Chromatography

Polynuclear Aromatic Hydrocarbons In Water By Automated Solid Phase Extraction and HPLC Analysis

Author: FMS, Inc on behalf of Fluid Management Systems Inc

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Introduction

Produced as the byproducts of fuel com-bustion, polynuclear aromatic hydrocarbons (PAHs) consist of fused aromatic rings. As pollutants, they are of concern because some polynuclear compounds have been identified as carcinogenic, mutagenic, and teratogenic.  PAHs are lipophilic and therefore found in the environment, primarily in soil, sediment, and oily substances. They also appear in surface and ground water, indicating a source of pollution.

Instrumentation and Consumables

  • FMS, Inc. TurboTrace™ SPE system (solid phase extraction)
  • FMS, Inc. SuperVap™ Concentrator
  • FMS, Inc. 1 gram PAH C18 cartridge
  • Waters Alliance 2695 HPLC, UV254

Method Summary

TurboTrace SPE

  1. Condition cartridge with 15 mL dichloromethane
  2. Condition cartridge with 15 mL methanol
  3. Condition cartridge with 35 mL water
  4. Load 1 liter of water sample
  5. Dry cartridge for 20 minutes
  6. Rinse sample bottle with 35 mL dichloromethane
  7. Elute sample from cartridge with
    bottle rinse
  8. Elute sample with additional 25 mL dichloromethane

SuperVap Concentrator

  1. Pre-heat temp:  60 ºC
  2. Pre-heat time:  20 minutes
  3. Heat in Sensor mode:  60 ºC
  4. Nitrogen pressure:  9 PSI

Procedure

Three, one liter samples were acidified to pH 2 with 6N hydrochloric acid and spiked with 5 μL of Restek 31458 MA EPH aromatic hydrocarbon solution. Samples were then loaded onto the FMS TurboTrace SPE system using vacuum adjusted to -10 psi and passed across an FMS PAH C18 cartridge. After sample loading, the cartridges were automatically dried using a stream of nitrogen until no residual water remained. The cartridges were subsequently eluted using dichloro-methane from both the automatic sample bottle rinse and from the elution solvent reservoir. The extracts were concentrated to 1.0 mL and 5 mL acetonitrile was added for solvent exchange. The sample was concentrated to a final volume of 1 mL for HPLC analysis.

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