EI6501 Analytical instruments Dept.

of EIE and ICE 2016-2017

EI6501-ANALYTICAL INSTRUMENTS
UNIT I COLORIMETRY AND SPECTROPHOTOMETRY

Part A
1. Difference between single beam and double beam instrument? (Dec 2014)
Advantages of Single Beam Systems
Single beam instruments are less expensive
High energy throughput due to non-splitting of source beam results in high sensitivity of detection
Disadvantages
Instability due to lack of compensation for disturbances like electronic circuit fluctuations, voltage
fluctuations, mechanical component’s instability or drift in energy of light sources. Such drifts
result in abnormal fluctuations in the results.
Advantages of Double Beam Systems
Modern improvements in optics permit high level of automation and offer the same or even better
level of detection as compared to earlier single beam systems. Instability factors due to lamp drift,
stray light, voltage fluctuations do not affect the measurement in real-time.
Little or no lamp warm up time is required. This not only improves throughput of results but also
conserves lamp life
Disadvantages
The cost factor is more than offset by the advantages offered by modern double beam systems and
therefore these have become the preferred choice
2. What is absorption spectrum? (Dec 2014)
The electromagnetic spectrum, broken by a specific pattern of dark lines or bands, observed when
radiation traverses a particularabsorbing medium and through a spectroscope. The absorption
pattern of an element is unique and can be used to identify thesubstance of the medium.
3. State the limitations of absorption filters. (May 2014)
Absorption filters are made primarily from colored filter glass or synthetic gels, and represent the
largest class and most widely used type of filters for applications that do not require a precise
definition of transmitted wavelengths. The quality of glass or polymer used in the manufacture of
filters is important, and should be of optical grade and provide uniformity of density and color
over the entire surface of the filter. Filter glass or plastic attenuates light only through absorption,
so the spectral performance is dependent upon the thickness and optical density of the filter
material. Increasing the thickness will produce a corresponding increase in the blocking level of
unwanted wavelengths, but also reduces the peak in-band transmission, causing falloff at the
ends of absorption bands.
4. Why sensitive detector is required for spectrophotometer? (May 2014)
PDA detectors are more traditional linear detectors which consist of a set of individual
photodiodes that are arranged in a linear fashion.The advantage of PDA detectors is that the well
depth is much higher than the well depth of a CCD(Charge Coupled Devices); a typical PDA
detector well depth is ~156,000,000e- as compared to ~65,000e- for a standard CCD. The larger
well depth of PDA detectors causes them to have a very large dynamic range ~50,000:1 as well as
an extremely linear response. These properties make PDAs ideal for applications where it is
necessary to detect small changes in large signals, such as LED monitoring.
5. What is Spectrophotometer?
Spectrophotometer are dispersive analyzers where a prism is used to separate the spectral
components of the UV spectrum.
6. Name the main components of UV analyzer.
The main components of UV analyzer are Source, Mono Chromator, Sample Cell, Detector, and
Readout Device.
7. Give some example of radiation source used in UV region.
Cadmium, Mercury and Zinc Vapour sources that are used in the UV region are emission
line sources.
8. Name two sources used in NIR region.
i. Tungsten filaments ii. Quartzhalide lamps
9. What is the use of O-rings?
Sealing of cell is accomplished with O-ring gaskets.Viton, Ethylene-propylene and Kalrez are
commonly used.

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10. Name few detectors used in UV region.
i. Silicon photo diode ii. Photo Diode array
11. Classify UV analyzer based on design.
i. Single-beam analyzer
ii. Split-beam analyzer
iii. Dual beam- Single detector analyzer
iv. Dual beam- Dual detector analyzer
v. Flicker Photometer
vi. Photodiode Analyzer
vii. Retro reflector analyzer.
12. Define path length.
The distance between the windows in the sample cell defines the path length.
13. What is the purpose of sample cell?
The purpose of sample cell is to contain a representative sample from the process
stream.
14. Write the principle used in scanning spectrophotometer.
Scanning spectrophotometer are dispersive devices that normally utilize diffraction
gratings to scan across a spectral regions. Scanning devices can be used for multiple
component applications.
15. Give some applications of Photo diode array.
i. Analysis of Hydrogen sulphide and sulphur dioxide in sulphur recovery
ii. Determination of octane number are two examples of PDA applications
16. Give some applications of scanning spectrophotometer.
i. Measurement of multi component solvent mixture
ii.Determination of octane number for gasoline samples
17. Write the applications of atomic absorption Spectrophotometry.
Mercury is conveniently analyzed by atomic absorption technique because the elemental vapour
exists in atomic form under normal ambient conditions.
18. Write the features of single Beam configuration of IR Spectrophotometer.
i. Less expensive. But power variations or temperature changes can cause zero and span
drift and necessitates frequent re-zeroing. ii. Drift caused by dirt accumulation on the
windows is not a problem as the instrument is automatically re-zeroed on each revolution
of the chopper wheel.
19. What is FTIR spectrophotometer?
FTIR spectrophotometer are dispersive devices that are being used for on-line analysis in
the near infrared region. Instead of separating different wavelengths for measurement, the
complete spectrum is encoded as an interferogram in a few seconds of measurement time,
and the spectrum computed by fast Fourier transform.
20. What are the basic components of Infra-red Spectrometer?
i.Source of radiation, ii.Monochromator for dispersing the radiation
iii.Detector which registers the residual intensity after selective absorption by the sample.
21. Write the detector used in Infrared radiation.
i. Thermal detector ii. Photo conductive cells
22. Define wave number.
Wave number is defined as the number of wavelengths per-centimeter and it is expressed
as cm-1
23. What are the advantages of double beam spectrophotometers
a) speed of operation
b) automatic compensation for variation in lamp output
c) solvent absorption at various 8
d) changes in detector sensitivity
e) spectra scan
24. Mention the application of Colorimeter.
Essentially, a colorimeter is a scientific instrument that measures the amount of light passing
through a solution relative to the amount that passes through a sample of pure solvent.
Colorimeters have many applications in the fields of biology and chemistry

