DOCSLIB.ORG

A Rapid Procedure for the Determination of C60 and C70 Fullerenes in Soil and Sediments by Ultrasound-Assisted Extraction and HPLC-UV

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
A Rapid Procedure for the Determination of C60 and C70 Fullerenes in Soil and Sediments by Ultrasound-Assisted Extraction and HPLC-UV ANALYTICAL SCIENCES MAY 2013, VOL. 29 533 2013 © The Japan Society for Analytical Chemistry A Rapid Procedure for the Determination of C60 and C70 Fullerenes in Soil and Sediments by Ultrasound-assisted Extraction and HPLC-UV Rosa Ana PÉREZ, Beatriz ALBERO, Esther MIGUEL, José Luis TADEO, and Consuelo SÁNCHEZ-BRUNETE† Departamento de Medio Ambiente, INIA, Ctra de la Coruña, 7, 28040 Madrid, Spain In this work, a rapid and sensitive method, based on ultrasound-assisted extraction of samples with a small volume of toluene, has been developed for the quantification of C60 and C70 fullerenes in soil and sediments. Good extraction efficiencies were obtained at all of the fortification levels studied (200, 100, 20 and 2 ng/g), which ranged from 72 to 104%. An important effect of the extraction temperature was observed on C60 recoveries, and an acceptable decrease in the recovery rates was observed in aged samples. In the case of wet samples, the extraction can be done by percolating a small volume of acetonitrile before extraction. The extraction yields of the developed method for the extraction of C60 and C70 from soil were compared with those obtained by pressurized liquid extraction. Finally, analyses of fullerenes in agricultural and industrial soils and sediments were carried out, but no fullerene residues were found. (Received October 15, 2012; Accepted March 6, 2013; Published May 10, 2013) synthesis and application of fullerene materials, but quantitative Introduction information describing the occurrence, behavior, and transport of fullerenes is still lacking. As a result of the ongoing advances in nanotechnology and the Soxhlet extraction and ultrasonic assisted extraction (UAE) increasing use and production of engineered nanoparticles are the procedures most commonly used to extract fullerenes (ENPs) for different purposes, the release of substantial amounts from environmental samples;3,6,9 although for solid samples, of ENPs into the environment is growing, and it is expected to extraction methods such as shaking10 and pressurized liquid increase considerably in the future. Fullerenes are carbonaceous extraction (PLE)3,11 have been reported, too. In general, the nanoparticles made entirely of carbon that may contain methods described above used large amounts of organic solvent pentagonal and hexagonal rings, being C60 (an icosahedral in the extractive process. structure) the most common form and C70, with an oblong Although fullerenes show a poor solubility in most organic form, the next stable fullerene.1,2 Fullerenes have been detected solvents, some aromatic solvents and carbon disulfide, among at very low concentrations in geological materials and in a wide others, are commonly used.12–14 Nowadays, toluene is the most range of extraterrestrial materials;3 therefore, the natural widely used solvent for the solution and extraction of fullerenes, presence of fullerenes has been related to materials affected by and was employed in the extraction methods reported above. high-energy events.4 The use of these compounds in a great Most analytical methods use liquid chromatography (HPLC), variety of commercial products and in many biomedical and combined with ultraviolet-visible detection (UV) or mass industrial applications is expected to be due to their optical and spectrometry (MS) for the detection of fullerenes in geological, electrochemical features, as well as to other properties, such as, environmental or biological samples.4,7 In order to achieve high their high strength and radical scavenging capability.5 As a selectivity and sensitivity in the quantitative analysis of result of the growing industrial applications and increasing fullerenes in environmental samples, HPLC-MS and tandem household usage of fullerenes, there is