SCES3362 : TEKNIK-TEKNIK INSTRUMENTASI DALAM KIMIA INTRUMENTAL TECHNIQUES IN 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 2014/2015 : SEMESTER 2 ACADEMIC SESSION 2014/2015 : SEMESTER 2 SCES3362 : TEKNIK-TEKNIK INSTRUMENTASI DALAM KIMIA INTRUMENTAL TECHNIQUES IN CHEMISTRY Jun 2015 June 2015 Masa : 2 jam Time : 2 hours ARAHAN KEPADA CALON : INSTRUCTIONS TO CANDIDATES : Jawab semua soalan. Answer all questions. Untuk soalan 4, sila jawab di atas kertas soalan dan kertas soalan haruslah dihantar bersama skrip jawapan. For question 4, please answer on the question paper and question paper must submit it together with answer scripts. (Kertas ini mengandungi 8 soalan dalam 7 halaman yang dicetak) (This question paper consists of 8 questions on 7printed pages)

2 1. Seperti yang dibincangkan dalam kuliah, Pembelauan sinar-x adalah satu teknik yang penting untuk menentukan struktur molekul dalam keadaan pepejal. Apakah keperluannya supaya teknik ini boleh digunakan untuk menentukan struktur. As discussed in lectures, X-ray crystallography is a vital technique for the determination of molecular structure in the solid-state. What are the requirements to enable the use of this technique for structure determination? (7 markah/marks) 2. Seperti teknik analisis lain, Pembelauan sinar-x mempunyai kelebihan dan keburukannya. Berikan tiga contoh kelebihan dan tiga contoh keburukan untuk teknik ini. As with all analytical techniques, X-ray crystallography has advantages and disadvantages. Give examples of three advantages and three disadvantages of this technique (6 markah/marks) 3. Dalam Pembelauan sinar-x, simetri adalah sangat penting. Dalam soalan ini anda dikehendaki memberi definasi dan contoh untuk setiap jenis simetri yang berikut: In X-ray crystallography, symmetry is all-important. In this question you need to provide definitions and examples of each of the following: Kumpulan titik Point Group (ii) Paksi skru screw axis (iii) Satah gelangsar Glide plane (10 markah/marks) 2/7

3 4. Peralatan Pembelauan sinar-x adalah ditunjukkan seperti gambar rajah di bawah. Kenalpasti setiap komponen berikut: The image below is of an X-ray diffraction apparatus. On the diagram, identify each of the following components: (a) Goniometer (b) Kepala goniometer (c) CCD Goniometer Goniometer head CCD (d) Tiub sinar-x Mo (e) Kollimator (f) Beam Stop Mo X-ray tube Collimator Beam stop (g) Muncung gas N 2 (h) Shutter Gaseous N 2 nozzle Shutter Paksi/bulatan omega (j) Pin tembaga Omega axis/circle Brass pin (10 markah/marks) 3/7

4 5. Berikut adalah gambar rajah ORTEP untuk molekul dikloromethana: The following is an ORTEP diagram of a dichloromethane molecule: Bincangkan maksudnya bentuk bola yang digunakan untuk mewakili atom dalam gambar rajah ini. Bagaimana anda menganggap hablur diklorometana telah terbentuk? Discuss the meaning of the shapes of the balls used to represent the atoms in this diagram. How do you suppose crystals of dichloromethane were formed? (12 markah/marks) 6. Pembelauan sinar-x serbuk adalah teknik penting dalam saringan fasa sampel hablur. Dengan menggunakan gambar rajah di bawah yang menunjukkan struktur molekul [Pd(S 2 CO-iPr) 2 ] (gambar di sebelah kiri) dan corak PXRD dari eksperimen (bahagian atas, gambar di sebelah kanan) dan corak berdasarkan kepada keadah simulasi struktur hablur tunggal (bahagian bawah, gambar di sebelah kanan): Powder X-ray diffraction (PXRD) is a crucial technique in screening the phase of bulk samples of crystals. Consider the images below obtained for [Pd(S 2 CO-iPr) 2 ] (left-hand image): Right-hand images: Experimental (upper trace) and simulated based on the single crystal structure (lower trace) PXRD patterns. 4/7

