Method of quantitatively detecting chloromethyl methyl ether and/or bis-chloromethyl ether with improved sensitivity

Claim 1

The improved method of quantitatively determining the presence of chloromethyl methyl ether or bis-chloromethyl ether in a fluid which comprises: bringing a sample of said fluid into intimate admixture, in lower alcohol medium, with an alkali metal salt of a lower alcohol and with a readily detectable organic hydroxy compound selected from 1. a compound of the formula R-OH wherein R is a halo-lower alkyl, a halophenyl, unsubstituted phenyl, an alkoxy halophenyl, an alkoxy phenyl, an alkyl halophenyl, an alkylphenyl or 2. a halothiophenol or thiophenol or 3. a halopyridinol or unsubstituted pyridinol, the molar ratio of said salt to said hydroxy compound being in the range of from about 0.2:1 to about 5:1, the total moles of said salt present in said lower alcohol medium being at least equal to the sum of the moles of chloromethyl methyl ether plus two times the moles of bis-chloromethyl ether present, and the total moles of said hydroxy compound present in said lower alcohol medium being at least equal to the sum of the moles of chloromethyl methyl ether and bis-chloromethyl ether present; adding to the admixture, (1) an aqueous medium selected from the group consisting of (a) water and (b) an aqueous solution of a salt former, and (2) an immiscible organic solvent; agitating the admixture and allowing the phases to separate; drawing off at least a portion of the solvent phase containing ether derivative; directing said solvent portion onto a suitable gas chromatographic column; eluting with inert gas the solvent portion from the column and into an electron capture detector capable of detecting the said ether derivative; and displaying the output of said detector on a readout device.