CONFIDENTIAL, TIME ASIDEC 2018/CHM260 UNIVERSITI TEKNOLOGI MARA FINAL EXAMINATION COURSE BASIC INSTRUMENTAL ANALYSIS: COURSE CODE : CHM260 EXAMINATION : DECEMBER 2018 2 HOURS INSTRUCTIONS TO CANDIDATES This question paper consists of thirteen (13) questions. ‘Answer ALL questions in the Answer Booklet. Start each answer on a new page. Do not bring any material into the examination room unless permission is given by the invigilator. The use of calculator is allowed. Please check to make sure that this examination pack consists of i) the Question Paper il) a one-page Appendix iii) an Answer Booklet — provided by the Faculty ‘Answer ALL questions in English. DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO This examination paper consists of 5 printed pages (© Hak Cipta Universiti Teknologi MARA CONFIDENTIAL,CONFIDENTIAL 2 ASIDEC 2018/CHM260 QUESTION 1 a) Calculate the energy of an electromagnetic radiation with a wavelength of 322 nm. (2 marks) b) A 20.5 mg sample of a dark-orange compound (molecular mass = 536.89 gol") was dissolved with a solvent in a 100 mL volumetric flask. The absorbance of this solution at 451 nm was 0.856 in a 1.00-cm cuvette. Calculate the molar absorptivity of this compound. (3 marks) QUESTION 2 a) Define the term ‘chromophores’ (1 mark) b) The following is the block diagram of a single beam instrument. Identify the components labelled A, B, C and D. 8 Photo- Source ea— A ——+|¢ |] |—-[ iene J D > (4 marks) QUESTION 3 Differentiate between the cause of Beer's Law real and instrumental devi nin UV-Vis analysis. (6 marks) QUESTION 4 a) Illustrate a well-labelled energy diagram of four (4) possible electronic transitions for an ‘organic compound in the UV-Vis region. (4 marks) b) Based on your answer in (a), select which two (2) electronic transitions occur in the C=O functional group. (2marks) (© Hak Cipta Universiti Teknologi MARA CONFIDENTIAL,CONFIDENTIAL 3 ASIDEC 2018/CHM260 ¢) Distinguish between the types of compounds analysed using UV-Vis and IR spectroscopy. (4 marks) QUESTION 5 a) State the characteristic of an IR active molecule. (2 marks) b) Describe the preparation procedures for the analysis of pure citronellal oil using the IR instrument. (3 marks) QUESTION 6 a) Arrange the given bonds in the order of increasing frequency. C=O, C-0, OH, C=C (2 marks) b) Predict the bond which is responsible for the strong absorption at 3100-3000 om" in the IR spectrum of toluene. Given Toluene CH. (1 mark) c) Based on the following IR data, relate about the structure of the given compound. Molecular formula : CsH;z0 IR spectrum A broad and strong absorption peak at 3600-3200 cm” : No absorption peak at 1760-1670 cm (2 marks) (© Hak Cipta Universiti Teknologl MARA CONFIDENTIALCONFIDENTIAL 4 ASIDEC 2018/CHM260 QUESTION 7 a) Define the terms ‘volatilization’ and ‘atomization’ in flame atomic absorption spectroscopy. (3 marks) b) Briefly explain the function of a chopper in a flame atomic absorption spectrometer. (2 marks) QUESTION 8 a) Determine the type of interference which is caused by the presence of another atomic absorption line close to the spectral line of the element of interest. (2 marks) b) Provide any two (2) possible methods to prevent the interference described in question 8a) above: (3 marks) QUESTION 9 Separation of lemongrass oil using gas chromatography produced two major compounds Which are G and H. For compound G, the retention time was 5.2 min with the width at baseline of 1.6 min. While for compound H, the retention time was 7.8 min with the width at baseline of 1.4 min. A non-retained compound generated a peak at 0.8 min after injection. Calculate: a) The capacity factor (k’) for compound G and H. (3 marks) b) The resolution (R,) achieved of compound G and H. (2 marks) QUESTION 10 a) Briefly explain why molecules such as Nz and propadiene (Molecular formula: CH,=C=CH,) do not absorb IR radiation (2 marks) b) Describe any two (2) methods which can improve the efficiency of a chromatographic column in a gas chromatography (GC) separation. (3 marks) (© Hak Cipta Universiti Teknologi MARA CONFIDENTIALCONFIDENTIAL, 5 ASIDEC 2018/CHM260 QUESTION 11 a) Isothermal run was used for the separation of ethanol (bp: 78.4°C) and isopropyl alcohol (bp: 82.6°C) in a GC experiment. Propose why an isothermal run was selected rather than the temperature programming method. (bp = boiling point) (2 marks) b) Write the suitable GC detector for each of the following sample: R - Saturated, unsaturated and aromatic hydrocarbons S - Nitriles, quinones and nitro compounds (3 marks) QUESTION 12 a) List any two (2) reasons why sometimes it is necessary to use gradient elution in HPLC. (3 marks) b) Suggest the suitable liquid chromatography technique for the separation of water- insoluble polymers in which the component with the highest molecular weight is collected as the first fraction. (2marks) QUESTION 13 The experimental condition of a reversed-phase liquid chromatography is as follows: Length of column: 25 cm Stationary phase : C18 bonded phase particles Mobile phase —_: 60% water, 40% methanol Flow rate 20.4 mLimin a) Based on the information above, relate why it is categorized as reversed-phase liquid chromatography. (2 marks) b) Propose the elution order of a mixture containing aromatic hydrocarbon, ester and alcohol using the given HPLC condition. (3 marks) END OF QUESTION PAPER (© Hak Cipta Universiti Teknologi MARA CONFIDENTIALCONFIDENTIAL, APPENDIX 1 ASIDEC 2018/CHM260 SOME CHARACTERISTIC IR ABSORPTION BANDS Wavenumber, cm* Bond Functional Group 2960-2850(s) C-H (sp) | Alkanes zr aon ga -200060, 1c | arts 3080 — 3020 (m) C-H (sp*) | Alkenes 3100 - 3000 (rm) C-H__ | Aromatic Rings 3333 - 3267 (s) C-H (sp) | Alkynes 1680 — 1640 (m, w) C=C | Alkenes 2260 - 2100 (m) C=C | Alkynes 1600, 1500 (w), usually shows C=C __ | Aromatic Rings ‘several peaks 1400 - 1090 (s) C-0 | Alcohols, Ethers, Esters 1320 ~ 1210 (m) C-0 | Carboxylic acids 4760 ~ 1670 (s) c=0 | Aldehydes, Ketones, Carboxylic acids, pee see a eae reeceereonaed Alcohols, 3400 ~ 2500 (b) O-H | Carboxylic acids 3500 — 3300 (m) N-H_ | Amines 1340 — 1020 (m) C-N | Amines 2260 ~ 2220 (m) CEN | Nitriles Intensities: s = strong, m = medium, w = weak, b = broad h=6.63 x 10™ Js 1.00 x 10°ms* (© Hak Cipta Universiti Teknologi MARA CONFIDENTIAL