CH6501 Instrumental Methods Of Analysis Chemical 2015-

Engineering St.
16 Joseph’s College of Engineer

INSTRUMENTAL METHODS OF ANALYSIS

UNIT-I

PART-A (Questions & Answers)

1. Discuss instrumental method of analysis.

Instrumental method is a technique based on instrument which convert chemical information to a
form that is more observable. It plays an important role in the production and evaluation of new
products and in the protection of consumers and the environment .
2. What is a read out device?
It is a transducer that converts information from an electrical domain to a domain that is
nderstandable by a human observer.
3. What are the four basic functions of instrumental analysis?
The four basic function of instrumental method of analysis are
1) Generation of a signal 2) Signal transduction 3) amplification of the transformed signal and
4) Presentation of signal.
4. What are the basic functions of Instrumentation?
Instrument may be regarded as a communication device which is accomplished by several steps
such as
1.Generation of a signal 2. Transformation of a signal to one of a different nature
3.Amplification of a transformed signal 4.Presentation of the signal as a displacement on a scale
or on the chart of the recorder.
5. Classify the instrumental techniques.
Most instrumental techniques are divided into three principal areas.
1.Spectroscopy, 2. electrochemistry, and 3.chromatography.
6. Define instrumental method of analysis.
This is a newer methods use for separating and deterring chemical species.
Example: chromatography and electrophoretic techniques used to replace distillation, extraction and
precipitation for the separation of components of complex mixtures prior to their qualitative or quantitative
determination.
7. What is the basis of instrumental methods?
Instrumental methods are based on the theory of relations between the content and the
corresponding physico-chemical and physical properties of the chemical system being analyzed.
8. Classify the sources of noise in instrumental analysis.
i. Chemical noise
ii. Instrumental noise
 Thermal noise or Johnson noise
 Shot noise
 Flicker noise
 Environmental noise.
9. How a thermal noise is caused?
It is caused by the thermal agitation of electrons or other charge carriers in resistors, capacitors,
radiation transducers, electrochemical cells, and other resistive elements in an instrument.
10. When a shot noise is encountered?
It is encountered wherever electrons or other charged particles cross a junction.
11. What is flicker noise?
It is characterized as having a magnitude that is inversely proportional to the frequency of the
signal being observed.
St.Joseph’S College Of Engineering ISO9001:200
8
12. List out the read out devices available.
i. Oscilloscopes
ii. Cathode-ray tubes
iii. Horizontal and vertical control plates.
13. Define sensitivity.
It is a measure of its ability to discriminate between small differences in analytic concentration.
14. What are the factors that limit sensitivity?
i.The slope of the calibration curve ii. The reproducibility or precision of the measuring device.
15. What is the relation between wavelength and energy of electromagnetic radiation?
(May/June 2012)
c =  E = h E = (hc)/  E 1/ 
16. What type of noise can be reduced by hardware techniques? (May/June 2012)
Environmental Noise, flicker noise, noise in transducer.
17. Distinguish between sensitivity and detection limit. (May/June 2012,2014)
Sensitivity: It is a measure of its ability to discriminate between small differences in
analyticconcentration.
Detection limit: Detection Limit (Limit of detection, LOD): The minimum concentration
ofanalytic that can be detected with a specific method at a known confidence level.
18. Define signal to noise ratio. (May/June 2013)
S/N ratio is defined as the ratio of average amplitude of signal to the average amplitude of the noise.
S/N = Avg. amplitude of signal / Avg. amplitude of noise 19. Give the
sources of:IR radiation -Nernst glower and Globar widely used,
Nichrome wire, A tungsten filament lamp for near IR.
UV-radiation -Hydrogen gas lamps and deuterium lamps
Visible radiation -Incandescent tungsten filament lamp.
20. Sort out the ideal requirements of source.
a. It should provide continuous radiation.
b. It should be stable
