Three-dimensional in vivo ESR imaging in rats

The first experiment of tridimensional in vivo ESR imaging at 1.2 GHz is described in this paper. The tails of rats weighing 300-350 grams were visualized using 1 cc of a 50 * 10(-3) M solution of nitroxide free radical injected in the caudal vein. In an even distribution of spin label is assumed this would correspond to a final concentration of about 10(-4) M. A reconstruction from projections was used to obtain the images. The apparatus utilizes stationary field gradients. Projections were obtained by sweeping the main field. For 3D reconstructions, the projections were collected along 32 * 8 field gradient orientations. The whole procedure takes approximately 18 minutes.     

Open resonators for low dielectric loss measurements

Open resonators are studied based on the scattering theory. In particular, a theory of open resonators with a dielectric plate is constructed. This theory is used to develop a technique for measuring small dielectric loss. Measurements of the loss tangent in diamond plates show that the volume absorption in the best samples is ≈7×10^?6 in the high-frequency part of the millimeter-wave range. A significant absorption in thin surface layers that is caused by surface treatment techniques (polishing, vacuum soldering, etc.) is revealed.     

Continuous-wave far-infrared ESR spectrometer for high-pressure measurements

We present a newly-developed microwave probe for performing sensitive high-field/multi-frequency electron spin resonance (ESR) measurements under high hydrostatic pressures. The system consists of a BeCu-made pressure-resistant vessel, which accommodates the investigated sample and a diamond microwave coupling window. The probe’s interior is completely filled with a pressure-transmitting fluid. The setup operates in reflection mode and can easily be assembled with a standard oversized microwave circuitry. The probe-head withstands hydrostatic pressures up to 1.6 GPa and interfaces with our home-built quasi-optical high-field ESR facility, operating in a millimeter/submillimeter frequency range of 105–420 GHz and in magnetic fields up to 16 T. The overall performance of the probe was tested, while studying the pressure-induced changes in the spin-relaxation mechanisms of a quasi-1D conducting polymer, KC₆₀. The preliminary measurements revealed that the probe yields similar signal-to-noise ratio to that of commercially available low-frequency ESR spectrometers. Moreover, by observing the conduction electron spin resonance (CESR) linewidth broadening for KC₆₀ in an unprecedented microwave frequency range of 210–420 GHz and in the pressure range of up to 1.6 GPa, we demonstrate that a combination of high-pressure ESR probe and high-field/multi-frequency spectrometer allows us to measure the spin relaxation rates in conducting spin systems, like the quasi-1D conductor, KC₆₀.     

Modified surface-coil-type resonators for EPR measurements of a thin membranelike sample

Surface-coil-type resonators (SCRs) equipped with a circular single-tum coil (conventional SCR), a circular spiral coil (spiral SCR), and a plate-type single-turn coil (plate-type SCR) were fabricated. By using these SCRs, the electron paramagnetic resonance (EPR) sensitivities of thin membranelike samples were investigated. For a non-dielectric-loss phantom, filter paper containing 1,1-diphenyl-2-picrylhydrazyl was used. For a high-dielectric-loss phantom, gauze containing an aqueous solution of 3-carbamoyl-2,2,5,5-tetramethylpyrrolidine-1-oxyl (carbamoyl-PROXYL) was used. For a biological sample, a pea leaf impregnated with the carbamoyl-PROXYL solution was used. The sensitivity (signal-to-noise ratio) of the spiral and plate-type SCRs for the non-dielectric-loss phantom was significantly greater than that of the conventional SCR. Under these conditions, the sensitivity of the spiral SCR was relatively higher than that of the plate-type SCR. For the high-dielectric-loss phantom, the sensitivity of the plate-type SCRs was significantly greater than that of the conventional SCR, but there were no differences in sensitivity between the spiral and conventional SCRs. The sensitivity of the plate-type SCR in the EPR measurement of a pea leaf was significantly greater than that of the conventional SCR. These findings show that the spiral and plate-type SCRs are suitable for measuring EPR of thin membranelike samples, especially when the former is used for the non-dielectric-loss sample and the latter for high-dielectric-loss sample, including the leaf.     

Longitudinally detected ESR magnetometer for wide-range measurements of low fields

A new magnetometer utilizing a longitudinally detected ESR (LODESR) method was developed. The probe head of the LODESR magnetometer is equipped with a single-turn coil (8 mm in diameter) which has a very wide bandwidth because the reactance of the coil is always smaller than the resistance of the transmission line (50 ohm) at frequencies less than 700 MHz. Thus, an absolute magnetic field could be measured over a wide range (2 to 9 mT) using this magnetometer without changing the probe head.     

