SCES3311/ SCES3141 : KIMIA ANALISIS II/ KIMIA ANALISIS LANJUTAN ANALYTICAL CHEMISTRY II/ ADVANCED ANALYTICAL CHEMISTRY

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1 UNIVERSITI MALAYA UNIVERSITY OF MALAYA PEPERIKSAAN IJAZAH SARJANA MUDA SAINS EXAMINATION FOR THE DEGREE OF BACHELOR OF SCIENCE SESI AKADEMIK 2013/2014 : SEMESTER 2 ACADEMIC SESSION 2013/2014 : SEMESTER 2 SCES3311/ SCES3141 : KIMIA ANALISIS II/ KIMIA ANALISIS LANJUTAN ANALYTICAL CHEMISTRY II/ ADVANCED ANALYTICAL CHEMISTRY Jun 2014 June 2014 MASA : 2 jam TIME : 2 hours ARAHAN KEPADA CALON : INSTRUCTIONS TO CANDIDATES : Kertas soalan ini mengandungi Bahagian A dan B. This paper consists of Section A and B. Jawab soalan mengikut arahan yang diberikan dalam setiap bahagian. Questions should be answered according to the instructions given in each section. (Kertas ini mengandungi 7 soalan dalam 5 halaman yang dicetak) (This question paper consists of 7 questions on 5 printed pages)

2 Jawab SEMUA soalan dalam Bahagian ini Answer ALL questions in this Section BAHAGIAN A ( 50 MARKAH) SECTION A ( 50 MARKS) 1. Tuliskan persamaan van Deemter bagi kromatografi gas (GC). Dengan menggunakan persamaan itu, tunjukkan bagaimana ia boleh digunakan untuk mengoptimumkan kederasan aliran gas pembawa/fasa bergerak dan memaksimumkan kecekapan dalam pemisahan GC. Write down the van Deemter equation for gas chromatography (GC). Using this equation show how it can be employed to optimize the flow rate of the carrier gas/mobile phase and to maximize the efficiency in a GC separation. 2. Bincangkan peranan saiz zarah dalam sesuatu turus HPLC merujuk kepada kecekapan, resolusi dan masa analisis. Discuss the importance of particle size in the HPLC column with reference to efficiency, resolution and analysis time. 3. (a) Terangkan bagaimana eksperimen voltammetri perlucutan anod (ASV) boleh dilakukan ke atas analisis logam surih seperti Pb, Cd dan Zn dalam sesuatu sampel air. Explain how the anodic stripping voltammetric (ASV) experiment is carried out for the determination of trace metals such as Pb, Cd and Zn in a water sample. Apakah parameter-parameter yang boleh mempengaruhi ketepatan keputusan-keputusan yang diperolehi dari eksperimen ASV? Terangkan. What are the factors which can influence the reproducibility in an ASV experiment? 4. Dalam percubaan-percubaan pemisahan yang berikut, tuliskan tertib elusi bagi sebatian-sebatian yang diberikan, mulai dengan sebatian yang mempunyai masa penahanan yang paling rendah. In the following separation experiments write the elution order of the compounds, beginning with the compound of the lowest retention. 2/5

3 (a) Kromatografi gas ke atas suatu campuran gas asli yang mengandungi n- pentan, metan, n-heksan, n-butan, iso-pentan, 3-metilpentan, etan, propan, iso-butan dan 2,2-dimetilbutan dengan menggunakan suatu turus 30 m x 0.53 mm yang diisikan dengan SE-30 sebagai fasa pegun pada 30 ºC. Gas chromatography on a natural gas mixture containing n-pentane, methane, n-hexane, n-butane, iso-pentane, 3-methylpentane, ethane, propane, iso-butane and 2,2-dimethylbutane using a 30 m x 0.53 mm column with SE-30 as the stationary phase at 30 C. HPLC ke atas suatu campuran yang mengandungi n-propilbenzen, toluen, benzen, n-butilbenzen, dan etilbenzen dengan menggunakan suatu turus 25 cm X 4.6 mm Nucleosil C18 dan 20:80 (v/v %) air/metanol sebegai fasa bergerak yang mengalir sebanyak 1.2 ml/min. HPLC on a mixture containing n-propyl benzene, toluene, benzene, n- butyl benzene and ethylbenzene using a 25 cm x 4.6 mm Nucleosil C18 column with 20:80 (v/v %) water/methanol as the mobile phase and a flow rate of 1.2 ml/min. 3/5

4 BAHAGIAN B ( 50 MARKAH) SECTION B ( 50 MARKS) Jawab SEMUA soalan Answer ALL questions 5. (a) Apakah sebab yang menyebabkan kemerosotan atau kehilangan analit dalam eksperimen analisis? What are the possible causes of degradation or lose of analytes in an analytical experiment? Nyatakan beberapa masalah biasa yang dihadapi dalam proses pencernaan basah dan proses pencernaan kering untuk sampel dalam analisis surih? State the common problems which are usually encountered in wet digestion processes and dry digestion processes for samples in trace analysis? (c) Terangkan kaedah kelalang oksigen pembakaran. Describe the oxygen flask combustion method. 6. (a) Dua larutan sampel natrium telah disediakan untuk dianalisa menggunakan spektroskopi pemancaran nyala. Keamatan pemancaran garis natrium pada dan nm didapati adalah lebih tinggi dalam larutan sampel yang mengandungi KCl daripada larutan kedua, di mana KCl tidak hadir. Cadangkan penjelasan untuk pemerhatian ini. Two solutions of sodium samples were prepared for analysis using flame emission spectroscopy. The emission intensities of sodium lines at and nm were found to be greater in a sample solution that contains KCl than the second solution, in which KCl is absent. Suggest an explanation for this observation. Apakah spektrometri penyerapan atom? Terangkan prinsip dan instrumentasi spectrometer penyerapan atom (dengan bantuan gambarajah). What is atomic absorption spectrometry? Describe the principle and instrumentation of a typical atomic absorption spectrometer (with help of a diagram). 4/5

5 (c) Huraikan bagaimana sampel bukan logam boleh disediakan dan dianalisa menggunakan spektroskopi sumber percikan. Describe how non-metallic samples are prepared and analyzed using the spark source spectroscopy. (d) Bincangkan mengenai interferens spektroskopi jisim di dalam spektrometri jisim-inductively coupled plasma (ICP-MS). Discuss the mass spectroscopic interferences in Inductively coupled plasma-mass spectrometry (ICP-MS). 7. (a) Terangkan bahagian utama penganalisisa auto. Describe the main parts of an auto analyzer. (25 markah/marks) Nyatakan faktor yang mempengaruhi rekabentuk penganalisa klinikal automatik. State the factors affecting the design of the automated clinical analyzer. TAMAT END 5/5

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