GC-MSによる1ppbオーダーの塩化メチル水銀の同定;蒸発法によるベンゼン溶液試料濃縮

概要

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A method of final confirmation of methylmercury chloride (MMC) in waste water at the level of 1 ppb has been established by a combination of the concentration technique and the gas chromatographymass spectrometry (GC-MS). First, MMC in water sample of 500 ml was concentrated about 175 times to benzene phase of 1 ml according to a solvent extraction method developed by Nishi. Further concentration was, however, required for the present purpose, because of the still lower sensitivity of the modern GC-MS apparatus. Various concentration techniques were examined, but the following evaporation method was found to be practical for the purpose : 1 ml of the benzene sample solution was taken in a stoppered test tube of 9 mm i. d. × 8 cm tapered at the position of 6 cm from the top to 1.5 mm i. d. and evaporated at 70°C for 3 hours by blowing the tube with air from a hot air blower. This enables us to prepare a benzene solution of 20 μl containing MMC concentrated more than 5000 times and identify MMC at the level of 1 and 0.1 ppb by the mass spectrometry and the fragmentgraphy in GC-MS, respectively.
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