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Microplastic (MP) contamination in natural water circulation is a concern for environmental issues and human health. Various types of polymer materials have been identified and were detected in MP analytic test procedures. Beyond MP polymer type, particle size and form play a major role in water analysis due to possible negative toxicologic effects on flora and fauna. However, the correct quantitative measurement of MP size distribution over several orders of magnitude is strongly influenced by sample preparation, filtration materials and processes, and microanalytical techniques, as well as data acquisition and analysis. In this paper, a reference methodology is presented aiming at an improved quantitative analysis of MP particles. An MP analysis workflow is demonstrated including all steps from reference materials to sample preparation, filtration handling, and MP particle size distribution analysis. Background-corrected particle size distributions (1–1000 µm) have been determined for defined polyethylene (PE) and polyethylene terephthalate (PET) reference samples. Microscopically measured particle numbers and errors have been cross-checked with the total initial mass. In particular, defined reference MP samples (PE, PET) are initially characterized and applied to filtration experiments. Optical microscopy imaging on full-area Si filters with subsequent image analysis algorithms is used for statistical particle size distribution analysis. To quantify the effects of handling and filtration, several blind tests with distilled water are carried out to determine the particle background for data evaluation. Particle size distributions of PE and PET reference samples are qualitatively and quantitatively reproduced with respect to symmetry, and maximum and cut-off diameter of the distribution. It is shown that especially MP particles with a radius of >50 µm can be detected and retrieved with high reliability. For particle sizes <50 µm, a significant interference with background contamination is observed. Data from blank samples allows a correction of background contaminations. Furthermore, for enhanced sampling statistics, the recovery of the initial amount of MP will be qualitatively shown. The results are intended as an initial benchmark for MP analytics quality. This quality is based on statistical MP particle distributions and covers the complete analytic workflow starting from sample preparation to filtration and detection. Microscopic particle analysis provides an important supplement for the evaluation of established spectroscopic methods such as Fourier-transform infrared spectroscopy or Raman spectroscopy.
The elemental dissolution of Cu-Zn alloys was investigated as a function of Zn content ranging from 0 to 45 wt%. Atomic emission spectroelectrochemistry (AESEC) was utilized to directly monitor Cu2+ and Zn2+ release and oxide growth as function of time during potentiodynamic experiments. It was determined that Cu dissolution undergoes a simultaneous mechanism of Cu2O formation and Cu2+ release. The addition of Zn in Cu-Zn alloy does not measurably change the dissolution mechanism of Cu2+ and the rate of aqueous Cu2+ was only dependent on the potential. Zn dissolution was however blocked by the formation of a Cu(0) film which shifted the Zn dissolution in the anodic direction.
The elemental dissolution of Cu-Zn alloys was investigated as a function of Zn content ranging from 0 to 45 wt%. Atomic emission spectroelectrochemistry (AESEC) was utilized to directly monitor Cu2+ and Zn2+ release, oxide growth, and the enrichment of Cu metal as function of time during potentiodynamic experiments. It was determined that Cu dissolution undergoes a simultaneous mechanism of Cu2O formation and Cu2+ release. The addition of Zn in Cu-Zn alloy does not measurably change the dissolution mechanism of Cu2+ and the rate of aqueous Cu2+ was only dependent on the potential. Zn dissolution was however blocked by the formation of a Cu(0) film which shifted the Zn dissolution in the anodic direction.
Five stainless steel alloys were tested and compared to find a test method for the qualification of stainless steel used in drinking water systems. Determination of the pitting/critical potentials from the conventional cyclic polarization results was shown to be difficult when stainless steels have high Mo and Cr content. The electrochemical impedance data indicated that results received with the conventional methods do not necessarily reflect the steady state. The low frequency time constant determined from the impedance measurements showed that the anodic polarization should be conducted with very slow scan rate to get information about the mechanism. The steady state investigations were compared with the conventional electrochemical results to propose an electrochemical-based route as a standard qualification method. The qualification method was tested to be valid by a European round-robin-test.