Pharmaceutical Analysis-II (Volume-II : Instrumental Methods)
  by P.C. Kamboj
 
About The Book
Contents
Reviews
Related Books
Order Now by Email

   ISBN 978-81-85731-52-0; 1st Ed. 2010; Rpt 2015 pp.xvi+504

   Delhi price: 290      Outside Delhi price: 305      Overseas price : 870

 About The Book  


   The Volume II involves "Instrumental Methods of Analysis". The major objective of this text (both theory and practicals). The use of statistical methods in judging the accuracy and precision of the data.

The text includes 22 chapters and provides the modern techniques of chromato-graphy, refractometry, polarimetry, ORD and CD spectra, radiochemical analysis, thermal and X-ray methods in a simple and easy to learn manner. Basic principles, methodologies and applications given with diagrams. Data tables, solved examples, questions, practical exercises included. Satistical treatment of data, standards, calibration and method validation etc., also described. Eight important appendices and a detailed index is included.

 Content


1 Introduction to Analytical Chemistry
What is Analytical Science?
Qualitative, Quantitative and Structural Analyses
Various Fields Where Analytical Chemistry is Applied
Definition of Analytical Chemistry
Areas of Applications
Steps in an Analysis
Drug Characterisation by Physico-chemical Methods
   Analytical Terminology
   Sample Size

2 Errors and Computation of Analytical Data
Introduction
Units and Dimensions
Mathematical Symbols
Exponents
Extensive, Intensive and Proper Quantities
Dimensional Analysis
Logarithm
Atomic Masses, Mole and Avogadro’s Number
Significant Figures
Precision and Accuracy
Classification of Errors
Minimisation of Errors
Testing for Significance
Confidence Limit
Rejection of a Result
How to Report Analytical Data
Statistical Parameters and Analytical Data
Propagation of Determinate Errors
       of Indeterminate Errors

3 Some Definitive Terms, Random Errors and Quality Assurance
Glossary of Terms
Random Error Sources (Normal Error Curve)
Histogram and Frequency Polygon
Statistics of Random Errors
Area Under a Gaussian Curve
Accuracy, Standardisation, and Calibration
External Standard Calibration
   Method of least square (regression method)
       Errors in
Internal Standard Method
Standard Addition Method
Quality Assurance and Method Validation

4 Chromatographic Separations–An Introduction
Introduction—What is Chromatography
Chromatographic Methods (Classification)
Chromatographic Separations (Various Mechanisms)
Adsorption, Partition, Ion-exchange, Affinity
Gel permeation (size-exclusion / molecular sieving)
Chromatographic Separations (Basis)
Sorption Isotherms
Development of the Chromatograms
Frontal analysis, Displacement development, Elution analysis
   Column Efficiency in Chromatography
Retention time, Retention factor, selectivity factor
Band-Broadening and Column Efficiency
Column efficiency
Plate height
Peak Tailing or Fronting (How to reduce)
Column Performance (Band-Broadening), Kinetic Factors
Van Deemter Equation
    Eddy diffusion, Longitudinal (axial) or molecular
    diffusion term , Mass transfer coefficients
Optimisation of Column Performance
Resolution, Relationship among retention factor, selectivity factor, number of plates and resolution
Problems Faced in Chromatographic Separations
   (General elution problem)
Applications of Chromatography
Qualitative and quantitative analyses
Peak height, Peak areas, Calibration and series
of standards Area normalisation method, Internal standard
   Chromatographic Terminology
   Symbols, Terms and Relationships in Chromatography (Table)
   Questions and Problems

5 Liquid Phase Column Chromatography (Classification)
Liquid-Solid Adsorption Chromatography
Liquid-Liquid Partition Chromatography
Reversed Phase Liquid Partition Chromatography
Bonded Phase Liquid Partition Chromatography
Counter-Current Chromatography
Ion-Exchange Chromatography
Gel (or Size Exclusion) Chromatography
Affinity Chromatography
Metal-Chelate Affinity Chromatography
High Performance Liquid Chromatography

6 Adsorption Chromatography
Introduction
Principles and Mechanism
Adsorption Isotherms
Adsorbents
Mobile Phase (Eluents)
Operational Details; Separation of a mixture; Columns; Preparation of columns; How to use
Dry Columns
Glass Columns
Nylon Columns
Flash Chromatography
Microscale Adsorption Chromatography
Applications
Experimental Determinations
   Determination of the percentage (w/w) of strychnine
   Separation of dyes on alumina
   Determination of phytomenadione in its injection

7 Partition Chromatography
Introduction
Stationary Mobile Phases and Types of Partition
   Chromatography
Bonded Phase Partition Chromatography
   Applications
   Counter-Current Chromatography

8 Size Exclusion Chromatography
Introduction
Principles
Techniques
Structures and Properties of Gels (Stationary Phase)
Column Preparation
Monitoring of Eluate
Mechanism of Separation
   Applications
Affinity Chromatography
Applications
Metal Chelate Affinity Chromatography