c. It must generate beam with sufficient power for ready detection and measurement.
21. Arrange the different types of electromagnet
They are –cosmic rays < r-rays x-rays < UV rays < visible light < infrared rays < microwave and
< radio wave
22. What is electromagnetic radiation?
Electromagnetic radiation is a form of energy that is transmitted through space at a enormous velocity.
23. Name the materials of which sample containers are made?
Quartz or fused silica -in UV region below 350nm Silicate glasses –350 –2000nm.
Plastic containers in visible regions.
24. Name the two filters employed in wavelength selection?
Interference filters and Absorption filters.
25. Define monochromator.
They are the units which are used to separate a polychromatic radiation into a monochromatic form.
26. List out the components of monochromators.
An entrance slit-a collimating lens-a prism-a focusing element-an exit slit
27. Explain about crystal monochromator.
A crystal monochromator is made up of a suitable crystalline materials positioned in the x-rays beam and
satisfies the Bragg’s equation.
28. State the ideal properties of a transducer.
High sensitivity-a high signal-to-noise ratio,and a constant response over considerable range of wavelengths.
In addition it would exhibit a fast response time and a zero output signal in the absence of illumination.
29. List out the types of radiation transducers.
Two general types of transducers are: one responds to photons, the other to heat.
30. List out the types of photon transducers.
Photovoltaic cells -in which the radiant energy generates a current at the interface of a semiconductor layer
and a metal.Phototubes -in which radiation causes emission of electrons from a photosensitive solid surface.
Photomultiplier tubes -which contain a photo emissive surface as well as several additional surfaces that emit
a cascade of electrons when struck by electrons from photosensitive area. Photoconductivity transducers -in
which absorption of radiation b a semiconductor produces electrons and holes.Silicon photodiodes –in which
photons increase the conductance across a reversed biased pn junction.
31. Why is thermal noise called as White noise? (May/June 2014)
Because thermal noise is independent of absolute frequency.
PART B
1. What is meant by instrumental noise? What are the types of noise? Explain each with example. (May/June
2013)
2. Discuss about signal to noise ratio and the sources of noise in instrumental analysis.
3. Describe the Software techniques for Signal to noise enhancement. (May/June 2012)
4. Explain in detail the Hardware techniques available for S/N ratio enhancement.
5. Explain about wavelength selectors. (May/June 2012 & 13)
6. Describe the principle, working methodology of Fourier transform measurements.
7. Explain the types of optical instruments. (May/June 2012)
8. Describe the principle, working methodology of Fourier transform measurements.
9. Explain the general principle and design of optical methods.
10. Explain the terms: reflection, refraction, diffraction and scattering.
11. Discuss the radiation transducers in detail.
UNIT 2
PART A
1. Explain Beers Law.(May/June 2012).
Beer's law states that the absorbance is directly proportional to the concentration of a solution. If you plot
absorbance versus concentration, the resulting graph yields a straight line.
2. Explain the term chromophore and give two examples.(May/June 2012)
A chromophore is the part of a molecule responsible for its color. The color arises when a molecule
absorbs certain wavelengths of visible light and transmits or reflects others. The chromophore is a region in
the molecule where the energy difference between two different molecular orbitals falls within the range of
the visible spectrum.Examples: Lycopene, Beta carotene, azo dyes.
3. What is Lambert’s(May/June2014) law?
When a beam of light is allowed to pass through a transparent medium, the rate of decrease of intensity(I)
with the thickness(t) of medium is detect proportional to the intensity
-dI / dt = KI or It= I0e –kt
4. What is absorbance?
The absorbance(A) is the logarithm to the base of the reciprocal of the transmittance.
A= log(1/ T) = -log T or log I0 / It
5. What is absorptivity, Explain?
