Instrumental Methods of Chemical Analysis

Front Cover
Krishna Prakashan Media, 2000 - Air - 308 pages
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Contents

into an organic phase 39 Advantages of solvent extraction 41 Applications of liquid
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FUNDAMENTAL PRINCIPLES OF SPECTROSCOPY 367
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Comparison with indicators in buffers 72 Potentiometric determination
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surements with the glass electrode 79 Advantages of glass electrode 80 Disadvantages
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voltaic cells or Barrier layer cells 86 Photoemissive vacuum tubes 87 Photomultiplier
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Photoelectric spectrophotometers 100 Sources of errors
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Presentation of spectral data 105 Special spectrophotometric tech
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Effect of conjugation on chromophores 134 Choice of solvent
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Spectroscopy 11 Advantages of spectroscopy 12 Wave properties
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Basic separation methods 5 Chromatography 9 Definitions 10 Classification
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Emission spectra 13 Born Oppenheimer approximation 13 Interaction of electro
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Thermal radiation 27 Practical sources of radiation 28 Particle properties of radiation
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Factors affecting extraction 27 Technique for solvent extraction 34 Com
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Detectors 40 Photometric analytical methods 42 Spurious radiation 43
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Signal indicator 43 Natural line width and natural line broadening including
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COUNTER CURRENT EXTRACTION 5757
C-57

