Semivolatile Compounds, EPAMethod 8270
Column: HP-5ms 19091S-133 30 m x 0.25 mm, 0.50 µm
Carrier: Ramped flow 1.2 mL/min for 0.0 min Ramp at 99 mL/min to 2.0 mL/min 2.0 mL/min for 0.35 min Ramp at 10 mL/min to 1.2 mL/min
45 37 22, 23 33 29 38 18 16 4, 5 10 8 3 1, 2 24 6 7 12
11 9
14 13 20 19 17
15 18
34 21 28
25 26
27 30
31 32 35 36 42 40 43
39 41
52
4851 56 50
55 58
62 67 63 64 66 65 70 68, 69 61 72 73 78
47 46
54 53
57 5960 71 77 79 80 82 81 83 74 76 Suggested Supplies
Septum: Advanced Green, 5183-4759 Liner: Splitless, single taper, deactivated, 4 mm ID, 5181-3316
Syringe: 10 µL tapered, FN 23-26s/42/HP, 5181-1267
Oven: 40°C for 1.0 min 40-100°C at 15°C/min 100-240°C at 20°C/min 240-310°C at 10°C/min
Sample: 1 µL of 50 ng standard 75
Injection: Splitless, 250°C 30 mL/min purge flow at 0.35 min
Detector: 5973 MSD, 310°C transfer line Scan range 35-500 amu, 3.25 scans/sec
4
6
8
1. n-Nitrosodimethylamine 2. Pyridine 3. 2-Fluorophenol 4. Phenol-d5 5. Phenol 6. Aniline 7. Bis(2-chloroethyl) ether 8. 2-Chlorophenol 9. 1,3-Dichlorobenzene 10. 1,4-Dichlorobenzene-d4 11. 1,4-Dichlorobenzene 12. Benzyl alcohol 13. 1,2-Dichlorobenzene 14. 2-Methylphenol 15. Bis(2-chloroisopropyl) ether 16. 4-Methylphenol 17. n-Nitroso-di-n-propylamine 18. Hexachloroethane 19. Nitrobenzene-d5 20. Nitrobenzene 21. Isophorone 22. 2-Nitrophenol
10
12
14 Time (min)
23. 2,4-Dimethylphenol 24. Benzoic acid 25. Bis(2-chloroethoxy) methane 26. 2,4-Dichlorophenol 27. 1,2,4-Trichlorobenzene 28. Naphthalene-d8 29. Naphthalene 30. 4-Chloroaniline 31. Hexachlorobutadiene 32. 4-Chloro-3-methylphenol 33. 2-Methylnaphthalene 34. Hexachlorocyclopentadiene 35. 2,4,6-Trichlorophenol 36. 2,4,5-Trichlorophenol 37. 2-Fluorobiphenyl 38. 2-Chloronaphthalene 39. 2-Nitroaniline 40. Dimethylphthalate
41. 2,6-Dinitrotoluene 42. Acenaphthylene 43. 3-Nitroaniline 44. Acenaphthene-d10
45. Acenaphthene 46. 2,4-Dinitrophenol 47. 4-Nitrophenol 48. Dibenzofuran 49. 2,4-Dinitrotoluene 50. Diethylphthalate 51. 4-Chlorophenyl-phenyl ether 52. Fluorene 53. 4-Nitroaniline 54. 4,6-Dinitro-2-methylphenol 55. n-Nitrosodiphenylamine 56. Azobenzene 57. 2,4,6-Tribromophenol 58. 4-Bromophenyl-phenylether 59. Hexachlorobenzene 60. Pentachlorophenol 61. Phenanthrene-d10 62. Phenanthrene 63. Anthracene 64. Carbazole 65. Di-n-butylphthalate 66. Fluoranthene
16
18
20
22
24 GCES015
67. Pyrene 68. Terphenyl-d14 69. Benzidine 70. Butylbenzylphthalate 71. 3,3'-Dichlorobenzidine 72. Benzo[a]anthracene 73. Chrysene-d12 74. Chrysene 75. Bis(2-ethylhexyl) phthalate 76. Di-n-octylphthalate 77. Benzo[b]fluoranthene 78. Benzo[k]fluoranthene 79. Benzo[a]pyrene 80. Perylene-d12 81. Indeno[1,2,3-cd]pyrene 82. Dibenz[a,h]anthracene 83. Benzo[g,h,I]perylene
A variety of Agilent HP-5ms and DB-5ms columns can be used for 8270 and similar semivolatiles applications. The column shown above was chosen to maximize inertness and robustness to residues with a thicker 0.5 µm film, but the price paid is a slightly longer run time. An HP-5ms, 30 m x 0.25 mm ID, 0.25 µm, P/N 19091S-433 would give shorter run times, with slightly less inertness and robustness. A DB-5ms, 30 m x 0.25 mm ID, 0.25 µm, P/N 122-5532, would give slightly less inertness, but offer better resolution of PAHs such as Benzo[b]fluoranthene and Benzo[k]fluoranthene. A DB-5ms, 20 m x 0.18 mm x 0.18 µm, P/N 121-5522, can offer significantly reduced run times with a modest loss of inertness.
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