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ABOUT THE AUTHOR
R S Khandpur is the former Director General of Science City, Kapurthala, a joint project of the
Government of India and Government of Punjab. He has steered the development of the Science City
from almost its very beginning.
A former Director General of Centre for Electronics Design and Technology of India of Ministry of
Information and Communication Technology, Government of India (CEDTI), Dr. Khandpur is the founder
Director of Centre for Development of Advanced Computing, (C-DAC) Mohali (Punjab). He has served
as scientist for 24 years in CSIR-CSIO (Central Scientific Instrument Organisation), Chandigarh as Head
of Medical Instrument Division (1975–1989) and Electronics Division (1985–1989).
He has been AICTE/NAE Distinguished Visiting Professor, Member IEEE, USA; Fellow, IETE; and
Member, Society for Engineering in Medicine and Biology, USA.
He has authored eight books of international repute, four of which has been published by McGraw
Hill, USA. These books have gone into several re-prints and new editions. He holds seven patents for
innovative designs and has published over 60 research and review papers.
Handbook of Analytical Instruments
Third Edition
R S Khandpur
Head,
Medical Electronics Division
CSIR-Central Scientific Instruments Organization
Chandigarh
and
Former Director,
Centre for Development of Advanced Computing (C-DAC),
Mohali (Chandigarh) Punjab
Information contained in this work has been obtained by McGraw Hill Education (India), from sources believed to be
reliable. However, neither McGraw Hill Education (India) nor its authors guarantee the accuracy or completeness of
any information published herein, and neither McGraw Hill Education (India) nor its authors shall be responsible for
any errors, omissions, or damages arising out of use of this information. This work is published with the understanding
that McGraw Hill Education (India) and its authors are supplying information but are not attempting to render
engineering or other professional services. If such services are required, the assistance of an appropriate professional
should be sought.
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CONTENTS
3. Infrared Spectrophotometers
3.1 IR Spectroscopy
3.2 Basic Components of IR Spectrophotometers
3.2.1 Radiation Sources
3.2.2 Monochromators
3.2.3 Entrance and Exit Slits
3.2.4 Mirrors
3.2.5 Detectors
3.3 Types of IR Spectrophotometers
3.3.1 Optical Null Method
3.3.2 Ratio Recording Method
3.4 Sample Handling Techniques
3.4.1 Gas Cells
3.4.2 Liquid Cells
3.4.3 Variable Path Length Cells
3.4.4 Sampling of Solids
3.4.5 Micro-sampling
3.5 Fourier Transform Infrared Spectroscopy
3.5.1 FTIR spectrometers
3.5.2 Major Components of FTIR Spectrophotometer
3.5.3 Advantages of FTIR
3.6 Calibration
3.7 Attenuated Total Reflectance Technique
4. Flame Photometers
4.1 Principle of Flame Photometry
4.2 Basic Flame Photometer
4.3 Constructional Details of Flame Photometers
4.3.1 Emission System
4.3.2 Optical System
4.3.3 Photosensitive Detectors
4.3.4 Recording System
4.4 Clinical Flame Photometers
4.5 Accessories For Flame Photometer
4.6 Expression of Concentration
4.7 Interferences in Flame Photometry
4.7.1 Flame Background Emission
4.7.2 Direct Spectral Interference
4.7.3 Self-Absorption
4.7.4 Effect of Anions
4.7.5 Effect of Ionisation
4.7.6 Solution Characteristics
4.8 Procedure For Determinations
4.8.1 Calibration Curve Method
4.8.2 Internal Standard Method
7. Raman Spectrometer
7.1 The Raman Effect
7.2 Raman Spectrometer
7.2.1 The Source
7.2.2 Sample Chamber
7.2.3 The Spectrometer
7.2.4 The Detector
7.2.5 Computer
7.3 PC-Based Raman Spectrometer
7.4 FT Raman Spectrometer
7.5 Infrared and Raman Microspectrometry
9. Mass Spectrometers
9.1 Basic Mass Spectrometer
9.2 Principle of Operation
9.3 Types of Mass Spectrometers
9.3.1 Magnetic Deflection Mass Spectrometer
9.3.2 The Time-of-Flight Mass Spectrometer
9.3.3 Radio Frequency Mass Spectrometer
9.3.4 Quadrupole Mass Spectrometer
9.4 Components of a Mass Spectrometer
9.4.1 The Inlet Sample System
9.4.2 Ion Sources
9.4.3 Electrostatic Accelerating System
9.4.4 Ion Detectors and Recording of Mass Spectrograph
9.4.5 Vacuum System
9.5 Inductively Coupled Plasma Mass Spectrometer
9.6 Trapped Ion Mass Analyzers
9.7 Quadrupole Ion Trap Mass Spectrometer
9.8 Fourier Transform Mass Spectrometry (FT-MS)
