<p>This study evaluates the applicability of single particle inductively coupled plasma mass spectrometry (spICP-MS) for the quantitative detection of small microplastics (MPs) through monitoring of the carbon signal in tap water. To overcome high background signal originating from dissolved inorganic carbon typically present in tap water at elevated levels, a sample pretreatment procedure was developed to remove inorganic dissolved carbon while preserving the physicochemical properties of MPs. The optimized protocol involved mild acidification with 0.05% HNO₃ followed by ultrasonication for 60&#xa0;min. This treatment effectively reduced the concentration of dissolved inorganic carbon by up to 97%, achieving background carbon levels comparable to those of ultrapure water, and enabling the detection of MPs smaller than 2 μm. The impact of the pretreatment on MPs was evaluated using polystyrene (PS) MPs in the 1&#xa0;–&#xa0;4.5&#xa0;µm size range. In addition, systematic optimization of spICP-MS instrumental parameters was conducted across four configurations differing in sample introduction system and torch injector inner diameter. Among the tested setups, the combination of a conventional concentric nebulizer and a 2.5&#xa0;mm torch injector provided the most reliable performance for detecting MPs. Under optimized conditions, the spICP-MS method was used for MPs spiked to tap water, followed by the proposed pretreatment, which showed the procedure had negligible effects on particle concentration, size distribution, morphology, and surface characteristics. This was also confirmed by field-emission scanning electron microscopy (FE-SEM). The proposed pretreatment strategy, coupled with optimized spICP-MS conditions, shows potential for the first assessment of the contamination of tap water with MPs.</p>

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Development and evaluation of a pretreatment procedure for single particle ICP-MS quantitative analysis of microplastics in inorganic-carbon-rich water samples

  • Pia Leban,
  • Aljaž Iveković,
  • Janja Vidmar

摘要

This study evaluates the applicability of single particle inductively coupled plasma mass spectrometry (spICP-MS) for the quantitative detection of small microplastics (MPs) through monitoring of the carbon signal in tap water. To overcome high background signal originating from dissolved inorganic carbon typically present in tap water at elevated levels, a sample pretreatment procedure was developed to remove inorganic dissolved carbon while preserving the physicochemical properties of MPs. The optimized protocol involved mild acidification with 0.05% HNO₃ followed by ultrasonication for 60 min. This treatment effectively reduced the concentration of dissolved inorganic carbon by up to 97%, achieving background carbon levels comparable to those of ultrapure water, and enabling the detection of MPs smaller than 2 μm. The impact of the pretreatment on MPs was evaluated using polystyrene (PS) MPs in the 1 – 4.5 µm size range. In addition, systematic optimization of spICP-MS instrumental parameters was conducted across four configurations differing in sample introduction system and torch injector inner diameter. Among the tested setups, the combination of a conventional concentric nebulizer and a 2.5 mm torch injector provided the most reliable performance for detecting MPs. Under optimized conditions, the spICP-MS method was used for MPs spiked to tap water, followed by the proposed pretreatment, which showed the procedure had negligible effects on particle concentration, size distribution, morphology, and surface characteristics. This was also confirmed by field-emission scanning electron microscopy (FE-SEM). The proposed pretreatment strategy, coupled with optimized spICP-MS conditions, shows potential for the first assessment of the contamination of tap water with MPs.