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The in-situ graphitization of an as-made, large pore silica mesostructure templated by nonionic Pluronic 123 surfactant micelles provides a low cost pathway to the nanocasting of linear carbon nanotubes.
Palladium-bacteriopheophorbide (WST09), a novel bacteriochlorophyll derivative, is currently being investigated for use as a photodynamic therapy (PDT) drug due to its strong absorption in the near-infrared region and its ability to efficiently generate singlet oxygen when irradiated. In this study, we determined the pharmacokinetics and tissue distribution of WST09 in female EMT6 tumour-bearing Balb/c mice in order to determine if selective accumulation of this drug occurs in tumour tissue. A total of 41 mice were administered WST09 by bolus injection into the tail vein at a dose level of 5.0 +/- 0.8 mg kg(-1). Three to six mice were sacrificed at each of 0.08, 0.25, 0.5, 1.0, 3.0, 6.0, 9.0, 12, 24, 48, 72, and 96 h post injection, and an additional three control mice were sacrificed without having been administered WST09. Terminal blood samples as well as liver, skin, muscle, kidney and tumour samples were obtained from each mouse and analyzed for palladium content (from WST09) using graphite furnace atomic absorption spectroscopy (GFAAS). The representative concentration of WST09 in the plasma and tissues was then calculated. Biphasic kinetics were observed in the plasma, kidney, and liver with clearance from each of these tissues being relatively rapid. Skin, muscle and tumour did not show any significant accumulation at all time points investigated. No selective drug accumulation was seen in the tumour and normal tissues, relative to plasma. Thus the results of this study indicate that vascular targeting resulting from WST09 in the circulation, as opposed to selective WST09 accumulation in tumour tissues, may be responsible for PDT effects in tumours that have been observed in other WST09 studies.
A novel method for the manufacturing of microchips for on-chip combinations of electrochemistry (EC) and sheathless electrospray ionisation mass spectrometry (ESI-MS) is described. The technique, which does not require access to clean-room facilities, is based on the incorporation of an array of gold microcoil electrodes into a poly(dimethylsiloxane)(PDMS) microflow channel equipped with an integrated graphite based sheathless ESI emitter. Electrochemical measurements, which were employed to determine the electroactive area of the electrodes and to test the microchips, show that the manufacturing process was reproducible and that the important interelectrode distance in the electrochemical cell could to be adequately controlled. The EC-ESI-MS device was evaluated based on the ESI-MS detection of the oxidation products of dopamine. The results demonstrate that the present on-chip approach enables full potentiostatic control of the electrochemical cell and the attainment of very short transfer times between the electrochemical cell and the electrospray emitter. The transfer times were 0.6 and 1.2 s for flow rates of 1.0 and 0.5 microL min(-1), respectively, while the electrochemical conversion efficiency of the electrochemical cell was found to be 30% at a flow rate of 0.5 microL min(-1). To decouple the electrochemical cell from the ESI-MS high voltage and to increase the user-friendliness, the on-line electrochemistry-ESI-MS experiments were performed using a wireless Bluetooth battery-powered instrument with the chip floating at the potential induced by the ESI high voltage. The described on-chip EC-ESI-MS device can be used for fundamental electrochemical investigations as well as for applications based on the use of electrochemically controlled sample pretreatment, preconcentration and ionisation steps prior to ESI-MS.
Carbon nanotubes (CNTs) are promising materials for use in amperometric biosensors. The defect sites at their ends, and on their sidewalls, are considered to be edge plane-like defects and show high electrocatalytic activity toward several biological molecules. However, electrocatalytic activity toward H(2)O(2) has not been compared among bamboo-structured CNTs (BCNTs), which have many defect sites; hollow-structured CNTs (HCNTs), which have few defect sites; edge plane pyrolytic graphite (EPG); and traditional glassy carbon (GC). The advantages of using CNTs in electrodes for biosensors are still equivocal. To confirm the utility of CNTs, we analyzed the electrochemical performance of these four carbon electrodes. The slope of the calibration curve for H(2)O(2) at potentials of both +0.6 V and -0.1 V obtained with a BCNT paste electrode (BCNTPE) was more than 10 times greater than the slopes obtained with an HCNT paste electrode and a GC electrode, reflecting the BCNT's larger number of defect sites. Although the slope with the EPG electrode (EPGE) was about 40 times greater than that with BCNTPE at +0.6 V, the slopes with these two carbon electrodes were nearly equivalent at -0.1 V. EPGE demonstrated excessive electrochemical activity, detecting currents on the basis of consumption of oxygen and oxidation of ascorbic acid, even at -0.1 V. In contrast, BCNTPE could dominantly detect a cathodic current for H(2)O(2) at -0.1 V, even when interfering molecules were added. BCNTPE possesses appropriate electrochemical activity and is an effective electrode materials for developing interference-free oxidase-based biosensors operated by the application of an appropriate potential.