9.8.1 Ion Cyclotron Resonance (ICR) Mass Spectrometery
9.8.2 Orbitrap Mass Spectrometry
9.9 Tandem Mass Spectrometry (MS/MS)
9.10 Resolution in Mass Spectrometry
9.11 Applications of Mass Spectrometry
References
Index
PREFACE TO THE THIRD EDITION
I am delighted to place before you the third and enlarged edition of my popular book Handbook of
Analytical Instruments. This edition is totally revised and updated based on the technical advances
which have penetrated the field of analytical sciences during the last decade. Each chapter has been
revisited, obsolete material deleted and latest material based on new developments included at various
places, so that the reader gets the best from the new edition.
Three new chapters have been added to the book. For observing and analysing the surface micro-
structure of a sample, very sophisticated imaging instruments have become available. These instruments
enable the users to look into and work at atomic level. The new topics which have been included as
separate chapters are: Scanning Electron Microscope and Scanning Probe Microscope (Scanning
Tunneling Microscope and Atomic Force Microscope). Particle size analysers play an important role in
research and development and for quality control in many industries such as pharmaceuticals, ceramics,
cement, paints and emulsions etc. Realizing the need of the users in these areas, a new chapter on
particle size analysers and counters has been included.
Several new topics have been incorporated in the revised text, some of which are:
• Brief introduction to the use of MEMS in analytical instrumentation, leading to Lab-on-a-Chip
technology.
• Rising trends in portable spectrophotometers using fibre optics.
• Use of Fourier transform with conventional instrumentation such as Infrared Spectroscopy,
Raman Spectrometry, NMR Spectrometry, Mass Spectrometry etc.
• Neutron Activation Analysis Technique.
• Liquid Chromatography-Mass Spectrometry.
• Flow injection automated analysis system, semi-automated clinical chemistry analyser and point
of care instrumentation.
• Thermo-mechanical analysis instrumentation.
• Capillary electrophoresis instrumentation including DNA sequencer.
• Integrated chips for modern pH metres.
• Process gas analysers including online quantitative analysis of industrial gases.
• Various levels of power supplies.
• Embedded systems and digital signal processors.
• Popular software packages which find applications in analytical instrumentation, interfacing
techniques, computer networking and smart laboratory concepts.
While the basic principles of instrumentation and techniques are generated by researchers, their
practical utilisation gets established when they are commercially produced by various manufacturers.
Therefore, it is more pertinent for the users to understand the way an instrument is designed, the
placement of the various subsystems inside it and the precautions needed during its operation. Inclusion
of information from the manufacturers on the typical instruments thus, indicates the practical aspects of
the technology utilised in the instruments. It is for this reason that efforts have been made to include
information on some of the popular commercially available instruments. It, however, does not imply that
the instrument described is superior to the competing ones. The motive is to illustrate the instruments
typical of their class or possessing features of special interest for intended applications.
A distinctive feature of the third edition is the improved visual impact of the illustrations and
photographs of latest commercial equipment. The list of references has been greatly expanded in the
book, which will be found useful by those who would like to know more about the latest research in the
field.
The book continues to enjoy an enviable position in the field of analytical instrumentation both in
India and abroad for which I feel obliged to the students and the teachers for patronising the book. I, on
my part, have endeavoured to make the text more lucid and illustrations more meaningful.
I thank the readers once again for sending me the feedback and suggestions, formally and informally,
which I have tried to incorporate in the revised edition. I do hope that the present book would be found
even more useful to students and professionals in the field of analytical instrumentation.