rising interest regarding MS have been recently applied in the determination of fullerenes their presence, behavior and effects in the environment.1,2,4–7 in water and suspended material of wastewater effluents,15 in rat Although C60 is the main fullerene studied as an emerging tissues and blood16 or in aerosol samples.6 contaminant,8 Sanchís et al.6 found that C70 was the most Although the separation of C60 and C70 can be carried out frequently detected fullerene in airborne particulate matter from with various stationary phases,12 most of the studies available in the Mediterranean Sea. In general for ENPs, and particularly the literature were performed by the separation of these for fullerenes, it is necessary to develop or improve the compounds using C18 columns, or columns that had specifically methodology for their detection and quantification in different designed ligands for fullerene separation.16–19 Despite their good environmental matrices. Thus, in a critical review, Isaacson separation properties and capacity to retain fullerenes with a et al.4 pointed out that many reports had been published on the 100% toluene mobile phase, the main drawback of these specifically designed columns is their high price in comparison † To whom correspondence should be addressed. to a C18 column. Thus, an increase in the use of a C18 column E-mail: [email protected] for fullerenes analysis has been observed.6,11,20,21 534 ANALYTICAL SCIENCES MAY 2013, VOL. 29 The extraction of fullerenes from solid environmental matrices, temperature until spiked. The characteristics of the soil were: such as soil or sediments, has been scarcely reported due to their pH 7.7, moisture content 1%, total organic matter content complexity. Shareef et al.11 reported an analytical method for 0.97%, sand 44.34%, silt 37.44% and clay 18.22%. Surface soil the determination of C60 in soil using PLE followed by from agricultural fields (horticultural and forested) located in HPLC-UV. The main drawbacks of this method were that only different Spanish regions and industrial soils from the area of one fullerene was evaluated, and the relatively high limit of Bilbao, an important industrial region, were sampled, air dried, detection (LOD) achieved (20 μg/kg). In a recent publication, sieved and stored frozen (–18°C) in glass containers until their Wang et al.5 used an artificial sediment to develop an analytical evaluation. method to quantify C60 using HPLC-UV, where the extraction Sediments were obtained from different rivers of Madrid was carried out by shaking using a high solvent volume (40 mL), (Manzanares, Jarama, Henares, Guadarrama and Lozoya). and a high limit of quantification (LOQ) was reported for C60 Sediments were collected into glass containers, previously (0.15 mg/kg) with this methodology. To the best of our rinsed several times with acetone, and stored refrigerated during knowledge, these are the only methods reported for the transport to the laboratory. Before analysis, sediments were determination of fullerenes (C60 only) in soil and sediments. dried at room temperature, sieved and kept frozen at –18°C. In this context, the main objective of our study was to develop a fast and sensitive method for the analysis of C60 and C70 in Extraction procedures soil and sediments by UAE, using a low volume of extraction UAE method. Sieved soil or sediment (5 g ± 0.001) were solvent and without the need of sophisticated extraction weighed into a 10 mL weighing funnel and placed in a glass instrumentation. The effects of the extraction temperature and column (20 mL), 10 cm × 20 mm i.d. (Normax, Portugal), with time, soil moisture and the residence time of residues in soil on a polyethylene frit of 2 cm diameter and 20 μm pore size the recoveries of both compounds by UAE were studied. For (Supelco, Madrid, Spain) at the end. Luer tips of the columns comparative purposes, PLE was applied for the extraction of were closed with 1-way stopcocks. For recovery studies, soil C60 and C70 from soil samples, and both methods were samples were previously spiked with a mixture of fullerenes to compared. Finally, the