Absorptivity (a) is the ratio of the absorbance to the product of the concentration and length of
optical path. It is a constant characteristic of ( a= A / bc) substance and wavelength. The alternate
of this term is extinction coefficient or absorbance index.
6. What are the reason for deviation from Beer
Deviation from the Beer’s law aree ther reported the as resultant curve is concave upwards or concave
downwards. The factors involved in deviation from Beer’s law may be chemical, instrumental
7. Define colorimeter.
Any instrument used for measuring absorption in the visible region is generally
called colorimeter.
8. Define spectrophotometer.
The instrument which measures the ratio or a function of the two, of the radiant power of two
electromagnetic beam over a large wavelength region.
9. Define monochromators.
A monochromators used to isolates band of interest of wavelengths. It allows the light of the
required wavelength to pass through but absorb the light of other wavelengths. It contains
entrance slit, dispensing elements and exit slit.
10. What is Detector and what are the detectors used in visible spectroscopy?
Detector is used for measuring the radiant energy transmitted through the sample.
There are three types of photo devices used 1) photovoltaic cell 2) phototube and
Photomultiplier tubes.
11. What is meant of single and double beam spectrophotometer?
Single beam have only one light path. Involve three controls: wavelength, zero adjustment and
100 per cent adjustment. The double-beam design provides two equivalent paths for radiation,
both originating with the same source. One of these beams passes through the sample and other
through reference. The two beams are measured separately, ether by duplicate detector or rapidly
alternating use of the same detector.
12. What are the application of IR spectroscopy?
To estimation of organic compounds, inorganic compounds, geometrical isomerism, presence of
water in the samples, shape of symmetry of a molecules, determination of purity etc.
13. Discuss about the sources of AA spectroscopy.
The most successful line spectra source for AA is the hollow-cathode lamp.
14. What are the applications AA?
AA is useful in the determination of a large number of metals ,specially at trace levels. 2) It is
widely used in such field as water and pharmaceutical analysis and in metallurgy.
15. Mention the basic components of instruments that measure transmittance
or absorbance.
1. A stable light source
2. Monochromator
3. Sample containers for sample and solvent
4. A radiation detector
5. A signal indicator.
16. State the advantages of spectroscopy.
1. More rapid and less time consuming
2. Gives more information.
3. Requires small amount of the compound to be anlysed
4. Precise and reliable
5. More selective and sensitive
6. Continuous operation is often possible.
17. Explain molecular spectroscopy.
This is deals with the interaction of electromagnetic radiation with molecules. The results in
transition between rotational and vibrational energy levels in addition to electronic transition.
Molecular spectra extend from the visible through infrared into the microwave region.
18. Define transmittance.
It is the ratio of the radiant power transmitted by the sample (It) to the radiant power incident on
the sample (I0), both being measured at the same spectral position and with the same slit width.
This transmittance T is defined by It/ I0 .
19. Discuss atomic absorption.
This is most powerful technique for the quantitative determination of trace metals in liquids. e.g.
total sodium content of a water. The sample should be gaseous state and volatilization of liquids
or solid followed by the dissociation of molecules to give free atoms.
20. What are amphiprotic compounds? Give examples.
Can act as both acid or base. example: amino acids, water, proteins.
21. Proportionality: how it is used in the determination of unknown concentration?
(May/June 2013)
Absorbance Varies linearly with the change i law).
22. The absorptivity of a compound is 1.5M -1 -1
cm . What is the concentration of solution of
this compound if 2cm sample has an absorbance of 1.20? (May/June 2013)
A = abc -1 -1
Where, a= 1.5M B=1.2cm; A=1.2 ; C=? Answer:C=0.4
cm ;
23. What is interference?
Interference are confined mainly to phenomena that affect the number of atoms in the flame