9 Ion-Exchange Chromatography
Introduction
Types of Ion-Exchangers
Ion Exchange Resins (Preparations)
Cations or anions exchange properties;
Resins with chelating ligands
Other ion-exchange materials
Functions of Ion Exchangers
Ion Exchange Mechanism
Ion Exchange Equilibria and Selectivity
Experimental Details
   Preparation of the column; Technique;
Analysis of the eluate
Applications of Ion-Exchange Chromatography
Water softening and demineralization;
Isolation of alkaloids; Assay of total halogenic salts
Pharmaceutical Applications
Separation of lanthanides and actinides
   Separation of metals (effect of complexing agents)
Separation of amino acids (Effect of pH)

10 Ion Chromatography
Introduction
Separation Mechanisms Employed
Resins (structure and characteristics)
Eluents Used in Separation
Suppressor Columns
Detectors / Monitors Used
Instrumentation
Analytical Applications
No Suppressor Column
Ion Pair Chromatography
Ion Exclusion Chromatography

11 Thin Layer Chromatography
Introduction
What Makes it Different
Stationary Phases
Mobile Phases
Techniques of TLC
   Thin layer plates;
   General method; Special effects;
   Sample application; Development of the chromatogram
Two Dimensional Development
Location of the spots
Evaluation of the Chromatogram,
   Rf value; Use of an authentic substance
Quantitative Analysis
   Radioactive detection techniques
Applications of TLC
High Performance Thin Layer Chromatography (HPTLC)
Experiments in TLC
   Amino acid identification
   Detection of p-chloroacetanilide in paracetamol
   Separation and recovery of dyes
   Separation and identification of Ni2+ & Co3+ present together

12 Paper Chromatography
Introduction
Special Papers for PC
Ascending and Descending Techniques
Radial (circular) Paper Chromatography
Practical Details
   Choice of the chromatographic paper; Proper developing solvent; Application of the sample to paper; Development of the chromatogram; Drying of the chromatogram; Location of separated spots; Calculation of Rf values
Some Typical Separations
   Amino acids identification
   Separation of a mixture of sugars
   Separation of a mixture of dyes
   Separation of the plant pigments
   A study of food colours
   Two Dimensional Development

 
13 High Performance Liquid Chromatography
Introduction
Principles
Scope of HPLC
Instrumentation
Solvent delivery system; Pumping systems, (a) Constant flow reciprocating pumps,(b) Displacement pumps, (c) Pneumatic pumps; Sample injection systems; HPLC columns (a) Guard and scavenger column; Column thermostat; Stationary phase (column packing), (a) Microporous (or diffusive) particles, (b) Perfusion packing, (c)Non Porous packings, (d) Chiral Stationary phases, (e) Microbore columns (fast and efficient HPLC); Mobile phases; Effect of temperature; Detectors; Types of Detectors, Ultraviolet detectors, Refractive index detector; Evaporative light scattering monitor (ELSD), Fluorescence detector. Electorchemical detectors Infrared detectors,
HPLC - Mass Spectrometry
   Thermospray ionisation interface (TSI)
   Particle beam interface (PBI)
   Atmospheric pressure Chemical ionisation interface (APCI)
   Electrospray ionisation interface (ESI)
Derivatization
Optimisation of the HPLC Separations
Applications
Assessment of fruit juices for vitamin C using HPLC
      Analysis of analgesics using HPLC
   Assay of Hydrocortisone in the cream/ointment formulation
Questions

14 Gas Chromatography
Introduction
Gas-solid chromatography
Gas-liquid chromatography
Principles of Gas-Liquid Chromatography
Basic Components of a Gas Chromatograph
1. Carrier gas, Flow meter, Oven temperature programmer, Sample injection port, Heated analytical column, Detector, Recorder Basic Methodology
Components of a Gas Chromatograph (details)

1. Mobile phase and flow controls; Sample injection systems; Columns; Open tubular columns; Wall coated open tubular column(WCOT); Support coated open tubular (SCOT) columns; Porous layer open tubular (PLOT) columns; Fused silica open tubular (FSOT) columns; Stationary phases; Detectors; Thermostated compartment and temperature programmer Specialised Techniques in GC for Optimisation of a Separation
    (1) Temperature programming; (2) Derivatization; (3) Pyrolysis gas chromatography; (4) Thermal desorption; (5) Head-space analysis; (6) Purging and trapping
Applications of GLC
Qualitative identification; Quantitative analysis (peak height and peak area);
Interfacing Gas Chromatograph with spectroscopic Techniques
GC-mass spectrometry; GC-infrared spectrometry
Applications
Experimental Section
   Determination of elements in organic/organometallic compound
   Analysis of a tertiary mixture of hydrocarbons
   Determination of sucrose as its trimethylsilyl derivative
   Assay of caffeine and cylizine hydrochloride in the tablet
Questions

15 Supercritical Fluid Chromatography and Extractions
Introduction
Characteristics of Supercritical fluids
Supercritical Fluid Chromatography, Applications
Comparison of SFC with HPLC and GLC
Supercritical Fluid Extractions