UAE method was applied to the analysis reach final concentrations of 200, 100, 20 and 2 ng/g, whereas of C60 and C70 fullerenes in soil and sediment samples sediment samples were spiked with fullerenes at 20 and 2 ng/g. collected in different areas of Spain. As far as we know, this is Then, they were covered with aluminum foil and left in dark the first reported method for the simultaneous determinations of conditions at room temperature for 24 h to allow solvent C60 and C70 in soil and sediment by a fast and miniaturized evaporation. The samples were protected from light during the extraction method. whole extraction procedure. Extractions were carried out with an ultrasonic water bath (Raypa, Barcelona, Spain) at room temperature, where water level was adjusted to equal the Experimental extraction solvent level inside the columns. Samples were extracted with 4 mL of toluene in an ultrasonic water bath Reagents and chemicals (15 min). Then the columns were placed on a multiport vacuum Toluene and propan-2-ol, HPLC grade, were purchased from manifold (Supelco, Visiprep, Madrid, Spain) where the solvent Lab Scan, Analytical Science (Poland). Acetonitrile (ACN) was collected in 10 mL graduated tubes. Another 4 mL of gradient 240 nm/far UV, HPLC grade and n-hexane, residue toluene were added to the samples that were sonicated again for analysis grade, were obtained from Scharlab (Barcelona, Spain). 15 min. The solvent was filtered and samples were washed with Fat-free quartz sand was supplied by Buchi AG (Switzerland). 1.5 mL of additional solvent. The combined extracts were LabortechnikFullerene-C60 (99.5%) and [5,6]-fullerene-C70 concentrated to 1 mL using an evaporator Genevac EZ-2 (99%) were supplied by Sigma-Aldrich (Steinheim, Germany). (purchased from NET Interlab, S.A.L., Spain) and 1 mL of ACN Separate stock solutions of individual compounds were made up was added to the tube to obtain a final extract in toluene:ACN at 500 μg/mL in toluene. A working standard mixture containing (50:50, v/v).
Load more

Recommended publications
  • Calorimetric Studies of Solvates of C60 and C70 with Aromatic Solvents
    J. Phys. Chem. B 1999, 103, 1339-1346 1339 Calorimetric Studies of Solvates of C60 and C70 with Aromatic Solvents Mikhail V. Korobov, Andrej L. Mirakyan, and Natalia V. Avramenko Department of Chemistry, Moscow State UniVersity, 119899 Moscow, Russia Gerd Olofsson* Thermochemistry DiVision, Center for Chemistry and Chemical Engineering, Lund UniVersity, S-22100 Lund, Sweden Allan L. Smith* Chemistry Department, Drexel UniVersity, Philadelphia, PennsylVania 19104 Rodney S. Ruoff Physics Department, Washington UniVersity, St. Louis, Missouri 63130 ReceiVed: July 24, 1998; In Final Form: December 18, 1998 To improve the understanding of the solution properties of C60 and C70 in aromatic solvents, binary systems of C60 and C70 with benzene, toluene, 1,2- and 1,3-dimethylbenzene, 1,2,4- and 1,3,5-trimethylbenzene, bromobenzene, and 1,2- and 1,3-dichlorobenzene were studied using differential scanning calorimetry, solution calorimetry, and thermogravimetry. Solid solvates with different compositions were identified in many of the systems. The solvates were characterized by composition and by the temperature and the enthalpy of the incongruent melting transition. Enthalpies of solution of C60 in toluene, 1,2-dimethylbenzene, 1,2- and 1,3- dichlorobenzene, and 1,2,4-trimethylbenzene and of C70 in 1,2-dimethylbenzene and in 1,2- and 1,3- dichlorobenzene were determined. The formation-incongruent melting of solid solvates causes maxima in the temperature-solubility curves of fullerenes in aromatic solvents. Trends in solubility behavior of fullerenes were discussed in terms of thermodynamics of solution and solvate formation. Introduction solvate (II), or more probably, pure C60. Phase equilibrium conditions relate the mole fraction of C60, x(C60), to T (tem- The unusual temperature dependence of solubility of fullerenes perature) for both low- and high-temperature parts of the (ln x)- 1 in a number of solvents has attracted attention and provoked T curve.
