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Course Info for CHE260 - Instrumental Analysis

This course provides an intensive study of instrumental analysis for the evaluation, separation, isolation, and identification of the chemical components of a variety of both pharmaceutical and environmental samples.  Introductory topics covered are measurements, sampling protocol, methods involving the preparation of standards and the basic components common to most instruments.  Specific topics deal with sample preparation, instrument design, calibration, operation, data collection, spectral analysis and troubleshooting for each instrument being studied.  The instruments used in this course are UV/VIS, FTIR, AA, GC/MS and HPLC.  There are two hours of lecture and one three-hour laboratory per week.

PREREQUISITE:  

CHE112 - General Chemistry II or its equivalent

REQUIRED TEXTBOOK:

N/A

REQUIRED MATERIALS:  

Safety glasses are required for all on-campus sections.

COURSE OBJECTIVES:

As the result of instructional activities, students will be able to:

  • Obtain, store, log and prepare samples for instrumental analysis.
  • Obtain a fair amount of knowledge about environmental samples.
  • Prepare a variety of standards for use in instrumental analysis.
  • Calibrate a UV/VIS, FTIR, AA, GC/MS and HPLC.
  • Describe the theory of how each instrument works.
  • Operate a UV/VIS, FTIR, AA, GC/MS and HPLC.
  • Interpret spectral data of UV/VIS, FTIR, AA, GC/MS, and HPLC.
  • Troubleshoot when instrumental problems arise.

GENERAL TOPICS OUTLINE:

  1. Introduction to Chemical Instrumentation
  2. Measurements and Sampling Protocol
    1. Sampling
      1. Sampling & storage procedures
      2. Standard and sample preparation
      3. Basic units of measurement
    2. Instrument components
      1. Basic electronics
      2. Detectors
      3. Amplifiers and signal to noise ratio
      4. Microcomputers
      5. Data handling, display and storage
  3. Ultraviolet and Visible Spectroscopy (UV/VIS)
    1. Basic instrument design
    2. Sample preparation
      1. Standard curve
      2. Typical solvents used for analysis
      3. Cells and cruvettes
    3. Instrument operations
      1. Calibration
      2. Attenuation
      3. Zeroing
    4. Collection and interpretation of spectral data
      1. Basic chromophores
      2. Determining lambda max
      3. Beer's Law
      4. Interpolation and extrapolation of data
    5. Troubleshooting
  4. Gas Chromatography (GC)
    1. Basic instrument design
    2. Sample preparation
      1. Typical solvents used for analysis
      2. Internal and external standards
      3. Types of syringes and sample ports
    3. Instrument operations
      1. Carrier gases
      2. Column specifications
      3. Flow rates
      4. Calibration and theoretical plates
    4. Collection and interpretation of spectral data
      1. Rf values
      2. Peak height vs. area under the peak
      3. Determining unknowns
      4. Evaluation of spectra for successful separation of samples
      5. Evaluation of spectra for successful isolation of samples
      6. Evaluation of spectra for successful identification of samples
    5. Troubleshooting
  5. Mass Spectroscopy (MS)
    1. Basic instrument design
      1. Mass analyzers - quadrupole vs. ion trap
      2. Types of MS
    2. Sample preparation
    3. Instrument operations
      1. Calibration
      2. Signal processing
    4. Collection and interpretation of spectral data
      1. Mass-to-charge ratio
      2. Base peak determination
      3. Mass peak determination
      4. M+, M+2 and M+3 peaks
      5. Fragmentation patterns
    5. Troubleshooting
  6. GC/MS - Varian 2000 series
    1. Integration of the two instruments
      1. Method writing
      2. Separation and identification of samples
      3. Spectral analysis and reporting data
    2. Using the library
  7. High-Performance Liquid Chromatography (HPLC)
    1. Basic instrument design
    2. Sample preparation
      1. Typical solvents used for analysis
      2. Internal & external standards
      3. Mobile-phase preparation
      4. Polar vs. non-polar samples
    3. Instrument operations
      1. Determining mobile-phase reservoirs & treatment
        1. Isocratic vs. gradient elution
      2. Column specifications - normal vs. reverse phase
      3. Flow rates and pumps
      4. Detectors
      5. Calibration
    4. Collection and interpretation of spectral data
      1. Rf values
      2. Peak height vs. area under the peak
      3. Determining unknowns
      4. Evaluation of spectra for successful separation of samples
      5. Evaluation of spectra for successful isolation of samples
      6. Evaluation of spectra for successful identification of samples
      7. Improving separation efficiency
    5. Troubleshooting
  8. Fourier Transfer Infrared Spectroscopy (FTIR)
    1. Basic instrument design
    2. Sample preparation
      1. KBr pelleting
      2. 3M sample films
      3. "Neat" samples
      4. Rock salt cells
    3. Instrument operations
      1. Calibration
      2. IR sources & transducers
      3. Rotation and vibrational modes
      4. Optical system functions
    4. Collection and interpretation of spectral data
      1. Basic spectral analysis
        1. Functional group region analysis
        2. Fingerprint region analysis
        3. % Transmittance
        4. Wavenumbers
    5. Troubleshooting
  9. Atomic Absorption Spectroscopy (AA)
    1. Basic instrument design
      1. Flame atomization
      2. Graphite furnaces
      3. Lamps
    2. Sample preparation
    3. Instrument operations
      1. Calibration curves
      2. Standard addition method
      3. Flame control
      4. Detection limits
    4. Collection and interpretation of spectral data
      1. Method setup
      2. Spectral analysis
      3. Data reports
    5. Troubleshooting
Feel free to contact a member of the Science Department or the Science Department Chair.



 

 

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