CONFIDENTIAL ASIJAN 2018/CHMS74 UNIVERSITI TEKNOLOGI MARA FINAL EXAMINATION COURSE : BASIC INSTRUMENTAL ANALYSIS COURSE CODE : CHM571 EXAMINATION JANUARY 2018 TIME 2 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 invigiator 4 Please check to make sure that this examination pack consists of i) the Question Paper ii) aone— page Appendix ill) an Answer Booklet — provided by the Faculty 5. ‘Answer ALL questions in English. DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO This examination paper consists of 4 printed pages (© Hak Cipta Universiti Teknologi MARA CONFIDENTIALCONFIDENTIAL 2 ASIJAN 2018/CHM571 QUESTION 1 a) Briefly define spectroscopy and name two (2) types of radiation. (2 marks) b) Explain type interaction when the ultra violet radiation comes in contact with matter. (3 marks) ©) Calculate the frequency of infrared radiation of wavelength 67.5 um. (3 marks) 4) Differentiate between line and band spectra. (4 marks) QUESTION 2 a) Describe sigma (a), pi (11) and non-bonding (n) electron. Illustrate these three types of electron in formaldehyde (CH20) molecule. (6 marks) b) Explain the meaning of Beer Lambert Law. (3 marks) ©) The ultraviolet spectrum of benzonitrile shows a primary absorption band at 224 nm and a secondary band at 271 nm. The concentration of benzonitrile in water is 1 x 10“ mol L and the absorbance recorded is 1.30 in a 1.00 cm cell at 224 nm, calculate the molar absorptivity of this absorption band. If the same solution is then examined at 271 nm, calculate the new absorbance reading. (given € = 1000 L mot" cm”) (3 marks) d) Briefly explain a chromophore and the effect of an auxochrome when it is attached to a chromophore. (2 marks) QUESTION 3 a) Explain the criteria needed for a molecule to absorb infrared radiation. (4 marks) b) Distinguish between stretching and bending involve in infrared molecular vibrational mode. (2 marks) (© Hak Cipta Universiti Teknologi MARA, CONFIDENTIALCONFIDENTIAL 3 ASIJAN 2018/CHMS71 c) Using infrared spectroscopy, differentiate between pentene and pentanol. (4 marks) d) Define neat liquid and its sample preparation for infrared spectroscopy analysis. (3 marks) e) Sample X is a solid that is not soluble in infrared transparent solvent and not convenient to make a KBr pellet. Suggest sample preparation for sample X in infrared analysis. (2 marks) QUESTION 4 a) Name the most common line source used in atomic absorption spectrophotometer. State the function of this line source in atomic absorption spectroscopy. (2 marks) b) Explain the working mechanism of a Hollow Cathode Lamp. (6 marks) ¢) One of the advantages of plasma sources in emission spectroscopy is little chemical interferences. Discuss how this interference can be minimized by using these plasma sources. (4 marks) QUESTION 5 a) Explain the principle involves in gas chromatography (GC) analysis from sample introduction to the output of the chromatogram. (4 marks) b) The following GC data was obtained for a mixture separated using a 50.0 cm long column at a column temperature 190°C. _ Compound Retention time, te (min) — Peak width, W (min) A 4.124 0.07_ B = 3.021 0.41 cl - 4.356 0.13) | Calculate the number of plate and resolution for species B and C. Explain whether or not it is a baseline separation. (4 marks) ©) Elaborate the methodology in qualitative analysis performed by gas chromatography (GC). (4 marks) (© Hak Cipta Universiti Teknologi MARA CONFIDENTIALCONFIDENTIAL 4 ASIJAN 2018/CHMS71 QUESTION 6 a) The solvents in High Performance Gas chromatography (HPLC) must be degassed prior to use. Explain the reason behind this procedure. (2 marks) b) Define gradient elution in HPLC. State advantage of gradient elution over isocratic elution. (mans) ©) Compare and contrast between guard column and analytical column used in HPLC. (5 marks) d) State two (2) criteria for choosing a solvent as a mobile phase in HPLC. (2 marks) ) Benzene is eluted from a reverse phase Cis column in 13 minutes with a mobile phase consisting of 50 % acetonitrile and 50 % water. Predict what will happen to the retention time if the mobile phase is changed to 70 % acetonitrile and 30 % water. Explain your answer. (3 marks) END OF QUESTION PAPER (© Hak Cipta Universiti Teknologi MARA CONFIDENTIALCONFIDENTIAL APPENDIX 4 ASIJAN 2018/CHMS71 SOME CHARACTERISTICS OF IR ABSORPTION BANDS Wavenumber, cm* Intensity Structure 730 - 770; 690 - 710 m Mono (aromatic) 1090 - 1400 | s C—O (inethers, alcohols and esters) 1315 - 1475 m-s C -H (in alkanes) . C=C bond in aromatic ring (usually shows Te) a several peaks) 1620 - 1680 m }c=c 2100 - 2200 m c 4690 - 1750 s | C = 0 (in carbonyl compounds and esters) 1740 - 1725 s C =O (in aldehydes) 4700 - 1730 | s C = 0 (in carboxylic acids) 4320 - 1210 m C - 0 (in carboxylic acids) 2760 - 2700 2860 . 2800 w C -H (of aldehyde group, a pair of bands) 2400 - 3400 s, vb O-Hin COOH 3000 - 3100 m | C-H (Cis part of aromatic ring) 3300 s | C-H (sp) 3020 - 3080 m C-H (sp) 2800 - 3000 | m-s CH (sp) 3200 - 3600 s,b O —H (in H-bonded ROH and ArOH) Intensities: s=strong m=medium w=weak b=broad vb = very broad h=6.63 x10 J.s c= 3.00 x 10®ms* (© Hak Cipta Universiti Teknologi MARA CONFIDENTIAL