This book deals with the principles and applications of analytical chemistry, and is useful for BSc chemistry students and those working in analytical research laboratories of drug, pesticide and other chemical industries. The topics discussed include the procedures to be followed in analytical work, solvent extraction as a tech-nique in the isolation and purification of compounds, and chromatographic techniques (TLC, column, paper, ion-exchange, and HPLC) that are used for identification, purification, quantitative analysis and for monitoring the progress of reactions.
Evaluation of Analytical Data 1.1 Introduction 1.1.1 Errors 1.1.2 Classification of errors: Their detection-Determinate and indeterminate errors 1.1.3 Normal law of distribution of indeterminate errors 1.1.4 Correction and minimization of errors
1.2 Accuracy and Precision: Methods for their Expression 1.2.1 Accuracy 1.2.2 Determination of accuracy as relative error 1.2.3 Precision
1.3 Significant Figures and Computation 1.3.1 Significant figures 1.3.2 Significance of zero in the computation of analytical data 1.3.3 Rules of computation
1.4 Calibration 1.4.1 Calibration of weights 1.4.2 Calibration of volumetric apparatus 1.4.3 Calibration of standard flask 1.4.4 Calibration of burette 1.4.5 Calibration of pipette
2. Separation Methods: Solvent Extraction 2.1 Introduction 2.2 Principles and Process of Solvent Extraction 2.3 Techniques of Solvent Extraction 2.4 Batch Extraction 2.4.1 Batch extraction of liquid 2.4.2 Batch extraction of mixtures with active solvents 2.5 Continuous Extraction of Liquids 2.6 Extraction of Solids 2.6.1 Batch process of extraction of solids 2.6.2 Continuous solid-liquid extraction (soxhlet extraction apparatus) 2.7 Countercurrent Extraction 2.8 Advantages of Solvent Extraction Technique
3. Separation Methods: Chromatography 3.1 Introduction 3.1.1 Classification of chromatographic methods 3.2 Column Chromatography 3.2.1 Adsorption phenomenon: Nature of adsorbents 3.2.2 Solvent systems 3.2.3 Differential migration 3.2.4 Separation of a mixture of o-/p-nitro anilines (A demonstration experiment) 3.3 Thin-Layer Chromatography (TLC) 3.3.1 Coating materials and preparation of TLC plates 3.3.2 Solvents for development 3.3.3 Detection of compounds in TLC 3.3.4 Rf values in TLC 3.3.5 Applications of TLC in chemistry 3.3.6 Preparative TLC 3.3.7 Demonstration experiment in TLC 3.4 Ion-Exchange Chromatography 3.4.1 Theory and apparatus 3.4.2 Applications of ion-exchange chromatography 3.5 Paper Chromatography 3.5.1 Nature of paper-support, stationary phase 3.5.2 Application of sample, solvent systems: Mobile phase 3.5.3 Theoretical basis (principles) of paper chromatography 3.5.4 Detection of the spots 3.5.5 Rfvalues in paper chromatography 3.5.6 Various modes of development: Ascending, descending and horizontal 3.5.7 Two-dimensional paper chromatography and applications
3.6 High-Performance Liquid Chromatography (HPLC) 3.6.1 Applications of HPLC 3.6.2 HPLC instrument 3.6.3 Stationary phases in HPLC 3.6.4 Normal and reversed phase HPLC: A comparison 3.6.5 Normal phase HPLC: Principle 3.6.6 Retention times in HPLC 3.6.7 Reversed phase HPLC: Principle
4. Instrumental Methods of Analysis: UV-Visible Spectroscopy 4.1 General Features of Absorption Spectroscopy 4.1.1 Interaction of UV-visible radiation with organic and inorganic compounds 4.1.2 Recording the UV-visible spectra of a compound
4.2 Quantitative Aspects of UV-Visible Absorption Measurements 4.2.1 Terms employed in absorption spectroscopy
4.3 Laws of Absorption of Radiation 4.3.1 Lambert’s law 4.3.2 Beer’s law 4.3.3 Beer-Lambert’s law 4.3.4 Beer-Lambert’s calibration graph for quantitative analysis by the UV-visible method 4.3.5 Deviations and limitations of Beer-Lambert’s law
4.4 General Design of Instruments for Absorbance Measurements 4.4.1 Visual comparison 4.4.2 Visible photometer or colourimeter 4.4.3 Spectrophotometry 4.4.4 Single-beam spectrophotometer 4.4.5 Double beam spectrophotometer 4.4.6 Comparison of visible photometers, single-beam and double-beam spectrophotometers
4.5 Quantitative Applications of UV-Visible Spectroscopy 4.5.1 Determination of Fe (III) using thiocyanate 4.5.2 Determination of Fe (III) using the standard addition method
4.6 Extension of Beer’s Law to Mixtures 4.6.1 Simultaneous determination of permanganate and dichromate 4.6.2 Determination of the composition of a complex
5. Analysis of Water 5.1 Introduction 5.1.1 Impurities in water 5.1.2 Physical properties of water 5.1.3 Hardness of water 5.1.4 Units of hardness of water 5.1.5 Industrial uses of water
5.2 Water-Softening Methods for Industrial Purposes 5.2.1 Lime-soda process of softening of water 5.2.2 Zeolite or permutit process 5.2.3 Ion-exchange resin process-Softening of water by synthetic ion -exchange resins or by de ionization or demineralization process
5.3 Formation of Scales and Sludge 5.3.1 Boiler feed water 5.3.2 Scales and sludge 5.3.3 Chemical composition of scales and sludge 5.3.4 Disadvantages of scales and sludge formation 5.3.5 Prevention of scales and sludge formation 5.3.6 Priming and foaming 5.3.7 Caustic embrittlement 5.3.8 Corrosion 5.3.9 Protective measures against corrosion
5.4 Biological Oxygen Demand (BOD) and Chemical Oxygen Demand (COD) 5.4.1 Introduction 5.4.2 Biological oxygen demand (BOD) 5.4.3 Determination of BOD 5.4.4 Chemical oxygen demand (COD) 5.4.5 Determination of COD
5.5 Effluent (Sewage) Water Treatment 5.5.1 Sources of industrial pollution 5.5.2 Sewage treatment 5.5.3 Harmful effects of sewage and industrial wastes