Evaluation of sub-microsecond recovery resonators for in vivo electron paramagnetic resonance imaging

Time-domain (TD) electron paramagnetic resonance (EPR) imaging at 300MHz for in vivo applications requires resonators with recovery times less than 1 micros after pulsed excitation to reliably capture the rapidly decaying free induction decay (FID). In this study, we tested the suitability of the Litz foil coil resonator (LCR), commonly used in MRI, for in vivo EPR/EPRI applications in the TD mode and compared with parallel coil resonator (PCR). In TD mode, the sensitivity of LCR was lower than that of the PCR. However, in continuous wave (CW) mode, the LCR showed better sensitivity. The RF homogeneity was similar in both the resonators. The axis of the RF magnetic field is transverse to the cylindrical axis of the LCR, making the resonator and the magnet co-axial. Therefore, the loading of animals, and placing of the anesthesia nose cone and temperature monitors was more convenient in the LCR compared to the PCR whose axis is perpendicular to the magnet axis.     

Optical bistability and temporal symmetry-breaking instability in nonlinear fiber resonators

In this work we analyze two different behaviors in a nonlinear passive fiber ring cavity with a synchronously pulsed pump iterating the infinite-dimensional Ikeda map. First, we show optical bistability with normal and anomalous dispersions. The obtained numerical results are compared with the cw pump case. Secondly, these cavities are subject to a temporal symmetry-breaking instability with anomalous dispersion. This instability is described and the range of parameters for its appearance is shown and discussed.     

Submillimeter-wave ESR measurements of low-dimensional quantum spin systems

Temperature-dependent electron spin resonance (ESR) measurements of two low-dimensional quantum spin systems, theS = 1/2 spin-ladder system Cu₂(1,4-diazacycloheptane)₂Cl₄ (Cu₂(C₅H₁₂N₂)₂Cl₄) and the gaplessS = 1 bond-alternating one-dimensional antiferromagnettrans-Ni(333-tet)(N₃)(ClO₄), have been performed. X-band electron spin resonance (ESR) measurements of single-crystal Cu₂(C₅H₁₂N₂)₂Cl₄ show the increase of linewidth and anisotropicg-shifts below 8 K similar to those known for one-dimensional antiferromagnet. On the other hand, Ni(333-tet)(N₃)(ClO₄) has broad line-width and ESR has been observed for the first time by our high-field ESR. Its linewidth increases as the temperature is decreased, while theg-shift seems to be isotropic and theg-value decreases as the temperature is decreased. Thisg-shift can be connected to the quantum fluctuation of the system.     

Acoustical measurements of expression devices in pipe organs

In this investigation, three different swell systems known in pipe organs, the swell box, the crescendo wheel, and the historic wind swell were measured and compared to each other. The dynamic range of the crescendo wheel was found to be most effective, and for frequencies near 2 kHz the increase in sound pressure level could be up to 50 dB between the softest and the loudest adjustment. The maximum dynamic range for the wind swell and the swell box were found to be 10-20 dB in the same frequency range. With its step-wise crescendo procedure, the crescendo wheel simulates the type of orchestra crescendo which is reached by successively adding further musical instruments. In contrast, the swell box and the wind swell produce a crescendo effect similar to the crescendo in which individual musical instruments perform a dynamic movement. This type of crescendo requires a continuous level increase but allows a smaller dynamic range. The disappearance of the wind swell is not surprising because it offers no advantage over the swell box, while being restricted to stops with free reeds.     

Concentration by centrifugation for gas exchange EPR oximetry measurements with loop-gap resonators

Measurement of the bimolecular collision rate between a spin label and oxygen is conveniently carried out using a gas permeable plastic sample tube of small diameter that fits a loop-gap resonator. It is often desirable to concentrate the sample by centrifugation in order to improve the signal-to-noise ratio (SNR), but the deformable nature of small plastic sample tubes presents technical problems. Solutions to these problems are described. Two geometries were considered: (i) a methylpentene polymer, TPX, from Mitsui Chemicals, at X-band and (ii) Teflon tubing with 0.075 mm wall thickness at Q-band. Sample holders were fabricated from Delrin that fit the Eppendorf microcentrifuge tubes and support the sample capillaries. For TPX, pressure of the sealant at the end of the sample tube against the Delrin sample holder provided an adequate seal. For Teflon, the holder permitted introduction of water around the tube in order to equalize pressures across the sealant during centrifugation. Typically, the SNR was improved by a factor of five to eight. Oxygen accessibility applications in site-directed spin labeling studies are discussed.     

