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Determination of N-cyclohexyl-diazeniumdioxide (HDO) containing compounds in treated wood using GC-MS

Applications |  | GL SciencesInstrumentation
GC/MSD, Thermal desorption, GC/IT
Industries
Materials Testing
Manufacturer
Thermo Fisher Scientific, GL Sciences

Summary

Significance of the Topic


The reliable analysis of organic wood preservative compounds in solid matrices is critical for environmental risk assessment and regulatory compliance under biocidal directives. Traditional extraction-based approaches are time-consuming and may introduce interferences from wood constituents. A direct thermal desorption GC-MS method provides a rapid and sensitive solution for detecting N-cyclohexyl-diazeniumdioxide in treated timber.

Objectives and Study Overview


This work aims to develop and validate a thermal desorption GC-MS procedure for identification and quantification of HDO in impregnated wood. Key objectives include optimization of desorption conditions, demonstration of method reproducibility across various formulations, and determination of practical detection limits.

Methodology and Instrumentation


Wood specimens are milled to a uniform particle size (≤3 mm) and weighed (≈15–20 mg) into thermal desorption vials. Samples are rapidly heated to 200 °C within the GC oven, releasing volatile analytes directly onto a capillary column. Separation is achieved under a controlled temperature program, and HDO is identified by characteristic retention time (~3.48 min) and mass spectral fragmentation (m/z range 35–150). Instrumentation includes an ATAS autosampler, thermal desorber unit, Finnigan GC system, and Finnigan mass spectrometer.

Main Results and Discussion


A distinct chromatographic peak corresponding to HDO was observed in both K-HDO and Cu-HDO treated samples, with mass spectra confirming expected fragment patterns. Untreated wood produced background peaks but without spectral match to HDO. Signal intensity showed a linear relationship with initial HDO concentration, supporting quantitative capability. The estimated detection limit for HDO in wood is approximately 50 ppm.

Benefits and Practical Applications


  • Minimal sample preparation without solvent extraction
  • Rapid analysis with direct thermal desorption in the GC oven
  • High selectivity and sensitivity via mass spectral confirmation
  • Suitable for routine quality control of wood preservative treatments

Future Trends and Possibilities for Application


Further research may expand this approach to diverse wood species and additional organic biocides. Calibration strategies will enhance quantitative accuracy. Adapting thermal desorption GC-MS to composite materials, coatings, and other environmental matrices could extend its utility.

Conclusion


The developed thermal desorption GC-MS method offers a fast, reliable, and direct technique for detecting HDO in treated wood with minimal interference. Its quantitative potential and low detection limits make it a valuable tool for regulatory compliance and industrial quality assurance.

References


  • Ferlazzo DE 1999 Analysis of tebuconazole in wood treated with Tanalith E Int Res Group Wood Pres Doc IRGWP9920158
  • Horn W Marutzky R 1994 Rapid pyrolytical method for determination of wood preservatives Fresenius J Anal Chem 348 832835
  • Hübschmann HJ 1996 Handbuch der GCMS Grundlagen und Anwendung VCH Verlag Weinheim
  • Karpe P Kirchner S Rouxel P 1995 Thermal desorption GCMS FID sniffer for odorous VOC determination J Chromatogr A 708 105114

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