Atomic emission spectroscopy In Pharmacy Education ppt

Spectroscopy-Pharmacy

1. ATOMIC EMISSION SPECTROSCOPY Prepared By D.Mahendra,Mpharm (PA&QA) Asst.Professor – NCOP-T7 DEPT- PHARMACEUTICAL ANALYSIS Mail id :- [email protected]

2. INTRODUCTION

3. Used as standard method for the metal analysis In atomic emission small part of sample is vaporized forms free atom that attain energy form excitation source results in transition from lower to higher energy state on returning back emit a photon of radiation

4. ) PRINCIPLE OF ATOMICEMISSION SPECTROSCOPY AND S C HE M A TIC D I AG RA M OF INS T R UME N TA T I ON

5. Principle The electrons of an atom moves from higher energy level to lower energy level, they emit extra amount of energy in the form of light which is consist of photons.

6. Instrumentation Comprises on: Source & Sample Atomizer Monochromator Detector & readout device

7. Schematic Diagram Of Instrumentation

8. COMPONENTS 1. Light source Inductively coupled plasma (ICP) Direct current plasma (DCP) Flame Arc and spark

9. Plasma Source “ Plasma is defined as a neutral gas containing significant number of both positive and negative ions or free electrons”

10. Continue Light source Arc and spark Laser induced breakdown Laser induced plasma Microwave induced plasma

11. Laser Beam Excitation

12. A T OMI Z ER AND SAMPLE HANDLING

13. A t omi z er Elements to be analyzed needs to be in atomic state. Atomization; Conversion of sample (maybe; solid or liquid) into free gaseous atom. Atomizer; Device used for atomization

14. TYPES OF ATOMIZER FLAME ATOMIZER C ON T I NUO US D I S C R E T E E L E C T R O- T H ERM A L ATOMIZER

15. 1. Flame Atomizer To produce flame, required oxidant gas and flame gas. Mostly the air-acetylene flame or nitrous oxide- acetylene flame is used. Liquid or dissolved samples are typically used with flame atomizer.

16. Flame Atomization

17. Sub-types Of Flame Atomization Continuous Atomization; sample penetrate the atomizer at constant speed. not used for dissolved solid.* Discrete Atomization; measured amount of sample enters atomizer. – effective when sample volume islimited.

18. 2. Electro-thermal Atomizer Also known as “Graphite Furnace Atomizer” More convenient to uses a non-flame method i.e. electrically heated graphite tube.

19. Atomization Of Sample drying of sample into solid deposit. by heating graphite tube at 110 ºC. DRYING ASHING conversion of organic matter in CO 2 and H 2 O &volatilization of inorganic matter. by heating graphite tube at 350-1200 ºC. ATOMIZATION leads to gaseous atom by raising the temperature up to 2000-3000 ºC.

20. Advantages; Small sample size Little or no sample preparation required Enhanced sensitivity Direct analysis of solid samples Disadvantages; Loss of analyte during ashing stage Incomplete atomization

21. Sample Handling The droplets of sample introduced in atomizer should be of constant size. The temperature should be maintained to obtain good reproducibility. The speed of introducing sample must be equal to certain permissible band values. Sufficient sample volume should be available for maximum efficiency

22. MONOCROMATORS Prism Diffraction grating

23. M o noc h r o m a t or It is a device use to transmit narrow band of wavelength which is chosen from wavelength of wider range available. Types of monochromator: Prism Monochromator Grating Monochromator

24. a. Prism When the light pass through prism it emerges out in form of two lines or beam. To overcome this drawback two half prism are placed. When light pass through first prism it splits into two beams, when it reaches second half prism recombines two beam into single beam

25. b. Diffraction grating It gives better result and resolution. It replaced prism give linear dispersion. Problem occurred during the identification of wavelength of emission lines on photographic plate solved through grating monochromator. Once we identify known reference line and other lines identified automatically.

26. DETE C T ORS

27. Phototube (Photo Electric Cell) Glass filled or vacuum tube Sensitive to light Depend on frequency and intensity of incoming photon Need amplifier. But are replaced by photomultiplier detectors.

28. Photo Multiplier Detector Vacuum phototubes, are extremely sensitive detectors of light in the ultra violet, visible, and near-infrared region ranges of the electromagnetic spectrum.

29. A P P L IC A TIONS

30. A ppl i ca t i o ns It is used for rapid analysis of multi-component pharmaceutical tablet. It is used for elemental analysis. It is used primarily for the identification and determination of metals in traces amount.

31. It is used for determination of mineral composition of igeous and metamorphic rock. It is used for routine analysis of wear metals in lubricating oils. It is used for the analysis of sodium, potassium and lithium.