    [Show full text]
  • Polymer Solar Cells Based on Poly(3-Hexylthiophene) and Fullerene: Pyrene Acceptor Systems
    Polymer solar cells based on poly(3-hexylthiophene) and fullerene: Pyrene acceptor systems a a a a, * Alessandra Cominetti , Andrea Pellegrino , Luca Longo , Riccardo Po , Alessandra a a a b, 1 Tacca , Chiara Carbonera , Mario Salvalaggio , Michele Baldrighi , Stefano Valdo b Meille a Research Center for Renewable Energies and Environment, Istituto Donegani, Eni S.p.A, Via Fauser 4, IT-28100 Novara, Italy b Dipartimento di Chimica, Materiali e Ingegneria Chimica “G. Natta”, Politecnico di Milano, via Mancinelli 7, IT-20131 Milano, Italy Received 12 May 2014 Received in revised form 30 January 2015 Accepted 27 March 2015 Available online 4 April 2015 1. Introduction The literature on novel materials for polymer solar cells [1e3] deals mainly with the development of the donor components of the active layer [4e9], while much fewer papers are devoted to novel acceptors [10,11]. [6,6]-phenyl-C61-butyric acid methyl ester * Corresponding author. E-mail address: [email protected] (R. Po). 1 Present address: Istituto Italiano di Tecnologia (IIT), via Morego 30, IT-16163 Genova, Italy. (PCBM) is the oldest [12], the most used [13] and, to date, still one filtered, and the solvent was distilled under reduced pressure. 1.03 g of the most effective acceptors for bulk heterojunction polymer (yield 84%) of a pale yellow oil were obtained, which became a solar cells. The popularity of PCBM, aside from its unique electronic white solid after 24 h of storage at þ4 C in a refrigerator. ¼ 1 0 properties, is mainly due to its good solubility in many organic Tm 37.4 C (DSC).
    [Show full text]
  • Decontamination of Surfaces Exposed to Carbon-Based Nanotubes and Nanomaterials
    Hindawi Publishing Corporation Journal of Nanomaterials Volume 2014, Article ID 249603, 9 pages http://dx.doi.org/10.1155/2014/249603 Research Article Decontamination of Surfaces Exposed to Carbon-Based Nanotubes and Nanomaterials Paul Su,1 Babak Haghpanah,2 William W. Doerr,1 Zahra Karimi,2 Syed Hassan,2 Louis Gritzo,1 Ahmed A. Busnaina,2 and Ashkan Vaziri2 1 FMGlobal,Norwood,MA02062,USA 2 DepartmentofMechanicalandIndustrialEngineering,NortheasternUniversity,Boston,MA02115,USA Correspondence should be addressed to Paul Su; [email protected] Received 10 October 2013; Accepted 12 December 2013; Published 16 January 2014 Academic Editor: Aiying Wang Copyright © 2014 Paul Su et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Contamination of surfaces by nanomaterials can happen due to accidental spillage and release or gradual accumulation during processing or handling. Considering the increasingly wide use of nanomaterials in industry and research labs and also taking into account the diversity of physical and chemical properties of different nanomaterials (such as solubility, aggregation/agglomeration, and surface reactivity), there is a pressing need to define reliable nanomaterial-specific decontamination guidelines. In this paper, we propose and investigate a potential method for surface decontamination of carbon-based nanomaterials using solvent cleaning and wipes. The results show that the removal efficiency for single- and multiwalled carbon nanotubes from silicon wafers sprayed with water-surfactant solutions prior to mechanical wiping is greater than 90% and 95%, respectively. The need for further studies to understand the mechanisms of nanomaterial removal from surfaces and development of standard techniques for surface decontamination of nanomaterials is highlighted.
