scholarly journals Analiza mikrośladów trinadtlenku triacetonu (TATP) w fazie gazowej z zastosowaniem TD-GC/MS

2021 ◽  
Vol 13 (24) ◽  
pp. 250-276
Author(s):  
Rafał Jurczak

W artykule opisano metodykę wykrywania trinadtleneku triacetonu (TATP) w postaci par oraz śladów powierzchniowych z wykorzystaniem chromatografi gazowej sprzężonej ze spektrometrią mas wyposażoną w system do termodesorpcji (TD-GC/MS). Rozwiązania techniczne aparatury analitycznej umożliwiają wybór jednej z dwóch metod wprowadzenia par analitu w celu identyfikacji – pośrednio ze złoża TENAX TA lub bezpośrednio z obiektów badań. Dodatkowo zastosowanie elementu GERSTEL CIS odgrywającego rolę koncentratora substancji powoduje, że jest możliwa identyfikacja już nawet nanośladowych ilości TATP. W artykule przedstawiono schemat działania termodesorpcji w TD-GC/MS z jednoczesnym zwróceniem uwagi na cechy fizyczne substancji warunkujące osiągnięcie zadowalających wyników. Micro-traces analysis of triacetone triperoxide (TATP) in the form of vapours using TD-GC/MS The article discusses the method of detecting triacetone triperoxide (TATP) in the form of vapours and surface traces using gas chromatography with a thermal desorption system of mass spectrometry (TD-GC/MS). The technical solutions of analytical equipment make it possible to choose one or two methods for introducing analyte vapour for identification – indirectly from the TENAX TA deposit or directly from the research objects. In addition, the use of the GERSTEL CIS element as a substance concentrator renders identification of even nano-trace amounts of TATP possible. The article presents the experimental procedure of the thermal desorption TD-GC/MS and simultaneously draws attention to physical properties of the substance determining the achievement of satisfactory results.

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 683 ◽  
Author(s):  
Yukihiro Ouchi ◽  
Hiroyuki Yanagisawa ◽  
Shigehiko Fujimaki

This study describes a methodology for evaluating regulatory levels of phthalate contamination. By collecting experimental data on short-term phthalate migration using thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS), the migration of di(2-ethylhexyl) phthalate (DEHP) from polyvinyl chloride (PVC) to polyethylene (PE) was found to be expressed by the Fickian approximation model, which was originally proposed for solid (PVC)/liquid (solvent) migration of phthalates. Consequently, good data correlation was obtained using the Fickian approximation model with a diffusion coefficient of 4.2 × 10−12 cm2/s for solid (PVC)/ solid (PE) migration of DEHP at 25 °C. Results showed that temporary contact with plasticized polymers under a normal, foreseeable condition may not pose an immediate risk of being contaminated by phthalates at regulatory levels. However, as phthalates are small organic molecules designed to be dispersed in a variety of polymers as plasticizers at a high compounding ratio, the risk of migration-related contamination can be high in comparison with other additives, especially under high temperatures. With these considerations in mind, the methodology for examining regulatory levels of phthalate contamination using TD–GC–MS has been successfully demonstrated from the viewpoint of its applicability to solid (PVC)/solid (PE) migration of phthalates.


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