Optima 2100 dv instrument

Inductively coupled plasma-optical emission spectrometry (ICP-OES) was performed on an OPTIMA 2100 DV instrument (PerkinElmer, Waltham, MA, USA). X-Ray diffraction (XRD) patterns were obtained using a Texture Analysis D8 Advance Diffractometer (Bruker, Billerica, MA, USA) with Cu Kα radiation. The TEM and HRTEM images were obtained on a 2100F microscope (JEOL, Tokyo, Japan) equipped with an EDX detector INCA x-sight (Oxford Instruments, Abingdon, UK).

Inductively coupled plasma-optical emission spectrometry (ICP-OES) was performed on an OPTIMA 2100 DV instrument (PerkinElmer, Waltham, MA, USA). X-Ray diffraction (XRD) patterns were obtained using a Texture Analysis D8 Advance Diffractometer (Bruker, Billerica, MA, USA) with Cu Kα radiation. Transmission electron microscopy (TEM) and high-resolution TEM microscopy (HRTEM) images were obtained on a 2100F microscope (JEOL, Tokyo, Japan). Scanning electron microscopy (SEM) imaging was performed on a TM-1000 microscope (Hitachi, Tokyo, Japan). To recover the biohybrids, a Biocen 22 R (Orto-Alresa, Ajalvir, Spain) refrigerated centrifuge was used. X-ray photoelectron spectroscopy (XPS) spectra were determined through a SPECS GmbH electronic spectroscopy system with a UHV system (pressure approx. 10–10 mbar), with a PHOIBOS 150 9MCD energy analyzer, monochromatic X-ray sources. The analysis of the same was carried out using the CasaXPS program.

In each site, 23 trace elements (Al, As, Ba, Bi, Cd, Cr, Co, Cu, Fe, Ga, Hg, In, Li, Mn, Mo, Ni, Pb, Se, Sr, Ti, Tl, V, and Zn) were detected in the whole bodies of macrobenthic invertebrates [35 (link)] by inductively coupled plasma-optic emission spectrometry (ICP-OES) using a Perkin Elmer Optima 2100 DV instrument (PerkinElmer, Inc., Shelton, CT, USA), coupled with a CETAC U5000AT+ ultrasound nebulizer (Cetac Technologies, Inc., Omaha, NE, USA) for mercury. All these elements can affect organisms; thus, it is important to assess their bioavailability in freshwater [30 (link)]. We analyzed the whole-body concentrations (gut contents included), since analysis of tissue concentrations alone does not allow for the detection of trace elements in sites with very low metal concentrations [51 (link)].
All samples were homogenized and microwave-digested using a Milestone ETHOS ONE oven using 4-mL nitric acid and 1-mL hydrogen peroxide. All reagents were from Merck, Darmstadt (Germany); acids were of Suprapur grade [52 (link)]. Analytical results are reported as ug g⁻¹ wet weight (w.w.). Quality assurance tests performed during analysis included the recovery rate and blank and certified material analyses; all quality results were within acceptable ranges. Table S1 presents the limit of detection (LOD), the reference material values, and the percentages of recovery.