    [Show full text]
  • Ep 2 098 549 A1
    (19) & (11) EP 2 098 549 A1 (12) EUROPEAN PATENT APPLICATION published in accordance with Art. 153(4) EPC (43) Date of publication: (51) Int Cl.: 09.09.2009 Bulletin 2009/37 C08G 61/00 (2006.01) C01B 31/02 (2006.01) C09D 201/02 (2006.01) H01L 51/30 (2006.01) (2006.01) (21) Application number: 07860265.3 H01L 51/42 (22) Date of filing: 26.12.2007 (86) International application number: PCT/JP2007/075036 (87) International publication number: WO 2008/081845 (10.07.2008 Gazette 2008/28) (84) Designated Contracting States: (72) Inventors: AT BE BG CH CY CZ DE DK EE ES FI FR GB GR • TANAKA, Katsutomo HU IE IS IT LI LT LU LV MC MT NL PL PT RO SE Kitakyusyu-shi SI SK TR Fukuoka 806-0004 (JP) • TAKAGI, Masatoshi (30) Priority: 27.12.2006 JP 2006351751 Yokohama-shi Kanagawa 227-8502 (JP) (71) Applicants: • Frontier Carbon Corporation (74) Representative: Vossius & Partner Fukuoka 806-0004 (JP) Siebertstraße 4 • Mitsubishi Chemical Corporation 81675 München (DE) Tokyo 108-0014 (JP) (54) FULLERENE FILM USING FULLERENE DERIVATIVE AS RAW MATERIAL, FULLERENE POLYMER AND THEIR PRODUCTION METHODS (57) A fullerene film and a fullerene polymer both produced from a fullerene derivative are provided which can be easily formed by a wet process and can retain the intact properties inherent in the fullerene. Also provided are processes for producing the film and polymer. A solution of a fullerene derivative decomposing at a temperature lower than the pyrolysis temperature of the fullerene, e.g., the fullerene derivative represented by the following formula, is applied to a substrate.
    [Show full text]
  • Dispersion of Fullerenes in Natural Water and Their
    DISPERSION OF FULLERENES IN NATURAL WATER AND THEIR BEHAVIOR IN WATER TREATMENT PROCESS A Thesis Presented to The Academic Faculty by Hoon Hyung In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the School of Civil and Environmental Engineering Georgia Institute of Technology August 2008 DISPERSION OF FULLERENES IN NATURAL WATER AND THEIR BEHAVIOR IN WATER TREATMENT PROCESS Approved by: Dr. Jae-Hong Kim, Advisor Dr. Seung Soon, Jang School of Civil and Environmental School of Material Science and Engineering Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Joseph B. Hughes Dr. Vernon L. Snoeyink School of Civil and Environmental School of Civil and Environmental Engineering Engineering Georgia Institute of Technology University of Illinois Dr. Michael H. Bergin School of Civil and Environmental Engineering Georgia Institute of Technology Date Approved: June 11, 2008 [To Se-Eun and Juhee] ACKNOWLEDGEMENTS Firstly, I would like to thank my advisor, Dr. Jae-Hong Kim. He not only provided me a chance to become a piece of this great legacy of Georgia Tech., but also showed me the example of a great advisor with extensive knowledge, creative mind, and friendliness. I acknowledge my thesis committee, Dr. Joseph Hughes, Dr. Vernon Snoeyink, Dr. Michael Bergin, and Dr. Seung Soon Jang for agreeing to be my committee and providing invaluable comments and advices on my research. All the members of Dr. Kim and Dr. Huang’s groups and Korean graduate students in the environmental engineering program are greatly appreciated. It was very nice to share friendship with them in and out of the campus and discussions and advices from them brought me valuable idea on my research.