5 (ii) (iii) (iv) (v) (vi) Bandingkan dan bezakan eksperimen Pembelauan sinar-x hablur tunggal (SCXRD) dengan Pembelauan sinar-x serbuk (PXRD) apakah maklumat yang diperolehi daripada setiap teknik ini? Compare and contrast single crystal X-ray diffraction (SCXRD) experiments with powder X-ray diffraction (PXRD) experiments what information does each give? Bagaimana teknik SCXRD dan PXRD saling membantu satu sama lain? How do the SCRXD and PXRD techniques complement each other? Dengan merujuk kepada corak PXRD di atas, apakah kesimpulan yang boleh diperolehi daripada perhubungan diantara corak SCXRD simulasi dengan corak PXRD eksperimen? Referring to the PXRD patterns shown in the image above, what can one conclude about the relationship between the simulated SCXRD and experimental PXRD patterns? Apa maksudnya jika puncak yang kurang diperhatikan dalam corak di bahagian atas? What would it mean if less peaks were observed in the upper trace? Apakah maksudnya jika lebih puncak diperhatikan dalam corak di bahagian atas? What would it mean if more peaks were observed in the upper trace? Apakah maksudnya jika tiada puncak diperhatikan dalam corak di bahagian atas? What would it mean if no peaks were observed in the upper trace? (17 markah/marks) 7. Soalan ini ada berkaitan dengan ciri terma untuk pepejal dan anda perlu memberi jawapan kepada soalan berikut: This question relates to the thermal characterisation of solids and requests you provide answers to the following questions: (ii) Berikan satu definasi untuk DSC dan terangkan apakah maklumat yang boleh didapati daripada sesuatu eksperimen DSC? Give a definition of DSC and describe what information can be gained from a DSC experiment? Dengan merujuk kepada gambar di bawah yang dihasilkan daripada eksperimen DSC untuk pridopidin hidroklorida, bincangkan bagaimana kedua-dua puncak tertimbul. Referring to the image below, obtained for pridopidine hydrochloride, discuss how the two peaks might arise. 5/7

6 (iii) Apakah perhubungan diantara TGA dengan DSC untuk sampel yang sama? What is the relationship between TGA and DSC performed on the same sample? (8 markah/marks) 8. Apabila anion metilxanthat, - S 2 COMe berkoordinat kepada palladium(ii), dua polimorf akan terbentuk: satu polimorf yang tidak mempunyai simetri seperti dalam molekul yang ditunjukkan dalam bentuk I, manakala polimorf yang kedua menunjukkan atom palladium terletak di pusat penyongsangan, bentuk II. When the methylxanthate anion, - S 2 COMe, is coordinated to palladium(ii), two polymorphs are formed, one with no symmetry in the illustrated molecule, form I, and the other where the palladium atom is located on a centre of inversion, form II. Bentuk I/ Form I Diberi parameter geometri yang penting untuk [Pd(S 2 COMe) 2 ] dalam bentuk I seperti di bawah: Significant geometric parameters for the independent molecule in form I of [Pd(S 2 COMe) 2 ] are given below: Parameter Pd S1 /Å (15) Pd S2 /Å (15) Pd S3 /Å (15) Pd S4 /Å (15) Dengan merujuk kepada data di atas, berikan jawapan dan justifikasi kepada soalan berikut: 6/7

7 Referring to the data above, provide answers, giving justification, to the following questions: (ii) (iii) (iv) (v) (vi) Berikan satu definasi untuk polimorf Give a definition for a polymorph Berikan data metrik untuk mentakrifkan satu sel unit triclinik. Give the metric data defining a triclinic unit cell. Bincangkan ciri RMN karbon-13 dalam keadaan pepejal dan keadaan larutan yang dijangka untuk [Pd(S 2 COMe) 2 ] dalam polimorf bentuk I. Discuss the expected solution and solid-state carbon-13 NMR characteristics expected for [Pd(S 2 COMe) 2 ] in form I of [Pd(S 2 COMe) 2 ]. Bincangkan ciri RMN karbon-13 dalam keadaan pepejal dan keadaan larutan yang dijangka untuk [Pd(S 2 COMe) 2 ] dalam polimorf bentuk II. Discuss the expected solution and solid-state carbon-13 NMR characteristics expected for [Pd(S 2 COMe) 2 ] in form II of [Pd(S 2 COMe) 2 ]. Dengan mempertimbangkan panjang ikatan Pd-S dalam bentuk I, adakah jarak Pd-S1 dan Pd-S4 berbeza secara eksperimen? Tunjukkan jalan kerja dan berikan jawapan yang wajar. Considering the Pd S bond lengths for form I, are the Pd S1 and Pd S4 distances experimentally distinct? Show your working and justify your answer. Apakah akan terjadi kepada molekul ini jika pengiraan pengoptimuman geometri digunakan? What would happen to the molecule if it was subjected to a geometry optimisation calculation? (30 markah/marks) TAMAT END 7/7

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