1. Environmental Health Laboratories Yongtao B. Li, Ed J. George, Earl M. Hansen, and Jerry J. Thoma and Werner Martin and Peter D. Smith (LEAP Technologies) An Innovative Automated Microscale Solid Phase Extraction Technology Coupled with GC-MS for Online Analysis of Water Samples Pittcon 2000 March 14, 2000

2. Environmental Health Laboratories Large Volume Injection (LVI) GC and GC-MS

3. Environmental Health Laboratories LVI-GC Conditions Injection Vol.:50 µL eluate Injector Temp.:80 ºC for 1 min, 80-280 ºC at 300ºC/min, 280 ºC for 34 min Vent Valve: 0-0.6 min open, 0.6-3.5 min closed, 3.5- 37 min open Vent Flow: 85 mL/min Column Temp.:45 ºC for 3 min, 45-160 ºC at 50 ºC/min, 160-260 ºC at 5 ºC/min, 260-330 ºC at 6 ºC/min, 330 ºC for 1 min Helium: 26 cm/s at 100 ºC

4. Environmental Health Laboratories SPE Twin-PAL LVI-GC-MS

5. Environmental Health Laboratories Extraction and Collection Plates

6. Environmental Health Laboratories SPE Twin-PAL LVI-GC-MS Running Sequence

7. Environmental Health Laboratories SPE Twin-PAL LVI-GC-MS Running Sequence

8. Environmental Health Laboratories Automated SPE Conditions Cleaning:500 µL 1:1 dichloromethane:ethyl acetate Conditioning:500 µL methanol & 500 µL reagent water Extraction:10 mL samples Washing:1 mL reagent water Drying:5 min nitrogen gas Elution:160 µL 1:1dichloromethane:ethyl acetate Mixing:~ 90 µL eluate + 10 µL internal standard Injection:50 µL

9. Environmental Health Laboratories Automated Multi-Step Elution 160 µL 1:1 dichloromethane:ethyl acetate at 10 µL/s. –70 µL solvent, then soak for 60 s; –30 µL solvent, then soak for 30 s; –30 µL solvent, then soak for 30 s. Flush with nitrogen gas at 15 psi for 5 s.

10. Environmental Health Laboratories SPE Twin-PAL LVI-GC-MS Calibrations Environmental Health Laboratories 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 0246810 Heptachlor Bromacil Heptachlor Epoxide gamma-Chlordane alpha-Chlordane trans-Nonachlor Dieldrin Endrin 0.05-10 ug/L, 50 uL R 2 = 0.999-1.000 Concentration, ug/L Sample Area/Standard Area

11. Method Sensitivity, Accuracy and Precision

12. Online Analysis of Treated Well Water

13. Online Analysis of Untreated Well Water

14. Online Analysis of Tap Water