THE UNIVERSITY OF THE WEST INDIES

ST. AUGUSTINE


EXAMINATIONS OF APRIL/MAY 2008


Code and Name of Course: CHEM 3468 (C31F) ADVANCED ANALYTICAL CHEMISTRY

Date and Time: Duration: Three (3) hours

INSTRUCTIONS TO CANDIDATES: This paper has FIVE ( 5) pages and Seven (7) questions

The University of the West Indies Course Code CHEM 3468 (C30F) 2007/2008/.
___________________________________________________________________________________________________________

DO NOT WRITE OR TYPE ON THE BACK OF THIS SHEET: USE ONE SIDE ONLY

INSTRUCTIONS: Each page must be signed by the Examiners and where applicable, the University Examiner and/or
the External Examiner. Where the examination does not require a University Examiner, the form must be signed by the First
and Second Examiners. Completed forms should be handed to the Assistant Registrar (Examinations). The EXTERNAL
EXAMINER is requested to sign the question paper and return it with comments, it any, (on a separate sheet), to the Assistant
Registrar (Examinations).

. ..
First Examiner University Examiner

.
Second Examiner External Examiner (where applicable)

Date: 20/../.. Date: 20..//
1




Answer FIVE (5) Questions, at least TWO (2) from each section


Non-programmable calculators with statistical functions
may be used in this examination.



Statistical tables and graph paper are to be provided.


























PLEASE TURN TO THE NEXT PAGE

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The University of the West Indies Course Code CHEM 3468 (C30F) 2007/2008/.
___________________________________________________________________________________________________________

DO NOT WRITE OR TYPE ON THE BACK OF THIS SHEET: USE ONE SIDE ONLY

INSTRUCTIONS: Each page must be signed by the Examiners and where applicable, the University Examiner and/or
the External Examiner. Where the examination does not require a University Examiner, the form must be signed by the First
and Second Examiners. Completed forms should be handed to the Assistant Registrar (Examinations). The EXTERNAL
EXAMINER is requested to sign the question paper and return it with comments, it any, (on a separate sheet), to the Assistant
Registrar (Examinations).

. ..
First Examiner University Examiner

.
Second Examiner External Examiner (where applicable)

Date: 20/../.. Date: 20..//
2
S E C T I O N A


1. A medium size local manufacturing company, which produces a popular range of preserved mango
relishes, wishes to export its products to a European supermarket chain.
However, accurate labeling of artificial food colorants and preservatives in food products is required by
law in the buyers country. In addition, the buyer insists that the local manufacturer must provide
assurance of the ongoing quality of its products.

Suggest how the manufacturer can meet these requirements for export to its new customer in the shortest
possible time. Pay special attention to the costs to be incurred in implementation of the quality systems
required, versus their potential benefits.
(20 marks)

2. (a) Describe how Shewart control charts may be used to monitor and control the quality of
laboratory analyses.
Provide suitable equations, examples and fully labeled diagrams to illustrate your answer.
(12 marks)

(b) A container load of bathroom soap, consisting of 12,000 tablets, is selected from two batches of
7,500 and 6,500 tablets respectively.

The mass per tablet of the soap is set at 120 + 2g and the shipment of soap is to be inspected at
AQL 1.0 at Inspection Level II. Describe how you would undertake this inspection to decide
whether the batch meets this product specification, with special emphasis on the sampling,
inspection and the criterion for decision-making. (Tables to be supplied)

(8marks)



PLEASE TURN TO THE NEXT PAGE
Page




The University of the West Indies Course Code CHEM 3468 (C30F) 2007/2008/.
___________________________________________________________________________________________________________

DO NOT WRITE OR TYPE ON THE BACK OF THIS SHEET: USE ONE SIDE ONLY

INSTRUCTIONS: Each page must be signed by the Examiners and where applicable, the University Examiner and/or
the External Examiner. Where the examination does not require a University Examiner, the form must be signed by the First
and Second Examiners. Completed forms should be handed to the Assistant Registrar (Examinations). The EXTERNAL
EXAMINER is requested to sign the question paper and return it with comments, it any, (on a separate sheet), to the Assistant
Registrar (Examinations).

. ..
First Examiner University Examiner

.
Second Examiner External Examiner (where applicable)

Date: 20/../.. Date: 20..//
3
3. Using appropriately labeled diagrams, describe briefly the designs and mechanisms of operation of
two (2) of the following sources used in emission spectroscopy (ES).

