Detail publikace

Overcoming the BSTFA: Study on Trimethylsilylation Derivatization Procedures for Chemical Weapons Convention-Related Alcohols in Field Analysis

ROZSYPAL, T. ZITOVÁ, K. MRAVCOVÁ, L.

Originální název

Typ

článek v časopise ve Web of Science, Jimp

Jazyk

angličtina

Originální abstrakt

After the use of chemical weapons, there is a gradual spontaneous decomposition of chemical warfare agents (CWAs), and only degradation products can be present at the time of sample collection. Depending on the type of parent compound, these are most often acids, alcohols, or thiols. This article deals with the development and optimization of methods for the trimethylsilylation of controlled alcohols that outperforms the currently widely used method with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) prior to gas chromatographic identification. Thiodiglycol (TDG) was chosen as a model alcohol for the development and optimization of methods. Nine trimethylsilylating agents were tested as derivatization agents. For each reagent, the method was optimized in terms of reaction medium (seven tested solvents), reaction time, and temperature. The temporal stability of the resulting derivatives and the effect of the addition of the reaction catalyst were also monitored. Subsequently, optimal methods were applied in the derivatization of N-ethyldiethanolamine, N-methyldiethanolamine, triethanolamine, 2-diisopropylaminoethanol (DIAE), and 3-quinuclidinol. The developed methods were compared in all monitored properties with the standard BSTFA-method (in acetonitrile for 30 min at 60 °C). From the developed methods, three were selected that showed similar or better sensitivity parameters than BSTFA, and at the same time were less demanding to perform. Trimethylsilylation via trimethylsilyl cyanide (TMSCN) appears to be the most successful method. In conclusion, the selected methods were applied in the analysis of contaminated environmental and urban samples – sand, acrylic paint, asphalt-aluminum paint, and concrete. The samples were measured on both a benchtop and a field gas chromatograph.

Klíčová slova

chemical warfare, chemical weapons, silylation

Autoři

ROZSYPAL, T.; ZITOVÁ, K.; MRAVCOVÁ, L.

Vydáno

16. 8. 2023

Nakladatel

Taylor and Francis online

ISSN

0003-2719

Periodikum

ANALYTICAL LETTERS

Ročník

august

Číslo

2023

Stát

Spojené státy americké

Strany od

Strany do

Strany počet

URL

https://www.tandfonline.com/doi/full/10.1080/00032719.2023.2281587?scroll=top&needAccess=true

BibTex

@article{BUT185532,
  author="Tomáš {Rozsypal} and Kristýna {Zitová} and Ludmila {Mravcová}",
  title="Overcoming the BSTFA: Study on Trimethylsilylation Derivatization Procedures for Chemical Weapons Convention-Related Alcohols in Field Analysis",
  journal="ANALYTICAL LETTERS",
  year="2023",
  volume="august",
  number="2023",
  pages="17",
  doi="10.1080/00032719.2023.2281587",
  issn="0003-2719",
  url="https://www.tandfonline.com/doi/full/10.1080/00032719.2023.2281587?scroll=top&needAccess=true"
}