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DEPARTMENT OF CHEMISTRY MSC SEM-1 (2012-13) ANALYTICAL CHEMISTRY

CLASSIFICATION OF ANALYTICAL METHODS


PRESENTED BY

PATEL SANJEEVKUMAR L

Analytical Chemistry deals with methods for

determining the chemical composition of samples.

Qualitative Analysis (identification) provides information about the identity of species or functional groups in the sample (an analyte can be identified). Quantitative Analysis provides numerical information of analyte (quantitate the exact amount or concentration).

Classification of Analytical Methods

1. Classical methods
Qualitative identification by color, indicators, boiling or melting points, odour

Quantitative mass or volume (e.g. gravimetric, volumetric)

Gravimetric Methods the mass of the analyte or some compound produced from the analyte was determined. Titrimetric Methods the volume or mass of a standard reagent required to react completely with the analyte was measured.

2. Instrumental methods Qualitative chromatography, electrophoresis and identification by measuring physical property (e.g. spectroscopy, electrode potential) Quantitative measuring property and determining relationship to concentration (e.g. spectrophotometry, mass spectrometry)

Spectroscopy:
Spectroscopy measures the interaction of the molecules with electromagnetic radiation. Spectroscopy consists of many different applications such as atomic absorption spectroscopy, atomic emission spectroscopy, ultraviolet-visible spectroscopy, x-ray fluorescence spectroscopy, infrared spectroscopy, Raman spectroscopy, nuclear magnetic resonance spectroscopy, and so on.

Mass spectrometry:
Mass spectrometry measures mass-to-charge ratio of molecules using electric and magnetic fields. There are several ionization methods: electron impact, chemical ionization, fast atom bombardment, and others.

Electrochemical method:
Electroanalytical methods measure the potential (volts) and/or current (amps) in an electrochemical cell containing the analyte.These methods can be categorized according to which aspects of the cell are controlled and which are measured. The three main categories are

Potentiometry: The difference in electrode potentials is

measured. The result of the analysis can be computed directly from the voltage of the cell, or the equivalence point of a titration known as potentiometric titration

Coulometry :

In these experiments, the total current passed is measured directly or indirectly to determine the number of electrons passed. Knowing the number of electrons passed can indicate the concentration of the analyte or, when the concentration is known, the number of electrons transferred in the redox reaction.

Voltammetry:The cell's current is measured while

actively altering the cell's potential. This method can reveal the reduction potential of an analyte and its electrochemical reactivity.

Conductometry:Methods based on electrical

conductance measurements are grouped under the term conductometry.

Optical Methods:
i) Emission Spectroscopy:
Emission spectroscopy is the method where the characteristic spectrum produced by excitation of elements is applied to qualitative and quantitative analysis

ii) Absorption Spectrometry:

Absorption spectrometry is based on the measurement of the absorption of electromagnetic radiation by matter.

iii) Ultraviolet and Visible Absorption Spectroscopy: Analytical methods which involve
the measurement of absorption of ultraviolet and visible radiation (wavelength range from 180 to 780 nm) by an atomic, ionic, or molecular species are known as ultra violet and visible spectroscopic

iv) Turbidimetry and Nephelometry:

These methods are applied to determine the concentrations of suspensions where small solid particles are homogeneously dispersed in the liquid medium.

v) Raman Spectroscopy :Raman spectroscopy

involves the scattering of electromagnetic radiation by a liquid (solution) following Raman effect (scattering with change of wavelength). Some other optical methods, namely, flame photometry, refractometry, polarimetry find applications in analytical laboratory

Thermal Methods:

Calorimetry and thermogravimetric analysis measure the interaction of a material and heat.

i) Thermogravimetric Analysis (TGA)


:Thermogravimetric

analysis (TGA) involves the measurement of mass of a sample as its temperature is increased at a linear rate. Plot of mass versus temperature known as thermogram persuits determination of thermal stabilities and sample compositions at different temperatures.

ii)Calorimetry :It involve measuring

the heat of chemical reactions or physical changes.

Separation Method:
i) Chromatography :Choromatography is a multistage
separation process in which the sample is applied on a stationary phase over which a mobile phase is percolated. Various solutes present in the sample are separated on the basis of differential migration. e.g, paper chromatography, thin-layer chromatography, liquid chromatography, high performance liquid chromatography, gas chromatography, gel chromatography, partition chromatography, ion exchange chromatography, etc

ii) Solvent Extraction :In solvent extraction, a desired

solute can be isolated/extracted by distributing it between two immiscible liquids.

iii) Electrophoresis: The movement of charged

particles in the influence of an electric field, in general, is known as electrophoresis.

iii) Ion Exchange :

Ion exchange is a stoichiometric process in which a solid (insoluble) material, known as ion exchanger, when comes in contact with an electrolyte solution takes either positive or negative ions and releases the ions of like charge (to maintain the stoichiometry) to the solution

REFERENCE
Principal of instrumental analysisSkoog , Holler & Crouch

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