which are given as –spectral interference-caused by overlapping of any radiation of the test
elements to be estimated, chemical interference-due to presence of chemicals, it may be cationic
or anionic etc.
PART B
1. Discuss about the Jablonski’s Diagram.
2. Explain the important components of Infrared spectroscopy with diagram. (May/June 2013)
3. Explain about various componenets of UV spectroscopy. (May/June 2012)
4. Describe how IR is useful in analytical spectroscopy as well as in the other instrumentations
relevant to biological research.
5. Explain the theory, instrumentation and applications of Raman spectroscopy. (May/June 2014)
6. Discuss the Biological applications and uses of Raman spectroscopy.
7. Draw and explain the block diagram of an infrared spectrophotometer. (May/June 2012)
8. Give an account on sampling of solids, liquids and gases for IR analysis.
9. What are the advantages of raman spectroscopy over infrared spectroscopy. (May/June 2012)
10. Explain the deviations in detail on Beer’s law.
11. Differentiate stokes from antistokes. Explain the principle and procedure involved in raman
spectroscopy. (May/June 2013)
12. (i) How will you calculate transmittance when absorption is provided?
(ii) Explain the significant features of UV and visible spectrophotometer. (May/June 2013)
UNIT 3
PART A
1.What is NMR spectroscopy?
Is one of the most powerful tool, based on the measurement of absorption of electromagnetic radiation in
the radio-frequency region of roughly 4 to 900 MHz.
2.Compare NMR with UV, Visible and IR absorption spectroscopy.
In contrast to UV, Vis and IR absorption, nuclei of atoms rather than outer electrons are involved in the
absorption process.
3.What are the uses of NMR spectroscopy?
A powerful tool available to chemists and biochemists for elucidating the structure of chemical species. The
technique is also useful for the quantitative determination of absorbing species.
4.List the types of NMR spectroscopy.
Two general types of spectrometers are currently in use, continuous-wave(CW) and pulsed or Fourier-
Transform(FT-NMR).
5.What are the various types of NMR spectra?
Wide line spectra, high resolution spectra.
6.List the factors that decide the type of NMR spectra?
Kind of instrument used –type of nucleus involved –the physical state of the sample –the environment of
the analyte nucleus and the purpose of the data collection.
7.Define wide line spectra of NMR.
Wide line spectra are those in which the bandwidth of the source of the lines is large enough that the fine
structure due to chemical environment is obscured.
8.List the uses of wide line NMR spectra.
Are useful for the quantitative determination of isotopes and for studies of the physical environment
of the absorbing species.
9.Define high-resolution spectra.
Most NMR spectra are high resolution and are collected by instruments capable of differentiating between very
small frequency differences of 0.01 ppm or less.
10. What are the two types of relaxation processes important in NMR spectroscopy?
Spin-lattice or longitudinal relaxation and spin-spin or transverse relaxation.
11. Define relaxation time.
Is the measure of the average life time of the nuclei in the higher-energy state.
12. What is meant by free induction decay?
In Fourier Transform NMR, free induction decay (FID) is the observable NMR signal generated by non-
equilibrium nuclear spin magnetization precessing about the magnetic field(conventionally along z).
13. What is a NMR spectrum?
The NMR spectrum is a plot of the intensity of NMR signals Vs Magnetic Field (Frequency) in reference to
TMS.
14. List the components of NMR instrument.
Sample holder, Permanent magnet, magnetic coils, sweep generator, radio frequency transmitter and radio
frequency receiver and read out systems.
15. Name some solvents used in NMR spectroscopy.
The following solvents are normally used in NMR in which hydrogen is replaced with deuterium.
CCl4- carbon tetrachloride,
CS2- carbon disulfide, D2O- deuterium oxide,
CDCl3 –Deuteriochlorofor& C6D6 - HexaDeutriobenzene.
16. Define Chemical shift.
A chemical shifht is defined as the difference in parts per million (ppm) between the resonance
frequency of the observed proton and tetramethylsilane (TMS) hydrogens.