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25. What are the applications of flame photometry?
1).Analyze wide variety of materials such as environmental biological fluids, solids, plant
materials and industrial cement, ferrous metals, glasses etc,
2). It is used for determining sodium, potassium, Aluminum, Calcium, and Iron in soil.
26. List the advantages of Fourier transform spectrometer.
1. Signal to noise ratio is high 2. Retrieval of data is possible.3. Information could be obtained
on all frequencies. 4. Processing speed of data is high. 5. High reliability and good sensitivity.
27. What are the disadvantages of Fourier transform spectrometer?
1. Cost is the major problem. 2. Maintenance of the instrument.
28. What is total internal reflection in spectrometry? (May 2013)
is a sampling technique used in conjunction with infrared spectroscopy which enables samples to
be examined directly in the solid or liquid state without further preparation.
29. State Beer-Lambert law. (May 2013, May 2015)
The Beer-Lambert law is the fundamental law for quantitative analysis by absorption
spectroscopy. This law states A= abc
where A = absorbance, a = Molar absorptivity, b = Sample path length,
c = Concentration of absorbing species
30. Name the types of detectors used in IR spectrometry. (Nov 2013)
i.Bolometers ii.thermocouples iii.thermistors iv.golay cell v.pyroelectric transducer
vi.photoconductivity cell.
31. Write the wavelength range of IR radiation ( May 2015)
700 nm – 1 mm
32. What are the two basic requirements of radiation sources in absorption photometry ( Dec
2015)
The radiation source must emit the line spectrum of that element. It should provide high
sensitivity

33. Define interference filters (Dec 2015)

An interference filter or dichroic filter is an optical filter that reflects one or more spectral bands
or lines and transmits others, while maintaining a nearly zero coefficient of absorption for all
wavelengths of interest

Unit-I Part B
1. Explain FTIR spectrophotometers in detail with necessary diagram. (Dec 2014, Dec 2015)
2. Write short notes on: (Dec 2014)
(i) Attenuated total reflectance flame photometers (8)
(ii) Atomic absorption spectrophotometers. (8)
3. What are the limitations of visual calorimeter? Explain the working principle of a double beam
calorimeter with a schematic diagram. (16) (May 2014)
4. With a block diagram, explain the operation of flame photometer. List the advantages of flame
photometry. (May 2014 ,May 2015)
5. State and derive Beer’s law from basic principles. Discuss the limitations of it.
6. With a schematic diagram explain the atomic emission spectroscopy.
7. Explain flame emission photometer with its instrumentation.
8. Explain mono-chromators and detectors (Dec 2015)
9. Explain about photo multiplier tube.
10. Explain Fourier transform infra-red spectrometers.
11. Explain different radiation source in absorption spectrophotometry.
12. Explain the working principle of various radiation sources and detectors in IR
Spectrophotometers.
13. With a neat diagram, explain the instrumentation setup of Atomic absorption spectroscopy
(MAY 2013)
14. With a neat sketch, explain the instrumentation setup and working principle of IR spectrometer.
(May 2013)
15. Draw and Explain the schematic diagram of a typical double beam spectrophotometer and write
it advantages over single beam configuration (Nov 2013, May 2015)

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16. What are non-dispersive spectrophotometers? Explain in detail the FTIR spectrometer. Also
specify the advantages of the FTIR spectrophotometer. (Nov 2013)

