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CONFIDENTIAL UNIVERSITI KUALA LUMPUR, Malaysian Institute Of Chemical & Bioengineering Technology FINAL EXAMINATION JANUARY 2012 SESSION SUBJECT CODE : LD 10402 SUBJECT TITLE : ANALYTICAL CHEMISTRY LEVEL : DIPLOMA DURATION : 2HOURS INSTRUCTIONS TO CANDIDATES . Please read CAREFULLY the instructions given in the question paper. . This question booklet has information printed on both sides of the paper. This question booklet consists of two sections; Section A and Section B. |. Answer ALL questions in Section A in the OMR Form. 3. Answer THREE (3) questions in Section B in the answer booklet provided. THERE ARE 12 PAGES OF QUESTIONS, INCLUDING THIS PAGE. JANUARY 2012 CONFIDENTIAL SECTION A (Total: 25 marks) INSTRUCTION: Answer ALL questions. Please use the OMR FORM provided. Analytical chemistry is known as @ scientific discipline used to study the following parameters EXCEPT A. study of high precision measurement B. find composition and identity of chemicals ©. physical properties of a sample only D. structure of components in a sample ‘Choose the BEST statement that describe about Chromatographic method A. Widely used method to identity the present or absent of functional group. B. Separation involves the usage of stationary phase and mobile phase. C. Separation wil need the measuring of ight produced or absorbed by an atom. D.—_Alom or molecule must undergo an electrenic transition for the separation to happen. ‘The following statements are referring to absorbance EXCEPT A. Absorbance infinity when transmittance is 0%. when alt ight absorbed by the sample ‘Absorbance Is zero when transmittance is 100%, whan no light absorbed by the sample ‘Absorbance is a logarithm function of transmittance. Absorbance is widely used to identify the present or absent of functional group. The principle method that used separation technique te mezsure concentration of an analytes in @ sample is called A gravimery . chromatography B, _ titimetry spectroscopy ChB 10402 ANALYTICAL CHEMISTRY JANUARY 2012 CONFIDENTIAL ‘Absorption of UV VIS radiation by an atom or molecule is result from ...... ‘A. the-excitation of electrons from excited state to ground state. 8. the vibration of moleculer bonds at various frequencies. C. the excitation of electron from higher frequency to lower frequency. D. the excitation of electrons from the ground state to the excited state Choose the CORRECT siatements about Beer’s Lambert Law. | Absorbance is proportional te the pathlength and the concentration of the Nl Absorbance is expressed as. = 2 ~log T. Ul, Absorption of molecules must undergo a net change ina dipole moment. TV. Absorbance is zero when transmittance is 100%. A. Land IV only 6. A. lland iv aniy B itand Il only D, Lilt and iv Select the advantage of laminar flow atomizer in AAS compared to turbulent flow sstomizer. ‘A. Nebulization occurs et the flame tip B. Large amount of sample reaches the flame Quist flame D. Lower sensitivity ‘At 580.nm, the wavelength of its maximum absorption, 0.175 NM of complex FeSCN" has an absorbance of 0.735 when measured in @ $ mm path length, Calculate the ‘molar absorptivity far this compound, AQ 4870.10? M" em" C0841 M cmt B. O49t Mem DB. 2.040 81" cm” ‘A requirement for a molecule to be absorbed in infra red region is... A. absorption can only occur when the molecule absorbs a photon of light B. the molecule must be able to rotate and vibrate C. it must be a non — polar molecule D, the molecule must possess a net change in the dipole moment 10402 ANALYTICAL CHEMISTRY 5 JANUARY 2012, “CONFIDENTIAL 10, In the context of infra red spectroscopy, wavelength is measured in “wavenumbers” The relationship between wavenumber and wavelength can be expressed a5 A 1 Wavenumber = —————___ wavelength (um) 1 ‘wavelength (em) Wavenumber = wevelength | Wavenumber = frequency frequency Wavenumber = ‘wavelength Choose the wavenumber range for “fingerprint region” in infra red radiation, A 4000-1500 m+ G.