of ----------.
i. Flame photometer ii. Atomic absorption
spectrophotometer iii. UV-Vis spectrophotometer iv. none of these

(15) In measuring the absorbance of a compound at 250 nm on a

spectrophotometer, we have to use
i. a tungsten lamp ii. a hydrogen lamp
iii. IR sensitive tube iv. a mercury lamp

(16) Metals and metalloids are detected by

i. Flame photometer ii. Atomic absorption
spectrophotometer iii. UV-Vis spectrophotometer iv. all of these
140
(17) The present of solvent in a crystalline sample of a compound could
be detected and quantified using:
i. AAS ii. UV-Vis iii. TGA iv. ESR-MS

(18) What is the name of an instrument used to measure the

absorbance of a coloured compound in solution?
i. colorimeter ii. colourmeter iii. calorimeter iv. coulometer

(19) In AAS, which of the following is generally used as radiation

source?
i. Tungsten lamp ii. Xenon mercury are lamp
iii. Hydrogen or Deuterium dischargr lamp iv. Hollow cathode lamp

(20) Methods requiring the measurement of absorbance in the UV

region of the electromagnetic spectrum require that the sample
cuvette is made of
i. glass ii. quartz iii. plastic iv. sodium chloride
141
(21) The unit of molar absorptivity's is
i. L mol-1 cm-1 ii. mol L-1 cm iii. mol L-1s-1 iv. S mol-1 m2

(22) In what instrumental method(s), the sample must be in solution?

i. Flame pfotometry ii. AAS iii. Uv-Vis spectroscopy
iv. all of these

(23) In GLC, using a polar stationary phase, the elution times of polar
compounds from a mixture are _______ those of non-polar
compounds.
i. longer than ii. shorter than iii. the same as iv. all of
these

(24) What is a blue shift?

i. The shifting of an absorption to longer wavelength.
ii. The shifting of an absorption to higher energy
iii. The shifting of an absorption to lower energy
iv. None of these 142
(25) The UV and visible regions of the electromagnetic spectrum lie
between wavelength of
i. 200-400 nm ii. 400-700 nm iii. 200-700 nm iv. 340-850 nm

(26) The wavelength of absorption is 495 nm, In what region of the

electromagnetic spectrum does this lie?
i. IR ii. UV iii. visible iv. microwave

(27) In Gas chromatography, the stationary phase is

i. Gas ii. Liquid iii. Solid iv. Both I & ii

(28) According to the Beer-Lambert’’s law, absorbance is

i. inversely proportional to the concentration
ii. directly proportional to the concentration
iii. directly proportional to the transmittance
iv. directly proportional to the log of concentration

143
1. Construct the electrochemical cell for potentiometry.
2. Write the disadvantages of the following
i. Atomic Absorption Spectroscopy ii. IR spectroscopy
3.Explain the vibrational coupling occurred in molecules by the
absorption of IR radiation.
4. Write the instrumentation and applications of NMR spectroscopy.
5. Write a note on microwave spectroscopy.
6. Explain the different types of vibration of a molecule with suitable
representations.
7. Write the applications and disadvantages of IR spectroscopy.
8. What is cyclic voltametry? Write the electrodes and their functions
in cyclic voltametry.
9. Write the instrumentation of IR spectroscopy.
10. What are the types of electronic transition and molecular
vibrations?
11. What is chromatography? Write two differences between HPLC
and GLC techniques.
12. Write a note on the thermogravimetric analysis. 144