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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