The self-organization of multicomponent tetrarosette assemblies into ordered nanostructures on graphite surfaces has been studied by atomic force microscopy (AFM). Real-space information on the level of individual molecules allowed us to analyze the underlying structure in unprecedented detail. In highly ordered nanorod domains, tetrarosettes 1(3) x (DEB)(12) arrange in the form of parallel rows with a spacing of 4.6 +/- 0.1 nm. High resolution AFM revealed the internal packing of the tetrarosette assemblies in these rows, which can be described by an oblique lattice with a = 2.5 +/- 0.3 nm, b = 5.0 +/- 0.1 nm, and gamma = 122 +/- 3 degrees. The results, together with recent improvements in synthetic approaches, contribute to the development of a general strategy to develop H-bonding-based nanostructures with molecular precision.
A method for the determination of the basic penicillins, amoxicillin and ampicillin, in animal tissue is described. The method used aqueous extraction with tungstate to remove proteins followed by cation exchange solid phase extraction (SPE) clean-up. This extract was further purified using porous graphitic carbon (PGC) SPE. Extracted residues were derivatized with acetic anhydride followed by triazole/mercuric chloride prior to reversed phase HPLC with UV determination at 325 nm. At the Maximum Residue Limit of 50 micrograms/kg in fortified cattle muscle validation gave mean recoveries for amoxicillin of 57% and 50% on two different days with relative standard deviations of 19% and 15% respectively. For ampicillin the recoveries were 72% and 59% with relative standard deviations of 15% and 19% respectively.
The voltammetric oxidation of adenosine-3',5'-cyclic monophosphate (3',5'-CAMP) has been studied in the pH range 2.13-10.07 using pyrolytic graphite electrode (PGE). Voltammetric, coulometric, spectral studies, and product characterization indicate that the oxidation of 3',5'-CAMP occurs in an EC reaction involving a 6H+, 6e process at pH 7.24. Electrooxidized products were seperated by semipreparative high performance liquid chromatography (HPLC) and were characterized by mp, 1HNMR, FTIR, and GC-mass as allantoin cyclic ribose monophosphate and 3 dimers as the major products. A detailed interpretation of the redox mechanism of 3',5'-CAMP also has been presented to account for the formation of various products.
The physical and chemical properties of the particulate fraction of carbon-graphite/epoxy advanced composite material (cgeACM) smoke were measured to address concerns regarding potential health hazards posed by the release of fibers during pyrolysis of this material. Filter, low-pressure cascade impactor, and electrostatic precipitator samples were collected from cgeACM smoke in which the aerosol concentration ranged from 0.20 to 5.39 g/m3. Fibers were found in the smoke among individual, spherical, or nearly spherical particles and chain aggregates. The fibers had a mean count diameter of 0.54 micron and an average length of 2.84 microns. However, fibers accounted for approximately 0.3% of the particles counted. The smoke aerosols (including fibers) had mass median aerodynamic diameters (MMAD) ranging from 1.4 to 1.9 microns with standard geometric deviations ranging from 1.6 to 1.8, and hence more than 88% of the particles were in the thoracic size range (MMAD < or = 4.0 microns). All particles were composed primarily of carbon, silicon, sulfur, and oxygen with traces of other metals. By comparison fibers were composed almost exclusively of silicon.
The characteristics of thermoluminescent dosemeters prepared from graphite mixed with sintered MgB4O7:Dy are presented for beta ray dosimetry. These dosemeters are attractive for beta ray dosimetry since the material combines low transparency with near tissue equivalence and high sensitivity, thus enabling skin dose to be assessed from low energy beta emitters in accordance with the ICRP recommendations. Results from practical field experiments are also presented.