UNIT II CHROMATOGRAPHY
Part A
1. Define retention time. (Dec 2014, May 2015)
The interval between the instant of injection and the detection of the component is known as
retention time. The time required for each of the components to emerge from sample or mixture is
also called retention time. It is used to identify the component through qualitative analysis.
2. What is chromatography? (Dec 2014, May 2015)
Chromatography is defined as the physical ( is based on the difference in solubility of
substance between a mobile and stationary phase )and chemical method of separation between
various components of a mixture into a pure fractions or bands of each component.
3. Define dead time in chromatograph. ( May 2014)
Dead time is the time required for a molecule of mobile phase to pass through the column.
4. Specify the various types of Chromatographic column. (May 2014)
 Standard column ƒ
 Radial compression column ƒ
 Narrow-bore column ƒ
 Short ,fast column ƒ
 Guard columns and in-line filters.
5. What is Chromatography?
Chromatography describes a physical method of separation that is based on the difference
in solubility ( or adsorption ) of substance between a mobile and stationary phase.
6. Define Chromatogram.
The individual components register a series of signals which appear as successive peaks
above a base line on the recorded curve is called Chromatogram.
7. What are the different components of Gas Chromatography?
The basic parts of a gas chromatograph are
i. carrier gas supply along with pressure regulator and flow monitor ii. Sample injection
system, iii. Chromatographic column iv. Thermal compartment or thermostat v. Detection system,
vi. The strip-chart recorder
8. Name the detectors used in liquid Chromatography.
i. UV-Visible Spectrophotometric detectors ii. Fluorescence Detector iii. Refractive Index
detectors, iv. Adsorption Detector v. Electrical Conductivity detector vi. Thermal Detector
9. Name some source carrier gas used in Gas Chromatography.
Hydrogen, Helium, Nitrogen, Argon and CO2.
10. Write the limitations in FID.
i. Does not respond to inert gas and inorganic compounds
ii. The emerging compound get destroyed in the flame
iii. The response to sample weight has to be separately determined for each component.
11. What are the different components of Liquid Chromatography?
i. A High pressure pump system to force the liquid mobile phase through the column.
ii. A gradient elusion or solvent programmer iii. The sample injection system
iv. The column v. The detection system including display or recording devices.
12. Write the choice of a particular type of detector in Gas Chromatography .
i. Detectors should have high sensitivity , to be sufficient enough to provide an adequate
signal for all components with a small sample.
ii. The response of the detector should be linear over the whole range
iii. The detector should give good reproducibility
iv. Detector should be insensitive to changes in the rate of flow of the carrier gas
13. Write the application of argon Ionization detector.
Responds to most of the organic and Inorganic Compounds.
14. Write the methods used in sample injection system in liquid Chromatography( Dec
2015)
i. Syringe Injection method ii. Injection valve method.
15. What are the factors to be considered when a detector is interfaced with
Liquid Chromatography?
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i. Good sensitivity- to deal with low concentration of typical analyses.
ii. The volume of the detector must be small to avoid additional band broadening due to
extra column., iii. Detector must be able to function in the presence of a large background
signal and be able to null out this signal.
16. State the principle used in refractive Index detectors.
Refractive Index detectors depends on Snell’s law. It is based on refraction, reflection or
interference of light beams.
17. Write the principle of adsorption detector.
This detector depends on the measurement of the evolution of the heat of adsorption and
heat uptake at desorption as the solutes in the effluent stream comes in contact with an
adsorbent.
18. Write the factors affecting Gas flow rate.
The rate of the gas flow depends upon column diameter. The flow rate is generally in the range
10-400ml/ minute. Very low and very high flow rate affect the efficiency adversely.
19. Define dead time and dead volume.
Dead time is the time required for a molecule of mobile phase to pass through the column.
Dead volume Vm is the volume of the mobile phase from the point of injection through the
column to the detector.
20. Write advantages of HPLC over gas chromatography.
i) Gas chromatography is in need of conversion of nonvolatile substances into volatile, such
conversion is not needed in HPLC.
ii)Gas chromatography is not applicable to thermally unstable substances. but liquid
chromatography can be applied to thermally unstable substances.
21. Define thin layer chromatography
A method of separating two or more chemical compounds in a solution through their
differential migrations across a thin layer of adsorbent spread over a glass or plastic plate.
22. What are the applications of HPLC?
1. It is applied in the process of isolation and purification of compounds. The information that is
obtained from this includes identification, quantification and resolution of a compound.
2. Chemical separation can be accomplished using HPLC by utilizing the fact that certain
compounds have different migration rates with respect to the particular column and mobile phase.
The degree of separation is mostly determined by the choice of stationary and mobile phase.
23. What are the applications of gas chromatography?
Gas chromatography is applicable for the analysis of the solute in both qualitatively and
quantitatively.
24. What do you mean by open tubular column?
Capillary column are the open tubular column constructed from fused silica ( a very high purity
glass).The length of the column from 30 to 300m and a diameter of 1mm or less.
25. Name the detectors used in Gas Chromatography.(May 2013)
i. Katharometer or Thermal Conductivity detector ii. Flame Ionisation Detector
iii. Differential flame Ionisation Detector iv. Electron Capture detector
v. Argon Ionisation Detector vi Cross-Section Ionisation Detector
26. What is HPLC? (May 2013)
High Pressure Liquid chromatography. The most widely used analytical separations technique.
Utilizes a liquid mobile phase to separate components of mixture. uses high pressure to push
solvent through the column.
27. What is Pyrolysis? (Nov 2013)
Pyrolysis offers a technique for injection of certain types of materials which are low or
non-volatile. This is a valuable technique for sample injection in rubber, plastics, polymers
and adhesive industries.
28. What are the properties of carrier gas? (Nov 2013)
a) The carrier gas must be chemically inert. That is otherwise it should not react with the sample
or stationary phase.
b) It should be suitable for the detector employed and the type of sample analysed.
c) It should give best column performance consistent with required speed of the analysis.
d) It should be free from the risk of fire.
29. Describe classification of stationary phases ( Dec 2015)
Liquid phase,Solid phase
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Unit-II Part B
1. Explain high pressure chromatographs in detail.(Dec 2014)
2. Explain with sketches the operation of any two detectors used in gas chromatography.(Dec
2014)
3. Give in detail the classification of Chromatography. Briefly explain liquid chromatography.
(May 2014)
4. With block diagram, explain the Gas chromatography. State the factors to be considered in
Carrier Gas supply system.(May 2014)
5. Draw the schematic diagram of a gas chromatography and explain the different parts in Gas –
chromatography.(May 2013), (Nov 2013)
6. Describe a gas liquid chromatography with a schematic diagram. Explain how it works.
7. Give a typical chromatogram. Discuss some applications of gas liquid chromatography.
8. Explain in detail the following detectors used in Gas Chromatography.
a).Thermal conductivity detector b).Flame ionization detector
9. With a neat schematic diagram discuss the separation principle of HPLC. (May 2013)
10. What are the requirements of HPLC pumping system and enumerate the application of HPLC.
11. Give in detail the classification of chromatography. Explain liquid chromatography (Dec 2015)
12. Explain various detectors used in liquid chromatography.
13. Explain about Refractive index detector and electrochemical detector
14. Explain with neat diagram about flame photometric detector, photo ionization detector and
electron capture detector.
15. Draw the general block diagram of HPLC and explain its operation principle. (May 2015, Dec
2015)
16. Explain two types of chromatographic column used in Gas chromatography (May 2015)

