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Modern Instrumental Methods of Analysis
J.R. Mudakavi
Dept. of Chemical Engineering
Indian Institute of Science, Bangalore
Qualitative analysis
Quantitative analysis
characterization
Method development
Multidisciplinary
Problem solving
Broader perspectives
Ions,organics,titrations
Gravimetry,
Limited physical properties
M.P,B.P,Viscosity
Classical & Modern
Instrumental techniques
Statistics, electronics
Computers
Quditative schemes
Tools
Routine Analysis Cutting edge Technology
Tools
ANALYTICAL SCIENCE
ANALYTICAL CHEMISTRY
2. Analytical Chemistry in Action
2.1 Automobile exhaust analysis
Sub-ppb analysis of PAHS
2.2 APXS sensor on Mars
Analysis of soils and rocks on Mars by
Rutherford backscattering
X-ray fluorescence
Nuclear reactions
2.3 SPADNS Method for fluoride determination
Development of APHA standard Method
Interlaboratory and intralaboratory analysis
Development of standard Reference material(SRM)
Data handling – statistical evaluation
1.Identify the problem
Determine type of information needed
(qualitative,quantitative,characterization,
or fundamental)
Identify context of the problem
2.Design the experimental procedure
Establish design criteria (accuracy,
Precision, scale of operation, sensitivity,
Selectivity, cost, ,speed )
Identify interferents
Select method
Establish validation criteria
Establish sampling strategy
5.Propose a solution
Conduct external evaluation
4.Analyze the experiment data
Reduce or transform data
Analyse statistics
Verify results
Interpret results
3.Conduct an experiment
Calibrate instruments and
equipment
Standardize reagents
Gather data
Feedback
loop
Marching ahead
• Resolving the contradictory evidence of a sportsman taking steroids
• Evaluating the endosulphan exposure to farmers, children and
pregnant ladies
• Developing rapid and sensitive detectors for chemical warfare
agents.
• Real time modeling and monitoring of an oil spill near a port.
• Developing miniaturized sensors for real time air quality monitoring
Problem solving – Multiple source, interactions
• Accuracy,precision,sensitivity and detection limit
• Amount of sample available, collection ,storage, transport and
pretreatment of the sample
• Number of samples to be analysed
• Validation of the method, equipment and results
• Report presentation, problem solution and external evaluation
• Cost considerations based on the above
Analytical inputs
9 What exactly is the analytical problem?
9 What type of input information is to be collected?
9 What criteria are to be considered in designing the experiment ?
9 What interferences are expected and how to eliminate the same?
9 How to collect ,store, transport and pretreat the samples
9 Validation of results
9 Can a successful solution is feasible at this stage?
Characteristic Properties Instrumental Methods
• Emission of radiation
• Absorption of radiation
• Scattering of radiation
• Refraction of radiation
• Diffraction of radiation
• Rotation of radiation
• Electrical potential
• Electrical charge
• Electrical current
• Electrical resistance
• Mass
• Mass-to-charge ratio
• Rate of reaction
• Thermal characteristics
• Radioactivity
• Emission spectroscopy (X-ray, UV, visible,
electron, Auger); fluorescence, phosphorescence,
and luminescence (X-ray, UV, and visible)
• Spectrophotometry and photometry (X-ray, UV,
visible, IR); photoaccoustic , spectroscopy
;nuclear magnetic resonance and electron spin
resonance spectroscopy
• Turbidimetry;nephelometry;Raman spectroscopy
• Refractometry;interferometry
• X-ray and electron diffraction methods
• Polarimetry;optical rotary dispersion;circular
Dichroism
• Potentiometry;chronopotentiometry
• Coulometry
• Amperometry;polarography
• Conductometry
• Gravimetry(quartz crystal microbalance)
• Mass spectrometry
• Kinetic methods
• Thermal gravimetry and titrimetry;differential
scanning calorimetry;differential thermal analyses;
thermal conductometric methods
• Activation and isotope dilution methods
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Absorption spectroscopy by Prof J R Mudakavi