Development of a Headspace-Solid Phase Micro Extraction Method for the Analysis of Volatile and Semi-Volatile Organic Compounds from Polyurethane Resins for Leather Finishing

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Antonia Flores
Silvia Sorolla
Concepció Casas
Rosa Cuadros
Anna Bacardit


Volatile organic compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) arise from the chemicals used in the various stages of the leather manufacturing process. An important aim of the tanning industry is to minimize or eliminate VOCs and SVOCs, without lowering the quality of leather.  

This paper shows the development of a new headspace-solid phase micro extraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS) method for the identification of VOCs and SVOCs emitted by newly designed polymers for the leather finishing operation. These new polymers are polyurethane resins designed to reduce the VOC and SVOC concentration. This method enables a simple and fast determination of the qualitative and semi-quantitative content of VOCs and SVOCs in polyurethane-type finishing resins. The chemicals that are of concern in this paper are the following: Dipropylene glycol Monomethyl Ether (DPGME), DBE-3 (a mixture of dibasic esters) and Triethylamine (TEA). The test conditions that have been determined to carry out the HS-SPME assay are the following: incubation time (2 hours), extraction temperature and time (40°C; 5 minutes) and the desorption conditions (280°C, 50 seconds). 

Ten samples of laboratory scale resins were tested by HS-SPME followed by gas chromatography (GC-MS). DPGME and DBE-3 (a mixture of dimethyl adipate, dimethyl glutarate and dimethyl succinate) have been identified effectively. The compounds are identified by a quantitative method using external calibration curves for the target compounds. The technique is not effective to determine the TEA compound, since the chromatograms shown poor resolution peaks for the standard. 

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