UNIT III INDUSTRIAL GAS ANALYSER AND POLLUTION MONITORING

INSTRUMENTS
Part A
1. What is the use of gold films in H2S analyzer? ( Nov 13 ,Dec 2014)
Gold films absorb hydrogen sulfide and register the concentration by a proportional change in
their electrical resistance. It is available in ppb range and is not sensitive to interferences by SO 2,
CO2 or CO.
2. What are the sources of error in oxygen analyzer? (Dec 2014)
i. The filament temperature is affected by changes in the thermal conductivity of the carrier gas,
ii. The cross tube must be horizontal to avoid an error due to gravitational chimney-flow effects.
iii. Hydrocarbons and other combustible gases in the sample stream react on the heated filaments
causes changes in temperature and therefore their resistance, which results in large error.
3. What are the properties of Gas used for the measurement of Quantity? (May 2014)
The properties of Gas used for the measurement of Quantity are pressure, density,
temperature, internal energy, viscosity, heat conductivity, and diffusivity.
4. State the principle of Dust measurement in Thermal power plant. (May 2014)
Photocell is used for the dust measurement which works on “obscuration” principle. The
variation of the obscuration of light source due to smoke and dust in flue gas generates a signal
in the photocell circuit. The variation in the signal which is a measure of dust in the flue gas is
processed further by electronic circuit and displayed in the control unit.
5. Classify gas analyzer based on principle.
i. No interaction of intramolecular energy states, ii. With excitation of intramolecular
energy states, iii.With chemical or electrochemical reaction
6. Explain paramagnetic property .Give some example.
It does not have strong magnetism as permanent magent but it is attracted into a magnetic field.
Ex: O2, NO, N O2
7. Write the drawbacks of CO monitor.
i. Sources must be balanced either electrically or mechanically. ii. Unbalanced chopper causes
failure of chopper motor bearings iii. Difficult to maintain and expensive to replace
8. Define thermal conductivity of a gas.
It is defined as the quantity of heat (calories) transferred in unit time (secs) in a gas between two
surfaces 1 sq.cm in area and 1 cm apart with a temperature difference between the surface 1°C.

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9. Write the advantage of using thermistor in thermal conductivity analyzer.
i. It is sensitive to minute changes in temperature. ii. High negative temperature coefficient
of resistance
10. Write the considerations in industrial process analyzer.
i. Simple to design and easy to maintain, ii. Ability to withstand harsh plant environment
(mechanical shocks, vibration, dust and weather). iii. Decreasing the analyzer sizes
facilitates the installation and reduces the cost. iv. Reliability is important.
11. Write the methods used in electrochemical analyzer.
i. Galvanic method ii. Polographic method iii. conduct metric method
12. Write the methods used for measurement of Nox in Industry.
i. Infrared analysis ii. Ultraviolet Analysis iii. Chemiluminescent Analysis
iv. ElectroChemical Analysis v. Gas Chromatography
13. Write the methods used for measurement of Nox in ambient gas.
i. Coulometric analyzer ii. Calorometric analyzer
14. What are the different types of Hydrogen Sulfide Analyzer?
i. Electrochemical diffusion ii. Solid state or gold film sensors
iii. UV Photometric iv. Gas Chromatography
15. Why thermistors are used in thermal conductivity analyzer as a heat sensing elements?
Thermistors possess the advantage of being extremely sensitive to relatively minute changes in
temperature and have high negative temperature coefficients. The speed of response is also high.

16. What are the applications of thermal conductivity gas analyzer?

a. It is used in the measurement of hydrogen in blast furnace gases
b. In the determination of argon in Oxygen in the process of air decomposition
c. In the determination of sulphur dioxide in roasting gases in the production of sulphuric acid.
17. How is nitrogen-di-oxide prepared by chemiluminescence?
The nitric oxide reacts with ozone to form nitrogen-di-oxide with chemiluminescence .
NO + O3 ----> NO2 + hv (light 0.6- 3μ)
18. What are the advantages of Hydrogen Sulfide analyzer?
i. It do not require pumps or aspirators to pull in the sample
ii. They are unaffected by wind or variations in relative humidity.
19. What are the applications of oxygen analyzer?
i. It is used in the areas of oxygen absorption studies on plants and tissues.
ii. It is used in food processing industries.
iii. It is also used in respiratory studies.
20. Explain the different analysis methods of Nitrogen Oxide.
i. Infrared ii. Ultraviolet iii. Chemiluminescent iv. Colorimetric v. Electrochemical
21. What are the applications of Electrochemical and Infrared sensors?
i. Electrochemical sensors are used for ambient air monitoring
ii.Infrared sensors are used for stack gas concentration
22. Explain the detection methods of Carbon Monoxide Analyzer.
i. Non dispersive method ii. Mercury Vapour
iii. Catalytic Oxidation iv. Electrochemical fuel cell
23. Explain the calibration methods used in NO2 analyzer.
The calibration methods are Dynamic calibration & Static calibration. Dynamic calibration
requires preparation of inert gas containing a known concentration of NO2. This may be
accomplished by gas dilution techniques. Static calibration is carried out with standard solutions
of nitrite.
24. Mention the uses of IR analyzer
1. It is used for single component analysis such as ethylene, CO, acetylene, methane etc,
2. Multiple component for cereal, meat and paper could also be analyzed
25. What is the need of carbon monoxide in flue gas?
The carbon monoxide is colorless, odorless, poisonous gas that has an affinity for hemoglobin,
which is 210 times that of oxygen. By combining with hemoglobin in the blood it inhibits the
delivery of oxygen to the body’s tissues, thereby causing asphyxia or shortness of breath.
26. Write the principle of smoke meter. (Nov 2013)
Smoke meter is based on the principle of absorption / obscuration of light which is indicative of
the quality of smoke. The light beam passes through a smoke cell and onto a silicon photo