To derive the absorbed dose to water from a standard of absorbed dose to graphite, the metrology laboratories which apply such a method usually make use of cavity ionization chambers as transfer instruments. In addition, the BNM-LPRI has tested, as such instruments, two types of Fricke dosimeter in its cobalt-60 beam. The two procedures are compared and their results are found to be in good agreement (the difference is less than 0.1%). Both procedures are then taken into account for the calculation of the reference value of absorbed dose to water.
The basic equation for establishing a 60Co air-kerma standard based on a cavity ionization chamber includes a wall correction term that corrects for the attenuation and scatter of photons in the chamber wall. For over a decade, the validity of the wall correction terms determined by extrapolation methods (K(w)K(cep)) has been strongly challenged by Monte Carlo (MC) calculation methods (K(wall)). Using the linear extrapolation method with experimental data, K(w)K(cep) was determined in this study for three different styles of primary-standard-grade graphite ionization chamber: cylindrical, spherical and plane-parallel. For measurements taken with the same 60Co source, the air-kerma rates for these three chambers, determined using extrapolated K(w)K(cep) values, differed by up to 2%. The MC code 'EGSnrc' was used to calculate the values of K(wall) for these three chambers. Use of the calculated K(wall) values gave air-kerma rates that agreed within 0.3%. The accuracy of this code was affirmed by its reliability in modelling the complex structure of the response curve obtained by rotation of the non-rotationally symmetric plane-parallel chamber. These results demonstrate that the linear extrapolation technique leads to errors in the determination of air-kerma.
The realization of the unit of absorbed dose at LNE-LNHB is based on calorimetry with the present GR8 graphite calorimeter. For this reason the calorimetric technique must be maintained, developed and improved in the laboratory. The usual quasi-adiabatic operating mode at LNHB is based on the thermal feedback between the core (sensitive element) and the jacket (adjacent body). When a core-jacket temperature difference is detected, a commercially available analogue PID (Proportional, Integral, Derivative) controller sends to the jacket an amount of electrical power to reduce this difference. Nevertheless, the core and jacket temperatures increase with irradiations and electrical calibrations whereas the surrounding is maintained at a fixed temperature to shield against the room temperature variations. At radiotherapy dose rates, fewer than ten measurements, or electrical calibrations, per day can be performed. This paper describes the new constant-temperature operating mode which has been implemented recently to improve flexibility in use and, to some extent, accuracy. The core and the jacket temperatures are maintained at fixed temperatures. A steady state is achieved without irradiation. Then, under irradiation, the electrical power needed to maintain the assigned temperature in the core is reduced by the amount of heat generated by ionizing radiation. The difference between these electrical powers, without and with irradiation, gives the mean absorbed dose rate to the core. The quality of this electrical power substitution measurement is strongly dependent upon the quality of the core and jacket thermal control. The core temperature is maintained at the set value using a digital PID regulator developed at the laboratory with LabView software on PC for this purpose. This regulator is versatile and particularly well suited for calorimetry purposes. Measurements in a cobalt-60 beam have shown no significant difference (<0.09%) between the two operating modes, with an equivalent reproducibility (1sigma < 0.06%). These results corroborate the negligible difference of heat transfer between steady and irradiation periods when working in quasi-adiabatic mode with thermal feedback between the core and the jacket. The new constant-temperature mode allows numerous and fully automated measurements. The electrical calibration is an integral part of the measurement; no extra runs are needed. It also allows faster thermal equilibrium before starting runs. Moreover the quality of vacuum within the gaps between the bodies is less important.
A simple and rapid determination of tin in biological materials (blood, brain, liver, kidney, etc,) by atomic absorption spectrometry (AAS) with a graphite furnace is described. Suppression of interferences by direct addition of ascorbic acid in wet-ashed biological materials was investigated for the determination of tin. This method involves no extraction with organic solvent for removal of the interferences, and therefore it is neither time consuming nor error prone, and is suitable for large sample sizes and small sample volumes. The limit of detection of this method is 0.002 microgram/mL, equivalent to a limit of detection in the materials of 0.02 microgram/g. The calibration graph is linear up to 1 microgram/mL of tin.
