A new proton NMR method has been developed for micro-amount determination of aqueous hexamethylenetetramine (HMT) alone, in the presence of large amounts of formaldehyde, and in urine. The method is based on the direct determination of HMT in [2H3]acetonitrile containing anisole as the internal reference standard. HMT is determined in the range 5–50 µg using a 5 mm NMR tube.
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