17. Name the reference compound mostly used in TMS.

TMS (tetramethylsilane) is the most reference compound in NMR, it is set at
18. List the factors affecting chemical shift.
Electronegative groups –magnetic anisotropy–hydrogenbondingof. π electrons
19. What is n+1 rule?
The multiplicity of signal is calculated by using n+1 rule. This is one of the rule to predict the
splitting of proton signals. This is considered by the nearby hydrogen nuclei. Therefore, n =
number of protons in the nearby nuclei.
20. Define spin-spin coupling (splitting).
The interaction between the spins of neighboring nuclei in a molecule may cause the splitting of
NMr spectrum. This is known as spin-spin coupling or splitting. The splitting pattern is relted to
the number of equivalent H-atom at the nearby nuclei.
21. List the rules for spin-spin coupling.
 Chemically equivalent protons do not show spin-spin coupling.
 Only nonequivalent protons couple.
 Protons on adjacent carbons normally will couple.
 Protons separated by four or more bonds will not couple.
22. Define coupling constant.
The distance between the peaks in a given multiplet is a measure of the splitting effect known as
the coupling constant. It is denoted by the symbol J, Expressed in Hz. Coupling
1
constants are the
measure of the effectiveness of spin-spin coupling and very useful in H NMR of complex
structures.
23. Define NOE.
NOE: Nuclear Overhauser Effect, caused by dipolar coupling between nuclei. The local field at
one nucleus is affected by the presence of another nucleus. The result is a mutual modulation of
resonance frequencies. The intensity of the interaction is a function of the distance between the
nuclei according to the following equation :

24. Give the general applications of NMR spectroscopy.


NMR is used in biology to study the biofluids, cells, per fused organs and
biomacromolecules such as Nucleic acids (DNA, RNA), carbohydrates, proteins and
peptides. And also labeling studies in biochemistry.

NMR is used in physics and physical chemistry to study high pressure diffusion, liquid
crystals, liquid crystal solutions, membranes and rigid solids.

NMR is used in food science.

NMR is used in pharmaceutical science to study pharmaceuticals and drug metabolism.

