Krzysztof Jankowski

A fast and green approach for the non-chromatographic assaying of volatile metalorganic compounds (VMOCs) is presented, involving the use of thermal desorption microwave-induced plasma optical emission spectrometry for the multi-species simultaneous determination of VMOCs in wastewater plant samples after headspace solid-phase microextraction (HSSPME-TD-MIP-OES), and optimized as a tool for the assessment of ambient exposure to hazardous VMOC pollutants. With the aim of VMOC monitoring, all species are separated and quantified within 10 s in comparison with about 10–20 min required by conventional GC-based procedures. Calibration against aqueous standards was carried out for several metalorganic species. The method was successfully applied for the quantitative extraction of As, Bi, Hg, Sb, Si and Sn compounds. Limits of detection ranging from 5 to 30 ng L⁻¹ and relative standard deviations lower than 4% were obtained. The method is appropriate for high-sample-throughput measurements, and it proved to be suitable for the analysis of wastewater and sewage sludge samples.

The effects of 5.8-GHz microwave (MW) irradiation on the synthesis of mesoporous selenium nanoparticles (mSeNPs) in aqueous medium by reduction of selenite ions with ascorbic acid, using zinc nanoparticles as a hard template and cetyltrimethylammonium bromide (CTAB) as a micellar template, are examined for the first time with a particular emphasis on MW-particle interactions and the NPs morphology. This MW-assisted synthesis is compared to 2.45 GHz MW heating method and conventional hydrothermal method at around 100 °C to produce the nanoparticles of different morphology and particle size distributions. The NPs morphology is tailored by varying the temperature ramp characteristics and the MW irradiation time. Under mild synthesis conditions only spherical particles are formed. Enhancing temperature ramp rate in the presence of CTAB micelles increases the metal–semiconductor hybrid particles growth rate and promotes the formation of nanorods and branched shapes. The effect is MW frequency dependent and non-thermal to some extent. Multi-step mechanism of mSeNPs formation is proposed based on derivative UV–Vis spectrophotometry and scanning electron microscopy (SEM) data. Both the stability of the chemical composition at a single particle level and the high efficiency of zinc template removal are determined by single particle microwave plasma optical emission spectrometry (SP-MWP-OES). After Zn template removal mSeNPs can be loaded with antifungal carbamate agent, hence the application as a nanopesticide is suggested.

The ability of microwaves to heat various kinds of substances has been known for decades [1] . Today, this phenomenon is used in many technological and scientific fields, such as food processing (both in home-use microwave ovens and large industrial installations) [2] , wood drying [3] , medicine (microwave ablation treatment) [4] , and waste recycling (pyrolysis) [5] , just to name a few. Opportunities for new applications are emerging with technological advances allowing for increasingly precise manipulation of microwave signals.

Novel multi-species analyzer based on thermal desorption and digitally-controlled plasma optical emission spectrometry followed by solid-phase microextraction has been developed for determining various organometallics in sediment samples. A helium plasma source operating at 10 kHz and an integrated small-sized spectrometer with a charge-coupled device detector is installed for cost-effective atomic emission measurement and signal acquisition. Moreover, the analyzer size of a portable device is achieved, while the system is capable of absorbing large amounts of measurement data. Specifically, the analyzer has been applied for the speciation of mercury species in sediments. Method detection limits for MeHg and Hg²⁺ are 35.4 and 9.6 ng L⁻¹. Thus, sediments containing above 0.2 µg kg⁻¹ of mercury can be analyzed with precision 1–3.5% of RSD. The developed methods are validated by the analysis of estuarine sediment certified reference material ERM CC580, GBW 07405 Chinese soil. [AQ1]