Chromatography Forum

Hallo, excuse me for my bad english....
Have anybody some experience with extraction of PCB and organochlorous pesticides from water by SPE? I get bad recoverys... and i dont know what to do...

I used: SPE C18 500mg

Conditions: add 5 ml of methanol, then 5 ml isopropanol (10%), then 5 ml of tube distiller water
Load: 500 ml of sample (water) very slowly (1 hour)
Wash: 5 ml isopropanol (10%)
Dry SPE: 1 hour in centrifuga at 4000 rpm
Elute: 2x 5 ml od dichloromethane

Eluate is evaporated under stream od nitrogen to dryness and reconstitute in hexan. Add internal standard and analyze by GC-MS.

Tanks for any answers.

Zdenek.

The Japanese have a validated method. Supelco sells the components to do the analysis. Give their technical service a call and they may be able to assist you.

best wishes,

Rodney George

Thank you, chromatographer1.

Dont know name of this Japanese metod? I have tried find this on google, but I cannt.

JSA JIS K 0311:2005
JSA JIS K 0312
Method for determination of tetra- through octachlorodibenzo-p-dioxins, tetra- through octachlorodibenzofurans
and dioxin-like polychlorinated biphenyls in stationary source emissions
Method for determination of tetra- through octachlorodibenzo-p-dioxins, tetra- through octachlorodibenzofurans
and dioxin-like polychlorinated biphenyls in industrial water and waste water limits

Call Supelco technical service and they have the hardware to do the extraction. I assisted in the preparation of the materials to perform this analysis.

They have a very informative PDF which details the procedure. Ask them for the Dioxin - PCB literatures

www.pdfxp.com/supelco-pdf.html another link.