Instrumental Analysis Student Competencies

Principles of Instrumental Analysis, 7th. ed., Douglas A. Skoog, F. James Holler, Stanley R. Crouch, 2018.

Chapter 1 Student competencies

Upon completion of this chapter, students should be able to:

• Differentiate between Classical Methods of Analysis and Instrumental Methods of Analysis.
• Describe the different domains through which data is passed within a sophisticated instrument.
• Understand the terms detector, transducer, and sensor.
• Have a general knowledge of how to select an analytical method for chemical analysis.
• Calculate and interpret analytical figures of merit, including accuracy, precision, signal-to-noise ratio, sensitivity (calibration and analytical), limit of detection (LOD), linearity via log-log plots, and linear dynamic range (LDR)
• Utilize calibration, standard addition, and internal standard methods of analysis, as introduced in Quantitative Analysis.

Chapter 2 Student competencies

Upon completion of this chapter, students should be able to:

• Utilize the basic laws of electricity, including Ohm's Law, Kirchoff's current and voltage laws, and the power law to find voltage, current, resistance or wattage.
• Determine the total resistance in a series circuit or calculate voltage at various points in a voltage divider.
• Determine the total resistance in a parallel circuit or calculate the current at various points in a current divider.
• Differentiate between dc and ac circuits.
• Work with expressions for sinusoidal currents, including terms related to amplitude, period, frequency, angular velocity, and phase angle.

Chapter 3 Student competencies

Upon completion of this chapter, student should be able to:

• Understand purpose of an operational amplifier in instrument measurement including general structure of these integrated circuits.
• Understand difference between inverting and non-inverting inputs.
• Understand the operational modes used including comparator, voltage follower, and current follower.
• Know how operational amplifiers are used for current & voltage amplification.

Chapter 5 Student competencies

Upon completion of this chapter, students should be able to:

• Determine and interpret the meaning of the signal-to-noise ratio.
• Explain sources of instrumental noise, including shot, flicker, and environmental noise, and factors that influence the magnitude of each.
• Classify an instrument as shot or flicker noise limited.
• Understand the various hardware techniques used to reduce environmental and external electronic noise sources.
• Describe the purpose of differential and instrumental amplifiers in instrumental design as well as contrast the advantages and disadvantages of each type of amplifier
• Describe the purpose of high pass; low pass; and narrow band pass analog filters in instrument design.
• Discuss the technique of modulation/demodulation in noise reduction of dc signals.
• Describe how a lock-in amplifier works.
• Understand the various software techniques used to reduce noise including ensemble averaging, boxcar averaging, digital filtering, and Fourier transform.

Chapter 6 Student competencies

Upon completion of this chapter, students should be able to:

• Describe the wave and particle properties of electromagnetic radiation.
• Inter-convert between wavelength, frequency, period, energy, and wavenumber.
• Describe the relative ordering of the electromagnetic spectral regions and the types of transitions that occur in each region.
• Describe the superposition of wave theory, and how this relates to Fourier transform
• Describe diffraction of radiation.
• Define coherent radiation, blackbody radiation, fluorescence, phosphorescence, resonance fluorescence, Stokes and Anti-Stokes Shifts.
• Contrast line, band, and continuum spectra.
• Inter-convert between transmittance and absorbance data.
• Utilize Beer's Law to determine concentrations from absorbance data, and vice versa.

Chapter 7 Student competencies

Upon completion of this chapter, students should be able to:

• Describe and diagram the basic components in absorption, emission, and luminescence optical spectrometers
• List and describe some common light sources used in the infrared, visible, and UV regions of the electromagnetic spectrum
• Describe the differences between line, continuum, and quasi-continuum light sources, and the applications of each.
• Describe the components of a laser.
• Describe the four mechanisms involved in a laser and which processes contribute to or attenuate laser power.
• Describe various wavelength selectors including absorption filters, interference filters, and monochromators (Bunsen, Czerny-Turner, and Echelle.
• Describe how diffraction gratings disperse light.
• Utilize the grating formula to calculate wavelengths at various incident and reflected angles for various orders.
• Understand the terms single channel and multi channel radiation transducer.
• List and describe phototubes, photomultiplier tubes, and silicon photodiodes.
• List and describe linear diode arrays, charge coupled devices, and charge injection devices.

Chapter 13 Student competencies

Upon completion of this chapter, students should be able to:

• Differentiate between radiant power and intensity.
• Define and calculate transmittance and absorbance.
• Differentiate between absorptivity and molar absorptivity in Beer's Law
• Derive Beer's Law.
• Give limitations to Beer's Law
• Utilize Beer's Law in solving for concentration of mixtures and equilibrium concentrations.
• Describe what is meant by photometric error.
• Describe the components and arrangements of a single beam and double beam spectrophotometer and the purpose of each design.
• Describe common sources and detection systems used in molecular UV/Vis spectrometry.

