Development of a GC/MS method for the qualitative and quantitative analysis of mixtures of free fatty acids and metal soaps in paint samples

Analytica Chimica Acta
Jacopo La NasaIlaria Bonaduce

Abstract

In this paper we present a new analytical GC/MS method for the analysis of mixtures of free fatty acids and metal soaps in paint samples. This approach is based on the use of two different silylating agents: N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1,1,1,3,3,3-hexamethyldisilazane (HMDS). Our experimentation demonstrated that HMDS does not silylate fatty acid carboxylates, so it can be used for the selective derivatization and GC/MS quantitative analysis of free fatty acids. On the other hand BSTFA is able to silylate both free fatty acids and fatty acids carboxylates. The reaction conditions for the derivatization of carboxylates with BSTFA were thus optimized with a full factorial 32 experimental design using lead stearate and lead palmitate as model systems. The analytical method was validated following the ICH guidelines. The method allows the qualitative and quantitative analysis of fatty acid carboxylates of sodium, calcium, magnesium, aluminium, manganese, cobalt, copper, zinc, cadmium, and lead and of lead azelate. In order to exploit the performances of the new analytical method, samples collected from two reference paint layers, from a gilded 16th century marble sculpture, and from a paint tube belonging ...Continue Reading

Citations

Mar 23, 2019·Critical Reviews in Analytical Chemistry·Li-Xia LiuXue-Song Feng
Feb 28, 2020·Studies in Conservation = Études De Conservation·Christine RomanoJia-Sun Tsang
May 1, 2021·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Eliise TammekiviIvo Leito
Jul 11, 2021·Scientific Reports·Francesca NardelliIlaria Bonaduce
Sep 18, 2021·ChemistryOpen·Francesca Caterina IzzoElisabetta Zendri

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