Joint temporal density measurements for two-photon state characterization

We demonstrate a technique for characterizing two-photon quantum states based on joint temporal correlation measurements using time-resolved single-photon detection by femtosecond up-conversion. We measure for the first time the joint temporal density of a two-photon entangled state, showing clearly the time anticorrelation of the coincident-frequency entangled photon pair generated by ultrafast spontaneous parametric down-conversion under extended phase-matching conditions. The new technique enables us to manipulate the frequency entanglement by varying the down-conversion pump bandwidth to produce a nearly unentangled two-photon state that is expected to yield a heralded single-photon state with a purity of 0.88. The time-domain correlation technique complements existing frequency-domain measurement methods for a more complete characterization of photonic entanglement.     

Dielectric resonator-based resonant structure for sensitive ESR measurements at high-hydrostatic pressures

We present a newly developed microwave probe head that accommodates a gasketed sapphire anvil cell (SAC) for performing sensitive electron spin resonance (ESR) measurements under high-hydrostatic pressures. The system was designed around commercially available dielectric resonators (DRs) having the dielectric permittivity of approximately 30. The microwave resonant structure operates in a wide-stretched double-stacked geometry and resonates in the lowest cylindrical quasi TE(011) mode around 9.2 GHz. The most vital parts of the probe's microwave heart were made of plastic materials, thus making the resonant structure transparent to magnetic field modulation at 100 kHz. The overall ESR sensitivity of the probe was demonstrated for a small speck of 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) positioned in the gasket of the SAC, using water as the pressure-transmitting medium. The system was also used for studying pressure-induced changes in spin-relaxation mechanisms of a quasi-1D-conducting polymer, K(1)C(60). For small samples located in the sample hole of the gasket the probe reveals sensitivity that is only approximately 3 times less than that yielded by regular ESR cavities.     

Simultaneous ESR and optical absorption measurements of K in solid Ar

An apparatus was developed for simulataneous electron spin resonance (ESR) and optical absorption experiments on atoms imbedded in rare gas matrices. In a first application the temperature dependence of ESR signals and of optical absorption spectra of K atoms in Ar matrices were studied. One of the numerous ESR lines could be unambiguously assigned to the so-called red triplet absorption due to their identical annealing behaviour at 12–14 K. The correspondence of other ESR lines to optical absorptions is discussed.     

Mass measurements of relativistic projectile fragments in the storage ring ESR

Two experimental methods of measuring masses of exotic nuclei in the storage ring ESR are presented. Bismuth and nickel fragments were produced via projectile fragmentation, separated and investigated with the combination of the fragment separator FRS and the ESR: (i) Direct mass measurements of relativistic projectile fragments were performed using Schottky mass spectrometry (SMS), i.e., exotic nuclei were stored and cooled in the ESR. Applying electron cooling, the relative velocity spread of circulating low intensity beams can be reduced below 10⁻⁶. Under this condition a mass resolving power of up to m/Δm=6.5·10⁵ (FWHM) was achieved in a recent measurement. Previously unknown masses of more than 100 neutron-deficient isotopes have been measured in the range of 60≤Z≤84. Using known Q _α values the area of known masses could be extended to more exotic nuclei and to higher proton numbers. The results are compared with mass models and extrapolations of experimental values. In a second experiment with ²⁰⁹Bi projectiles the area of the measured masses was extended to lower proton numbers. Due to various improvements at the ESR the precision of the measurements could be raised. (ii) Exotic nuclei with half-lives shorter than the time needed for SMS (present limit: T _1/2 ≈ 5 sec) can be investigated by time-of-flight measurements whereby the ESR is operated in the isochronous mode. This novel experimental technique has been successfully applied in first measurements with nickel and neon fragments where a mass resolving power of m/Δm=1.5·10⁵ (FWHM) was achieved.     

Usability of tartaric acid in dose measurements: an ESR study

Unirradiated tartaric acid samples do not exhibit any ESR signal. However, the ESR spectra of irradiated samples contain many resonance signals. The dose–responce curves of the resonance signals, denoted as I ₁, I ₂, I ₃ and I ₄ in the present study, were found to increase linearly with the applied radiation dose in the range of 0.04–25 kGy. Adjusting the microvawe power and modulation amplitudes of 1.0 mW and 1.0 mT, respectively, was found to increase the sensitivity of tartaric acid. From the dose–response curves and room temperature decay data, it was concluded that the I ₃ resonance signal of tartaric acid can be used for dose measurements at intermediate (0.04–0.4 kGy) and high dose (0.5–25 kGy) levels.     