—-4000-600 cm* 2000-1000 en” BD. 1800-609 em” Figure 1 below shows a vibrational made of a molecule Figure 1 The type of vibrational made does the molecule undergo is Called joss. ss 0 A. in plane scissoring 8, asymmetrical stretching C. symmetrical stretching Din plane reeking A process in which an atom will spontaneausly return to the ground state and release light energy due to the instability of the excited state is called ...... A. emission Cc. — absorption 8. excitation D. fluorescence (CUD A402 ANALYTICAL CHEMISTRY JANUARY 2012 CONFIDENTIAL 14, 15, 16 (Cup 102 ANALVFICAL CHEMIST Select the main saurce of light used in atomic absarption spectroscopy A. Hollow cathode lamp CC. Photomultiplier tube B. Tungsten lamp DB. Dewietum tamp Diagram in Figure 2 belaw shows an I spectrum of a compound. om won ‘Wavemanter a) Figuie 2 By referring to the correlation chart in the appendix, predict the major IR absorption that present in the spectrum. A C=O Cc CHH B c-o DB O-H Choose the significant reasons why “characteristic concentration’ check is used in AAS. |. To make sure the overall conditions of the instrument are optimized, I. To. determine ifthe instrument is performing up to the specification I, To. predict the absorbance range and concentration range to produce optimum absorbance level. Iv, It shows the gensitivity of the instrument AL land i Cc i lland iv 8 | Mend Dil illand v JANUARY 2012 CONFIDENTIAL 17. Chromatographic method can be classified into two basic types, They are ‘A column chromatography and atamic chramatography ‘atomic chromategraphy and molecular chromatography B, C. column chromatography and planar chromatography o. planar chromatography and molecular chromatography In atomic absorption method, samples can be prepared using procedures below EXCEPT A wet digestion 8 hydride generation C. Nujor tut D. cold vapor mercury Separation process in chromatographic method involves interaction between packing material and sample. Choose the best statement that describes the interaction. ‘A. Components that have strong interaction with the stationary phase will move slower to the detector Components that have weak interaction with the mobile phase will move faster to the detector Components that are strongly interacts with the stationary phase will move: faster to the detector Components that are weakly interacts with the stationary phase will move slower to the detector Classification of a spectroscopy technique is described as below. the most powerful tec! for identifying types of chemical bonds (functional groups) give information about identity of structure of molecules a molecule must undergo a net change in a dipole moment a8 a consequence of its vibrational or retational metion Itis best describe about... A. infra rad spectroscopy B _UVEvis spectroscopy C. atomic spectroscopy D. nuclear magnetic resonance CLD 10402. ANALYTICAL CHEANSTRY JANUARY 2012 (CONFIDENTIAL, a 22, 23, 24, 25. cum lina chromatogram, the number of peaks correlates with while the area under each peak correlates with the relative amount of that component in the sample A. the flaw rate of the components B. the retention time of each component C. the temperature of the columa D. the number ef components in the sample ln the context of infrared spectroscopy, wavelength is measured in AL absorbance, A . transmittance, T 8. wavenumber, om" ‘D. frequency, Hz Following are the types of materials normally used for sample container or cuvettes EXCEPT A Plastic cells ©. Plastic quartz B Quartz silica D. Silicate glass ‘Select a detector that ig NOT suitable for HPLC. A. Refractive index detector C. Ultraviolet detector B. Fluorescence detector D. Thermal conductivity detector ‘A solvent delivery system in HPLC consist of ca A an injection port and a pump B. a series of solvent reservairs and a pump ©. aninjection port and a nebulizer D. pressurized tank and a solvent reservoir 2 ANALYTICAL CHEMISTRY 7 JANUARY 2012, ‘SECTION B (Total: 75 marks) INSTRUCTION: Answer only THREE questions. Please use the answer booklet provided. ‘Question 1 a) Brawa schematic diagram of UV-Vis spectrometer. Label all the components. (5 marks) Slale and define the equation for Beer's Lambert Law. (4 marks) In UV-Vis spectroscopy, analysis