A simple method of deproteinizing whole blood with an 0.8M (5%, v/v) nitric acid solution containing Triton X-100 (0.1%, v/v) is described. The resulting supernatant is used for the measurement of lead by Zeeman graphite furnace atomic absorption spectrometry using calibration with aqueous standards. Recoveries ranged from 97.7-105.6% when an aqueous lead solution was added to a deproteinized sample supernatant and from 98.5-104.5% when whole blood control material was added to a whole blood sample. At a blood lead concentration of 11.2 micrograms/dL, the within- and between-run coefficients of variation were both approximately 5%. Comparison of the proposed method versus one using a recommended matrix modifier gave a regression equation of Y(proposed) = 0.99x(matrix modifier)-0.36, with a correlation coefficient of r = 0.994 (n = 54).
A revised procedure for processing a capillary blood sample collected on filter paper (FP) for analysis by graphite furnace atomic absorption spectrometry (GFAAS) is described. A 1/4-in. diameter disk of the dried FP sample was used, and a correlation of 0.975 with a false-positive rate of 0.8% and a false-negative rate of 1.7% was found when the results from the FP sample and its corresponding venous sample were compared. Several analytical variables were investigated, and the following was found: blood samples with hematocrit values of 30-39% did not show any significant differences between the paired FP and venous lead results; filter paper blank values were < 2 micrograms/dl with the use of aqueous standards without correction and 0.1 microgram/dl with paper blank correction; and during the collection of 163 samples from 6 different urban sites over a period of 1 year, no environmental lead contamination was encountered based upon the good agreement between all of the paired FP and venous lead results. The method described is easier to perform than an earlier version. All indications suggest that a fingerstick capillary blood sample collected on filter paper is suitable for lead screening. Proper precautions must always be taken to guard against contamination.
The SIGMA facility was set up at IRSN to provide thermal neutrons for metrology and dosimetry purposes. SIGMA consists of six Am-Be radioactive sources located in a 1.5 x 1.5 x 1.5 m3 graphite moderator block. The neutron field at the calibration position, situated at 50 cm from the west surface of the assembly was characterised experimentally and by Monte Carlo calculations. The thermal neutron fluence was determined by the activation of gold foils; the neutron fluence energy distribution above 240 keV was measured with proton recoil spectrometers and the neutron fluence energy distribution from thermal energies to 20 MeV was measured with a Bonner spheres spectrometer. A Monte Carlo simulation of the SIGMA assembly was undertaken using the MCNP4C code, and the calculated neutron fluence energy distribution was compared with the measurements. As a whole, the experimental data and the MCNP calculation are in a good agreement.
Brain abscess can develop at the site of retained intracranial foreign bodies many years after the injury. This report describes a 6 1/2-year-old child who presented with recurrent severe headaches and a focal seizure of the right upper extremity. Skull X-ray was normal. Computed tomography of the head showed a mass in the left temporoparietal region with a central area of high density and contrast enhancement, thought to be a neoplasm. The mass was seen on the radionuclide brain scan and was avascular on angiography. Craniotomy revealed a foreign body granuloma with a small abscess cavity and a retained piece of pencil graphite. No one in the family could recall if the child had had such an injury.
It has been demonstrated previously that Geobacter species can transfer electrons directly to electrodes. In order to determine whether electrodes could serve as electron donors for microbial respiration, enrichment cultures were established from a sediment inoculum with a potentiostat-poised graphite electrode as the sole electron donor and nitrate as the electron acceptor. Nitrate was reduced to nitrite with the consumption of electrical current. The stoichiometry of electron and nitrate consumption and nitrite accumulation were consistent with the electrode serving as the sole electron donor for nitrate reduction. Analysis of 16 rRNA gene sequences demonstrated that the electrodes supplied with current were specifically enriched in microorganisms with sequences most closely related to the sequences of known Geobacter species. A pure culture of Geobacter metallireducens was shown to reduce nitrate to nitrite with the electrode as the sole electron donor with the expected stoichiometry of electron consumption. Cells attached to the electrode appeared to be responsible for the nitrate reduction. Attached cells of Geobacter sulfurreducens reduced fumarate to succinate with the electrode as an electron donor. These results demonstrate for the first time that electrodes may serve as a direct electron donor for anaerobic respiration. This finding has implications for the harvesting of electricity from anaerobic sediments and the bioremediation of oxidized contaminants.