The elemental composition of the samples was analyzed by inductively coupled plasma (ICP) mass spectrometry for the determination of the metal contents and by combustion analysis (CHNS) for the sulfur content. For the ICP analysis the samples were dissolved in aqua regia in closed Ni-capsules to avoid extrusion of volatile Sn species. The capsules were heated in a microwave (CEM) at 180°C for 35 min. The ICP analysis was carried out using an ICP-OES spectrometer (Vista Pro) equipped with an axial plasma source, an Echelle-polychromator and a CCD detector (Agilent Technologies). For the analysis, the following emission lines were used: Cu 327.395 nm, Sn 283.998 nm and Zn: 206.200 nm. The analysis of the sulfur content was carried out using a Vario Micro Cube analyser (Elementar).
Vario micro cube analyser
Manufactured by Elementar
The Vario Micro Cube analyser is a compact and high-precision instrument designed for elemental analysis. It performs rapid and accurate determinations of carbon, hydrogen, nitrogen, and sulfur in a wide range of solid and liquid samples.
Automatically generated - may contain errors
3 protocols using vario micro cube analyser
1
Elemental Composition Analysis of Samples
2
Elemental Analyses of Carbon, Hydrogen, Nitrogen, and Sulfur
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Elemental analyses of carbon, hydrogen and nitrogen were performed with a Vario Micro Cube analyser (Elementar). For the sulfur analysis, the samples were combusted catalytically in a helium/oxygen atmosphere on a WO3/Al2O3 contact at approximately 1373 K. The sulfur from the sample was converted to a mixture of sulfur dioxide and sulfur trioxide. The sulfur trioxide was reduced in the mixture to sulfur dioxide on a copper catalyst at approximately 1123 K, and the sulfur dioxide was finally quantified with an IR detector for samples L001, L002 and L003 or a thermal conductivity detector for samples L004, L005 and L006.
3
Characterization of Compound Samples
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Reagents and solvents were obtained from Sigma-Aldrich, Alfa Aesar, Acros Organics, Fisher Scientic, Fluorochem or Manchester Organics, and were used without additional purication. Samples used for elemental analysis, thermogravimetric analysis and laboratory powder X-ray diffraction were ground into a powder using a mortar and pestle immediately prior to analysis, to ensure consistency of solvent content in the bulk material. For solution-phase NMR spectroscopic characterisation, the sample (ca. 3 mg) was acid-digested in 50 mL deuterium chloride (35% in D 2 O) in 1 mL DMSO-d 6 . Thermogravimetric analysis was performed in air using a PerkinElmer Pyris1 Thermogravimetric Analyser. Elemental analysis was performed by combustion in pure oxygen using a Perki-nElmer 2400 CHNS/O Series II Analyser or an Elementar Vario MICRO cube analyser. NMR spectroscopy (400 MHz) was performed using Bruker AVANCE III 400 HD or AVANCE 400 HD spectrometers.
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