NMR is used in chemistry to determine the enantiomeric purity, elucidate chemical structure of organic and
inorganic compounds1and macromolecules –ligand interaction
25. List the applications of H NMR spectroscopy.
1
H NMR mainly used for structure elucidation.To examine hydrogen bonding and acidity in polymers and
rubbers. To study about proteins and peptides.
26. Give the applications of NMR in medicine.
MRI is the specialist application of multi-dimensional fourier transformation NMR. Anatomical imaging-
measuring physiological gunctions-flow measurements and angiography-tissue perfusion studies-tumors.
26. What is shielding in NMR?
When the magnetic moment of an atom blocks the full induced magnetic field from surrounding nuclei.
27. Define mass spectroscopy.
Is one of the primary spectroscopic methods for molecular analysis available to organic chemist. It is a
microanalytical technique requiring only a few nanomoles of the sample to obtain characteristic information
pertaining to the structure and molecular weight of the analyte.
28. Give the basic principle involved in mass spectroscopy.
In this technique, molecules are bombarded with a beam of energetic electrons. The molecules are ionized and
broken up into many fragments some of which are positive ions. Each kind of ions has a particular ratio of mass
to charge. i.e. m/e ratio (value). For most ions, the charge is one and thus, m/e ratio is simply the molecular
mass of the ion.
29. State Stevensons rule.
When an ion fragments, the positive charge will remain on the fragment of lowest ionization potential.
30. List the factors influencing fragmentation process.
 Bombardment energies
 functional groups
 Thermal decomposition.
31. Define EPR spectroscopy.
Is a technique for studying materials with unpaired electrons.
PART B
1. When does nuclear magnetic resonance occur? Explain the working of NMR spectrometer with a
schematic diagram. 1 13
2. Write the applications of H NMR and C NMR spectroscopy in detail.
3. State the basic principles of mass spectroscopy. Write about different types of ions produces in a mass
spectrometer.
4. What are the general rules of fragmentation pattern in molecules in mass spectroscopy?
5. Explain in detail about the EPR spectroscopy with its principle and instrumentation technique.
6. Write the applications of Mass spectroscopy with suitable examples.
7. Explain in detail the theory of NMR? Comment on NMR spectra in general.
8. Describe in detail the environmental effects on NMR spectra.
9. Elaborate the ionization techniques followed in mass spectroscopy.
10. Define g value. How will you calculate it? Write notes on spectral parameters involved in EPR
spectroscopy.
UNIT 4
PART A
1. What is chromatography?
It is a broad range of physical methods used to separate and or to analyze complex mixtures.
The components to be separated are distributed between two phases: a stationary phase bed and a
mobile phase which percolates through the stationary bed.
2. What is a packed bed and open tubular column?
PTC: it is comprised of a stationary phase which is granular form and packed onto the column as a
homogeneous bed. The stationary phase completely fills the column.
OTC: An open tubular column’s stationary phase is a thin film or layer on the column wall. There is a passage
way through the center of the column
3. What are mobile and stationary phases?
The mobile phase is comprised of a solvent into which the sample is injected. The solvent and
sample flow through the column together; thus the mobile phase is often referred to as the carrier
fluid. The stationary phase is the material in the column for which the components to be eparated
have varying affinities. The materials which comprise the mobile and stationary phases vary
depending on the general type of chromatographic process being performed.
4. What are types of chromatography?
 Gas chromatography .
 Liquid chromatography
 Ion exchange chromatography
 Affinity chromatography
5. What is an adsorption chromatography?
Adsorption chromatography is probably one of the oldest types of chromatography around. It
utilizes a mobile liquid or gaseous phase that is adsorbed onto the surface of a stationary solid
phase. The equilibrium between the mobile and stationary phase accounts for the separation of
different solutes.
6. What is partition chromatography?
This form of chromatography is based on a thin film formed on the surface of a solid support by
a liquid stationary phase. Solute equilibrates between the mobile phase and the stationary liquid.
7. What is an Ion exchange chromatography?
In this type of chromatography, the use of a resin (the stationary solid phase) is used to
covalently attach anions or cations onto it. Solute ions of the opposite charge in the mobile liquid
phase are attached to the resin by electrostatic forces.
8. What is molecular exclusion chromatography?
Also known as gel permeation or gel filtration, this type of chromatography lacks an attractive
interaction between the stationary phase and solute. The liquid or gaseous phase passes through a
porous gel which separates the molecules according to it size.
