HyperSep Column Applications

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EPA Method 8330B – Explosives and Residue Analysis –
Nitroaromatics, Nitroamines, Nitrate Esters
Using 500mg 6mL HyperSep Retain PEP Extraction Column (Part Number: 60107-206)
Sample Preparation
Soil
Add 2.0g of soil into a 25mL glass vial
Add 2g of sodium sulfate and mix
Add 0.1mL explosives soil surrogate to all samples,
(blanks/spikes)
Add 0.5mL explosives spike to the LCS, LCSD, matrix
spike, and matrix spike duplicate samples
Add 10mL of ACN
Mix/vortex 1 minute
Sonicate for 18 hours (<10°C)
Centrifuge 15 to 20 minutes
Remove solvent layer
Add solvent layer to 5mL (5.0 gram/L) CaCl2
Mix and leave to stand for 15 minutes
Filter through 1µm Teflon filter
Discard the first 3mL, retain the remainder
Discard the first 3mL and retain the remainder in an
appropriately labeled 12mL vial
Store in a refrigerator
Aqueous matrices
Do not concentrate explosives residue to dryness as they
may detonate
1L of sample water
Add 5.0mL of methanol and surrogate standards to all
samples and blanks
Add matrix spikes standards to sample replicates
Glass Apparatus Washing
Explosives
1 x 5mL ACN
1 x 15mL IPA
1 x 15mL CH3 OH
Nitramines, Nitroaromatics
1 x 5mL ACN
1 x 15mL ACN
Draw solvents through the cartridge under low vacuum
Condition HyperSep Hypercarb Extraction Column
Use an all glass vacuum manifold
Explosives
1 x 20mL ACN
1 x 20mL ACN
1 x 50mL DI H 2O
1 x 50mL DI H 2O
Nitramines, Nitroaromatics
1 x 15mL ACN
1 x 30mL DI H 2O
Apply Sample
Load sample at 10mL/min
Dry column under vacuum for 15 minutes
Elute
Explosives
1 x 4mL ACN
Collect eluate at low flow
Store in freezer
Nitramines, Nitroaromatics
1 x 5mL ACN
Collect eluate at low flow
Store in freezer
Evaporation
Evaporate eluates to 0.7mL under a gentle stream of
nitrogen <40°C
Analysis
Add internal standard to 0.7mL sample
Inject 100µL onto LC/MS
Flow rate: 0.50mL/minute
Mobile phase: 50:50
Recommended HPLC Columns Part Number
Hypersil GOLD 5µm, 250 x 4.6mm 25005-254630
Hypersil GOLD C8 3µm, 150 x 4mm 25203-154030
Hypersil GOLD CN 5µm, 250 x 4.5mm 25805-254630
Betasil Phenyl Hexyl 5µm, 250 x 3mm 73005-253030
Environmental
Applications