Kertas ini dibahagikan kepada Bahagian A dan Bahagian B. This paper is divided into Section A and Section B.

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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 2010/2011 : SEMESTER 2 ACADEMIC SESSION 2010/2011 : SEMESTER 2 SCES3362 : Teknik-teknik Instrumentasi Dalam Kimia Instrumental Technique in Chemistry April/Mei 2011 April/May 2011 Masa : 2 jam Time : 2 hours ARAHAN KEPADA CALON INSTRUCTIONS TO CANDIDATES : Kertas ini dibahagikan kepada Bahagian A dan Bahagian B. This paper is divided into Section A and Section B. Sila patuhi arahan yang diberikan dalam setiap bahagian semasa menjawab. Please follow the instruction given in each section. (Kertas soalan ini mengandungi 9 soalan dalam 6 halaman yang dicetak) (This question paper consists of 9 questions on 6 printed pages)

2 SCES3362/02 BAHAGIAN/SECTION A (50 MARKAH/MARKS) Jawab SEMUA soalan. Answer ALL questions. 1. Apakah yang anda faham dengan plat teori dalam HPLC? Hitung nombor plat teori (N) daripda kromatogram HPLC berikut menggunakan formula N = 5.5 [t r /W] 2. What do you understand by theoretical plates in HPLC? Calculate number of theoretical plates (N) from the following HPLC chromatogram using the formula N = 5.5 [t r /W] mm 12 mm [8 markah/marks] 2. Dengan ringkas terangkan sebutan berikut: Briefly describe the following terms: (i) (ii) (iii) (iv) (v) Isipadu bahan fasa pegun Vs Stationary phase material volume V S Isipadu gelonggong Vo Void volume Vo Isipadu elusi minima Vm Minimal elution volume Vm Isipadu elusi diukur secara eksperimen Vr Experimentally measured elution volume Vr Pemalar K Constant K (vi) Faktor muatan - k Capacity factor-k (vii) Sebutan kepilihan α Selectivity term- α

3 SCES3362/03 (viii) (ix) (x) Resolusi R Resolution R Masa penahan t r Retention time-t r Keluasan puncak dasar W Width of peak base line-w dan terbitkan persamaan: and derive the equation: R = t starting from V r = V m + K V s (W 1 + W 2 ) 1/2 [12 markah/marks] 3. Apakah yang anda faham dengan kaedah pemisahan yang dikenali sebagai SDS-PAGE? Jelaskan dengan bantuan gambarajah pemisahan protin dengan menggunakan kaedah elektroforetik. Bagaimana dapat anda bandingkan elektroforesis dan elektroforesis kapilari? What do you understand by the separation technique known as SDS-PAGE? Explain with the help of diagrams separation of proteins by using this electrophoretic technique. How would you compare electrophoresis with capillary electrophoresis? [10 markah/marks] 4. (a) Jelaskan dengan bantuan gambarajah bagaimana data TLC boleh digunakan untuk meramalkan sifat elusi turus dan bagaimana jumlah isipadu turus diperlukan (ΔCV) dalam kromatografi kilat dalam meramalkan jumlah maksima beban sampel. Explain with the help of a diagram, how the TLC data can be used to predict column elution behavior and how total number of column volumes required (ΔCV) in flash chromatography plays a role in predicting maximum sample loading. (4 markah/marks)

4 SCES3362/04 Kira ΔCV bagi tiga puncak berikut dalam kromatografi kilat yang mempunyai nilai R f : Calculate ΔCV for the following two peaks in a flash chromatogram having R f values: R f A = 0.22, R f B = 0.14 (3 markah/marks) (c) Jejari turus bulat adalah 5 inci dan tinggi turus adalah 10.2 inci. Apakah isipadu turus (Vc)? The radius of a circular column is 5 inches and the height of the column is 10.2 inches. What is the volume of the column (Vc)? (3 markah/marks) 5. (a) Bagaimana anda membezakan tiga kaedah kromatografi berikut? How would you differentiate the following three chromatographic techniques? (i) (ii) (iii) High Performance Liquid Chromatography HPLC Gas Liquid Chromatography GLC Supercritical Fluid Chromatography SFC (6 markah/marks) Lukis gambarajah fasa dan jelaskan femomena dalam supercritical fluids. Draw a phase diagram and explain the phenomenon of supercritical fluids. (4 markah/marks)

5 SCES3362/05 BAHAGIAN/SECTION B (50 MARKAH/MARKS) Jawab semua soalan. Answer all Questions 6. (a) Terangkan hubungan diantara corak pembelauan dengan susunan atom 3D dalam bahan berhablur. Relate the diffraction pattern to the 3D arrangement of atoms in a crystalline material. Nyatakan penggunaan pembelauan serbuk menggantikan pembelauan hablur tunggal. When is powder diffraction used in place of single crystal diffraction? 7. (a) Nyatakan Hukum Bragg. Terangkan bagaimana hukum ini dikaitkan dengan ketiadaan bersistem corak pembelauan. State Bragg s Law. How does it relate to systematical absences? Pemantulan mempunyai index Miller (1,2,3) memantul pada 2 = 20.0 dengan jarak d pada Å. Berapakah panjang gelombang X-ray, λ? Berapakah jarak d pada pemantulan (2,4,6)? A reflection has Miller indices of (1,2,3) diffracts at 2 = Its d spacing is Å. What is the wavelength, λ of the X-rays? What is the d spacing for the (2,4,6) reflection? 8. (a) Apakah faktor stuktur dan bagaimanakah ia berhubungkait dengan kepadatan electron? What is a structure factor and how is it related to the electron density?

6 SCES3362/06 Berapakah system kristal yang diguna untuk mengenal pasti kristal tunggal? Apakah ciri-ciri untuk unit sel ortorombik? How many crystal systems are used to identify single crystals? What are the characteristic of an orthorhombic unit cell? (c) Jika sesuatu molekul menghablur dalam Iba2, apakah operasi simetri yang boleh disimpulkan daripada kumpulan ruang tersebut? If a molecule crystallizes in the Iba2, what symmetry operations can you conclude from the space group? (2 markah/marks) (d) Namakan 2 kaedah untuk penyelesaian stuktur hablur dan bezakan antara kedua-dua kaedah ini. Name two methods for solving crystal structures and differentiate these two methods. (e) Apakah faktor R dan apakah implikasinya dalam penghalusan stuktur hablur? What is an R-factor and how it is used in refinements? (3 markah/marks) 9. Terangkan bagaimana hablur tunggal boleh dibezakan daripada hablur berkembar. Berdasarkan Hukum Berkembar, nyatakan jenis hablur berkembar yang mungkin. Describe briefly how can one tell if a crystal is a single crystal or is a twinned crystal? Based on the twin law, elaborate the possible twin arrangements. ******************* (10 markah/marks)

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