Analytical Chemistry I

GENERAL OBJECTIVES:

1. Understand the principles of analytical separations and their applications

2. Understand the principles of spectrophotometric techniques and their applications

1.1 Describe the principles of extraction using partition coefficients and separate phases.

1.2 Discuss the effects of pH on extraction

1.3 Discuss the basic principles of chromatography

1.4 List the different types of chromatography: adsorption; partition, ion-exchange; molecular exclusion/gel permeation; affinity chromatography.

1.5 Understand the fundamental differences between the types of chromatography in 1.4 above.

1.6 Calculate the retention time of a solute from a chromatogram

1.7 Discuss the relationship between retention time and the partition coefficient

1.8 Calculate the average volume percent of a compound from the peak areas

1.9 Explain the basic principles of gas chromatography

1.10 Draw a schematic diagram of a gas chromatograph

1.11 Understand the differences between packed and open tubular columns and when they may be used.

1.12 Discuss the different types of detector used with GC, e.g. electron capture, flame ionization, flame photometric.

1.13 Discuss the basic principles of HPLC

1.14 Draw a schematic diagram of a HPLC

1.15 Discuss stationary phases: polar and non polar and understand the difference between normal and reverse phase chromatography 1.16 Discuss the different types of detector: spectrophotometric, refractive index, evaporative lightscattering, electrochemical.

1.17 Discuss the criteria used to optimise separation: capacity factor, resolution, peak shape, operating pressure

1.18 Discuss the principles of ionexchange chromatography

1.19 Describe different types of resins and their applications

1.20 Discuss selectivity coefficients of resins and how this aids selection for analyte

1.21 Discuss the Donnan equilibrium and its role in ion-exclusion chromatography

1.22 Discuss the principles of ion chromatography for anion analysis

1.23 Discuss the principles of molecular exclusion/gel permeation chromatography

1.24 Discuss the types of gels used

1.25 Discuss the effect of molecular mass and shape on elution

1.26 Discuss the principles of capillary electrophoresis

1.27 Draw a schematic diagram of the apparatus used for capillary electrophoresis

1.28 Discuss the basic principles of electroosmosis

1.29 Calculate the apparent mobility using the electrophoretic mobility and electroosmotic mobility

1.30 Calculate the number of theoretical plates

1.31 Discuss experimental factors affecting the condition of the capillary wall

1.32 Discuss the type of sample injection: hydrodynamic and electrokinetic.

1.33 Discuss the process of stacking and its effect on the resulting chromatogram

1.34 Discuss the type of detectors used with CE and their application

1.35 Discuss the basic principles of Micellar electrokinetic chromatography

2.1 Explain the principle involved in qualitative identification of substances using flame tests.

2.2 Describe the three types of emission spectrometry.

2.3 Draw a schematic diagram of a flame photometer.

2.4 Describe the operation and working of a direct reading flame photometer.

2.5 Explain the error and interferences inherent in flame photometric analysis.

2.6 Describe the evaluation methods used in flame photometry.

2.7 Describe methods of preparing sample and stock solutions of standards in flame photometry.

2.8 Describe the general applications of flame photometry and its limitations in relation to AAS.

2.9 Explain the working principles of Atomic Absorption Spectrophotometer (AAS).

2.10 Draw the schematic diagram of AAS instrument.

2.11 Explain the errors and interferences in AAS.

2.12 Explain the advantages and disadvantages of AAS over flame photometer.

2.13 Discuss the use of graphite furnaces and inductively couples plasmas as the method of atomisation

2.14 Discuss the effect of temperature on AAS including the Boltzmann distribution

2.15 Discuss the use of background correction

2.16 Discuss the types of interference that may occur: spectral, chemical, ionisation

2.17 Explain the evaluation methods used in AAS.

2.18 Describe the preparation of sample and stock solutions of standards.

2.19 List the applications of atomic absorption spectrometry.

2.20 Explain the fundamental principles of infra-red spectroscopy (highlighting liberation of diatomic molecules and polyatomic molecules).

2.21 Classify molecular vibrations.

2.22 Describe the characteristic absorption frequency (group frequency) of certain groups in the molecules e.g. -OH; -COOH; -NH2; CO.

2.23 Explain how CO group frequencies are independent of the nature of the rest of the molecule.

2.24 Describe the components of an infra-red spectrometer e.g. light source, detector, monochromater etc.

2.25 Describe diagrammatically the outlay of IR spectrophotometer (single and double beam spectrophotometer).

2.26 Discuss the use of Fourier Transform (Michelson Interferometers)

2.27 Describe the preparation of substance for infra-red analysis using Nujol emulsion and KBr pellets etc.

2.28 Explain the use of infrared (IR) in elucidation of structure of molecules.

2.29 Explain the limitations of IR in analytical work.

2.30 Solve problems on IR spectroscopy.

2.31 Explain the fundamental principles of UV - Visible absorption spectrometry.

2.32 Classify electron transitions with relationship to UV-Visible absorption.

2.33 Explain the theory of light - absorption and transmission (Beer - Lambert’s law)

2.34 Apply the expression E1%1cm = A/C for intensity of absorption

2.35 Describe the spectra of the main classes of organic compounds - alkenes, unsaturated compounds, nitrogen compounds, nitrocompounds, aromatic compounds and heterocyclics.

2.36 Define the terms frequency used in the discussion of electronic spectra (e.g. chromophoresis, anxochromic shift, hypochromic shift, hyperchromic effect).

2.37 Illustrate diagrammatically the layout of UV - Visible spectrophotometer (power supply, light sources monochromators, detectors and measuring device).

2.38 Describe the optical layout of a double - beam UV - Visible spectrophotometer.

2.39 List the advantages of double beam over the single beam spectrophotometer.

2.40 Describe the operation of UV - Visible spectrophotometer.

2.41 Describe sample preparation for UV - Visible analysis.

2.42 Record the spectra of a sample

2.43 Outline the main applications of colorimetric and spectrophotometric analysis:

(a) spectrophotometric titration

(b) determination of pKa

(c) determination of pH of a given sample.

2.44 Explain the terms true fluorescence, phosphorescence, chemiluminescence and bioluminescence.

2.45 Differentiate between UV and fluorescence with respect to change in absorption maximum.

2.46 Explain how the intensity of fluorescence is proportional to the concentration of the substance in dilute solutions.

2.47 Explain the term “quantum yield”.

2.48 Explain the tem “quenching”.

2.49 Describe the various units of a spectrofluorimeter e.g. light source, photo-multiplier, recorder.

2.50 Describe diagrammatically the outlay of a spectroflourimeter.

2.51 Describe methods of preparation of a sample for analysis by spectroflourimetry.

2.52 Describe the operation of a flourimeter.

2.53 Explain the applications of flourimetry and its limitation in analytical work.