    [Show full text]
  • Sponge-Like Molecular Cage for Purification of Fullerenes
    ARTICLE Received 24 May 2014 | Accepted 13 Oct 2014 | Published 26 Nov 2014 DOI: 10.1038/ncomms6557 Sponge-like molecular cage for purification of fullerenes Cristina Garcı´a-Simo´n1, Marc Garcia-Borra`s1, Laura Go´mez1,2, Teodor Parella3,Sı´lvia Osuna1, Jordi Juanhuix4, Inhar Imaz5, Daniel Maspoch5,6, Miquel Costas1 & Xavi Ribas1 Since fullerenes are available in macroscopic quantities from fullerene soot, large efforts have been geared toward designing efficient strategies to obtain highly pure fullerenes, which can be subsequently applied in multiple research fields. Here we present a supramolecular nanocage synthesized by metal-directed self-assembly, which encapsulates fullerenes of different sizes. Direct experimental evidence is provided for the 1:1 encapsulation of C60, C70,C76,C78 and C84, and solid state structures for the host–guest adducts with C60 and C70 have been obtained using X-ray synchrotron radiation. Furthermore, we design a washing- based strategy to exclusively extract pure C60 from a solid sample of cage charged with a mixture of fullerenes. These results showcase an attractive methodology to selectively extract C60 from fullerene mixtures, providing a platform to design tuned cages for selective extraction of higher fullerenes. The solid-phase fullerene encapsulation and liberation represent a twist in host–guest chemistry for molecular nanocage structures. 1 Institut de Quı´mica Computacional i Cata`lisi and Departament de Quı´mica, Universitat de Girona, Campus Montilivi, Girona, Catalonia 17071, Spain. 2 Serveis Te`cnics de Recerca (STR), Universitat de Girona, Parc Cinetı´fic i Tecnolo`gic, Girona, Catalonia 17003, Spain. 3 Servei de RMN and Departament de Quı´mica, Facultat de Cie`ncies, Universitat Auto`noma de Barcelona (UAB), Campus UAB, Bellaterra, Catalonia 08193, Spain.
    [Show full text]
  • Extraction of Fullerenes in Organic Solvents and the Development of Superior Isolation Procedures
    Indian Journal of Chemistry Vol 31 MD, May 1992, pp. F32-F35 Extraction of fullerenes in organic solvents and the development of superior isolation procedures R Dhamodaran, I Kaliappam, N Sivaraman, T G Srinivasan, P R Vasudeva Rao & C K Mathews" Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102, Tamil Nadu, India Received 20 February 1992 Development of methods for the isolation of fullerenes depends to a great extent on the identifica- tion of suitable solvents. In the present work, extraction of fuUerenes from carbon soot by a number of aliphatic, alicyclic and aromatic solvents has been examined at a constant temperature of 60°C. The results indicate that the extraction power of aliphatic straight chain hydrocarbons increases with in- crease in carbon chain length. The aromatic solvents have superior extracting power as compared to the aliphatic solvents. The higher extraction power of the aromatic solvents is attributed to their better solubilising action. Based on the experimental data, it was possible to develop efficient procedures for the chromatographic separation of C60 and C70 employing cyclohexane and a normal paraffin hydro- carbon mixture with average carbon number of 12 as solvents. C60 and C70 could both be isolated completely in pure form in much smaller volumes of eluant than in the hexane system. The recent isolation of macroquannnes of C60 makes this separation procedure tedious, and and C70 bas led to a veritable explosion in scien- large volumes of solutions have to be handled. tific literature on the properties of these all-car- Further, the use of toluene means that for recycl- bon clusters called fullerenes.
    [Show full text]
  • Solvatochromism, Aggregation and Photochemical Properties of Fullerenes, C60 and C70, in Solution
    Journal of Photoscience (2003), Vol. 10(1), pp. 105−119 Solvatochromism, Aggregation and Photochemical Properties of Fullerenes, C60 and C70, in Solution Sukhendu Nath, Haridas Pal, Avinash. V. Sapre* and Jai. P. Mittal Chemistry Group, Bhabha Atomic Research Centre, Trombay, Mumbai 400085, India Fullerenes, C60 and C70, display interesting physicochemical properties in solutions, especially due to their unique chemical structures and their good electron accepting abilities. Solubility of fullerenes in different organic solvents and their unusual solvatochromic behavior, the ability of the fullerenes to form aggregates in solutions, and their electron transfer and charge transfer interactions with variety of electron donors, are the subjects of extensive research activities for more than one decade. Many research groups including ours have contributed substantially in the understanding of the solvatochromism, aggregation behavior, and the photoinduced electron transfer and charge transfer chemistry of fullerenes, in condensed phase. Present article is aimed to summarize the important results reported on the above aspects of fullerenes, subsequent to the earlier report from our group (D.K. Palit and J.P. Mittal, Full. Sci. & Tech. 3, 1995, 643-659). key words: Fullerene, Solvatochromism, Aggregation, Electron Transfer, Charge Transfer, Exciplex, CT Complex INTRODUCTION exotic three-dimensional structure of fullerenes with spherical hollow cage is responsible for their extraordinary behavior in Since the separation of the fullerenes, C60 and C70, in solution. Their ability to act as electron relays and to generate macroscopic quantities from the soots [1], extensive studies long lived excited states has made them an important class of have been carried out on the scientific and technological photochemically active compounds.
