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UNIVERSITI TEKNOLOGI MARA FINAL examination COURSE CHM510 APRIL 2010 3 HOURS INSTRUCTIONS TO CANDIDATES 1. This Question Paper consists of six (6) questions. 2. Answer ALL questions in the Answer Booklet. Start each answer on a new page. 3. Do not bring any material into the examination room unless permission is given by the invigilator.
UNIVERSITI TEKNOLOGI MARA FINAL examination COURSE CHM510 APRIL 2010 3 HOURS INSTRUCTIONS TO CANDIDATES 1. This Question Paper consists of six (6) questions. 2. Answer ALL questions in the Answer Booklet. Start each answer on a new page. 3. Do not bring any material into the examination room unless permission is given by the invigilator.
UNIVERSITI TEKNOLOGI MARA FINAL examination COURSE CHM510 APRIL 2010 3 HOURS INSTRUCTIONS TO CANDIDATES 1. This Question Paper consists of six (6) questions. 2. Answer ALL questions in the Answer Booklet. Start each answer on a new page. 3. Do not bring any material into the examination room unless permission is given by the invigilator.
FINAL EXAMINATION COURSE COURSE CODE EXAMINATION TIME ANALYTICAL SEPARATION METHODS CHM510 APRIL 2010 3 HOURS INSTRUCTIONS TO CANDIDATES 1. This question paper consists of six (6) questions. 2. Answer ALL questions in the Answer Booklet. Start each answer on a new page. 3. Do not bring any material into the examination room unless permission is given by the invigilator. 4. Please check to make sure that this examination pack consists of: i) the Question Paper ii) an Answer Booklet - provided by the Faculty DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO This examination paper consists of 6 printed pages Hak Cipta Universiti Teknologi MARA CONFIDENTIAL CONFIDENTIAL 2 AS/APR 2010/CHM510 QUESTION 1 a) Optimizing flowrate is one of the important steps in chromatographic analysis. Explain based on van Deemter plot. (6 marks) b) The separation of 4 compounds gave resolution values of 0.5, 1.8 and 10.5. Sketch the chromatogram and comment on the efficiency of separation. (5 marks) QUESTION 2 a) Give a reason for each of the following situation: i) In gas chromatography (GC) analysis, injection temperature is normally set higher than column temperature. (2 marks) ii) Identification of compound is more confirmative by using mass spectrometer as a detector compared to UV detector. (2 marks) iii) For the analysis of biological sample using HPLC, a guard column is normally required. (2 marks) iv) Pressure restrictor is vital in supercritical fluid chromatography (SFC) system. (2 marks) b) Discuss a suitable approach to separate a sample mixture containing volatile and non- volatile compounds with a wide range of polarity by using: i) Gas chromatography (GC) (4 marks) ii) High performance liquid chromatography (HPLC) (4 marks) iii) Supercritical fluid chromatography (SFC) (4 marks) Hak Cipta Universiti Teknologi MARA CONFIDENTIAL CONFIDENTIAL 3 AS/APR 2010/CHM510 QUESTION 3 Figure below shows a gas chromatogram of a sample mixture consisting of normal alkanes and chlorinated benzenes separated on a bonded phase column 100 m x 250 urn x 0.25 urn with helium as the carrier gas at 25 cm/s. The column temperature was 120 C. 1.0 uL of sample was injected using split ratio 1/25. 1.2 1 L 6 7 . < , , mm a) b) c) What does bonded phase column mean? Give the internal diameter of the above column. (2 marks) (1 mark) Assume that the first three peaks refer to chlorinated benzenes while the last four peaks refer to normal alkanes. i) Is the column used in the above separation a polydimethyl siloxane (PDMS) or polyethylene glycol (PEG)? Explain. (3 marks) ii) Is the detector employed in the above separation a flame ionization detector (FID) or electron capture detector (ECD)? Explain. (3 marks) Hak Cipta Universiti Teknologi MARA CONFIDENTIAL CONFIDENTIAL 4 AS/APR 2010/CHM510 d) Describe (with reason/s) the changes you expect in the chromatogram if i) the column temperature is increased to 160 C. (2 marks) ii) the carrier gas is changed to nitrogen using the same velocity. (2 marks) e) Can the injection mode be changed to splitless using the same GC conditions? Explain. (3 marks) f) The retention indexes for compounds 1-3 changed when the stationary phase is changed. However the retention indexes for compounds 4-7 remain unchanged. Explain why. (2 marks) g) Based on the above chromatogram, if compound 4 is heptane, give an approximate value of retention index for compound 3. (2 marks) QUESTION 4 a) A sample mixture containing acetophenone, phenol, 7-hydroxyphenol and methyl benzene was analyzed using HPLC with a mobile phase system of acetonitrile/water 80/20 and a UV detector set at a wavelength of 420 nm. Quantitative analysis was done using external standard method. Discuss the reason for each of the following problems encountered and suggest an approach to overcome the problem. i) Very low detection signals were obtained. (3 marks) ii) The first two peaks were not separated well. (In your discussion include the possible compounds for these peaks). (4 marks) iii) After doing five replicate measurements, the peak areas obtained vary considerably. (3 marks) Hak Cipta Universiti Teknologi MARA CONFIDENTIAL CONFIDENTIAL 5 AS/APR 2010/CHM510 b) Suggest and describe a suitable type of a specific liquid chromatography technique to separate two of the following samples (include the mobile phase, stationary phase, detector and principle of separation in the description): i) A dam water sample with pH 3 containing several basic metals. (6 marks) ii) A sample containing carbohydrates namely cyclodextrin compounds. (6 marks) iii) A sample mixture of alpha and gamma tocopherol compounds (fat soluble vitamins). (6 marks) QUESTION 5 a) Electroosmotic flow or EOF is the bulk flow of fluid in a capillary electrophoresis caused by migration of the dominant ions in the diffuse part of the double layer toward the anode or cathode. i) If the capillary was untreated, what is the direction of the EOF? (1 mark) ii) EOF is pH dependent. Explain why and how does this affect the migration time? (3 marks) iii) Give two steps that are necessary for the analysis of anions. (2 marks) b) Capillary zone electrophoresis (CZE), capillary gel electrophoresis (CGE) and micellar electrokinetic capillary chromatography (MEKC) are three different types of electrophoresis mainly used to separate ionic compounds. Explain how they complement each other in their applications. (6 marks) Hak Cipta Universiti Teknologi MARA CONFIDENTIAL CONFIDENTIAL 6 AS/APR 2010/CHM510 QUESTION 6 a) Liquid-liquid extraction (LLE), solid phase extraction (SPE) and solid phase microextraction (SPME) are three different techniques used to extract analytes from liquid samples. Each of these techniques produces extract with different quality which may or may not require clean up and pre-concentration step. Explain briefly. (6 marks) b) Explain why the recovery of analytes in supercritical fluid extraction (SFE) is simple compared to conventional solvent extraction. (3 marks) c) Pressurized liquid extraction method was used to extract atrazine pesticide from an agricultural soil sample. Methanol/water was chosen as the extraction solvents employed at high temperature and pressure. Nitrogen gas was also used in this method. After 10 minutes the sample extract was collected and was then filtered before injected into HPLC system for further analysis. i) Why was methanol/water chosen as the extraction solvents? (2 marks) ii) What was the function of the nitrogen gas? (2 marks) iii) If the methanol/water was employed at ambient temperature and pressure, what do you think might happen to the extraction? (2 marks) END OF QUESTION PAPER Hak Cipta Universiti Teknologi MARA CONFIDENTIAL