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detector which is continuously senses the intensity of the light incident on it and converts it into
a electrical signal which is further processed by precise signal handling circuits.
27. Brief the principle of dust monitor. (May 2013)(Nov 2013)
Dust monitor works on the principle of passing a focused light beam through the duct or
chimney on a photocell and the variations in the signal of the photocell circuit will be a measure
of the variation of the obstruction of the light source dust to the smoke and dust in the gases.
28. What is thermal conductivity? (May 2013)
A measure of the ability of a material to transfer heat. Given two surfaces on either side of a
material with a temperature difference between them, the thermal conductivity is the heat energy
transferred per unit time and per unit surface area, divided by the temperature difference.
29. What is magnetic Wind( May 2015)
A detector has two chambers, each of which has a heating wire element located at the center. A
magnetic field is provided only on the measurement chamber. Once the gas under measurement
is sent to the measurement chamber, oxygen is attracted by the magnetic field and then heated
with the heating wire element. Thus, the magnetization factor decreases and a continuous flow of
gas (magnetic flow) occurs. The magnetic flow cools the heating wire element as its intensity
varies in proportion to the concentration of oxygen. Therefore, the resistance changes during this
process are picked up as unbalanced voltage at the bridge to measure the concentration of
oxygen. This continuous flow of oxgen due to the demagnetization is called magnetic wind.
30. Define ionization (May 2015)
Ionization is the process by which an atom or a molecule acquires a negative or positive charge
by gaining or losing electrons to form ions, often in conjunction with other chemical changes.

Unit-III Part B
1. Draw and explain the measurement of dust and smoke in detail.( Dec 2014, Dec 2015)
2. Write short notes on Air pollution due to (Dec 2014)
a) Carbon monoxide (4)
b) Nitrogen oxide (4)
c) Hydrocarbons (4)
d) Sulphur dioxide (4)
3. Explain the working principle of Paramagnetic Oxygen Analyzer with a functional diagram.
Specify the need of oxygen measurement.(May 2014)
4. With a Schematic Diagram explain the method of measuring Sulphur dioxide SO2 estimation
using conductivity method.(May 2014)
5. With a neat sketch, explain the construction and working principle of parametric oxygen
analyzer. (May 2013)
6. With a block diagram, explain the method of measuring carbon monoxide using Non-dispersive
Infrared Analyzer. (Nov 2013, May 2015)
7. Explain how the NO2 analyzer is used. (May 2013)
8. Explain how the H2S analyzer is used.
9. Explain how the dust and smoke analyzer is used. (May 2013)
10. Explain how the IR analyzer is used.( Dec 2015)
11. With a suitable diagram explain the construction and working principle of thermal conductivity
analyzer. (Nov 2013, Dec 2015)
12. What are the sources of air pollution and explain in detail?
13. What are the type’s gas analyzers? Explain anyone with example.
14. Discuss the method of analysis based on ionization of gases.
15. With the instrumentation setups explain any one method to estimate sulphur-di-oxide present in
air.
16. Explain the photometric method of measuring dust and smoke measurement in thermal power
plant.
17. Why do we need temperature compensation in conductivity measurement? Describe a method of
temperature compensation
18. Draw the schematic diagram of hotwire thermal conductivity analyzer and explain its
operation (May 2015)

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UNIT IV pH METER AND DISSOLVED COMPONENT ANALYZER
Part A
1. Why ammonia gas is added to the sample in sodium analyzer?
The sodium selective glass electrode carries out the measurement in buffered solution above
10PH, where it responds specifically to value of the sample is sodium ion activity. So the PH
must be adjusted to within desired range .The PH value of the sample is maintained in the flow
cell by adding ammonia gas to the sample.
2. Give the characteristics of glass electrodes.
i. Sensitivity is above 95% ii. Fast response iii. Low melting point
iv. Relatively high electrical conductivity v. High horoscopy.
3. Mention the role of buffer solution in pH measurement.
A buffer solution is one which resists changes in pH when small quantities of an acid or an alkali
are added to it.
4. What are the difference between pH electrodes and Ion selective electrodes?
pH Electrode Ion selective electrodes
Hydrogen Electrode Primary ion selective
 Crystalline
 Non Crystalline
Gas Electrode Compound or multiple
membrane
 Gas sensing
 Enzyme Substrate
Calomel Electrode
Combination Electrode

