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ACADEMIC SESSION 2019/2020

CHEM1108

ADVANCED INSTRUMENTAL ANALYSIS

Q1.    Answer ALL parts of this question

(a)      Explain the meaning of the following NMR terms:

(i)       NOESY

(ii)      HSQC

In your answer critically discuss the experiments, describe both the typical results and the structural  information  that  may  be  obtained  by  using  these  techniques.  Include  a  fully annotated diagram of the 2D spectral profiles (topology) expected for (i) and (ii).

[22 marks]

(b)     In NMR spectroscopy what does PFG stand for? What hardware is

required to run PFG experiments and suggest two advantages of using this application over non-PFG experiments?

[5 marks]

(c)      From your knowledge of the scientific literature critically evaluate the TOCSY NMR experiment. In your answer, provide possible applications for this technique.

[6 marks]

[Total 33 Marks]

Q2.    Answer ALL parts of this question

(a)

(i)       Draw and label a schematic diagram for the main components comprising a mass spectrometer.

[5 Marks]

(ii)     What process does each region of a mass spectrometer perform in

order to collect mass spectrometry data?

[8 Marks]

(b)     Identify the three possible reactions that can occur when a neutral

molecule, M, undergoes Electron Ejection Ionisation, labelling all

species present.

[6 Marks]

(c)      Consider the mass spectrum below, along with the molecular formula Cm HnXY, where X and Y represent halogen atoms.

 

(i)       Identify X and Y from a calculation of relative isotope abundance.

[12 Marks]

(ii)      Identify the monoisotopic Molecular Ion Peak, by mass-to-charge

ratio, in the mass spectrum given above.

[2 Marks]

[Total 33 marks]

Q3.    Answer BOTH parts of this question


(a)      In relation to Localised Thermal Analysis (LTA) critically discuss, provide

examples  and  describe  the  use  of  Localised  Thermal  Analysis  (LTA)/  Nano/Micro Thermal  Analysis  (nTA/μTA)  in  pharmaceutical  research.  State  the  advantages  and disadvantages  of  LTA  compared  to  the  other  techniques  used  to  analyse  surface properties of materials.

[18 marks]

(b)     What are the main attributes of the samples and analytical method that

we need to consider when selecting any appropriate analytical method for analysis of our target samples, provide examples?

[15 marks] [Total 33 marks]

Q4.    Answer ALL parts of this question

The following questions are related to chiral separations:

(a)      Discuss why pharmaceutical companies care about the chiral purity

of their compounds.

[8 marks]

(b)     Discuss how enantiomeric mixtures are separated.

[15 marks]

(c)      If you need to validate a specific chromatographic methodology, discuss how you evaluate the key validation parameters.

[10 marks] [Total 33 Marks]