1.  Introduction to Instrumental Analysis (Upali)

 1. Describe following terms associated  measurements using an instrument:

a) *Precision & accuracy

b) Absolute error

c) Population mean 

d) *Population Standard Deviation 

2.  Describe following terms involved with an instrument

a) Data Domains

b) Detector

c) Transducer

d) Sensor

e) Monochromator 

3. Describe following terms and methods associated with instrumental analysis

a) *Standard sample

b)  Blank sample

c) *Calibration curve

d) *Dynamic range.

e) *Linear regression

f) Standard Addition Method

 4.  Describe following terms associated with instrumental analysis

a) *Sensitivity

b) *S/N ratio

c) *Fourier Transformation (FT) in increasing sensitivity and  S/N ratio

d) *Detection Limit,  DOL, and  DOQ.

e) Matrix and interference

9. Atomic Absorption and Atomic Fluorescence Spectrometry. (Upali)

1)* Describe following atomization techniques and compare their performance:

a) Flame atomization

b) Electrothermal atomization ( graphite furnace method)

       2. Describe how a hollow cathode lamp work as a radiation source for atomic absorption spectrometer.

       3. Describe how single and double beam atomic absorption spectrometers correct absorption or scattering due to flame.

      4.  Describe how two line, continuum-source and Zeeman-effect correct the back ground absorption in atomic absorption due to spectrometers.

      5. *Describe following interferences in atomic absorption and how it is minimized.

a) Spectral interferences

b) Chemical interferences

      6. Describe following chemical interferences due to:

      a) Low volatile compounds

      b) dissociation equilibria

      c) Ionization equilibira   

13. An Introduction to Ultraviolet/Visible Molecular Absorption Spectrometry. (Snow)

 1. *What is Beer's Law.

2. Derive the formula for Beer's Law.

3. *What are the limitations of Beer's Law. 

16. An Introduction to Infrared Spectrometry. (Frank)

1. *State the selection rule for infrared-active molecules. Also, give an example of a molecule that is IR-active and identify an IR-active bond in the molecule, as well as where one would find its transition (what frequency?).

2. *Discuss the effects of bond strength and reduced mass on the frequency of an IR transition. That is, how does the frequency depend on these parameters?

3. Explain why it is that one must ensure that solvents and analytes are dry before their use in IR spectrometry experiments. There are multiple reasons. For example, what happens to the sample container and how does that influence the quality of the data, both from a signal/noise/background point of view and a chemical point of view?

4. *Discuss whether IR spectrometry is a quantitative or qualitative technique (or both, and if both, when is this the case?).

 

19. Nuclear Magnetic Resonance Spectroscopy. (Upali)

  1. *Why are internal standards such as TMS added to samples?
  2. What is the structure of TMS, and why is it a good standard?
  3. Why is CDCl3 the most common nmr solvent?
  4. Why does a superconducting cryomagnet produce such a strong magnetic field?
  5. What temperature is the magnet? How is it maintained at that temperature?
  6. What is the temperature of the sample when it is in the magnet?
  7. Why is the magnet filled with liquid nitrogen every week?
  8. What are shim coils, and why are they necessary?
  9. Why is the sample tube spun?
  10. What frequency does our nmr use for proton spectra?
  11. What is meant by a "90o pulse?"
  12. *What is meant by "relaxation?"
  13. How does relaxation of nuclei generate a signal in the detector?
  14. What is the FID, or interferogram? Why does the detector substract the carrier frequency from the detected FID?
  15. Why does adding multiple scans increase the signal-to-noise ratio?
  16. *How does the signal-to-noise ratio vary with the number of scans?
  17. *Why is it necessary to lock onto the solvent?
  18. What does a Fourier transform accomplish?

20. Molecular Mass Spectrometry (Cox) 

1.    What units are used for the mass of molecular ion?

2.    What are the components of a mass spectrometer?

3.    *What methods are available in MS to produce  ions?

4.    *Compare chemical ionization (CI) and electron impact (EI) ionization methods.

5.    *What types of mass analyzers are used in mass spectroscopy?

6.    Describe quadruple and ion-trap mass analyzers.

7.    What types of detection methods are used in mass spectroscopy.

8.    Calculate the ratios of the (M+1)+ to M+ peak heights for the following compounds: dinitrogenbenzene(C6H4N2O4) and an olefin (C12H24),

9.    What is characteristic of fragmentation pattern of: 1) alcohols, and  2) carbonyl compounds?

10.     Describe the Nitrogen Rule” in Mass Spectrometry.

11.     *Interpret the mass spectra of following compounds.

 

27. Gas Chromatography. (Plamer)

1. *What are the four parameters that can be changed to achieve best separation of componenets in a GC experiment

2. *Whats the difference between FID and TCD?

3. *What criteria you use to select a column.


28. High-Performance Liquid Chromatography. (Elmore)[Bill B. Elmore

  1. List a reason the HPLC is designed to operate with minimal flow volumes and at high pressure.
  1. List two mechanisms used for separation in HPLC applications:

  

  1. What is “band-broadening”?
  1. Define the terms:
    1. Mobile phase—
    2. Stationary phase—

5.  True or False:          As packing particle size is decreased, the efficiency of the column (e.g. its ability to separate components) decreases.

           

 

31. Thermal Methods. (Upali)

1. Describe what quantity is measured and how the measurement is performed for each of the folowing techniques:

a) Thermogavimetric Analysus

b) Differential Thermal Analysis

c) Differential Scanning Calorimetry

2.*The following table summarizes some data about three iron(II) chlorides.

compound                 Molecular weight               Melting point

FeCl3. 6H2O                   270                               37

FeCl3. 5/2H2O                207                               56

FeCl3                                162                             306

Sketch the thermogravimetric curve anticipated if 25.0 mg sample of FeCl3. 6H2O is heated from 0 to 400 C

3) List types of physical and chemical changes that can yield exothermic and endothermic peaks in DAT and DSC?                   

12. Atomic X-Ray Spectrometry

1. *What are the three methods that are being used in X-ray analysis?

2. How do you produce a X-ray beam?

3. *What is X-ray Fluoresence Sepctroscopy?

4. Expalin how elemental analysis is carried out in X-ray Fluoresence Sepctroscopy?