Lecture 8

Elementorganic Toxins

Determination

Graphite furnace atomic absorption

Cold Vapor Atomic absorption and Fluorescence

ICP-MS

HPLC-ICP-MS

GC-MS

GC-ECD

Electrodeless Discharge Lamps

Sn, Cd, Hg, Zn, Pb, As, Sb, Bi, Tl, In Se, Te, Rb, and Cs

222

243 822552985 MnOHCOHgHMnOHgCH

+KMnO4 +NH3OH+

22343 6145865 MnOHNOHMnOOHNH

To convert organic mercury into Hg2+

To remove MnO4- ion:

To MHS-1530 min Overnight

0.1-0.3g

HNO3

@85oC

Digestion Procedure:

Sample

To cuvette

N2

SnCl2 Sample compartment

OHMnSnHMnOSn 224

42 8251625

4022 SnHgHgSn

PerkinElmer MHS-15 Mercury Analyzer

Hollow cathode Hglamp

Hg vapor

Monochromator

Detector

Data processing

Quarz cuvette253.6 nm

Thermo Jarrel Ash Smith-Hieftje 11AAS

ECD detector

ICP detector

F

PO

O

OO

PS

SOO

OO

OO

PS

OOO

OO

sarin

Malathion

Malaoxon

warfare agent

Organophosphorus Pesticides

GC

30. fenthion31. aspon32. parathion-ethyl33. chlorpyrifos34. trichloronate35. chlorfenvinphos36. merphos37. crotoxyphos38. stirofos39. tokuthion40. merphos oxidation product41. fensulfothion42. famphur43. ethion44. bolstar45. carbophenothion46. triphenyl phosphate (IS)47. phosmet48. EPN49. azinphos-methyl50. leptophos51. tri-o-cresyl phosphate52. azinphos-ethyl53. coumaphos

2. hexamethylphosphoramide3. mevinphos4. trichlorfon5. TEPP6. thionazin (IS)7. demeton-O8. ethoprop9. tributyl phosphate (SS)10. dicrotophos11. monocrotophos12. naled13. sulfotepp14. phorate15. dimethoate16. demeton-S17. dioxathion18. terbufos19. fonophos20. phosphamidon isomer21. diazinon22. disulfoton23. phosphamidon24. dichlorofenthion25. parathion-methyl26. chlorpyrifos methyl27. ronnel28. fenitrothion29. malathion

Organophosphorus PesticidesOven temp.: 100°C to 180°C @ 10°C/min. (hold 2 min.), to 300°C @ 18°C/min. Inj. / det. temp.: 250°C / 280°C FPDSolvent: hexane

OOH

O

ClCl

2,4-Dichlorophenoxyacetic acid (2,4-D)

OOH

O

ClCl

Cl

2,4,5-Trichlorophenoxyacetic acid (2,4,5-T)

O

O1

2

34 6

7

89

O

OCl

Cl

Cl

Cl

2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD)

1. 1,4,7,8-TCDD2. 2,3,7,8-TCDD3. 1,2,3,4-TCDD4. 1,2,3,75. 1,2,3,8-TCDD6. 1,2,7,8-TCDD

GC: 2.0μL splitless injection of TCDD isomers,approximately 0.5ng each isomerSplitless hold: 0.45 min ECD detector