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May 22nd, 2013, 1:44pm
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Oil and Grease (Read 373 times)
moeagle
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Oil and Grease
May 10th, 2012, 2:05pm
 
Our lab purchased a Xenosep Oil and Grease kit to test our wastewater effluent. The problem is my results are inflated and my blanks are even around 35 mg/l. I have isolated the interfence to the sodium sulfate column because there is always a white powderly substance left in the aluminum pan after drying. The manufacturer is not very cooperative, so I'm appealing for assistance. EPA says 0.45 micron filter paper should be used to prevent leakage, but there's no room for paper in the system. Is there a proper pretreatment procedure for preparing the sulfate columns?
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David S.
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Re: Oil and Grease
Reply #1 - May 10th, 2012, 3:43pm
 
What is sounds like is that you are getting too much water through your filter. If you overload the capacity of the sodium sulfate, some of the salt will dissolve into your extract and pull it through to the evaporation stage. You will notice your extract is very cloudy when this happens. There are a few things you can do to solve this problem. The first is to leave vacuum on your SPE filters for a longer period of time. You need to make sure you have pulled as much residual moisture out of the filters as possible. Be sure you have adequate vacuum for the number of samples you are extracting and leave the vacuum on the samples for 10-15 minutes or so after all the free liquid has pulled through. Then once you have added the hexane for extraction, if possible try to slow down the rate that the solvent is going through the sodium sulfate column. I don't know exactly how the Xenosep system is set up, but if there is a stopcock or valve of some sort, just open it partway so that the sodium sulfate has a chance to absorb the moisture instead of being absorbed by it. Also, you want to make sure the sodium sulfate is kept as dry as possible. Don't leave the bag open to the air, especially if you are in a humid environment.
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Re: Oil and Grease
Reply #2 - May 11th, 2012, 7:53am
 
Thanks David, I'll give it a try!
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Re: Oil and Grease
Reply #3 - May 11th, 2012, 9:33am
 
I agree with everything David says here.  I looked up what the Xenosep device looks like and one thing I would definitely keep an eye on would be your vacuum when pulling the solvent through the sodium sulfate cartridge.  If you pull too much of a vacuum your hexane will go through the cartridge too quickly leading to water and/or sodium sulfate getting through.  That is definitely a critical step in any extraction device so start there.
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