Chapter 15 Student competencies

Upon completion of this chapter, students should be able to:

• Explain the terms resonance fluorescence, Stokes shift, diamagnetic, paramagnetic, singlet state, doublet state, and triplet state.
• Draw energy level diagrams representing fluorescence and phosphorescence indicating absorption, internal conversion, vibrational relaxation, intersystem crossing, fluorescence, and phosphorescence.
• Distinguish between fluorescence and phosphorescence.
• Define quantum yield.
• Discuss variables that affect fluorescent and phosphorescent quantum yield including structure relationships, type of transition, dissolved oxygen, heavy atoms, temperature and pH.
• Explain relationship between fluorescent intensity and concentration leading to quantitative methods of analysis
• Discuss sources of deviation from linearity for fluorescence including self-quenching and self-absorption
• Explain the difference between Excitation and Emission Spectra.
• Describe the typical components and arrangement of a typical spectrofluorometer.
• Describe the components used for phosphorimetry.
• Discuss standardization of fluorescence instruments
• Discuss methods of analysis in molecular luminescence including the use of fluorescent derivatives and measurement of luminescent lifetime.
• Use calibration curve and standard addition methods of analysis for concentration determination from luminescence measurements

Chapter 16 Student competencies

Upon completion of this chapter, students should be able to:

• Describe the various types of molecular vibrations and the factors that lead to infrared radiation absorption.
• Describe and utilize mathematical relationships from the classical and quantum mechanical models for molecular vibration to calculate vibrational frequencies.
• Calculate the number of normal modes of vibration for linear and non-linear molecules.
• Describe vibrational coupling and its consequences.
• Discuss various components of infrared spectrometers.
• Explain time and frequency domain spectroscopy
• Describe the frequency problem in time domain IR spectroscopy and a Michelson interferometer.
• Use mathematical relationships to relate interferogram to source frequencies.
• Use mathematical relationships to calculate resolution in Fourier transform instruments.
• Compare dispersive and Fourier transform IR spectrometers.

Chapter 18 Student competencies

Upon completion of this chapter, students should be able to:

• Describe the mechanism leading to Raman and Rayleigh scattering, including definition of virtual state, leading to Stokes and Anti-Stokes shifts.
• Compare the factors that lead to Raman spectra with infrared spectra.
• Describe the components of a typical Raman spectrometer.
• Convert frequency shifts in Raman spectra to wavelength for a given source.
• Explain how a depolarization ratio is determined in Raman and the information gained.

Chapter 19 Student competencies

Upon completion of this chapter, students should be able to:

• Describe how a proton NMR spectrum arises quantum and classical descriptions, including calculation of transition frequency and influence of magnetic field strength.
• Use Boltzman calculation for population of excited state.
• Describe saturation and relaxation processes in NMR
• Describe Fourier transform in NMR.
• Describe environmental influences to NMR signals including chemical shift and spin-spin splitting.
• Discuss decoupling techniques in NMR
• Describe the components of a typical FT-NMR.
• Describe the purpose of locking and shimming an NMR spectrometer.
• Describe and show how NMR can be used for qualitative analysis.
• Apply NMR theory to carbon-13 nuclei.
• Discuss application of 2-D NMR to structure elucidation.

Chapter 26 Student competencies

This chapter will be covered quickly for review of separation concepts.  You should be familiar with these and be able to:

• Define chromatographic separation terms including partition coefficient, retention time, retention volume, adjusted retention time and volume, capacity factor, relative retention, number of plates, and plate height.
• Understand the major driving forces that lead to chromatographic band broadening, including multiple path, longitudinal diffusion, and mass transfer.
• Understand the factors that influence resolution in chromatographic systems.
• Apply chromatographic systems to problems of qualitative and quantitative analysis.

Chapter 29 Student competencies

Upon completion of this chapter, students should be able to:

• Describe supercritical fluids including properties relative to gases and liquids, such as density, diffusion, and viscosity.
• Draw a block diagram for SFC instrument.
• Give examples of types of detectors used in SFC.
• Compare advantages & disadvantages of SFC relative to HPLC and GC.
• Describe the effect of pressure on chromatograms.
• Describe the advantageous properties of supercritical carbon dioxide.
• Compare supercritical fluid and liquid-liquid extractions.

Chapter 30 Student competencies

Upon completion of this chapter, students should be able to:

• Describe the separation mechanism in electrophoresis.
• Describe current appliations of electrophoresis.
• Draw a block diagram of a CE system.
• Compare CE and slab electrophoresis.
• Relate migration velocity to field strength and electrophoretic mobility.
• Describe how the structural features of substances influence electrophoretic mobility.
• Calculate plate height and number of plates in a capillary.
• Describe the mechanism of electroosmotic flow, and the effect on positive, negative and neutral analytes.
• Use van Deemter's equation to compare separation efficiency of CE relative to HPLC & GC.
• Discuss electrokinetic and hydrodynamic (pressure) injection methods in CE.
• Give examples of common detectors used in CE.