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EPA 552.1 by Strata-X-A on a ZB-XLB-HT

Sample Preparation Details

Part No:8B-S123-EBJ
Solid Phase Extraction (SPE) procedure:Note: The solvent volumes shown below are for a 100 mg bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass.
Load:Water spiked with haloacetic acids ranging in conc. from 10ug/L to 100ug/L
Dry:None
Final Prep and Analysis:
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.
Inject: 1 µL on GC / Electron Capture (ECD) @ / (340 °C)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
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

Application Detail (App ID: 19322)

Part No:7HM-G024-11
Phase:Proprietary XLB Phase
Dimensions:30 meters x 0.32 mm x 0.25 µm
Oven Profile:30°C for 4 min to 50°C @ 30°C/min for 1 min to 70°C @ 15°C/min for 1 min to 115°C @ 20°C/min for 2 min to 200°C @ 30°C/min.
Carrier Gas:Constant Flow Helium, 2.3 mL/min
Injection:Pulsed :1 1 µL @ 250°C
Detection: Electron Capture (ECD) (340°C)
Note: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.


Analyte Details

Analyte Detail not available

1
Chloroacetic acid
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2
Bromoacetic acid
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3
Dichloroacetic acid
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4
Dalapon
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5
Trichloroacetic acid
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6
Bromochloroacetic acid
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7
1,2,3-Trichloropropane
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8
Dibromoacetic acid
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