5. What is a pH meter?
It is used to measure pH which is the hydrogen ion concentration in a test solution. It is defined
as the negative logarithm of hydrogen ion concentration.
pH= - log[H+]
6. Give the pH of water, acid, base.
Water pH=7, Acid pH<7, Base pH>7
7. What are the different electrodes used for pH measurement?
Hydrogen electrode, Glass electrode, Calomel electrode, Combination electrode.
8. What is the principle of a pH meter?
The measurement of hydrogen ion concentration in a test solution is made by measuring the
potential developed in an electrochemical cell. The electrochemical Ph cell consists of a
measuring electrode and a reference electrode both immersed in the solution under test. The two
electrodes are connected for measuring the instantaneous emf between the two electrodes. The
measuring electrodes are pH sensitive and the potential is proportional to the pH value of the
solution and the reference electrode always develops a constant electrical potential ,The potential
of the measuring electrode may be written as
E = Eo + 2.306 RT/F log C;
E = Eo – 2.306 RT/F pH
pH= pH value deviation from 7
C = hydrogen ion concentration
9. Define Sampling System.
The key to any continuous analysis is the sample transport system. Figure shows simple method
of continuous sensing used for variable such as pH, conductivity, dissolved oxygen and water
temperature.
10. What is the use of Conductivity Meter?
It measures the ability of the solution to carry electric current (conductivity of an electrolyte). If a
potential is applied to the electrode immersed in the solution, ions are accelerated towards the
electrode.
11. Define Cell constant.
Cell constant is given by Cell constant =L/A where, L= length A =area
Cell constant can be determined by the measuring the value of resistance of a solution of known
specific conductance.
12. Write the methods of measuring pH.
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i. Direct reading type ii. Null detector type
13. Define equivalent conductance.
Conductance =A/pl = K(a/l)
K=1/p = Specific conductance
Equivalent conductance: The ability of indiv9dual ions to conduct current is expressed as
equivalent conductance. It is the conductance of a solution containing 1 gram equivalent of an
electrolyte per cubic cm of a solution. This is represented as “^”
Relationship between “K” and ”^” ^ = 1000 K/C
14. Write the use of sodium analyzer.
i. To determine sodium ion concentration in boiler water
ii.Used for industrial water pollution monitoring
iii.Monitors and carries over detections of condenser leaks and the exhaustion of water treatment
plant cation exchange unit. Ion selective electrode is the most powerful tool for specific analysis.
It is used to determine the specific constituents like cyanide, fluoride, ammonia in a sample.
15. Write the methods of measuring oxygen.
1) Physical: a) Paramagnetic property of oxygen b) Thermal conductivity for quantitative
determination
2) Chemical: a) Potentiometry b) Catalytic combustion
16. Write the principle of silica analyzer.
A silica analyzer works on the calorometric principle. Ammonium molybdate solution (pH=7),
sulphuric acid and a reducing solution are added to a metered volume of a sample through
separate measuring cylinders to eliminate the precipitation of molybdic acid.
17. Define moisture.
It is defined as the amount of water vapour absorbed by a solid or adsorbed by a liquid.
18. Define ionic concentration and ionic activity.
Ionic activity: measures the number of free ions in the solution.
Ionic concentration: measures the free and bonded ions.
19. What is buffer solution?
It may be defined as the solution whose pH remains nearly a constant despite the addition of a
substantial quantity of acid or base. Buffers are employed for the standardization of a pH cell.
20. Write the advantage of direct reading type instruments.
1) simplicity of operation 2) speed of measurement
21. Why are glass electrodes preferred?
Glass electrodes are preferred because of their following characteristics
i. Low melting point ii. High hygroscopicity iii. High electrical conductivity
22. What are the considerations in diagramming a pH meter.
1) Internal resistance of glass electrode is very high.
2) Current should neither be drawn by the ph meter from the solution nor any current should
flow on the electrode which might result in the polarization of the electrode. Such polarized
electrodes give erroneous reading of pH values.
3) Meter should have a provision for compensating the charge in the pH reading due to
temperature change.
23. Write the applications of pH measurement.
i. Tanning industries ii. Chemical industries iii. Distillation plants
24. What are the advantages of hydrogen electrode
1. It is standard reference electrode with which the potentials of electrodes are calculated.
2. The results are highly accurate.3.It gives no salt error 4.The error due to electrical leakage is
negligible.
25. What are called bio-sensors?
A bio-sensor is a device that uses biological material to monitor the presence of various
chemicals in a substance or it can also be defined as it is a device for the detection of an analyze
that combines a biological component with a physiochemical detector component.
26. Define PH of a solution. (May 2013)
It is defined as the negative logarithm of hydrogen ion concentration.
pH= - log[H+]
27. List the demerits of glass electrode.(May 2013)
1) Measuring solutions containing particulate can damage the glass membrane and 2) the glass
membrane is easily broken.

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28. List the different types of electrodes used in PH measurement? (Nov 2013)
Glass electrode, platinum electrode
29. What is the use of blank in silica analyzer? (Nov 2013)
Blank calibration uses a method different from zero silica content water content. Generally the
blank is set by measuring the gap between absorbance of the normal measurement and that using
a double volume of molybdate reagent.
30. State the different type of electrodes? (May 2015)
a) Glass type b)Solid-state type c)Gas sensing type
31. What is galvanic cell (May 2015)
A galvanic cell, or voltaic cell, named after Luigi Galvani, or Alessandro Volta respectively, is
an electrochemical cell that derives electrical energy from spontaneous redox reactions taking
place within the cell.
32. Write the operational definition of PH (Dec 2015)
pH is a numeric scale used to specify the acidity or basicity (alkalinity) of an aqueous solution.
It is roughly the negative of the logarithm to base 10 of the molar concentration, measured in
units of moles per liter, of hydrogen ions. More precisely it is the negative of the logarithm to
base 10 of the activity of the hydrogen ion. Solutions with a pH less than 7 are acidic and
solutions with a pH greater than 7 are basic. Pure water is neutral, being neither an acid nor a
base.
33. What are the different types of calomel reference electrodes? (Dec 2015)
Calomel chloride with salt bridge solution of saturated lithium chloride.
Calomel electrode with open liquid junction, Calomel chloride with duplicate salt bridge

