How can I test for 4-Methylcyclohexane methanol?

On January 9th, approximately 5000 gallons of 4-Methylcyclohexane methanol (MCHM) seeped from a storage tank into the Elk River in southern West Virginia.  Eventually, the MCHM  (CAS #34885-03-5) made its way into the water supply prompting Governor Tomblin and President Obama to issue a state of emergency for the affected counties.  The story can be followed at The Charleston Gazette or WSAZ TV. 

 MCHM

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Since the spill, our tech service team has been receiving inquires about how to analyze MCHM along with the availability of MCHM reference standards.  Unfortunately, Restek does not have this as a reference standard, and there is no standard method, From what I understand, there are a handful of laboratories conducting analysis for the State of West Virginia.

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Until, Restek can conduct some experimental lab work on our end, below are two recommendations for anyone conducting method development:

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One might follow EPA Method 8260B with a purge & trap attached to a GC/MS.  Since MCHM is an alcohol, it will likely have a low purge efficiency similar to other alcohols listed in the method.  A heated purge cycle will be required to obtain the best purge efficiency.  A good starting point might be 45°C.  As for the analytical column, A Rtx-VMS with dimensions of 30 m x 0.25 mm x 1.40 µm would be a good choice.  One could set up their instrument much like Restek’s application for volatile organics on an Rtx-VMS. 

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Another option would be to use a charcoal SPE cartridge to trap the MCHM.  After conditioning the cartridge, a solvent such as dichloromethane could be used to elute the MCHM.  EPA 522 could be referred to as guidance for the extraction procedure.  The dichloromethane extract could then be analyzed by GC/MS.  If one has the capability of large volume injections (LVI), detection limits could potentially be lowered.       

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No matter what method one might develop, I would highly recommend matrix spike and laboratory control spikes using MCHM as a good laboratory practice.   

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I hope this recommendation helps provide some guidance.  For an update on testing, see Chris Rattray’s more recent post.

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