Goals are (1) to selectively synthesize MNFs in lieu of empty-cage fullerenes (e.g., C 60 , C 70 ) without compromising MNF yield and (2) to test our hypothesis that MNFs possess a different set of optimal formation parameters than empty-cage fullerenes. In this work, we introduce a novel approach for the selective synthesis of metallic nitride fullerenes (MNFs). This new method is "Chemically Adjusting Plasma Temperature, Energy and Reactivity" (CAPTEAR). The CAPTEAR approach with copper nitrate hydrate uses NO x vapor from NO x generating solid reagents, air and combustion to "tune" the temperature, energy and reactivity of the plasma environment. The extent of temperature, energy and reactive environment is stoichiometrically varied until optimal conditions for selective MNF synthesis are achieved. Analysis of soot extracts indicate that percentages of C 60 and Sc 3 N@C 80 are inversely related, whereas the percentages of C 70 and higher empty-cage C 2n fullerenes are largely unaffected. Hence, there may be a "competitive link" in the formation and mechanism of C 60 and Sc 3 N@C 80 . Using this CAPTEAR method, purified MNFs (96% Sc 3 N@C 80 , 12 mg) have been obtained in soot extracts without a significant penalty in milligram yield when compared to control soot extracts (4% Sc 3 N@C 80 , 13 mg Sc 3 N@C 80 ). The CAPTEAR process with Cu(NO 3 ) 2 ·2.5 H 2 O uses an exothermic nitrate moiety to suppress empty-cage fullerene formation, whereas Cu functions as a catalyst additive to offset the reactive plasma environment and boost the Sc 3 N@C 80 MNF production.

The yield of Sc3N@C80 metallofullerene and fullerene extract is dramatically increased via filling cored graphite rods with copper and Sc2O3 only; when compared to 100% Sc2O3 packed rods, improvements of factors of approximately 3 and approximately 5 have been achieved for Sc3N@C80 and fullerene extract produced, respectively, with the weight percent of Cu added to the rod affecting the type and amount of fullerene produced.

Herein, we address a need in the industrial and academic communities to reduce costs and environmental impact associated with the synthesis of select carbonaceous nanomaterials. In this effort, we have developed a method to recover Sc2O3 from carbonaceous “waste soot”, thereby alleviating the problem of waste disposal of fullerene depleted soot and tremendously reducing the costs and environmental impact of our synthetic process. The recovery process is based on the thermal oxidation and removal of carbon from waste soot as gaseous byproducts (e.g., CO2) to yield a recycled, reusable feedstock. The economic impact is measured in the cost savings of solid waste disposal fees and expensive reagents, such as scandium and some rare-earth metal oxides. Our recovery method is scalable and simple in design. Waste soot at different stages of thermal oxidation is characterized by thermogravimetric analysis (TGA) to determine optimal temperature and soak parameters. Corresponding X-ray photoelectron spectroscopy (XPS) analysis of these samples indicates a comparable chemical composition of Sc2O3 for recycled samples to virgin Sc2O3 controls. Recovered Sc2O3 material was used in our electric-arc reactor and resulted in statistically comparable fullerene product distributions.

Abstract. A mass spectrometry assay is presented here that allows for the simultaneous determination of yield and enantioselectivity in a single analysis. The assay makes use of molecules that are structurally similar to the analytes of interest as standards. The assay predicts the yields of the reactions reasonably well and with little error. For example, in the pig liver esterase catalyzed hydrolysis of one prochiral malonate, the yield predicted by the assay was 72%, while larger scale isolated reaction yields were within 5% of this value. This assay provides a fast method to determine yield and enantioselectivity in one analysis. The strengths and limitations of this method are discussed.

not Available.