(i) The inductively coupled plasma discharge lamp (ICP).
(ii) The DC arc.
(iii) The AC spark.

Which of the above sources are best suited for both qualitative and quantitative analysis. Give reasons
for your answer.
(2 x 10 marks)


4. Write short explanatory notes on Any TWO (2) of the following techniques, with special emphasis on
principles of operation and their applications in analytical separations:

(a) Supercritical Fluid Chromatography (SFC).
(b) Capillary Electrophoresis (CE).
(c) Ion Chromatography (IC) with membrane suppressors.
(2 x 10 marks)






END OF SECTION A






PLEASE TURN TO THE NEXT PAGE
Page




The University of the West Indies Course Code CHEM 3468 (C30F) 2007/2008/.
___________________________________________________________________________________________________________

DO NOT WRITE OR TYPE ON THE BACK OF THIS SHEET: USE ONE SIDE ONLY

INSTRUCTIONS: Each page must be signed by the Examiners and where applicable, the University Examiner and/or
the External Examiner. Where the examination does not require a University Examiner, the form must be signed by the First
and Second Examiners. Completed forms should be handed to the Assistant Registrar (Examinations). The EXTERNAL
EXAMINER is requested to sign the question paper and return it with comments, it any, (on a separate sheet), to the Assistant
Registrar (Examinations).

. ..
First Examiner University Examiner

.
Second Examiner External Examiner (where applicable)

Date: 20/../.. Date: 20..//
4
S E C T I O N B


5. A detergent manufacturing plant is suspected to be discharging levels of phosphate in its wastewater, in
violation of local environmental standards. You are required to undertake a project to monitor the
phosphate concentration in the companys wastewater over a 2-week period, with 2L of sample to be
taken every 4 hours, to verify whether the company meets the environmental standards. A report of the
project is expected within 14 days of completion of sampling.

Total phosphate is determined as follows:

(a) Pipette triplicate 5mL aliquots of each water sample into boiling tubes.
(b) Add 1mL concentrated nitric acid and reflux at 130
0
C for 4 hours.
(c) Cool, filter into 25mL volumetric flasks, make to volume with distilled water and mix well.
(d) Transfer 5mL of each extract into a test tube, add 0.2mL phosphomolybdate reagent and allow to
stand for 1 hour.
(e) Measure the blue color of a series of similarly prepared phosphate standard solutions at 800nm
with a spectrometer, followed by the sample solutions.
(f) Calculate the phosphate concentrations of the original sample solutions and compare them with
maximum allowed levels for discharged wastewater.

Describe how would you use batch and automated processing to achieve the projects objectives. Pay
special attention to personal and occupational health and safety requirements, statistical treatment of the
data generated and justification of the cost of any special equipment, instrumentation or software you
would use in the execution of this project. (20 marks)





PLEASE TURN TO THE NEXT PAGE
Page




The University of the West Indies Course Code CHEM 3468 (C30F) 2007/2008/.
___________________________________________________________________________________________________________

DO NOT WRITE OR TYPE ON THE BACK OF THIS SHEET: USE ONE SIDE ONLY

INSTRUCTIONS: Each page must be signed by the Examiners and where applicable, the University Examiner and/or
the External Examiner. Where the examination does not require a University Examiner, the form must be signed by the First
and Second Examiners. Completed forms should be handed to the Assistant Registrar (Examinations). The EXTERNAL
EXAMINER is requested to sign the question paper and return it with comments, it any, (on a separate sheet), to the Assistant
Registrar (Examinations).

. ..
First Examiner University Examiner

.
Second Examiner External Examiner (where applicable)

Date: 20/../.. Date: 20..//
5
6. Describe in detail the theoretical principles involved in the design and operation of a magnetic sector
analyzer used in Mass Spectrometry (MS).

A mass spectrometer with the above analyzer is often referred to as a single focusing instrument and
the resolution of the instrument is limited to R 2000 due to the inability of the magnetic field to bring
ions with different directional orientations and translational energies to focus.

Explain how this problem has been overcome in a double focusing instrument, where resolutions of up
to R = 10,000 is easily achieved.
(20 marks)


7. Provide a brief description of ANY TWO (2) of the following techniques:

(a) Electron microscopy of biological samples
(b) Velocity analysers in photoelectron spectroscopy
(c) X-Ray microanalysis
(d) Atomic force microscope cantilever tips

(2 x 10 marks)



END OF SECTION B


END OF EXAMINATION PAPER