    [Show full text]
  • Thermally Metastable Fullerenes
    THERMALLY METASTABLE FULLERENES IN FLAMES BY TAPESH KUMAR YADAV Subnutted to the Department of Cherical Engineering in partial fulfillment of the requirements for the degree of DOCTOR OF PHELOSOPHY at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY May 1994 1994 Massachusetts Institute of Technology All rights reserved Signature of Author j;/ I,- -, I I - IV - , I-4)eMl --------t of Chemical- Engineering March 10, 1994 Certified by Jack B. Howard I---- Thesis Supervisor Accepted by !;dence RobertETohen "" Department Committee for Graduate Students JUN 6 994 Thermally Metastable Fullerenes in Flames by Tapesh Yadav Submitted to the Department of Chemical Engineering on March 10, 1994 in partial fulfillment of the requirements for the Degree of Philosophy in Chemical Engineering. ABSTRACT Fullerenes are closed caged molecules of pure carbon. These carbon molecules are produced in abundant quantities by certain sooting processes. In particular, fullerenes are observed in large quantities in the soot produced by low pressure (100 Torr), inert environment, vaporization of pure carbon and in the soot produced by low pressure 40 Torr) laminar combustion of premixed benzene/oxygen/inert vapors. Along with the observation of large quantities of fullerenes, many more observations can be made from the soot of the two processes. One particularly significant observation is the presence of many thermally metastable fullerenes in the soot produced by flames. This thesis focuses on an experimental and modeling study of one of the many thermally metastable fullerenes. Specifically, this thesis establishes the true identity of one of the thermally metastable ftillerene produced in flames; the thesis investigates where in the flame the thermally metastable fullerene forms; the thesis reports thermochernical.
    [Show full text]
  • SOLUBILITY of FULLERENES C6o and C7 0 in WATER, D
    LPS XXVII 543 SOLUBILITY OF FULLERENES C6o AND C7 0 IN WATER, D. Heymann, Department of Geology and Geophysics, Rice University, Houston, TX 7725 7. e-mail: [email protected]. Fullerenes C60 and C70, the all-carbon molecules with closed-cage structures, have been found naturally in soot-rich clays and marls at the Cretaceous-Tertiary boundary [I].All were marine sediments which were permeated by water even after the consolidated rocks had become uplifted above sea level. Because of this, one would like to know the solubilities of C60 and C70 in water in order to evaluate how much of the fullerenes might have been leached from the sediments since their formation about 65 My ago. A direct measurement yielded essentially zero solubility. The solubilities of -C60 and C70 at 25 OC in seven normal alcohols obey the relationship InY = a + bX + cxZ, where Y is molefraction and X is the Hildebrand solubility parameter of the solvent. Extrapolation to the solubility parameter of water gave solubilities for C60 and C70 of 1.3~10-I and 1.3x10-~~ng/ml respectively with an uncertainty of one order of magnitude. Approximately 1 mg of C60 or C70 and about 5 ml of the alcohols were placed in screw-capped bottles. The bottles were stored for one month at 24.5 ? 0.5 OC, but were gently agitated twice every day which resulted in full equilibration. Also, 50 ml of water and fullerenes were stirred continuously in stoppered erlenmeyers for one month. Following filtration through 0.2 pm PTFE filters, the water was evaporated from the flask which was then rinsed repeatedly with a few ml HPLC toluene.