I am grateful to my wife Ramesh Khandpur for constant encouragement and support during the period
the book has been under revision. When the first edition of this book was published in 1989, my children
Vimal, Gurdial and Popila were all studying. By the time the second edition was out in 2006, they were
all married, well employed and had their own children. Today, my two granddaughters Ravleen and
Harsheen are in prestigious professional colleges, making me proud of their achievements. The other
three grandchildren Manmeet, Aashna and Gurtej, all millennium children born in the year 2000, are
school going. Each one of them has been getting motivated with my keen interest in their studies and I, in
turn with their inquisitive enquiries about what I do on my computer. Thanks are also due to McGraw
Hill Education (India) Pvt. Ltd. for bringing out an excellent publication.
R S Khandpur
PREFACE TO THE FIRST EDITION
Instruments used for analysis constitute the largest number of instruments in use today. Their range is
spectacular and variety baffling. It is difficult to imagine a field of activity where analytical instruments
are not required and used. They are used in hospitals for routine clinical analysis, drugs and
pharmaceutical laboratories, oil refineries, food processing laboratories and above all for
environmental pollution monitoring and control. This book has been designed to cater to the needs of a
wide variety of readers working in these areas. The postgraduate students of chemistry and physics
undergoing courses on instrumental analysis will find the book a useful text. It is also intended as a guide
for the scientific investigator who wishes to acquire knowledge about the more widely used analytical
instruments. The availability of a bewildering array of instrumental techniques and a large variety of
commercially available equipment have provided several courses of action to the investigator. The
student who undergoes this course will be in a position to select instruments for a particular problem
with some idea of their merits, demerits and limitations. The treatment of the subject is designed to be
sufficient to give the reader the necessary background to fruitfully discuss the more esoteric details of an
instrument with an expert in this area.
With the widespread use of analytical instruments, it has now become essential to have qualified and
sufficiently knowledgeable service and maintenance engineers. Besides having a basic knowledge of the
principle of operation, it is important for them to know the details of commercial instruments from
different manufacturers. A concise description of instruments of each type from leading manufacturers
has, therefore, been provided. Since rapid changes and improvements in instruments usually make some
of the description obsolete, an attempt has been made to describe the principles that are basic to the
various types of analytical instruments. The principles learned would enable the service engineers to
carry over to new equipment as it appears in the market.
The area of analytical instrumentation involves a multidisciplinary approach, with electronics and
optics forming the major disciplines. Highly populated printed circuit boards often have application-
specific integrated circuits mounted on them. This has necessitated a new approach to repair and
servicing involving replacement of the printed circuit card without having to repair the instrument at the
component level. Work of this nature requires a knowledge of the various building blocks of an
instrument, and this has been the approach in the preparation of the text. This approach will also be
advantageous to students of chemistry, physics, chemical engineering, instrumentation and electronics,
etc.
The book starts with an explanation of basic concepts in electronics and optics, with special
reference to operational amplifiers, digital integrated circuits and microprocessors. The chapter also
covers various types of display systems and laboratory recorders. The information in this chapter would
serve as a base for the description in the rest of the book.
The modern laboratory has a large number of analytical instruments churning out information.
Electronic procedures for handling the huge amount of data have become imperative. The marriage of
computers and instruments has offered tremendous possibilities of easing the burden on the scientists, as
well as optimising the performance of analytical instruments. Many of the leading instrument
manufacturers are producing systems for use in the laboratory, both for data acquisition and for control
purposes. The personal computer has been virtually responsible for a revolution in the methodology,
quantity, economy and quality of experiments performed. Taking into consideration the impact of
computers on analytic instruments, the topic is covered in the second chapter itself.
Colorimetry and spectrophotometry have become the central techniques of analytical chemistry.
Spectrophotometry, particularly in the ultraviolet region, offers a sensitive, precise and nondestructive
method of analysis of biologically important substances such as proteins and nucleic acids. The
introduction of spectrophotometers, especially in the visible region of the spectrum, led directly to the
explosion of analytical methodology, characterised by the use of an ever decreasing amount of sample
size and multi-sample analytical methods. The use of the double-beam principle helped in the
development of infrared spectroscopy, where direct recording of spectra is now routine. Similarly,
flame photometers and atomic absorption spectrophotometers have become almost indispensable tools
in clinical and research laboratories. These topics, along with fluorimeters and phosphorimeters,
photoacoustic and photothermal spectrometers, mass spectrometers, and Raman spectrometers, are
covered in the next part of the book.