Unit IV Part B
1. Explain in detail about construction and working principle of ammonia electrodes.(Dec 2014)
2. Write short notes on: (Dec 2014, May 2015, Dec 2015)
Sodium Analyzer(8)
Silicon Analyzer(8)
3. What is a reference Electrodes? What are the various types of Reference Electrodes? Compare
the properties of different types of Reference Electrodes?(May 2014)
4. State the principles of measuring Dissolved Oxygen in Boiler Feed Water. Explain any one
method to measure the dissolved oxygen. (May 2014)
5. Describe how a conductivity cell is used. Give the applications of conductivity measurement of a
liquid. Explain how the oxygen analyzer is used.
6. Describe the construction of a pH electrode. Draw the electronic circuit diagram for measuring
pH of a liquid and explain its working.
7. Discuss how pH values are measured. Explain the role of calomel electrodes in this
measurement.
8. Briefly explain about dissolved oxygen analyzer.
9. Discuss in detail the principle, characteristics of electrodes used in pH meters.
10. Describe with a neat sketch, the principle of operation of water purity meter.
11. Discuss the method of measuring electrical conductivity of a liquid. Also describe the techniques
for determining the purity of water.
12. Discuss how pH of a solution is measured using glass electrode and reference electrode with
necessary diagrams.
13. Explain about sodium analyzer in detail. (May 2013)
14. Explain about silica analyzer
15. Explain different types of ion selective electrodes. (Nov 2013)
16. List the types of electrodes used for pH measurement. Explain the construction details of Digital
pH meter. Also specify the need of reference electrode for pH measurement.
17. Describe a method of measuring dissolved oxygen content in the boiler feed water. Why
dissolved oxygen content is monitored in feed water? Also specify the cause of dissolved oxygen
content in feed water. (May 2013)
18. Explain the working principles of biosensors with a conceptual diagram. Also specify the
various parameters to be measured using Biosensor. (Nov 2013)
19. Explain the operating principle of kathrometer in measuring dissolved oxygen (May 2015)
20. Explain the operating principle principles of solid state sensors and liquid matrix electrodes
with neat diagrams ( Dec 2015)

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UNIT V ELECTRO MAGNETIC RESONANCE AND MICROSCOPIC TECHNIQUES

Part A
1. Write the principle of NMR spectrometer.
A radically different type of interaction between matter and electromagnetic forces can be
observed by subjecting a substance simultaneously to two magnetic fields, one stationary and
other varying at some radio frequency. At particular combinations of fields energy is observed by
the sample and the absorption can be observed as a change in signal developed by a radio
frequency detector and amplifier. The energy absorption can be related to the magnetic dipolar
nature of spinning nuclei.
2. What is Mass spectrometry?
Mass spectrometry is the most commonly used method which provides qualitative and
quantitative information about the atomic and molecular composition of organic and inorganic
materials. It produces charged particles that consist of the parent ion and ionic fragments of the
original molecule, and it sorts these ions according to their mass/charge ratio.
3. List the various types of semiconductor detectors.
1. Surface barrier Silicon detector. 2. Lithium drifted Silicon and Germanium detectors.
4. Why high intensity magnets are preferred for NMR?
The nuclear magnetic resonance (NMR) spectroscopy involves using energy in the form of
electromagnetic radiation which is generated by high intensity magnets, to pump the excess alpha
oriented nuclei into the beta state. Nuclear Magnetic Spectroscopy is based on the fact that when
a population of magnetic nuclei is placed in an external magnetic field, the nuclei become aligned
in a predictable and finite number of orientations. For 1H there are two orientations. In one
orientation the protons are aligned with the external magnetic field (north pole of the nucleus
aligned with the south pole of the magnet and south pole of the nucleus with the north pole of the
magnet) and in the other where the nuclei are aligned against the field (north with north, south
with south). The alignment with the field is also called the "alpha" orientation and the alignment
against the field is called the "beta" orientation.
5. Define state of resonance.
When a nucleus is placed in a system where it absorbs energy, it becomes excited. It then
loses energy to return to the unexcited state. It absorbs energy and again enters an excited state.
This nucleus which alternately becomes excited and unexcited is said to be in a state of
resonance.
6. Define Chemical shift.
The shift in the positions of NMR signals ( compared with a standard reference) resulting
from the shielding and deshielding by electrons are referred to as Chemical shift.
7. Write a method for measuring the Chemical shift.
To measure the magnitudes of chemical shifts of different kinds of protons, there must
be some standard signal with respect to which the measurement can be made.For this purpose
,Tetramethylsilane(TMS),(CH3)4Si is used as the reference or standard compound.It gives
only one signal which serves as fixed reference.
8. What are the factors that influence chemical shift?
The main factors which influence the chemical shift are ;
i. Inductive effect ii. Anisotropic effect iii. Hydrogen bonding
9. What is Spin-Spin coupling?
The interaction between the spins of the neighboring nuclei in a molecule may cause the
splitting of the lines in the NMR spectrum. This is known as spin-spin coupling which
occurs through bonds by means of a slight unpairing of the bonding electrons.
10. Give some applications of NMR spectroscopy.
i.Structural Diagnosis
ii.Quantitaive analysis – used to determine the molar ratio of the components in a mixture.
iii Hydrogen Bonding – Used to study the hydrogen bonding in metal chelates as well as in
organic compounds
iv.Structural determination
v.Intra molecular conversion
vi.Keto-enol Tautomerism
vii.Intermolecular Exchange reaction
viii.Elemental analysis- used for the determination of the total concentration of a given kind

