Formaldehyde Analysis by Spme on-Fiber Derivatization: A Study of the Kinetic Models of Adsorption for Divinylbenzene

Abstract

Solid-phase microextraction (SPME) via on-fiber derivatization with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine (PFBHA) and gas chromatographic determination is considered a technique of choice in many analytical fields for formaldehyde (FA) monitoring. Vapor phase adsorption models of experimentally loaded PFBHA on porous divinylbenzene (DVB) SPME were investigated at 60 °C, 35 cm s-1 of air velocity, in a 1-64 min range: with the fiber completely exposed, loaded PFBHA was about 276 µg. Among the models tested, i.e. heat transfer, pseudo-second-order (PSO), Elovich, intra-particle diffusion, extra-particle diffusion and Langmuir, PFBHA adsorption was best fit by the PSO model, showing agreement with experimental data (272 µg). The sampling rate of FA in our conditions, obtained with a permeation tube system, was in agreement with literature (17.4 and 18.3 mL min-1, respectively). Thus, an overall standardization of the sampling phase is presented, leaving the sampling time as the most crucial parameter to be set for future applications.

A New Perspective on SPME and SPME Arrow: Formaldehyde Determination by On-Sample Derivatization Coupled with Multiple and Cooling-Assisted Extractions

“…The recent applications involve coupling SPME with on-fiber derivatization [ 27 , 34 , 35 , 36 ]. In particular, several reports described the reaction of carbonyl compounds with o -(2,3,4,5,6-pentafluorobenzyl) hydroxylamine (PFBHA) and subsequent separation of PFB-oxime derivatives by GC coupled with different detectors [ 37 , 38 , 39 , 40 , 41 ], showing that the derivatives had outstanding chromatographic properties. Other derivatizing reagents are available on the market, such as 2,4-dinitrophenylhydrazine (DNPH) and 2,2,2-trifluoroethylhydrazine (TFEH).…”