9. Write down the basic operations in a chromatography system?
1. Feed injection
2. Separation in the column
3. Elution from the column
4. Detection
10. List out the application of size exclusion chromatography.
 Fractionation
 Separation of monomers from dimmers and higher aggregates.
 Estimation of molecular weight.
 Desalting
 Determination of equilibrium constants.
 Determination of molecular weight distribution of polymers
11. Define retention time.
Time taken by the solute to reach the detector from the moment of its injection into the column and
determined by measuring the distance between the sample injection point to the apex on the on-line
chromatogram. Denoted as tR
12. List out the factors affecting retention time.
 Nature of the stationary phase.
 Composition of the mobile phase.
 Column dimensions ( length and dia)
 Mobile phase flow rate (F).
13. Define retention volume.
VR defined as the volume of the mobile pohase required to transport a solute from the point of its injection into
the column and its passage through the column to the detector.
14. How does chromatographic development may be carried out?
Chromatographic development may be carried out by
 Elution analysis
 Gradient elution
 Frontal analysis
 Displacement analysis
15. List out few absorbent used.
Silica gel, aluminium oxide, calcium carbonate, magnesium carbonate, zinc carbonate, magnesium oxide and
cellulose.
16. What in the main function of binder?
To affect the chromatographic behavior of the thin layer by exhibiting adsorption properties.
17. Give examples for binders.
Binders such as plaster of paris, starch and carboxy methylcellulose are added to stationary phase.
18. List out the stationary phases used in HPLC?
Alumina, silicagel, polyamide. If molecular weight of component is larged on liquid stationary phases such as
amine, nitrile, octyl and octadecyl are used.
19. List out the detectors used in HPLC.
1. UV absorbance photometric detectors
2. Fluorescence detector
3. Refractive index detector
4. Electrochemical detector.
20. What are pumps?
They are used to pass mobile phase through column at high pressure and at a control flow rate.
There are two types 1. Constant pressure pump 2. Constant flow pump.
21. List out characteristics of pumps?
 Interior of pump should not be corroded by solvents
 A range of flow rates should be available
 Pulseless
 Easy to change from one mobile phase to another.
22. Gas solid chromatography is quite limited in its applications.
This is due to the following important reasons.
a. Because of the tailing caused by non-linear adsorption isotherm.
b. Partly because of the difficulty in reproducing surface conditions, and partly because of
excessive retention ofreactive gases which reduces the available area.
c. Surface catalysts may also play a restricting role.
23. List out the advantages of GC.
 Strong precision and accuracy
 Completed in a short time
 Sensitivity is high
 Cost low
 Wide range of applications.
24. Name the carrier gases used in GC?
Hydrogen,Helium,Nitrogen,Air are the carrier gases that are used in GC.
25. What characteristics are desirable for the carrier gas? (May/June 2012)
. Inert & Cheap/easily available ; Low risk of fire explosion ; High purity; Better column performance; should
be suitable for detector employed
26. What is the principle of ion exchange chromatography?
Ion exchange chromatography is based on the exchange of ions between solid-ion exchangers, and
substances in a solution with which these solids are brought into contact.
27. What are cation exchangers?
Cation exchangers are sorbents capable of cation exchange. They incorporate ionic groups of different
acidity, such as R-So3H, R-COOH, and R-OH, in which the hydrogen can be replaced by cations.
28. What are anion exchangers?
The anion exchangers are sorbents capable of anion exchange. They contain basic ionic groups capable
of exchanging their anions.
29. Name the types of stationary phases in ion exchange chromatography.
The four types are:
1. Pellicular with ion-exchange film
2. Superficially porous resin coated with exchanger beads
3. Macrorecticular resins bead
4. Surface sulfonated and bonded electrostatically with anion exchanger.
30. What is capillary electrophoresis?
Involves electrophoresis in very narrow tubes (50µm-300µm).used to separate biological molecules
incliding amino acids,peptides,DNA fragments.
31. Name the two methods of sample injection in capillary electrophoresis.
Two methods of sample intake: High voltage injection and pressure injection.
32. What is SFC?
It is Super critical Fluid chromatography: a hybrid of gas and liquid chromatography that combines some
of the best features of each.
33. What is meant by Rf value?(May/June 2012)
It is the retention factor and the ratio of the distance travelled by the solute to the solvent.
34. What is the principle used in size exclusion chromatography? (May/June 2013) Size-exclusion
chromatography (SEC) is a chromatographic methodin which molecules insolution are separated by their
size, and in some cases molecular weight.
35. What is Kovats index? (May/June 2013)