    [Show full text]
  • (12) Patent Application Publication (10) Pub. No.: US 2005/0136079 A1 Burangulov Et Al
    US 2005O136079A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2005/0136079 A1 Burangulov et al. (43) Pub. Date: Jun. 23, 2005 (54) COSMETIC COMPOSITIONS CONTAINING Related U.S. Application Data FULLERENE CLUSTERS (60) Provisional application No. 60/475,203, filed on May (76) Inventors: Nail Burangulov, St. Petersburg (RU); 30, 2003. Alexander P. Moravsky, Tucson, AZ (US); Yuiya V. Kulikova, St. Publication Classification Petersburg (RU); George I. Dyachuk, St. Petersburg (RU); Raouf O. Loutfy, (51) Int. Cl." .......................... A61K 7/021; A61K 33/44 Tucson, AZ (US) (52) U.S. Cl. ............................. 424/401; 424/125; 424/63 Correspondence Address: SCULLY SCOTT MURPHY & PRESSER, PC (57) ABSTRACT 400 GARDEN CITY PLAZA SUTE 300 The present invention is directed to a cosmetic composition comprising effective amounts of fullerene clusters in asso GARDEN CITY, NY 11530 (US) ciation with cosmetically acceptable carrier to prevent or (21) Appl. No.: 10/858,361 retard free radical oxidation processes in the skin and to the method of using Said composition for reducing damage to (22) Filed: Jun. 1, 2004 healthy Skin or mucous membranes by free radicals. Patent Application Publication Jun. 23, 2005 Sheet 1 of 2 US 2005/0136079 A1 FIGURE 1 Patent Application Publication Jun. 23, 2005 Sheet 2 of 2 US 2005/0136079 A1 Product Raw Material FIGURE 2 US 2005/O136079 A1 Jun. 23, 2005 COSMETIC COMPOSITIONS CONTAINING pure Co and Co fullerenes, higher order-fullerenes, their FULLERENE CLUSTERS mixtures, crystalline Solvates of fullerenes with aromatic molecules, fullerenes adsorbed on graphite, etc. CROSS REFERENCE TO RELATED 0007. The high strength of the fullerene molecular crys APPLICATIONS tals results in their drastically different chemical and bio 0001.
    [Show full text]
  • Probing the Solubility of Selected Nanoscale Building Blocks
    PROBING THE SOLUBILITY OF SELECTED NANOSCALE BUILDING BLOCKS USING MOLECULAR SIMULATION By Patrick Scott Redmill Dissertation Submitted to the Faculty of the Graduate School of Vanderbilt University in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOPSOPHY in Chemical Engineering December, 2008 Nashville, TN Approved: Peter T. Cummings Clare McCabe Scott Guelcher Eugene LeBoeuf M. Douglas LeVan To Mom and Dad SUPPORT LOCAL COLLEGE RADIO WRVU 91.1 FM ii ACKNOWLEDGEMENTS This work has been possible through the financial support of the National Science Foundation. Additionally, the simulations in this work were done using the computational resources at NERSC and ACCRE. I am grateful for the support, guidance, and patience I have received during my research from my advisors, Professor Peter T. Cummings and Clare McCabe. I would also like to thank the members of my Dissertation Committee for their time, valuable insights, and unique observations that they contributed to this work. Vanderbilt University, as a whole, deserves great thanks as well. I am very grateful for the exposure to some of the best educators in world that Vanderbilt provided. I truly consider Vanderbilt my academic home. I would like to thank Dr. Alberto Striolo, who was absolutely instrumental in initiating me to this work. Shannon Capps is also due special thanks for all of her hard work (i.e. things I didn’t want to do and passed off on a poor undergrad) while a student in the McCabe lab. Finally, I would like to thank my lab mates, in particular, Christina Payne, Peter Dyer, and Hugh Docherty.
    [Show full text]