For the detection of separate substances of 1-3C alkyl phenols, they are given an added internal standard, for narrow band condensation on a chiral column for gas chromatography and mass spectrometry

摘要

For the detection of separate substances of 1-3C alkyl phenols, the alkyl phenols for analysis are either in watery sample solutions or as solid matter. The sample is saturated with a salt which dissolves readily, and preferably sodium salt, using a headspace solid phase micro extraction (SPME) process together with an added acid. The acid has the same counter ions as the saturation salt matching the parameters of the detection threshold of the alkyl phenols to be analyzed. The prepared sample is contained within a glass vessel containing a gas zone equal to the sample volume, and a deuterized alkyl phenol as an internal standard for gas chromatography, closed by a syringe lid. The vessel is heated to 40-60 deg C and the temperature is maintained while an extraction fiber takes a sample from the gas volume, without immersion in the sample, for gas chromatography by adsorption. The removed fiber is placed in a split/splitless injector with total deactivation and the smallest possible liner at 200-300 deg C for complete cleaning and desorption, where the alkyl phenols and secondary matter are transferred to the liner for narrow band condensation on a chiral column of a permethyl- alpha -cyclodextrine type with helium. The alkyl phenols are separated on the chiral column by gas chromatography related to their temperature gradients for identification by mass spectrometry, to be quantified in relation to the internal standard.