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We have successfully applied coupled thermogravimetry, mass spectrometry, and infrared spectroscopy to the quantification of surface functional groups on single-walled carbon nanotubes. A high-purity single-walled carbon nanotube sample was subjected to a rapid functionalization reaction that attached butyric acid moieties to the nanotube sidewalls. This sample was then subjected to thermal analysis under inert desorption conditions. Resultant infrared and mass spectrometric data were easily utilized to identify the desorption of the butyric acid groups across a narrow temperature range and we were able to calculate the degree of substitution of the attached acid groups within the nanotube backbone as 1.7 carbon atoms per hundred, in very good agreement with independent analytical measurements made by inductively coupled plasma optical emission spectrometry (ICP-OES). The thermal analysis technique was also able to discern the presence of secondary functional moieties on the nanotube samples that were not accessible by ICP-OES. This work demonstrates the potential of this technique for assessing the presence of multiple and diverse functional addends on the nanotube sidewalls, beyond just the principal groups targeted by the specific functionalization reaction.
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PMID:Coupled thermogravimetry, mass spectrometry, and infrared spectroscopy for quantification of surface functionality on single-walled carbon nanotubes. 1983 81

A supramolecule, 6, based on an electron-donor zinc phthalocyanine (ZnPc) and an electron-acceptor perylene diimide (PDI) has been synthesized and characterized by elemental analysis, UV/Vis, IR, (1)H NMR and solid state (13)C CPMAS NMR and also MALDI-TOF and ICP mass spectrometry. The PDI appended ZnPc core brings about a geometrical constraint in the molecule with intriguing spectroscopic, electrochemical and photovoltaic properties. The first reduction process of 6 occurs on the PDI core while the first oxidation takes place on the Pc ring. These processes reflect a considerably small HOMO-LUMO gap of 1.50 eV, which has vital importance for optoelectronic applications. In addition, the PDI-based first and second reduction processes of 6 are accompanied by an electrochromic behaviour with colour changes from dark purple to blue and blue to turquoise, respectively. A photovoltaic cell involving 6 as the donor and [6,6]-phenyl C61 butyric acid methyl ester as the acceptor has been fabricated. The measurements of the effect of annealing temperature on its performance indicated that the annealing process gives rise to a significant increase in the open circuit voltage, the fill factor and the photoconversion efficiency.
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PMID:A conformationally stressed novel ball-type perylenediimide appended zinc(II)phthalocyanine hybrid: spectroelectrochemical, electrocolorimetric and photovoltaic properties. 2536 38

Only very limited information is available on measured environmental concentrations of nanoparticles. In this study, several environmental compartments in The Netherlands were probed for the presence of nanoparticles. Different types of water were screened for the presence of inorganic (Ag, Au, TiO2) and organic nanoparticles (C60, C70, [6,6]-phenyl-C61-butyric acid octyl ester, [6,6]-phenyl-C61-butyric acid butyl ester, [6,6]-phenyl-C61-butyric acid methyl ester, [6,6]-bis-phenyl-C61-butyric acid methyl ester, [6,6]-phenyl-C71-butyric acid methyl ester, [6,6]-thienyl-C61-butyric acid methyl ester). Air samples were analysed for the presence of nanoparticulate Mo, Ag, Ce, W, Pd, Pt, Rh, Zn, Ti, Si, B as well as Fe and Cu. ICP-MS, Orbitrap-HRMS, SEM and EDX were used for this survey. Water samples included dune and bank filtrates, surface waters and ground waters as well as influents, effluents and sludge of sewage treatment plants (STPs), and surface waters collected near airports and harbours. Air samples included both urban and rural samples. C60 was detected in air, sewage treatment plants, influents, effluents and sludge, but in no other aqueous samples despite the low detection limit of 0.1ng/L. C70 and functionalised fullerenes were not detected at all. In STP sludge and influent the occurrence of Ag and Au nanoparticles was verified by SEM/EDX and ICP-MS. In air up to about 25m% of certain metals was found in the nanosize fraction. Overall, between 1 and 6% of the total mass from metals in the air samples was found in the size fraction <100nm.
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PMID:Is there evidence for man-made nanoparticles in the Dutch environment? 2778 42