In vivo temporal EPR imaging for estimating the kinetics of a nitroxide radical in the renal parenchyma and pelvis in rats

The kinetics of a nitroxide radical in the renal parenchyma and pelvis in rats were investigated by employing an in vivo EPR imaging system equipped with a surface-coil-type resonator (SCR). The exposed kidney of a living rat was inserted into the single-turn coil of the SCR, with the renal major axis aligned with the direction of alternative magnetic field (B(1)). After the injection of nitroxide radical via the tail vein, EPR measurements were repeated. From the temporal EPR images of the kidney on the 2-D projection to the plane which is perpendicular to the direction of B(1,) the decay rate of nitroxide radical in the renal parenchyma and pelvis was estimated. The parenchymal decay rate was found to be significantly shorter than that for the pelvis.     

Tracking iron oxide nanoparticles in plant organs using magnetic measurements

Common bean plants were grown in soil and irrigated with water solutions containing different concentrations of \(\hbox{Fe}_3\hbox{O}_4\) nanoparticles (NPs) with a mean diameter close to 10 nm. No toxicity on plant growth has been detected as a consequence of Fe deficiency or excess in leaves. In order to track the \(\hbox{Fe}_3\hbox{O}_4\) NPs, magnetization measurements were performed in soils and in three different dried organs of the plants: roots, stems, and leaves. Some magnetic features of both temperature and magnetic field dependence of magnetization M(T, H) arising from \(\hbox{Fe}_3\hbox{O}_4\) NPs were identified in all the three organs of the plants. Based on the results of saturation magnetization \(M_\mathrm{s}\) at 300 K, the estimated number of \(\hbox{Fe}_3\hbox{O}_4\) NPs was found to increase from 2 to 3 times in leaves of common bean plants irrigated with solutions containing magnetic material. The combined results indicated that M(T, H) measurements, conducted in a wide range of temperature and applied magnetic fields up to 70 kOe, constitute a useful tool through which the uptake, translocation, and accumulation of magnetic nanoparticles by plant organs may be monitored and tracked.     

Rapid near-infrared Raman spectroscopy system for real-time in vivo skin measurements

A rapid dispersive-type near-infrared (NIR) Raman spectroscopy system and a Raman probe were developed to facilitate real-time, noninvasive, in vivo human skin measurements. Spectrograph image aberration was corrected by a parabolic-line fiber array, permitting complete CCD vertical binning, thereby yielding a 3.3-16-fold improvement in signal-to-noise ratio. Good quality in vivo cutaneous NIR Raman spectra free of interference from fiber fluorescence and silica Raman scattering can be acquired in less than 1 s, which greatly facilitates practical noninvasive tissue characterization and clinical diagnosis.     

Evaluation of some parameters which influence the ESR measurements for the fading study of alanine dosimeters

Since several years, with the evolution of ESR spectrometers, the measurement of low absorbed doses seems to be accessible by alanine dosimetry. Some laboratories have realized important progress in this domain, but the influence of external physical and chemical factors that modify the results (fading) is not well quantified for using them with a sufficient accuracy for national or international comparisons, typically less than 3%. The first experimental study of combined effects has been realized in our laboratory. A necessary multiparametric approach (experimental design) has shown the complexity of the problem to solve before creating a physico-chemical model of the observed phenomena. The chosen methodology permits us to give the first quantitative approach of the fading for applied metrology.     

Skeletal contribution in lung measurements for the in vivo assessment of 241Am

Physical phantoms used for the calibration of in vivo measurement equipments represent an approximate geometry of the body and usually contain a uniform distribution of radionuclides in the organ of interest. Numerical voxel phantoms allow an improvement of the calibration method by means of a more realistic definition of the phantom and the source. The distribution of the activity in the tissues evolves with time and it can be estimated by solving the specific biokinetic model of the radionuclide. Those results of predicted activity retained in the compartments of the model can be translated into the organs of a voxel phantom to be used as the source of radiation for a Monte Carlo radiation transport code. In this way, different patterns of contamination, according to different times after the intake, can be modelled and appropriate detection efficiencies can be obtained. In particular, it is studied the influence of the skeletal contribution in lung measurements in the in vivo assessment of ²⁴¹Am.