Separatory Funnel Liquid-Liquid Extraction

- 1 -CELPage 1 11/03/2018PCB WD Prep

PCB Oil Extraction

EPA SW-846 Method 3580

Procedure 6710.A

Description:

This procedure is applicable to samples that when submitted are soluable in hexane,and the concentration of PCB is being measured.After the sample aliquot has been diluted in hexane,several clean-up steps follow,starting with sulfuric acid to remove the PCB from the sample matrix and transfer it to the heane. It is applicable to,but limited to,transformer oils,solvents and other hydrocarbon-based samples.

Apparatus:

-40mL VOC Vial

-Pasteur Pipettes and bulbs

-2mL vials with crimp tops

Reagents:

-PCB surrogate and spiking mixture

-Hexane

-Sulfuric Acid

-Sodium Sulfate

Procedure:

1.0Extraction

1.1.1Label clean 40mL VOC Vials with sample information. Vials should be rinsed with hexane prior to use to remove any organic residue.

1.1.2The Blank and LCS consist of 1grams of sodium sulfate in the vial.

1.1.3Place 1gram of sample in the labeled vial (1gram of designated sample for MS, MSD also)

1.1.4Add 10mL Hexane to all vials.

1.1.5Add 50L surrogate to all and 50L spike to LCS, MS, and MSD.

1.1.6Add 1 Pasteur Pipette of concentrated Sulfuric Acid to each vial and mix on the Vortex mixer.

1.1.7Acid should turn dark and remain on the bottom of the vial.

Remove this acid discarding it into the acid waste bottle. Continue to add acid, shake, and remove until acid stops turning dark (4-5 washes are usually sufficient). A wash with water may be necessary after the acid washing to remove any residual acid. Again, the water layer will remain on the bottom of the vial. This should be removed and discarded. Be aware of removing too much hexane with the acid.

1.1.8Transfer 1mL of the hexane to a labeled 2mL vial; be careful not to transfer any acid to the vial. This should be passed through a disposable Pasteur pipette that has been plugged with glass wool, and contains layers of sodium sulfate, silica gel and activated copper. Each of these layers is designed to remove specific interferences. The sodium sulfate should remove any residual water. Silica gel is for any remaining large molecules, such as hydrocarbons, and the activated copper should turn dark in the presence of elemental sulfur. The capped and labeled vial is then submitted to the GC department for analysis. It should have the designation as “W/D” for waste dilution as its batch identification.

Reference SW-846 Method 3580A

Procedure 6710.A

Revised 04/07