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Automating the Fractionation of Extractable Petroleum
Hydrocarbons with a Scaled Down Sil...
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Automated fractionation of extractable petroleum hydrocarbons with a scaled down silica gel cartridge

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Petroleum products contain a complex mixture of aliphatic and aromatic components. The composition of hydrocarbons varies depending on the source, e.g. crude oil versus refined products. Not all components pose the same amount of health risk. Particularly the amount of polycyclic aromatic hydrocarbons (PAH) needs to be determined accurately.

In order to properly separate both aliphatic and aromatic fractions, a pre-fractionation with silica gel is carried out. The manual method is tedious and requires a very good
technique to obtain good recovery for the volatile PAH.

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Automated fractionation of extractable petroleum hydrocarbons with a scaled down silica gel cartridge

  1. 1. www.the-uninspired-scientist.com Automating the Fractionation of Extractable Petroleum Hydrocarbons with a Scaled Down Silica-Gel Cartridge Roel Wu�ts, Jef Leemans and Joeri Vercammen j.vercammen@is-x.com www.is-x.com Petroleum products contain a complex mixture of aliphatic and aromatic components. The composition of hydrocarbons varies depending on the source, e.g. crude oil versus refined products. Not all components pose the same amount of health risk. Particularly the amount of polycyclic aromatic hydrocarbons (PAH) needs to be determined accurately. In order to properly separate both aliphatic and aromatic fractions, a pre-fractionation with silica gel is carried out. The manual method is tedious and requires a very good technique to obtain good recovery for the volatile PAH. Fractionation is carried out automatically using the SmartPrep Extractor. Recoveries are acceptable for all components and range between 75% and 120% voor five replicate fractionations. Breakthrough of naphthalene is < 5%. Precisions are situated between 3 and 20%. A post run system flush is applied to reduce carry-over. Commercial SmartPrep Extractor (Horizon Technology) equipped with 6 mL silica gel cartridges (2.5 g). Cartridge is PTFE coated to eliminate cross contamination from hydrocarbon extractables and plasticizers. Custom sequence based on EPH reference methods*. Goals: - Process six extracts - Less than 5% breakthrough for naphthalene - Maximum recoveries for aliphatics and aromatics - High precision - Robust - No carry-over between samples * Consecutive elution with hexane (aliphatic phase) and hexane/DCM (aromatic phase). 2.3% Naphthalene breakthrough 82.4% C24 recovery 118.1% C9 recovery ANT recovery 73.8% I(123-cd)PY recovery 111.6% Aliphatic fraction Aromatic fraction 0 100 0 100 Typical chromatograms Minimal and maximal analyte recoveries (n=5)

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