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Organisationseinheit der BAM
We report a quantification approach for directly determining total tin and tin-based pollutants/species in sediments via electrothermal vaporization/inductively coupled plasma-mass spectrometry (ETV/ICP-MS) utilizing an on-line isotope dilution mass spectrometry (IDMS) approach. The method was developed and validated using an estuarine sediment reference material (BCR-277R), yielding a recovery of 106%. A relative standard deviation (RSD) of 14%, comparable to published data using a similar method, was obtained. A limit of quantification (LOQ) was estimated at 0.008 mg Sn kg−1 and sufficient for quantifying the total tin mass fraction of surface sediments along the tidal River Elbe course. Hereby, a decrease towards the river mouth, presumably due to dilution effects by less polluted marine sediment, was observed. Besides total tin, monitoring of organotin compounds (OTCs)/species is of interest in sediments due to their toxic effects on aquatic life. The method’s capability was extended by separating an OTC fraction in a sediment certified reference material (CRM) through the ETV temperature program. While spiking experiments with OTC standards confirmed the assignment, only a small fraction of the total certified OTC amount (3%), likely due to matrix effects, was recovered. However, applying the method to real-world samples, OTCs were detectable along the River Elbe course. By this, we demonstrated the potential of our method as a complementary fast-screening approach to species-specific analysis procedures.
A new elemental analytical approach for microplastic sum parameter analysis—ETV/ICP-MS with CO2
(2025)
Microplastics (MPs) are pervasive environmental pollutants and are considered one of the main challenges of our time. However, a fast and comprehensive analytical approach for MP analysis in complex matrices traceable to SI units is still lacking. In this context, we report a fast screening tool for the sum parameter analysis of MPs using electrothermal vaporization (ETV) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). In our proof-of-concept study, we observed size-independent detection of MPs as peaks above the 13C+ signal background in the nano- to micrometer range without limitations regarding the polymer type. Quantification of the 13C+ MP signals was accomplished via an external gas calibration utilizing dynamic dilution of carbon dioxide with argon, yielding recovery rates of 80–96% for MP reference material (RM) of polymer types commonly found in the environment. The applicability to a soil sample was demonstrated through spiking experiments with a polyethylene (PE) MP RM in soil. The limit of detection (LOD) was estimated to be 0.13 µg C, equaling the detection of a single spherical low-density-PE particle of about 70 µm, and a limit of quantification (LOQ) of 0.42 µg C.
Organic fluorine sum parameters are used to detect F-containing pollutants, e.g., per- and polyfluoroalkyl substances (PFASs), in the environment, within materials, or for monitoring technical processess, e.g., thermal decomposition of PFAS during municipal waste incineration. However, established approaches determining the extractable organic and adsorbable organic fluorine content (EOC and AOC) require laborious and error-prone sample preparation. We report a solid sampling-electrothermal vaporization (ETV) method for direct fluorine measurement based on the formation of [138Ba19F]+ with an inductively coupled plasma-triple quadrupole-mass spectrometer (ICP-QQQ-MS). Method development involved the instrumental setup for Ba introduction and fluorine-specific tuning of lens and collision-reaction cell (CRC) parameters. An inorganic fluorine fraction was detected in a cyclonic dust sample from a municipal waste incineration plant as a peak above a broad background signal. The content was estimated through standard addition using a NaF solution to 2300 mgg−1. With a limit of detection (LOD) of 130 mg g−1, which was below the reported value for an electrothermal vaporization/inductively coupled plasma-mass spectrometry (ETV/ICP-MS) approach, acquiring [19F]+. The method's potential for fractionation analysis was demonstrated by analyzing polytetrafluoroethylene (PTFE) powder.
