A High Throughput, Low Cost and Green Approach to Automated Extraction, Clean Up, and Concentration for Same Day POPs Analysis

Oral Presentation

Prepared by P. Bassignani
Fluid Management Systems, 580 Pleasant Street, Watertown, MA, 02472, United States

Contact Information: pbassignani@fms-inc.com; 617-393-2396


Persistent organic pollutants (POPs) are regulated under the Stockholm Convention. Since its entry into force in 2004, individual countries that ratified the convention have taken on obligations to monitor compounds such as polychlorinated dibenzo-p-dioxins, furans (PCDD/Fs) and biphenyls (PCBs), and pesticides. Hence, there is a continued interest in processing of samples containing these compounds. Laboratories around the world are interested in low cost, automated, high throughput equipment to assist them with these tasks.

Routine analysis of these compounds follows US EPA method 1613 (PCDD/Fs) and 1668 (PCBs). Traditionally sample processing has involved multi-day Soxhlet extraction and manual sample clean up using column chromatography. As an alternative to obtain faster and more reliable data, these steps have been automated.

Automated Pressurized Liquid Extraction using 50%/50% v/v dichloromethane/hexane (120oC, 1500psi, 20min) combined with automated column chromatography – using high capacity acid-base-neutral silica, alumina and carbon/celite columns – goes a long way towards completely eliminating the need for multiple day manual sample processing. With the extraction step limited to typically 1 h and the sample clean up step using versatile automated systems taking about the same amount of time, same day POPs analysis is easily achievable.

Matrices of interest have included various environmental (e.g., soil) and food applications. 13C labeled recoveries have been excellent for both PCDD/Fs and PCBs. New reduced volume programs use less than 325 mLs of solvent for the cleanup step. Different designs for both the European and North-American market (meeting different regulatory needs) have been developed.