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Bellefonte, PA, United States

Zhao Z.,Harbin Institute of Technology | Zhao Z.,Nanjing Southeast University | Zhao Z.,Pennsylvania State University | Cannon F.S.,Pennsylvania State University | And 3 more authors.
Carbon | Year: 2016

Sustainable biomaterial binders were developed from lignin and collagen to replace the conventional petroleum pitch and coal tar pitch binders that have been used when making specialty graphites and graphite electrodes. The team prepared lab-scale graphite electrodes by first creating green composites, by hot-pressing together the lignin, collagen, petroleum coke, and other additives, followed by carbonization and graphitization. Response Surface Methodology (RSM) experimental design was employed, based on Box-Behnken Design (BBD). This was employed to optimize the recipes and processing protocols for the green composite hot-pressing of 3.5 cm diameter × 19 cm long cylinder specimens. Relative to density, the apparent optimum conditions occurred with 13.0% lignin, 3.6% collagen, 27.4% petroleum coke fines, and the balance of petroleum coke particles plus some additives. The green hot-pressing protocol employed 30 MPa pressure at 400 °C for 2 h. Baking peaked at 800 °C, ramped up and down over 13 days. This baked product hosted an apparent density of 1.67 g/mL, and exhibited 6.2% puffing. Another baked product hosted 1.56 g/mL and 1.67% puffing. After the baked product was graphitized, we achieved an apparent density of 1.51 g/mL and resistance of 25–30 μΩm. These results approached the specifications for specialty graphites. © 2016 Elsevier Ltd

Ustinov E.A.,RAS Ioffe Physical - Technical Institute | Kukushkina J.,RAS Ioffe Physical - Technical Institute | Betz W.R.,Supelco Inc.
Langmuir | Year: 2011

A series of graphitized carbon blacks have been studied using argon and nitrogen adsorption at their boiling points. Analysis of adsorption isotherms was performed with nonlocal density functional theory (NLDFT) accounting for the Axilrod-Teller equation to describe the effect of nonadditivity of the gas-solid interaction. In our previous study [Ustinov, E. A. J. Chem. Phys. 2010, 132, 194703] we have shown that the nonadditivity effect decreases the attractive component of Ar-Ar interaction in the first molecular layer adjacent to the graphite surface by about 23%. This is a source of a large error (up to 40%) when a standard NLDFT is applied to fitting the low-temperature Ar adsorption isotherm on a graphitized carbon black. A new approach that incorporates the Axilrod-Teller equation into the standard NLDFT diminishes the relative error from 40 to 4%, which suggests that the nonadditivity correction should not be ignored in most adsorption systems including crystalline and amorphous solids. The present study is an extension of our approach to N 2 adsorption isotherms at 77.3 K on graphitized carbon blacks. We show that the approach allows to reliably determine the gas-solid molecular parameters, the gas-solid nonadditivity coefficient, the Henry coefficient, and the specific surface area. The surface areas of different carbon blacks determined with the N 2 at 77.35 K and Ar at 87.29 K are very close to each other, though in the former case the values proved to be slightly smaller presumably due to nonspherical shape of the nitrogen molecule. A comparison with the Brunauer, Emmett, and Teller method is provided. © 2010 American Chemical Society.

Vuckovic D.,University of Waterloo | de Lannoy I.,NoAb Biodiscoveries Inc. | Gien B.,NoAb Biodiscoveries Inc. | Yang Y.,NoAb Biodiscoveries Inc. | And 4 more authors.
Journal of Chromatography A | Year: 2011

