Fast Determination of 1-Methyl-1H-1,2,4-triazole in Soils Contaminated by Rocket Fuel Using Solvent Extraction, Isotope Dilution and GC–MS
1-Methyl-1H-1,2,4-triazole (MTA) is the most stable and abundant transformation product of dimethylhydrazine-based rocket fuel. Concentrations of MTA in soils affected by rocket fuel spills are regularly monitored using a number of available methods mainly based on GC–MS. Complex, time and labor intensive sample preparation makes quantification of MTA quite costly and unsuitable for on-site measurements. The goal of this study was to develop a new method for fast determination of MTA in soil samples based on solvent extraction and GC–MS. MTA extraction effectiveness using known polar organic solvents varies from 30 to 95 % for different soils. Isotope dilution method involving (1-trideuteromethyl)-1H-1,2,4-triazole (MTA-d3) provides efficient matrix effect control and analyte recovery in the range of 70–130 % for all tested solvents—acetone, methanol and acetonitrile. Any of the tested solvents may be used for the method depending on their affordability and accessibility in the lab. Addition of 3 g of 4Å molecular sieves to acetone extracts from soils removes 98 % of water and does not affect MTA/MTA-d3 concentrations ratio. Compared to the competitive SPME-based method, the developed approach does not require long-time equilibration of soils at elevated temperatures. The developed method is more suitable for determination of concentration at a level above 300 mg kg−1. MTA concentration in soils taken from the site of accidental “Proton” rocket crash in 2013 reached 600 mg kg−1. According to the method validation, its reproducibility and accuracy are below 9 and 23 %, respectively. Detection limit is below 2 mg kg−1 for all studied samples.
KeywordsGas chromatography Mass spectrometry Solvent extraction Isotope dilution 1-Methyl-1H-1,2,4-triazole Rocket fuel
This work was conducted under the program 0002/GOPCF-15 “Development of the environmental risks assessment system and methods for minimization of negative impact of space rocket activity on the environment and human health” funded by the Ministry of Education and Science of Kazakhstan. Authors are grateful to Dr. Nurzhan Kurmankulov and Dr. Kseniya Bortnikova (Institute of Chemical Sciences, Almaty, Kazakhstan) for synthesis of 1-methyl-1H-1,2,4-triazole and (1-trideuteromethyl)-1H-1,2,4-triazole.
Compliance with Ethical Standards
Conflict of Interest
The authors declare no conflicts of interest in relation to this research.
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