Suitability of the given binding agent for the moulding sands preparation depends on the one hand on the estimation of technological properties of the sand and the mould made of it and the obtained casting quality and on the other hand on the assessment of this sand influence on the natural and working environment. Out of moulding sands used in the foundry industry, sands with organic binders deserve a special attention. These binders are based on synthetic resins, which ensure obtaining the proper technological properties and sound castings, however, they negatively influence the environment. If in the initial state these resins are not very dangerous for people and for the environment, thus under an influence of high temperatures they generate very harmful products, being the result of their thermal decomposition. Depending on the kind of the applied resin (phenol-formaldehyde, urea, furfuryl, urea–furfuryl, alkyd) under an influence of a temperature such compounds as: furfuryl alcohol, formaldehyde, phenol, BTEX group (benzene, toluene, ethylbenzene, xylene), and also polycyclic aromatic hydrocarbons (PAH) can be formed and released. The aim of the study was the development of the method, selection of analytical methods and the determination of optimal conditions of formation compounds from the BTEX group. An emission of these components constitutes one of the basic criteria of the harmfulness assessment of binders applied for moulding and core sands. Investigations were carried out in the specially designed set up for the thermal decomposition of organic substances in a temperature range: 5000 C – 13000 C at the laboratory scale. The object for testing was alkyd resin applied as a binding material for moulding sands. Within investigations the minimal amount of adsorbent necessary for the adsorption of compounds released during the decomposition of the resin sample of a mass app. 15 mg was selected. Also the minimal amount of solvent needed for the desorption of compounds adsorbed in the column with adsorbent was found. The temperature range, in which the maximal amounts of benzene, toluene, ethylobenzene and xylenes are released from the resin, was defined. The qualitative and quantitative analyses of compounds from the BTEX group were performed by means of the gas chromatography combined with the mass spectrometry (GC/MS).