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of magnetic nucleus in a sample.
11. Write the limitation of NMR spectroscopy.
The limitations of NMR spectroscopy are :
i. Lack of sensitivity. The minimum sample size is about 0.1 ml having minimum
concentration of about 1%
ii. In some compounds, two different types of hydrogen atoms resonate at similar
resonance frequencies. This results in an overlap of spectra and makes such spectra
difficult to interpret.
iii. Only liquids can be studied by NMR spectroscopy, although polymers, when preheated
with various solvents, frequently become fluids which can be treated as liquids
12. Define mass spectrum.
The compound under investigation is bombarded with a beam of electrons which produce
an ionic molecule or ionic fragments of the original species. The resulting assortment of
charged particles is then separated according to their masses. The spectrum produced is
known as mass spectrum.
13. Define time of flight.
All ions leave the acceleration field with different velocities depending on their masses.
With magnetic focusing, the ions gets separated by changing their directions. However, if
these ions are allowed to travel in a straight line through a magnetic field – free region,
they will take different times to travel a given distance. The measurement of “this time of
flight” FORM the basis for the nonmagnetic separator.
14. What are the different types of mass spectrometer?
i. Magnetic Deflection mass spectrometer ii. Time of flight mass spectrometer
iii. Double focusing mass spectrometer iv. Quadrupole mass spectrometer
15. What are the different components of a mass spectrometer?
i. Inlet Sample System ii. Ion Sources iii. Electrostatic Accelerating System
iv. Ion detectors and Recording of mass spectrograph, v. Vacuum System
16. Write the components of electron spectroscopy.
a)A source of radiation to excite the sample. b)An electron energy analyzer.
c)An electron detector. d)Read out system. e)High vacuum system.
17. Give some applications of mass spectrometry.
i. Molecular mass can be accurately determined by the mass spectrometry.
ii. It is used to determine the amount of component of a complicated mixture.
iii. Method for the detection of impurities.
iv. Polymers can be characterized by mass spectrometry.
v. Molecular formulae can be determined from the mass spectrum either partially or exactly.
18. What are the types of NMR spectrometer.
a)Minimal type NMR spectrometer b) Multipurpose NMR spectrometer
c) Wideline NMR spectrometer
19. Write the advantages and disadvantages of time of flight mass spectrometer.
Advantages – It is simple and ruggedness. It can handle unlimited mass range.
Disadvantage – Limited resolution and sensitivity.
20. What are the types of detectors in mass spectrometer?
i. Electron multiplier ii. Faraday cup collector iii. Photographic plates
21. What are the two common designs of Double focusing mass spectrometer?
i. Nier - Johnson design ii Mattauch - Herzog geometry
22. What is the advantage of ESR Spectroscopy?
It is used to detect
1)Volume (300 mL) and concentration (1.0-0.01 mM) often low
2)Recording spectrum can be done quickly (usually no more than 15-20 min)
3)Spectrum is only of paramagnetic species
4)Spectrum is often simple to interpret
5)Spectrum often can be recorded in vivo
23. Write down the principle of Mass Spectrometry. (May 2013)
In Mass Spectrometer the sample to be analyzed is first bombarded with electron beam to produce
ions. These ions are then sorted out by accelerating them through electric and magnetic fields
according to their mass /charge ratio. Mass spectrometer separates the ions on the basis of their
mass to charge ratio. But most of the ions are singly charged, so the ratio is equal to the mass of

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the ions. A record of the number of different kinds of ions is called the mass spectrum.
24. Brief the principle of scanning electron microscope. (May 2013)
A normal scanning electron microscope operates at a high vacuum. The basic principle is that a
beam of electrons is generated by a suitable source, typically a tungsten filament or a field
emission gun. The electron beam is accelerated through a high voltage (e.g.: 20 kV) and pass
through a system of apertures and electromagnetic lenses to produce a thin beam of electrons.,
then the beam scans the surface of the specimen by means of scan coils (like the spot in a
cathode-ray tube "old-style" television).Electrons are emitted from the specimen by the action of
the scanning beam and collected by a suitably-positioned detector.
25. Write the principle of Electron Spin Resonance (ESR) spectrometer. (Nov 2013)
Electron Spin Resonance involves detecting the detection of a physical phenomenon of
absorption of electromagnetic radiation in the microwave region by paramagnetic species that
are subjected to magnetic field.
26. What is Nuclear magnetic resonance? (Nov 2013, Dec 2015)
The nuclei of atoms in a molecule on absorbing RF radiation may change their direction
of spin. The analytical field involved with the interaction between the nuclei and rf
radiation is called Nuclear magnetic resonance. (NMR )
27. Write few applications of electron spin resonance spectrometer (May 2015)
It’s used to study the molecular structure, reaction kinetics, molecular motion,crystal structure,
electron transport and relaxation properties.
28. What is TEM (May 2015)
Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons
is transmitted through an ultra-thin specimen, interacting with the specimen as it passes through
it.
29. Define wide-line NMR (Dec 2015)
The range of NMR spectrum from hundreds of kilohertz to tens of megahertz is called wide line
NMR.

Unit V Part B
1. Explain Scanning Electron microscope in detail and also give its applications. (Dec 2014)
2. Explain Transmission Electron Microscope in detail and also give its applications.(Dec 2014)
3. Explain the working principle of Electron spin resonance spectroscopy with a block diagram.
(May 2014)
4. What are the basic components of a Mass Spectrometer? Explain the functions of each
component. (May 2014, May 2015)
5. Draw the block diagram of an NMR spectrometer. Explain the function of each part and explain
how it is used to obtain NMR spectra. How are these spectra useful? (May 2013, May 2015)
6. What are Mass spectrometers? Describe magnetic deflection mass spectrometers. (May 2013)
7. Explain time of flight and quadrupole mass spectrometers.
8. Describe the working of double beam mass spectrometer and give its applications.
9. Explain the instrumentation and applications of Scanning Electron Microscope (SEM) and
Transmission Electron Microscope (TEM).
10. Describe how various samples are analyzed using NMR spectrometer with neat diagram.
11. Explain the construction and working principle of Electron Spin Resonance (ESR) spectrometer
with neat diagram.( Dec 2015)
12. Explain the construction and working of Radio frequency spectrometer with neat diagram.
13. Explain the various components of a mass spectrometer.
14. Explain in detail the construction and working principle of single focusing mass
spectrophotometers. (Nov 2013)
15. In NMR spectroscopy mention the advantages of using a magnet with as great field strength as
possible. Also explain the difference between a continuous wave and Fourier transform NMR.
16. With neat sketch explain the construction and working principle of mass spectrometer. (Dec
2015)
17. What are the basic components of electron Spectroscopy? Also explain the working principle of
Electron spectroscopy with a neat block diagram. (Nov 2013)

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