Mass Spectroscopy

Brief introduction about Mass Spectroscopy & its Instrumentation.

1. THE BASIC principle OF MASS SPECTROSCOPY & ITS INSTRUMENTATION 1 Chalapathi Institute Of Pharmaceutical Sciences Bhavana vedantam ,

2. Contents Applications Instrumentation Advantages & Disadvantages Introduction Basic principle 2 Chalapathi Institute Of Pharmaceutical Sciences

3. INTRODUCTION Mass spectroscopy deals with the study of the charged molecules & fragment ions produced from a sample exposed to ionizing conditions, & also of the relative intensity spectrum which results from the correlation of the ions with their mass to charge ratio. MS concept is first introduced by scientists Sir.J.J. Thomson and Wiens.

4. Principle When gaseous sample under 10 -7 to 10 -5 mm Hg pressure bombarded with electron beam(70ev), loss of electron from π orbital takes place resulting in the formation of ions and ion fragments. 4 Chalapathi Institute Of Pharmaceutical Sciences

5. Negative ions Fragment ions Meta stable ions Types of ions Molecular ions Rearrangement ions Isotopic ions Multiple charged ions 5 Chalapathi Institute Of Pharmaceutical Sciences

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7. Advantages & disadvantages 7 Chalapathi Institute Of Pharmaceutical Sciences

8. INSTRUMENTATION 8 Chalapathi Institute Of Pharmaceutical Sciences

9. Ion source Analyzers Detectors Sample inlet system BASIC Components 9 Chalapathi Institute Of Pharmaceutical Sciences

10. SAMPLE INLET SYSTEM Chalapathi Institute Of Pharmaceutical Sciences solid Directly into the chamber with low vapour pressure by means of probe. e.g. steroids, carbohydrates Liquid Vaporized with the help of heat inlet system. e.g. sugars , amino acids Gas Directly inleted & vaporized 10

11. Ionization techniques 11 Chalapathi Institute Of Pharmaceutical Sciences

12. Electron impact Ionisation: Electron beam(70ev) produced from electrically heated tungsten or rhenium filament is applied perpendicular to the sample and results in fragmentation. *sample destruction. 12 Chalapathi Institute Of Pharmaceutical Sciences

13. Chemical ionization: 13 Chalapathi Institute Of Pharmaceutical Sciences

14. Fast atom bombardment: 14 Chalapathi Institute Of Pharmaceutical Sciences

15. LASER DESORPTION TECHNIQUE: Eg : MALDI (Matrix Assisted Laser Desorption Ionization) TOF (Time Of Flight) analyzer Advantages : No direct contact of sample and electron Easy to operate laser 4-hydroxy cinnamic acid 15 Chalapathi Institute Of Pharmaceutical Sciences

16. + + + + - - - + + + + - - - - + + Analyte Matrix Laser + + + + + + Contd……. 16 Chalapathi Institute Of Pharmaceutical Sciences

17. MASS ANALYSERS Analyzers are used to deflect ions based upon m/e ratio. 17 Chalapathi Institute Of Pharmaceutical Sciences

18. Single focusing magnetic analyser 18 Chalapathi Institute Of Pharmaceutical Sciences

19. Double focusing magnetic analyser 19 Chalapathi Institute Of Pharmaceutical Sciences

20. Single focusing Double focusing 20 Chalapathi Institute Of Pharmaceutical Sciences

21. Time Of Flight(TOF) 21 Chalapathi Institute Of Pharmaceutical Sciences

22. Chalapathi Institute Of Pharmaceutical Sciences sensitive. 1000 times greater than faraday cup. Least sensitive. Cup will capture the ion. Most sensitive. Used for high resolution. Photomultiplier detector Photographic detectors 22 DETECTORS Faraday Cup detector

23. APPLICATIONS Chalapathi Institute Of Pharmaceutical Sciences 23

24. C onclusion Mass spectrometry is used for the study of charged molecules and fragment ions. Thus it is useful for the i dentification of an unknown compound. Chalapathi Institute Of Pharmaceutical Sciences

25. Elementary organic spectroscopy by Y.R.Sharma fourth edition 2007,by Rajendhra Ravindra printers page(280-291). Spectroscopy of organic compounds by P.S.Kalsi sixth edition, by New age international Pvt. Ltd. Page(415-439). Gurdeep R.Chatwal Sham K. Anand Instrumental Methods Of Analysis , Fifth addition, Himalaya publishing house Pvt . Ltd. Pharmaceutical analysis (INSTRUMENTAL METHODS) by Dr . A.V.Kasture, ninth edition. REFERENCES

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