Method 508.1: Determination of Chlorinated Pesticides and Herbicides Analysis by Liquid-Solid Extraction and Electron Capture GC
EPA Method 508.1 includes many of the same components as Method 505, but it also contains several other compounds, including chlorinated pesticides, herbicides, and organohalides. In order to increase sample throughput, an optimized method is shown here using a dual column configuration with the Rtx-CLPesticides/Rtx-CLPesticides2 column pair. These columns, used under the conditions shown, offer a unique selectivity that allows the target analytes to be resolved in approximately half the analysis time of the original method. Further, both columns easily passed the comprehensive system performance criteria adapted from 508.1 (see table below). The unique selectivity of the Rtx-CLPesticides/Rtx-CLPesticides2 column pair offers an ideal balance of speed and resolution for chlorinated pesticide, herbicide, and organohalide analysis.
Rtx-CLPesticides and Rtx-CLPesticides2 columns easily pass Method 508.1 performance criteria.
Test/Requirement | Analyte | Concentration (ppb) | Rtx-CLPesticides2 | Rtx-CLPesticides |
Inertness (breakdown <20%) | endrin | 50 | 0.9% | 1.4% |
Inertness (breakdown <20%) | 4,4'-DDT | 100 | 1.0% | 1.1% |
Sensitivity (S/N>3) | chlorpyrifos | 2 | 12.0 | 6.2 |
Chromatographic performance (0.8<PGF<1.15) | DCPA | 50 | 1.03 | 1.06 |
Column performance (resolution>0.50) | delta-BHC/ chlorothalonil |
40/50 | 9.9 | 26.8 |
Vendor | Column Pair | Analysis Time (min) | Coelutions | Restek Advantage |
---|---|---|---|---|
Restek | Rtx-CLPesticides / Rtx-CLPesticides2 |
23.5 / 24 | 2 / 2 |
|
Competitor A | column 1 / column 2 | 21 / 23 | 0 / 3 | |
Competitor B | column 1 / column 2 | 18 / 17 | 2 / 4 |
Comparison based on published competitor data. All columns tested were 0.32 mm ID.
24-minute analysis of Method 508.1 chlorinated pesticides, herbicides, and organohalides using Rtx-CLPesticides columns and a micro-ECD.
Peaks | |
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1. | Hexachlorocyclopentadiene |
2. | Etridiazole |
3. | Chlorneb |
4. | Propachlor |
5. | Trifluralin |
6. | Hexachlorobenzene |
7. | α-BHC |
8. | Simazine |
9. | Atrazine |
10. | Pentachloronitrobenzene (IS) |
11. | γ-BHC |
12. | β-BHC |
Peaks | |
---|---|
13. | δ-BHC |
14. | Heptachlor |
15. | Chlorothalonil |
16. | Metribuzin |
17. | Alachlor |
18. | Aldrin |
19. | 4,4'-Dibromobiphenyl (SS) |
20. | Metolaclor |
21. | DCPA methyl ester (Chlorthal-dimethyl) |
22. | Heptachlor epoxide |
23. | trans-Chlordane |
24. | Cyanazine |
Peaks | |
---|---|
25. | cis-Chlordane |
26. | Endosulfan I |
27. | 4,4'-DDE |
28. | Dieldrin |
29. | Endrin |
30. | Chlorobenzilate |
31. | 4,4'-DDD |
32. | Endosulfan II |
33. | 4,4'-DDT |
34. | Endrin aldehyde |
35. | Endosulfan sulfate |
36. | Methoxychlor |
37. | cis-Permethrin |
38. | trans-Permethrin |
Columns | Rtx-CLPesticides2 30 m, 0.32 mm ID, 0.25 µm (cat.# 11324) |
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and Rtx-CLPesticides 30 m, 0.32 mm ID, 0.32 µm (cat.# 11141) | |
using Rxi guard column 5 m, 0.32 mm ID (cat.# 10039) | |
with deactivated universal “Y” Press-Tight connector (cat.# 20405-261) | |
Standard/Sample | 50 ng/mL 508.1 calibration mix #1 (cat.# 32094) |
100 ng/mL 508.1 calibration mix #2 (cat.# 32095) | |
100 ng/mL 508.1 calibration mix #3 (cat.# 32096) | |
50 ng/mL pentachloronitrobenzene (cat.# 32091) | |
250 ng/mL 4,4'-dibromobiphenyl (cat.# 32092) | |
500 ng/mL atrazine (cat.# 32208) | |
500 ng/mL simazine (cat.# 32236) | |
Diluent: | Ethyl acetate |
Injection | |
Inj. Vol.: | 2 µL splitless (hold 0.75 min) |
Liner: | Cyclo double taper (4 mm) (cat.# 20896) |
Inj. Temp.: | 250 °C |
Oven | |
Oven Temp.: | 80 °C (hold 0.5 min) to 155 °C at 19 °C/min (hold 1 min) to 210 °C at 4 °C/min to 310 °C at 25 °C/min (hold 0.5 min) |
Carrier Gas | He, constant flow |
Linear Velocity: | 26 cm/sec |
Detector | Micro-ECD @ 325 °C |
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Notes | This chromatogram was obtained using an Agilent micro-ECD. To obtain comparable results, you will need to employ a micro-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight connector. |