Vario el analyzer

Particulate material fluxes were measured by weighing freeze-dried samples five times. The weight percentage of total carbon (% TC) in the exported material was measured with an Elementar Vario El analyzer on aliquots (15 mg) of freeze-dried sediment trap samples. A second aliquot (~ 20 mg) was acid digested (HNO₃/HF at 150°C) [43 ] before analysis by inductively coupled plasma atomic emission spectroscopy (ICP-AES). Assuming that particulate inorganic carbon (PIC) was mainly associated to calcium carbonate (CaCO₃), the measurement of calcium (% Ca) by ICP-AES allowed calculating the % of PIC (% Ca x 12/40, with 12 and 40 corresponding to molar masses of carbon (C) and calcium (Ca), respectively). The weigh percentage of POC (% POC) was then determined by subtracting % PIC from % TC. Results are expressed in mmol POC collected in each sediment trap. POC fluxes were then calculated considering the surface of the minicosms (0.36 m²) and daily fluxes were calculated considering the duration of the experiments (6 days). Using aluminum (Al) concentrations as a proxy for dust concentrations (Al = 4.12 ± 0.39% in the dust analog), the measurement of Al content (%) in the exported material by ICP-AES allowed to estimate the percentage of lithogenic particles recovered in the sediment trap and the fluxes of lithogenic particles over the course of the experiments.

Reagents were commercially available and used without further purification except otherwise stated. The monomer 4-pyC₂H₃ was distilled to remove polymerization inhibitor hydroquinone before use. ESI-MS was obtained using a Shimadzu LCMS-2010A mass spectrometer, for which samples were digested by sonication in a mixture of hydrochloric acid and MeOH after removal of the residual monomers by sublimation under vacuum. Elemental analyses (EA) were conducted using an Elementar Vario EL analyzer using guest-free samples (with a little water adsorbed from air). IR spectra were recorded on a Bruker TENSOR 27 FT-IR spectrometer in the 400–4,000 cm⁻¹ region with KBr pellets. ¹H NMR and ¹³C NMR spectra were recorded on a Bruker AVANCE III 400 MHz NMR spectrometer. Chemical shifts were quoted in p.p.m. referenced to the appropriate solvent peak or 0.0 p.p.m. for tetramethylsilicane. PXRD patterns were collected on a Bruker D8-Advance diffractometer with Cu Kα radiation and a LynxEye detector. Thermogravimetry analyses were performed on a TA Q50 system under N₂ at a heating rate of 5 °C min. N₂ sorption isotherms were measured by a Micromeritics ASAP 2020M physisorption analyzer.

All reagents were commercially available and used without further purification. 1,4-Benzenedi(1H-1,2,3-triazole (H₂bdt) was synthesized according to the method in the literature. Elemental analyses (EA) were conducted using an Elementar Vario EL analyzer. X-ray photoelectron spectroscopy (XPS) measurements were performed with a VG Scientific ESCALAB 250 instrument. Powder X-ray diffraction (PXRD) patterns were collected on a Bruker D8-Advance diffractometer with Cu Kα radiation and a LynxEye detector. Variable-temperature PXRD data were collected on a Rigaku SmartLab X-ray diffractometer (Cu-Kα, λ = 1.54056 Å). Thermogravimetric (TG) analyses were performed on a TA Q50 thermogravimetric analyzer under nitrogen gas at a heating rate of 10 °C min^–1. Scanning electron microscope (SEM) images were obtained from an ultra-high-resolution electron microscope (FE-SEM, SU8010). Gas sorption isotherms were measured on a Micromeritics ASAP 2020M instrument. Before the sorption experiments, the as-synthesized samples were first solvent exchanged with MeOH, and then activated for 12 h at 150 °C under vacuum. N₂ (99.999%) was used for all measurements. The temperature was controlled by a liquid nitrogen bath (77 K).

The chemicals used were of reagent grade. Removal of all solvents was carried out under reduced pressure. The ¹H and ¹³C NMR spectra were recorded in d6-DMSO 2% solutions on a “Bruker Avance III” (400.13 and 100.61 MHz) (Karlsruhe, Germany). Chemical shifts δ are given in ppm referring to the signal center using the solvent peaks for reference: d6-DMSO 2.50 ppm. IR spectra were recorded on a Spectrum 100 FT-IR spectrophotometer (PerkinElmer) using the universal ATR sampling accessory Agilent 5975C VL MSD (Waltham, MA, USA) with triple axis detector, performed using the method by Druta: temperature 60–320 °C, run time: 32.333 min, flow 1.1062 mL/min, pressure 9.418 psi and method steroid 250, temperature 180–250 °C, run time 29 min, flow 1.1062 mL/ min, pressure 16.528 psi. All products were analyzed by CHN elemental analysis (Elementar Vario EL analyzer) (Santa Clara, CA, USA). Melting points (uncorrected) were determined on a Boetius apparatus (Dresden, Germany). Thin-layer chromatography was carried out on Merck aluminum TLC plates, silica gel 60 coated with fluorescent indicator F254.