PART B
1. Explain the various chromatographic techniques in detail.
2. State and explain the van deemter equation in detail.
3. Explain the principle and procedure involved in gas chromatography.(May/June 2013)
4. Discuss in detail the principle and working of SFC.
5. Discuss in detail the characteristics and types of pumps used in HPLC.
6. Discuss in detail the types of detectors used in HPLC
7. Discuss the general principle underlying the capillary electrophoresis method for separation of mixture.
(May/June 2012)
8. Explain the different types of capillary electrophoresis.
9. Discuss the principle and applications of Ion exchange chromatography. (May/June 2012)
10. Explain the principle and procedure involved in IEC. (May/June 2013)
11. Explain the significant features of stationary and mobile phase used in Gas chromatography with its
advantages for the separation of molecules. (May/June 2014)
Unit 5
Part A
1. Define electrochemistry.
The area chemistry that deals with the interconversion of electrical energy and chemical energy.
2. Define electrochemical process.
Are redox reactions in which the energy released by a spontaneous reaction is converted to electricity or in
which electricity is used to drive a non-spontaneous chemical reaction.
3. What is a Galvanic or Voltaic cell?
Is an electrochemical cell that produces electricity as a result of spontaneous chemical change.
4. What is an electrochemical cell?
An arrangement which consists of electrodes dipped into an electrolyte in which chemical reaction
uses/generates electric current.
5. Definepotentiometry technique.
In potentiometry, the potential of an elcterochemical cell is measured under static conditions, because no
current flows while measuring a solution potential, its composition remains unchanged.
o
6. Write Nernst equation.
Ecell = E –(RT/nF) lnQ
Cell
7. What is a salt bridge in an electrochemical cell?
The two electrodes immersed in an electrolyte solution of EC cell, are joined by a salt bridge, which consists of
a tube filled with solution that is saturated with potassium chloride or, sometimes with a different electrolyte.
8. Define an anode and cathode of an EC cell.
The cathode of an EC cell is the electrode at which reduction occurs, and anode is the electrode where oxidation
takes place.
9. Define electrode potential.
An electrode potential is defined as the potential of a cell in which the electrode under investigation is the right
hand electrode and the SHE is the left hand electrode.
10. State Faradays’ law.
The amount of chemical reaction that occurs at an electrode id proportional to the current, called the Faradaic
current.
11. What is Voltammetry?
Voltammetry comprises a group of electrochemical methods in which information about the analyte is obtained
by measuring as a function of applied potential under conditions that promote polarization of an indicator, or
working electrode.
12. List the names of the three-electrode cell of a voltammeter.
Working electrode (WE), Reference electrode (RE) & a counter electrode (CE).
13. State the applications of Voltammetry.
Voltammetry is applicable to the analysis of many inorganic substances and for the study
and determination of organic compounds. Voltammetry is widely used by inorganic, physical
and biological chemists for non-analytical purposes.
14. How does the AFM work?
AFM provides a 3D profile of the surface on a nanoscale, by measuring forces between a sharp
probe (<10 nm) and surface at very short distance (0.2-10 nm probe-sample separation). The
probe is supported on a flexible cantilever. records the small force between the probe and the surface.
15. State Hookes’ Law.
F = -kX
Where, F = Force; K = Spring constant; X = cantilever deflection
16. What are probes made of in AFM?
Probes are typically made from Si3N4 or Si.
17. List the 3 primary imaging modes in AFM.
There are 3 primary imaging modes in AFM:
Contact AFM :< 0.5 nm probe-surface separation
Intermittent contact (tapping mode AFM): 0.5-2 nm probe-surface separation
Non-contact AFM :0.1-10 nm probe-surface separation
18. What are the limitations of AFM?
There are limitations in achieving atomic resolution. The physical probe used in AFM imaging is
not ideally sharp. As a consequence, an AFM image does not reflect the true sample topography,
but rather represents the interaction of the probe with the sample surface. This is called tip
convolution.
19. What are Force Curves?
Force curves measure the amount of force felt by the cantilever as the probe tip is brought close
to - and even indented into - a sample surface and then pulled away. In a force curve analysis the
probe is repeatedly brought towards the surface and then retracted.
20. What are the uses of Force curves?
Force curve analyses can be used to determine chemical and mechanical properties such as
adhesion, elasticity, hardness and rupture bond lengths.
21. What is STM?
A scanning tunneling microscope (STM) is an instrument for imaging surfaces at the atomic
level.
Part B
1. Describe in detail about scanning electron microscopes.
2. Explain with a neat diagram the principle and working of AFM.
3. Explain with a neat diagram the principle and working of STM.
4. Write in detail about potentiometry and its instrumentation.
5. Define Voltammetry? Write notes on Pulsed and Cyclic Voltammetry.
6. With a neat sketch explain in detail about electrochemical cells and its working procedure.
7. Explain the applications of Voltammetry and potentiometry in detail.
8. Describe in detail about Voltammetric instrumentation with a neat sketch.
9. Elaborate in detail about ion selective and molecular selective electrodes.
10. Highlight the three-electrodes used in a cell of a voltammeter with a schematic diagram
explain their uses.