can be performed either using @ single beam spectrometer or # double beam spectrometer, State TWO (2) advantages of single beam spectrometer. (2 marks) State TWO (2) advantages of double beam spectrometer. (2 marks) Discuss THREE (3) factors thal cause deviation from Beer-Lambert lav. (6 marks) Beryllum {if} forms a complex with acetyacetane (166.2 g/mol). Ithas 2 moter abisorptivity of 0.032 L mol * ein” at 295 am, Calculate the absorbance of 1.34 ppm solution ina 1 cm cuvette (3 marks} Calculate the %T af the solution, (3 marks) (CLD 10402 ANALYTICAL CHEMISTRY JANUARY 2012 CONFIDENTIAL Question 2 a) Draw a schematic diagram of High Performance Liquid Chramatography (HPLC). Label all the components, (5 marks) b) Explain how the separation cccurs in HPLC, (5 marks) ©) Briefly explain the purpose of mobile and stationary phase in HPLC. (5 marks) d) Identify and explain the parameter you would use to confirm the present of caffeine in unknown solution. (4 marks) €) Identity and briefly explain THREE (3) types of detectors in HPLC. (6 marks} Question 3 8) Draw a schematic diagram of Gas Chromatography (GC}. Label all the companents. (Smarts) b} Explain how the separation occurs in GC. (Smarks) ©) Briefly explain TW (2) tynes of the injection in GG. (Smarks) d) Name and briefly explain TWO (2) types of column usuelly used in GC. Use diagram to compare oth types of columns. (Smarks) ®) Ih @ chromatogram, the composition of every component in a mixture can be determined by measuring the area under esch peak. Sketch a chromatogram to show how to measure the area of a peak, (Smarks) (CLD 10402 ANALVFICAL CHEMISTRY . INSUARY 2612 CONFIDENTIAL Question 4 paracteristic concentration” is important in AAS for some purposes: Define the term “characteristic concentration”. (2 marks) Give the equation for this term. (3 marks) fed of diagram, briefly explain how the absorption occurs in AAS. (5 marks) Briefly compare the differences between TWO (2) types of atomizer (bumer head). (4 marks) ‘The Figure 1 shows type of bond detected at different IR wavelength range. (2 marks} Triple bond 1 ~ Fingerprint region 1. pede 4000 3000 2000 1500 1000 600 Wavenumber (em) Identify the types of chemical bond far X and ¥ repectively In infrared spectroscopy, molecular bonds vibrate at various frequencies depending on the elements and the type of bonds. Name TWO (2} major modes of vitsrational transition in a molecule that is infra red active (2 marks) Skeich all the types of vibrations for each made with a correct arrow (eirection) and label (6 marks) 2 ANALYTICAL CHEMISTRY JANUARY 2012 APPENDIX ‘CONFIDENTEAE Faaleeslpael] o- Te | au M te lias] Macs Force = 0.453892 kg 4 bt = 4.448222 N 1 ton = 2000 tm 1M = 0.224809 Ibf = 1 kg.mis* 2.20462 Ibm Densit 028317 m? kg im’ = 0.062428 tem! f° 1 L_= 0.001 m tm? =3532 1 1 om? = 0.06102 in? 1 gal =0.0037854 m’ 1 gallmin = 6.31 x 10% m/s Pressure 1 pascal (Pa) = 1 Ném? 1 atm = 760 mmlg = 760 torr 1 atm = 101.325 Pa CLD 10402 ANALYTICAL Co MISTRY JANUARY 2012 CONFIDENTIAL Table : Characteristic Infrared Absorption Frequencies Bond Compound Type Frequency range, em" 2960-2850(s) stretch 1470-1380(v) scissoring and bending [1380{m.w) - Doubiet - isopropyl, Hbutyl ‘3080-3020(m) stretch 1000-675(s) bend Aromatic Rings 3100-3900(m) stretch CH Bhenv! Ring Substitution Bands {870-675(s} bend Phenyl Ring Substitution Overtones 2000-1600(w) - fingerprint region — (3993-9267(8) stretch - CH Alkynes '700-610(b) bend C=C Alenes — 1640(m,y)) stretch COC Alkynes '2260-2100(w,sh} stretch (C=C Aromatic Rings 1600, 1800(w) str ‘€-O (Alcohols, Ethers, Carboxylic acids, Esters 1260-1000(s) stretch co Aldenydes, Ketones, Carboxylic acids '1760-1670{s) stretch Esters Monomeric = Alcahols, Phenols 1-31 60{ stretch O-H Hydrogen-tonded — Alcohols, Phenols _3600-3200(b) stretch ‘Carboxylic acids - (3000-2500{b) stretch '3500-3300im) sireich At tates 1650-1580 (m) bend 7340-1020{m) stretch 2260-22201u) sireich [7860-1 500(¢) asymmetrical stretch NO; Nitro Compounds 1380-1 260(5) symmetrical stretch v-variable, m- medium, s - strong, br - broad, w- weak CLD UOMO ANALYTICAL CHEMISTRY