Removal of oxygen 162 Agar salt bridge 163 Saturated calomel electrode 163 Con
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Analysis of inorganic complexes 166 Analysis of mixtures of absorbing
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Pilot ion procedure 166 Qualitative analysis 167 Inorganic polarographic
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Some spectrophotometric determination 176 Short answer questions 176 TrueFalse
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Infrared spectroscopy 220 Vibrational energies of diatomic molecules 222 Zero
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of electrochemical oxidation and reduction 238 Possible paths for electro reduction
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Reversed phase partition TLC 258 TLC on polyamides 258 TLC on dextran
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tomic molecules 250 Group frequencies and factors affecting band position
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Hadamard spectroscopy 269 Abridged spectrophotometers 269 Nondispersive pho
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Ethers 302 Esters 304 Acid halides 304 Carboxylic acids 305 Amines
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Important spectral regions in the infrared 311 Environmental effects
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Molecular shape 313 Applications of IR spectroscopy 314 Short answer questions
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Hints and explanations
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INFRARED SPECTROSCOPY 193333
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ATOMIC ABSORPTION SPECTROSCOPY
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answer questions 380 Truefalse questions 381 Fill in the blanks questions 381 Multi
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FLAME EMISSION SPECTROSCOPY OR FLAME PHOTOMETRY 421454
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sion intensity with the flame 424 Flame temperature 424 Chemical reactions in flames
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Single beam and double beam instruments 433 Calibration curve 434 Flame spectro
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Special applications 442 Some flame emission spectroscopic proce
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tion of emission spectrum 457 Origin of emission spectra 458 The emission process
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The spectra produced by electronic excitation 466 Units 468 Apparatus for emission
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Classification of spectrometers 479 Measures used for the comparison of prism instru
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Hints and explanations
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XRay fluorescence 499 Radioactive sources 499 Absorption of Xrays
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Xray instrumentation 503 Xray detection and measurement 508 Ionisation methods
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titative analysis 518 Applications of Xray emission 521 Xray absorption methods
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MOLECULAR LUMINESCENCE FLUOROMETRY AND PHOSPHORIMETRY 537575
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Theory 544 Relation between intensity of fluorescence and concen
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Applications of fluorometric analysis 558 Applications in inorganic chem
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Short answer questions 568 TrueFalse questions 570 Fill
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lometry and turbidimetry 578 Turbidity and colorimetry 578 Nephelometry and fluo
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Principles of XPS or ESCA 590 Instrumentation for XPS or ESCA
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Auger electron spectroscopy AES 602 Short answer questions
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toacoustic spectra 610 Instrumentation 610 Advantages of PAS over conventional
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Surface applications of PAS 613 Short answer questions 616 TrueFalse questions
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nance origin of NMR spectra 622 Theory of NMR spectroscopy 622 Precession
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and magnetic equivalence 676 Classification ABX AMX ABC A2B2 etc
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Double resonance spin spin decoupling and Nuclear Overhauser effect NOE
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nation of peak areas 691 Sample handling 694 Complicating factors 694 Spectro
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Carbon13 698 Boron11 701 Limitations of NMR spectros
S-734
Difference between ESR and NMR 741 Instrumentation 743 Electron nucleus cou
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Study of free radicals 754 Electronic structure and hyperfine splitting Spin den
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TrueFalse questions 770 Fill in the blanks questions 770 Multichoice questions
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plingnoise decoupling 779 Off resonance decoupling 781 Selective proton decoupling
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Chemical shifts for alkenes ppm from TMS 797 Chemical shifts for substituted alkenes
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gradient EFG and quadrupole coupling constant QCC 806 Splitting in
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Electron diffraction 819 Electron diffraction of gases and vapours
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structure of surfaces 825 Advantages of electron diffraction method over Xray
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solids and liquids 834 Diffraction of neutrons 835 Neutron diffraction theoret
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Hints and explanations
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Aromatic hydrocarbons 894 Alcohols 896 Aromatic alcohols 900 Phe
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Nitrogen rule 914 Ring rule 914 Qualitative applications 915 Quantitative applica
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paratus for Mossbauer spectroscopy 941 Lamb Mossbauer factor 942 Mossbauer
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Applications of Mossbauer spectroscopy 944 Iron proteins 947 Short answer questions
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TrueFalse questions 63 Fill in the blanks questions 64 Multichoice questions 64
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Continuous counter current separation 58 General theory of chromatographic processes
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Preparation of the coloured solution 71 Measurement of coloured solution
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of solid support for LLC 70 Selection of liquid liquid systems 71 Performance
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Reasons for deviations from Beers law 80 Techniques for colour comparison 80
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Ion exchange chromatography 81 Recycling chromatography 82 Ion pair chromatog
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adsorption column chromatography 98 Adsorbent 100 Solvent Eluting agent Mobile
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limitations of partition 114 Stationary phase 115 Impregenating the support 115
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Ion exchange resins 123 Cation exchange resins 124 Anion exchange resins 125
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exchange equilibrium 131 Basis for separations 131 Separation of organic mixtures
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niques of ion exchange chromatography 146 Separation factor 146 Factors affecting
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Packing of the column 163 Application of the sample 163 Theory of
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liquid chromatography 172 retention 176 Selectivity 176 Bonded phase chromatog
C-179
Alternating current polarography 179 Tensammetry 182 Chronopotentiometry 182
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liquid chromatography 183 Carrier gas 184 The injection port 185 Columns 186
C-186
The solid inert support 187 The stationary liquid phase 188 Column thermostatting
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Separation procedure 198 Theory and principle of gas liquid chromatography 202
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Factors affecting separation 204 Temperature programming 206 Applications of
C-212
or microwave spectrum 201 Microwave spectroscopy 201 Classification of mole
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Hints and explanations 224
C-224
Types of paper chromatography 226 Principle of paper chromatog
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Basic operations involved in TLC 243 Methods for the production of thin layer
C-247
Truefalse questions 265 Fill in the blanks questions 266 Multi choice
C-267
Zone electrophoresis or electrochromatography 270 Types of sup
C-278
HIGH PRESSURE OR PERFORMANCE LIQUID CHROMATOGRAPHY 286385
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RADIO CHROMATOGRAPHY 386388
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Measurement of conductance 6 Effect of temperature and pressure on con
M-7
tance measurement 11 Applications of conductance measurement 12 Conductometric
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Applications 35 Advantages 38 Disadvantages 39 Short answer questions
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Reversible and irreversible cells 43 Reversible electrodes 44 EMF and its measure
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POTENTIOMETRIC TITRATIONS 93132
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Solid state membrane electrodes 105 Precipitate membrane electrodes
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Acidalkali or neutralisation titrations 111 Methods of end point location 111 Graph
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Short answer questions 127 Truefalse questions 129 Multi choice
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Current voltage relationship 139 Polarograms 140 Interpretation of polarographic
M-147
Different kinds of currents contributing to the polarographic wave 147 The charging
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AMPEROMETRIC TITRATIONS 190209
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with two indicator electrodes 196 Instrumentation 198 Cell used 199 Volume cor
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Titration procedure 201 Amperometric and potentiometric titrations 202 Advantages
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Demonstration of polarisation 213 Remedy of polarisation 213
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Determination of copper lead and tin in brasses and bronzes by controlled potential
M-254
Mercury 260 Lead 260 Tin 260 Bismuth 260 Nickel in presence
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Precautions with oxygen hydrogen coulometer 265 Silver coulometer
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teristics of coulometric methods 267 Constant current coulometry or coulometric titra
M-273
Some other applications 279 Some nonanalytical applications of con
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Principle and apparatus for HPLC 189 Solvent delivery system 290
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Sample injection system 295 The column 297 Column packing materials
M-298
Optical activity 288 Specific rotation 289 Factors affecting angle of
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Hints and explanations 307
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Types of recording thermobalances 313 Sample holders 314
M-314
Theory 320 Simultaneous DTATGA curves 322 Instrumentation 323 Fac
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Acidbase titration 334 Precipitation titrations 334 Complexation
M-338
Xray absorption vs Xray emission 524 Advantages of Xray methods 525 Disadvan
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