EPA 552.1 by Strata-X-A on a ZB-XLB-HT
GC Conditions
Official Method
EPA 552
Column
Zebron ZB-XLB-HT, GC Cap. Column 30 m x 0.32 mm x 0.25 µm, Ea
Part No
7HM-G024-11
Phase Name
ZB-XLB-HT
Injection
Pulsed @ 250°C
Carrier Gas
Constant Flow Helium, 2.3 mL/min
Detection
Electron Capture (ECD) @ (340°C)
Detection Info
Sample Notes
Derivatization: Add 1mL of MTBE to the eluent in a screw cap vial or test tube. Heat the sample at 50ºC for 1.5 hours. Remove and allow the sample to cool to room temperature. Slowly add 10mL of saturated sodium bicarbonate and invert the sample several times releasing carbon dioxide gas frequently. Aspirate 100µL of the organic layer and transfer to a 2mL vial with insert. Add 10µL of internal standard (1,2,3-Trichloropropane) and inject into GC-ECD system.
Sample Preparation Details
Pretreatment Note
Elute: 1mL of 10% Sulfuric acid in methanol, eluent should be collected in a screw cap vial or test tube to accommodate derivatization. Note: Blank sample extract, post spiked was processed as above to prepare an extracted ref sample (Eref) for absolute recovery calculation Derivatization: Add 2mL of MTBE to the eluent in a screw cap vial or test tube. Heat the sample at 50ºC for 1.5 hours. Remove and allow the sample to cool to room temperature. Slowly add 10mL of saturated sodium bicarbonate and invert the sample several times releasing carbon dioxide gas frequently. Aspirate 100µL of the organic layer and transfer to a 2mL vial with insert. Add 10µL of internal standard (1, 2, 3-Trichloropropane) and inject into GC-ECD system.
Condition 1
2 mL Methanol at 1 mL/min
Condition 2
2 mL Water at 1 mL/min
Load
Load 100.00 mL Sample diluted in Water
Wash 1
1 mL Methanol at 1 mL/min
Dry
None
Elution 1
1 mL 10% sulfuric acid in methanol at 1 mL/min
Evaporation
Evaporate to dryness
Order Items Used in This Application
- 1. Chloroacetic acid
- 2. Bromoacetic acid
- 3. Dichloroacetic acid
- 4. Dalapon
- 5. Trichloroacetic acid
- 6. Bromochloroacetic acid
- 7. 1,2,3-Trichloropropane
- 8. Dibromoacetic acid
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