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Modern Instrumental Methods of Analysis
J.R. Mudakavi Dept. of Chemical Engineering
Indian Institute of Science, Bangalore
Qualitative analysisQuantitative analysis
characterization
Method development MultidisciplinaryProblem solvingBroader perspectives
Ions,organics,titrationsGravimetry,
Limited physical propertiesM.P,B.P,Viscosity
Classical & ModernInstrumental techniques
Statistics, electronicsComputers
Quditative schemes
Tools
Routine Analysis Cutting edge Technology
Tools
ANALYTICAL SCIENCEANALYTICAL 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 backscatteringX-ray fluorescenceNuclear reactions
2.3 SPADNS Method for fluoride determination
Development of APHA standard Method Interlaboratory and intralaboratory analysisDevelopment 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 interferentsSelect methodEstablish validation criteriaEstablish sampling strategy
5.Propose a solution
Conduct external evaluation
4.Analyze the experiment data
Reduce or transform dataAnalyse statisticsVerify resultsInterpret results
3.Conduct an experimentCalibrate instruments and
equipmentStandardize reagents
Gather data
Feedbackloop
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
What exactly is the analytical problem?
What type of input information is to be collected?
What criteria are to be considered in designing the experiment ?
What interferences are expected and how to eliminate the same?
How to collect ,store, transport and pretreat the samples
Validation of results
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;circularDichroism
• 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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contd
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contd
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contd
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