16 Capillary Electrophoresis and Capillary Electrochromatography
Introduction
Electrophoresis (Slab or zone)
Some Parameters Affecting a Zone Electrophoresis Separation
   Ionic migration; Temperature, pH and ionic strength;
Electro-osmosis; Support; Detection of components; Applications
   Electro-osmotic flow (EOF)
Capillary Electrophoresis (CE)
CE System and its working; Sample injection; Detection in CE;
   Variations in CE
   Modes of HPCE
Capillary zone electrophoresis; Capillary gel electrophoresis (CGE); Capillary isoelectric focusing electrophoresis (CIFE)
Capillary Electrochromatography (CEC)
Questions

17 Refractometry and Interferometry
Introduction
Factors Affecting Refractive Index
Specific and Molar Refractions
Calculation of Molar Refractions
Quantitative Analysis of a Binary Mixture
Types of Refractometers
Calibration of Refractometers
Some Experimental Determinations
Determination of refractive index of a liquid using ABBe's refractometer and to find the specific and molar refractions
Determination of molar refractivity of some organic liquids and thereby to calculate the refraction equivalents of C, H, and Cl atoms.
To study the variations of refractive index with composition for the mixtures of CCl4 and CH3COOC2H5.
Determination of the concentration of D(+)-glucose in solution using Abbe's refractometer.
Estimate the corrected refractive index of a liquid that has an observed refractive index of 1.430 at 35°C.
Applications
The Interferometers

18 Chirality and Polarimetry
Introduction
Light-An Electromagnetic Wave
Optical Activity
Epimerization
Mutarotation
Osazones
Configurational Nomenclature
Cahn-Ingold-Prelog Convention
   (or, R and S System)
E-Z Convention
Threo and Erythro Convention
Specific and Molar Rotations
The Main Parts of a Polarimeter
Lippich prism (Lippich polarimeter)
Half shadow device
Laurent half-wave plate (Biquartz Polarimeter)
Some Experimental Determinations
   Determination of the specific rotation of sucrose
   Determination of the concentration of the given unknown solution
   Determination of concentration dependence of specific rotation
Photoelectric spectropolarimeters
Chiral Drugs
Optical Purity
Applications

19 Optical Rotatory Dispersion and Circular Dichroism
Introduction
Optical Rotatory Dispersion (ORD)
   Circular dichroism
Instrumentation for ORD
Application of ORD Spectra to Organic Molecules
Circular Dichroism (CD)
Instrumentation for CD
Applications of CD

20 Radiochemical Methods of Analysis
Introduction
Stable and Radioactive Nuclides
Nuclear Structure
Nuclear Stability (N/P Ratio) and Binding Energy
Radioactive Decay Processes
Alpha decay; Beta decay; Positron decay;
Orbital or K-electron capture; Internal conversion (x-ray emission); Gamma decay (isomeric transition)
Kinetics of Radioactive Decay
   Units of radioactivity
Nuclear Bombardment Reactions
Growth and Decay of Radioactivity
Counting Statistics
Detection and Measurement of Radioactivity
Gas ionisation detectors; Geiger tube; Proportional counters; Scintillation counters; Semiconductor counters; Photographic detection
Auxiliary Instrumentation
Gamma-Ray Spectrometers
Carrier Precipitation Methods
Radiometric Titrations
Radioactivation Analysis
Radioisotope Dilution Methods
Radio Immuno Assay (RIA)

21 Thermoanalytical Methods
Introduction
Thermogravimetry (TG), or, Thermo-gravimetric Analysis (TGA)
Differential Thermal Analysis (DTA)
Applications of DTA
Differential Scanning Calorimetry (DSC)
   Power compensated DSC; Heat-flux DSC; Applications of DSC
Thermometric Titrations
   Application of

22 X-Ray Methods of Analysis
Introduction
Production of X-Rays
Origin of X-Rays and X-Ray spectra
Electron Bombardment of Atoms (other accompanying processes)
Emission and Absorption X-Ray Spectra
    Sources for X-Rays
    Instrumentation
 X-ray producing assembly; Collimators; Filters; X-ray monochromator; Bragg's equation; X-ray detectors; Photo counting, p Signal processors; Pulse height discrimination
X-Ray Fluorescence Spectrometry
Wavelength dispersive devices; Energy dispersive devices; Applications
X-Ray Absorption Methods
X-ray Diffraction Methods
Identification of crystalline compounds; Preparation of the sample; Automatic diffractometers; Photographic recording; Study of diffraction patterns; Applications of x-ray diffraction measurements

APPENDICES

I        List of Significant Abbreviations in Analytical Chemistry
II       Seven Fundamental Units (Definitions)
III      How to Draw the Graphs
IV     Compounds Used for the Preparation of Standard Solutions of Some Elements
V      Some Physical Constants and Refractive Indices of Some Liquids
VI     Formation Constants for Some Complex Ions
VII    Elution Solvents for Chromatography
VIII  Composition of Common Buffer Solutions and Hazardous Chemicals (Carcinogens)