Syllabus of Combined Geo-Scientist (Main) Examination
Stage-II (Descriptive Type)
Chemistry : Paper-III (Analytical and Organic)
PART-A (Analytical Chemistry)
A1. Errors in quantitative analysis:
Accuracy and precision, sensitivity, specific standard deviation in analysis,
classification of errors and their minimization, significant figures, criteria for
rejection of data, Q-test, t-test, and F-test, control chart, sampling methods,
sampling errors, standard reference materials, statistical data treatment.
A2. Separation Methods:
Chromatographic analysis: Basic principles of chromatography (partition,
adsorption and ion exchange), column chromatography, plate concept, plate
height (HETP), normal phase and reversed phase concept, thin layer
chromatography, frontal analysis, principles of High Performance Liquid
Chromatography (HPLC) and Gas Liquid Chromatography (GLC), and Ionexchange
chromatography.
Solvent extraction: Classification, principle and efficiency of the technique,
mechanism of extraction, extraction by solvation and chelation, qualitative and
quantitative aspects of solvent extraction, extraction of metal ions from aqueous
solutions.
A3. Spectroscopic methods of analysis:
Lambert-Beer's Law and its limitations.
UV-Visible Spectroscopy: Basic principles of UV-Vis spectrophotometer,
Instrumentation consisting of source, monochromator, grating and detector,
spectrophotometric determinations (estimation of metal ions from aqueous
solutions, determination of composition of metal complexes using Job’s method
of continuous variation and mole ratio method).
Infra-red Spectrometry: Basic principles of instrumentation (choice of source,
monochromator and detector) for single and double beam instruments,
sampling techniques.
Flame atomic absorption and emission spectrometry: Basic principles of
instrumentation (choice of source, monochromator, detector, choice of flame
and burner design), techniques of atomization and sample introduction, method
of background correction, sources of chemical interferences and methods of
removal, techniques for the quantitative estimation of trace level metal ions.
Basic principles and theory of AAS. Three different modes of AAS - Flame-AAS,
VG-AAS, and GF-AAS. Single beam and double beam AAS. Function of Hollow
Cathode Lamp (HCL) and Electrode Discharge Lamp (EDL). Different types of
detectors used in AAS. Qualitative and quantitative analysis.
A4. Thermal methods of analysis:
Theory of thermogravimetry (TG), basic principle of instrumentation, techniques
for quantitative analysis of Ca and Mg compounds.
A5. X-ray methods of Analysis:
Introduction, theory of X-ray generation, X-ray spectroscopy, X-ray diffraction
and X-ray fluorescence methods, instrumentation and applications. Qualitative
and quantitative measurements. Powder diffraction method.
A6. Inductively coupled plasma spectroscopy:
Theory and principles, plasma generation, utility of peristaltic pump, sampler–
skimmer systems, ion lens, quadrupole mass analyzer, dynode / solid state
detector, different types of interferences- spectroscopic and non-spectroscopic
interferences, isobaric and molecular interferences, applications.
A7. Analysis of geological materials:
Analysis of minerals and ores- estimation of (i) CaCO3, MgCO3 in dolomite (ii)
Fe2O3, Al2O3, and TiO2 in bauxite (iii) MnO and MnO2 in pyrolusite. Analysis of
metals and alloys: (i) Cu and Zn in brass (ii) Cu, Zn, Fe, Mn, Al and Ni in bronze
(iii) Cr, Mn, Ni, and P in steel (iv) Pb, Sb, Sn in ‘type metal’.
Introduction to petroleum: constituents and petroleum fractionation. Analysis of
petroleum products: specific gravity, viscosity, Doctor test, aniline point, colour
determination, cloud point, pour point. Determination of water, neutralization
value (acid and base numbers), ash content, Determination of lead in petroleum.
Types of coal and coke, composition, preparation of sample for proximate and
ultimate analysis, calorific value by bomb calorimetry.
PART B (Organic chemistry)
B1. Unstable, uncharged intermediates:
Structure and reactivity of carbenes and nitrenes and their rearrangements
(Reimer-Tiemann, Hoffman, Curtius, Lossen, and Schimdt,).
B2. Addition reactions:
Addition to C-C multiple bonds: Mechanism of addition involving electrophiles,
nucleophiles and free radicals (polymerization reactions of alkenes and
substituted alkenes), Ziegler-Natta catalyst for polymerization, polyurethane,
and conducting polymers; addition to conjugated systems (Diels-Alder reaction),
orientation and reactivity (on simple cis- and trans- alkenes).
Addition to carbon-heteroatom multiple bonds: Addition to C=O double
bond, structure and reactivity, hydration, addition of ROH, RSH, CN-,
bisulphite, amine derivatives, hydride ions.
B3: Reactions at the carbonyl group:
Cannizzaro, Aldol, Perkin, Claisen ester, benzoin, benzil-benzilic acid
rearrangement, Mannich, Dieckmann, Michael, Strobe, Darzen, Wittig, Doebner,
Knoevenagel, Reformatsky reactions.
B4. Oxidation and Reduction:
Reduction of C=C, Meerwein-Pondorf reaction, Wolff-Kishner and Birch
reduction.
Oxidation of C=C, hydration, hydroxylation, hydroboration, ozonolysis,
epoxidation, Sharpless epoxidation.
B5. Electrocyclic Reactions:
Molecular orbital symmetry, frontier orbitals of ethylene, 1,3-butadiene, 1,3,5-
hexatriene, allyl system, FMO approach, pericyclic reactions, Woodward-
Hoffman correlation diagram method and perturbation molecular orbital (PMO)
approach for the explanation of pericyclic reactions under thermal and
photochemical conditions. Simple cases of Norrish type-I and type-II reactions.
Conrotatory and disrotatory motions of (4n) and (4n+2) polyenes with emphasis
on [2+2] and [4+2] cycloadditions, sigmatropic rearrangements- shift of H and
carbon moieties, Claisen, Cope, Sommerlet-Hauser rearrangement.
B6. Spectroscopic methods of analysis:
Infrared spectroscopy: Characteristic frequencies of organic molecules and
interpretation of spectra. Modes of molecular vibrations, characteristic
stretching frequencies of O-H, N-H, C-H, C-D, C=C, C=N, C=O functions; factors
affecting stretching frequencies.
Ultraviolet spectroscopy: Chromophores, auxochromes. Electronic transitions
(σ−σ*, n-σ*, π-π* and n-π*), relative positions of λmax considering conjugative
effect, steric effect, solvent effect, red shift (bathochromic shift), blue shift
(hypsochromic shift), hyperchromic effect, hypochromic effect (typical examples).
Woodward rules. Applications of UV spectroscopy to conjugated dienes, trienes,
unsaturated carbonyl compounds and aromatic compounds.
Nuclear Magnetic Resonance Spectrometry: (Proton and Carbon-13 NMR)
Nuclear spin, NMR active nuclei, principle of proton magnetic resonance,
equivalent and non-equivalent protons. Measurement of spectra, the chemical
shift, shielding / deshielding of protons, upfield and downfield shifts, intensity
of NMR signals and integration factors affecting the chemical shifts: spin-spin
coupling to 13C IH-IH first order coupling: some simple IH-IH splitting patterns:
the magnitude of IH-IH coupling constants, diamagnetic anisotropy.
Mass spectrometry: Basic Principles, the mass spectrometer, isotope
abundances; the molecular ion, metastable ions. McLafferty rearrangement.