(Kertas ini mengandungi 5 soalan dalam 5 halaman yang dicetak) (This paper consists of 5 questions in 5 printed pages)

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1 UNIVERSITI MALAYA UNIVERSITY OF MALAYA PEPERIKSAAN IJAZAH SARJANA SAINS (MSc) KIMIA ANALISIS & ANALISIS BERALATAN EXAMINATION FOR THE DEGREE OF MASTER OF SCIENCE (MSc) IN ANALYTICAL CHEMISTRY & INSTRUMENTAL ANALYSIS SESI AKADEMIK 2016/2017 ACADEMIC SESSION 2016/2017 : SEMESTER I : SEMESTER I SCGS6115 : ANALISIS SPEKTROSKOPI ATOM ATOMIC SPECTROSCOPIC ANALYSIS Dis 2016/Jan 2017 Dec 2016/Jan2017 Masa: 2 jam Time: 2hours INSTRUCTION TO CANDIDATES: ARAHAN KEPADA CALON: Jawab SEMUA soalan. Answer ALL questions. (Kertas ini mengandungi 5 soalan dalam 5 halaman yang dicetak) (This paper consists of 5 questions in 5 printed pages)

2 SCGS (a) Berikan perbezaan asas di antara spektrometer alur tunggal dan alur dua. State the basic differences between a single beam spectrometer and a double beam spectrometer. Terdapat dua sumber sinar khusus yang sering digunakan untuk spektroskopi atom iaitu lampu katod berongga dan lampu nyahcas tanpa elektrod. Apakah kekurangan lampu katod berongga berbanding lampu nyahcas tanpa elektrod sebagai sumber sinar spektroskopi atom? The two common line sources in atomic spectroscopy are hollow-cathode lamp and electrodeless discharge lamp. What are the disadvantages of using hollow cathode lamps over electrodeless discharge lamps as a light source in atomic spectroscopy? 2. (a) Kaedah piawai dalaman adalah salah satu teknik penentukuran dalam spektroskopi atom. Apakah ciri-ciri piawai dalaman yang bagus? Terangkan bagaimana ia boleh meningkatkan ketepatan pengukuran spektrometri penyerapan atom dan kenapakah ia sering digunakan untuk teknik spektrometri pemancaran atom. Internal standards are used as a calibration method in atomic spectroscopy. What are the characteristics of a good internal standard? Explain how it can improve the precision of atomic spectroscopic techniques and why it is most commonly used for atomic emission techniques. (10 markah/marks) Kandungan kuprum dalam suatu sampel akues ditentukan dengan mempipetkan 10.0 ml larutan tersebut ke dalam setiap satu daripada lima kelalang volumetrik 50.0 ml. Pelbagai isipadu larutan piawai 30.0 ppm Cu ditambahkan ke dalam kelalang volumetrik dan dicairkan ke tanda senggatan. Kelima-lima larutan tersebut dianalisis dan bacaan yang diperolehi adalah seperti berikut: The copper content in an aqueous sample was determined by pipetting 10.0mL of the solution into each of five 50.0 ml volumetric flasks. Various volumes of a 30.0 ppm Cu standard solution were added to the flasks and the solutions diluted to the volume. The solutions were analysed and results were as follows: 2/5

3 Isipadu sampel (ml) / Unknown standard (ml) Piawai Cu (ml) / Cu standard (ml) SCGS6115 Bacaan keserapan / Absorbance (i) Apakah teknik penetukuran yang digunakan dalam eksperimen ini? What calibration method was used in this experiment? (1 markah/marks) (ii) Diberikan kecerunan geraf penentukuran adalah dan pintasan-y adalah , hitung kepekatan Cu (dalam ppm) dalam sampel asal. (Tunjuk jalan kerja) Given that the slope of the calibration curve is and the y-intercept is , calculate the concentration of Cu (in ppm) in the original unknown sample. (Show calculation) 3. (a) Dengan bantuan gambarajah blok, labelkan komponen peralatan utama spektrometer pendafluor atom. Terangkan fungsi setiap komponen. With the help of a block diagram, label the major instrumental components of atomic fluorescence spectrometer. Explain the function of each component. (8 markah/marks) Bagaimanakah susunan geometri peralatan tersebut meningkatkan nisbah isyarat terhadap hingar dan menurunkan had pengesanan dalam kaedah-kaedah berasaskan pendarfluor? How does the geometrical instrumentation setup provide a better signal-to-noise ratio and lower the detection limit of fluorescence based methods? (3 markah/marks) 3/5

4 (c) Bincangkan jenis-jenis peralihan pendafluor atom. Discuss the types of atomic fluorescence transitions. SCGS6115 (16 markah/marks) 4. (a) Nyatakan sama ada pernyataan di bawah adalah BENAR atau SALAH dan terangkan MENGAPA. Indicate whether the following statements are TRUE or FALSE and briefly explain WHY. (i) Spektroskopi penyerapan atom sesuai untuk digunakan dalam menganalisis bilangan sampel yang banyak dan berbeza komposisi unsurnya. Atomic absorption spectroscopy is suitable for use in analysing large numrber of samples of varying elemental composition. (ii) Kelebihan spektroskopi penyerapan atom relau grafit adalah had pengesanannya adalah kira-kira dua magnitud lebih baik daripada spektroskopi penyerapan atom nyala. The advantage of graphite furnace atomic absorption spectroscopy is that the detection limit is about two orders of magnitude better than that of flame atomic absorption spectroscopy. (7 markah/marks) (iii) Dalam penyerapan atom nyala dengan bahan api idrogen/oksigen, keserapan bagi Ca meningkat di dalam kehadiran kepekatan ion fosfat yang tinggi. In flame atomic absorption with a hydrogen/oxygen fuel, the absorbance for Ca increased in the presence of large concentrations of phosphate ion. (6 markah/marks) 4/5

5 SCGS6115 Gambarajah di atas menunjukkan gangguan latarbelakang semasa penentuan Ba dengan menggunakan spektroskopi penyerapan atom nyala. Cadangkan satu kaedah bagi mengatasi gangguan tersebut. The figure above shows background interference during the determination of Ba by using flame atomic absorption spectroscopy. Suggest one method of overcoming this interference. (3 markah/marks) 5. (a) Bincangkan perbezaan di antara spektroskopi penyerapan atom dan spektroskopi pemancaran atom dari segi a) Prinsip b) Peralatan c) Analysis. Discuss the difference between atomic absorption spectroscopy and atomic emission spectroscopy in terms of a) Principle b) Instrumentation c) Analysis. (15 markah/marks) Apakah itu plasma. Terangkan bagaimana plasma berkuasa RF berfungsi. What is a plasma? Describe the working of RF powered plasma. (15 markah/marks) TAMAT END 5/5

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