PBDEs by USEPA 1614

[chhubert]

Hi, I am wondering if anyone has lab experience using USEPA 1614 method in analysing PBDEs in environmental samples. We have experienced a significant loss of higher brominated BDEs, in particular BDE209 during cleanup. Is there any tips or tricks ? Thanks

[Don Shelly]

Since this is a performance based method. Can you share your extraction and clean-up procedure?

Don

[chhubert]

Extraction is performed by shaking and cleanup is pretty much followed the 1614 multi-silica column and alumina column cleanup. We did the blank spike for cleanup part with only 30% of 209 was recovered. All operation is done either under subdue light or covered by aluminum foil to reduce 209 photo decomposition. I just do know whether silica or alumina from some brands might absorb higher beominated BDE or else.

[Don Shelly]

Extraction is performed by shaking and cleanup is pretty much followed the 1614 multi-silica column and alumina column cleanup. We did the blank spike for cleanup part with only 30% of 209 was recovered. All operation is done either under subdue light or covered by aluminum foil to reduce 209 photo decomposition. I just do know whether silica or alumina from some brands might absorb higher beominated BDE or else.

Do you think that all of that clean-up is necessary? The easiest thing would be to skip the alumina.

Don

[chhubert]

Yup, it is necessary or it would cause big problem in instrumental analysis.

[Don Shelly]

I'm a little biased since I am in the SPE business. If you extract your samples with an endcapped C08 cartridge, you will extract all of your analytes with very little else, eliminating the need for so much clean-up.

Don

[krickos]

Avoid silanol groups throughout the analysis.

Mind you, 14 years since i participated in BDE-209 work, but recall already in that time it was known that silanol groups caused loss during sample preparation, so during the chromatography work (GC-ECD for me) we used deactivated: glassware, press fit connectors and SPI liners.

If you have acess to some articles by Jonas Björklund for example (around 2004) there is a some illustrative example where you get almost a complete loss of the BDE-209 peak just by picking the wrong column (non inert).

So recommend dig into what is written about sample clean up, sorry thats all I got on the topic.

[Steve Reimer]

It has been 8 years since I ran BDEs by GC-ECD. At that time I had a splitter on my HP 6890 with Restek CLPest and CLPest2 columns. The BDE-209 had pretty good response on the CLPest column but had erratic response on the CLPest2. Sometimes it had no peak at all, which is annoying when the run is 10 minutes longer just to get that one compound out.

[Don Shelly]

Avoid silanol groups throughout the analysis.

Mind you, 14 years since i participated in BDE-209 work, but recall already in that time it was known that silanol groups caused loss during sample preparation, so during the chromatography work (GC-ECD for me) we used deactivated: glassware, press fit connectors and SPI liners.

If you have acess to some articles by Jonas Björklund for example (around 2004) there is a some illustrative example where you get almost a complete loss of the BDE-209 peak just by picking the wrong column (non inert).

So recommend dig into what is written about sample clean up, sorry thats all I got on the topic.

In other words, no bare silica.

Don