Elemental Analysis by Inductively Coupled Plasma - MS and OES

Comparison between ICP-MS and ICP-OES
Instrumentation
Uses
Case Study
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1. Elemental analysis by ICP Guided by:- DR. Vaishali Shirsat Presented by:- Manali parab F.Y.M.PHARM PHARMACEUTICAL ANALYSIS DEPARTMENT 1

2. Instrumentation of ICP-MS 2

3. Flow diagram for ICP-MS Sample Introduction System Ionization System Detection System Interface 3

4. Sample Introduction Systems Pneumatic nebulisers 4

5. Concentric Nebulizers 5

6. Cross-flow nebulizers 6

7. High Solid Nebulizers 7

8. Ultrasonic Nebulizers These nebulizers use an ultrasonic generator at a frequency of between 200 kHz and 10 MHz to drive a piezoelectric crystal. 8

9. Spray Chambers The purpose of the spray chamber is to remove droplets produced by the nebulizer that are >8μm in diameter Faster wash out time depends on wettability of glass Water-cooled spray chambers may be used for volatile organic solvents They are externally cooled for thermal stability of the molecule Important advantage: to reduce oxide species, reduce solvent loading 9

10. Double pass Spray Chambers 10

11. Cyclonic spray chambers 11

12. Laser ablation ICP-MS 12

13. Nd: YAG LA system for ICP-MS 13

14. Sample and skimmer cones 14

15. Vacuum system Turbo molecular pump 15

16. ICP Torch 16

17. Torch configuration Axial View Radial View Dual View 17

18. The Lens System - Focusing Ions 18

19. Collision cell and Reaction Cell 19

20. Ion deflector devices- Quadrupole Mass Analyser 20

21. Ions collecting device and detecting system Photomultiplier Tube Faraday Cup 21

22. Application Simple metal analysis during metal based drug development Impurity limit tests Metals present in Active Pharmaceutical Ingredients Quality Control Tests of natural products for toxic impurities testing Monitoring metabolites of an administered drug Detection of metal impurities from leachable packaging material For elemental speciation Pharmaceutical Waste Water monitoring 22

23. ICP-OES 23

24. INSTRUMENTATION OF ICP-OES 24

25. Sample introduction system other than ICP-MS Hildebrand grid nebulizer (HGN) 25

26. Hydride generator Chemical reaction in generation of Hydride NaBH 4 + 3H 2 O + HCl H 3 BO 4 + NaCl + 8H 8H + E m+ EH n + H 2 (excess) HG is a very effective sample introduction technique for elements like arsenic, bismuth, germanium, lead, antimony, selenium, tin, and tellurium. 26

27. Electrothermal vaporisation 27

28. Detection of emission Concave grating placed on a Rowland circle 28

29. Echelle grating coupled with a prism order-sorting device Echelle Polychromator 29

30. Photomultiplier Tube 30

31. Array detectors 31

32. Type of detection Sequential Detection Simultaneous Detection 32

33. Applications Determination of metals in biological fluids (blood. urine) Environmental Analysis: Trace metals and other elements in water, soil and plants Pharmaceuticals: Traces of catalyst used Industry: Trace metal analysis in raw material Forensic science: Toxicological determination 33

34. Comparison between ICP-OES and ICP-MS ICP-OES ICP-MS Sample introduction for solution of inorganic salt is rapid and convenient Sample introduction of inorganic salt can be difficult (generally not volatile) Sample introduction is at atmospheric pressure Requires reduced pressure sample introduction Relatively large amount of dissolved solids can be tolerated Limited to less amount of dissolved solids by conventional method (<1%) Complicated spectra with frequent spectral overlap Relatively simple spectra Moderate sensitivity (ppm to ppb range) Excellent sensitivity (ppb to ppt range) Isotope ratio cannot be determined Isotope ratio determination possible 34

35. Case study THE ANALYSIS OF ECSTASY TABLETS BY ICP/MS AND ICP/AES by Stéphane COMMENT, Eric LOCK, Christian ZINGG1, Alfred JAKOB, Institute de Police Scientifique et de Criminologie, University de Lausanne, Switzerland AC Laboratories, Spiez, Switzerland In this study, Ecstasy tablets coming from different police seizures (in Switzerland) were analysed by ICP/MS and ICP/AES. The most frequent elements found were Ca, Mg, Na, K, Al, Si and Fe. Instrument used for ICP-OES: Perkin Elmer Emission Spectrometer Plasma 1000 Instrument used for ICP-MS: Perkin Elmer Elan 6000 35

36. DETECTION LIMITS FOR ICP/MS AND ICP/AES 36

37. 20 tablets coming from one batch (containing MDMA) and 20 other tablets coming from another batch (containing MDEA) were used The variation depends on the element analysed. The mean variation was found to be 20% for ICP/AES and 25% for ICP/MS. Therefore, these relative standard deviations represents the variation within batch including the instrument and quantification errors. RELATIVE STANDARD DEVIATIONS FOR ICP/MS AND ICP/AES 37