The use of solid-phase microextraction (SPME) for in vivo sampling of drugs and metabolites in the bloodstream of freely moving animals eliminates the need for blood withdrawal in order to generate pharmacokinetics (PK) profiles in support of pharmaceutical drug discovery studies. In this study, SPME was applied for in vivo sampling in mice for the first time and enables the use of a single animal to construct the entire PK profile. In vivo SPME sampling procedure used commercial prototype single-use in vivo SPME probes with a biocompatible extractive coating and a polyurethane sampling interface designed to facilitate repeated sampling from the same animal. Pre-equilibrium in vivo SPME sampling, kinetic on-fibre standardization calibration and liquid chromatography-tandem mass spectrometry analysis (LC-MS/MS) were used to determine unbound and total circulating concentrations of carbamazepine (CBZ) and its active metabolite carbamazepine-10,11-epoxide (CBZEP) in mice (n= 7) after 2 mg/kg intravenous dosing. The method was linear in the range of 1-2000 ng/mL CBZ in whole blood with acceptable accuracy (93-97%) and precision (<17% RSD). The single dose PK results obtained using in vivo SPME sampling compare well to results obtained by serial automated blood sampling as well as by the more conventional method of terminal blood collection from multiple animals/time point. In vivo SPME offers the advantages of serial and repeated sampling from the same animal, speed, improved sample clean-up, decreased animal use and the ability to obtain both free and total drug concentrations from the same experiment. © 2010 Elsevier B.V.

Souza-Silva E.A.,University of Waterloo | Gionfriddo E.,University of Waterloo | Shirey R.,Supelco Inc. | Sidisky L.,Supelco Inc. | Pawliszyn J.,University of Waterloo
Analytica Chimica Acta | Year: 2016

The main quest for the implementation of direct SPME to complex matrices has been the development of matrix compatible coatings that provide sufficient sensitivity towards the target analytes. In this context, we present here a thorough evaluation of PDMS-overcoated fibers suitable for simultaneous extraction of different polarities analytes, while maintaining adequate matrix compatibility. For this, eleven analytes were selected, from various application classes (pesticides, industrial chemicals and pharmaceuticals) and with a wide range of log P values (ranging from 1.43 to 6). The model matrix chosen was commercial Concord grape juice, which is rich in pigments such as anthocyanins, and contains approximately 20% of sugar (w/w). Two types of PDMS, as well as other intrinsic factors associated with the PDMS-overcoated fiber fabrication are studied. The evaluation showed that the PDMS-overcoated fibers considerably slowed down the coating fouling process during direct immersion in complex matrices of high sugar content. Longevity differences could be seen between the two types of PDMS tested, with a proprietary Sylgard® giving superior performance because of lesser amount of reactive groups and enhanced hydrophobicity. Conversely, the thickness of the outer layer did not seem to have a significant effect on the fiber lifetime. We also demonstrate that the uniformity of the overcoated PDMS layer is paramount to the achievement of reliable data and extended fiber lifetime. Employing the optimum overcoated fiber, limits of detection (LOD) in the range of 0.2-1.3 ng/g could be achieved. Additional improvement is attainable by introducing washing of the coatings after desorption, so that any carbon build-up (fouling) left on the coating surface after thermal desorption can be removed. © 2016 Elsevier B.V.

Mirnaghi F.S.,University of Waterloo | Chen Y.,Supelco Inc. | Sidisky L.M.,Supelco Inc. | Pawliszyn J.,University of Waterloo
Analytical Chemistry | Year: 2011

Biocompatible C18-polyacrylonitrile (PAN) coating was used as the extraction phase for an automated 96-blade solid phase microextraction (SPME) system with thin-film geometry. Three different methods of coating preparation (dipping, brush painting, and spraying) were evaluated; the spraying method was optimum in terms of its stability and reusability. The high-throughput sample preparation was achieved by using a robotic autosampler that enabled simultaneous preparation of 96 samples in 96-well-plate format. The increased volume of the extraction phase of the C18-PAN thin film coating resulted in significant enhancement in the extraction recovery when compared with that of the C18-PAN rod fibers. Various factors, such as reusability, reproducibility, pH stability, and reliability of the coating were evaluated. The results showed that the C18-PAN 96-blade SPME coating presented good extraction recovery, long-term reusability, good reproducibility, and biocompatibility. The limits of detection and quantitation were in the ranges of 0.1-0.3 and 0.5-1 ng/mL for all four analytes. © 2011 American Chemical Society.

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