The most important spectroscopic techniques for structural determination are nuclear magnetic
resonance and electron spin resonance spectrometry. These topics are covered in two chapters. Fourier
Transform NMR and spin decouplers are also concisely dealt with. A separate chapter on electron and
ion spectroscopy, important analytical tools for surface analysis, has been included.
Qualitative and quantitative analyses have been greatly facilitated by the increasing availability of
isotopically labelled compounds. The measurement of these has required the development of
increasingly complex equipment, usually capable of measuring and printing out the radioactive counts
from 100 or more samples wholly automatically. Multichannel counters, scanners and gamma cameras
are representative of the highly sophisticated equipment and richly deserve their place in the book. X-
ray spectrometers based on diffraction, absorption and fluorescence are also covered in detail. Analysis
procedures have been automated, with the result that a very large number of samples can be handled per
hour for a multiplicity of tests. Systems like auto-analysers have brought about tremendous procedural
and conceptual innovations. A complete description of the automated analysis systems has been
provided in a separate chapter.
Chromatography offers a unique method of separation of closely similar substances. Various methods
like liquid-liquid partition, gas-liquid partition, ion-exchange, molecular sieve, etc. have all provided a
basis for the same. Gas-liquid chromatography is perhaps the most widely used than any other single
analytical method for small- to medium-sized molecules. However, a liquid mobile phase possesses
certain advantages over a gaseous mobile phase since it can contribute to the separation achieved
through the specificity of its interaction with solutes. This advantage has resulted in the development of
high-pressure, high-performance liquid chromatography, using specialised column packing of very small
size. Two chapters are devoted to the different types of chromatograph instruments. Perhaps the most
sophisticated ultra-micro-scale analytical instrument is the combination of the gas chromatograph with
the mass spectrometer, and the same has been well illustrated in the chapter on mass spectrometry. A
separate chapter on thermo-analytical methods gives a brief introduction to these techniques.
Electrophoresis, as a medium-scale method for the separation of proteins and its development into
an ultra-micro method with the introduction of zone electrophoresis, is covered in the next chapter. The
continuous improvements in staining and optical visualisation methods have led to this technique being
applicable to the microgram level or even less. The chapter also covers spec-trodensitometers including
those based on microprocessors.
Electrochemical instruments, based on a variety of principles of operation, have undergone
considerable improvements in terms of accuracy, speed and automation. While the chapter on
electrochemical instruments covers various types of instruments like conductivity metres and
polarographs, the chapter on pH metres includes the latest in electronic circuitry, ion-selective
electrodes and bio-sensors. An exhaustive treatment has been given to blood gas analysers and industrial
gas analysers.
Awareness and concern about the deteriorating environment is increasing the world over. It is
necessary to monitor changes taking place in the quality of the environment for initiating efforts to
accomplish environmental pollution control. Many of the analytical tools used elsewhere in other areas
of applications could be profitably utilised for air and water pollution monitoring purposes. However, a
special chapter on this subject illustrates specific techniques employed for monitoring different
pollutants in air and water.
This book has a sufficient degree of comprehensiveness and depth to give the reader the most
important information without having to delve in more specialised books on the subject. I hope that the
material in the book would be found useful by a large number of readers working in different
disciplines.
I would also like to add that mention of the products of industrial manufacturers does not necessarily
imply that I consider them superior to competing items. The aim is to describe instruments typical of
their class, possessing some special features of interest as an illustration of the indicated principles and
intended application, rather than writing a catalog of analytical equipment.
I am indebted to the Director, CSIO, for his kind permission to publish the book and to Tata
McGraw-Hill Publishing Company Limited for excellent editing and printing. I am thankful to TAB
Books, USA, for their kind permission to reproduce some parts of my earlier book published by them. I
am also grateful to my wife Mrs Ramesh Khandpur and children Vimal, Gurdial and Popila for the help
they extended me during preparation of the manuscript and proofreading.
R S Khandpur
1
FUNDAMENTALS OF ANALYTICAL INSTRUMENTS