Synthesis of macrocycles incorporating azo‐bis(azofurazan) framework

A series of macrocycles containing four furazan rings bonded by three azo bonds 2, 5 and 7 have been synthesized from the common precursor, 3‐amino‐3′‐nitro(azofurazan) 3 . The macrocycles closure is a result of N?N bond formation at oxidative cyclization of corresponding bis(3‐aminofurazan‐4‐yl) precursors. X‐Ray crystal structures of macrocycles 2, 2 ?AcOH, 11 and 13 are reported.     

Towards a full reference library of MS(n) spectra. Testing of a library containing 3126 MS2 spectra of 1743 compounds

A library consisting of 3766 MS(n) spectra of 1743 compounds, including 3126 MS2 spectra acquired mainly using ion trap (IT) and triple-quadrupole (QqQ) instruments, was composed of numerous collections/sources. Ionization techniques were mainly electrospray ionization and also atmospheric pressure chemical ionization and chemical ionization. The library was tested for the performance in identification of unknowns, and in this context this work is believed to be the largest of all known tests of product-ion mass spectral libraries. The MS2 spectra of the same compounds from different collections were in turn divided into spectra of 'unknown' and reference compounds. For each particular compound, library searches were performed resulting in selection by taking into account the best matches for each spectral collection/source. Within each collection/source, replicate MS2 spectra differed in the collision energy used. Overall, there were up to 950 search results giving the best match factors and their ranks in corresponding hit lists. In general, the correct answers were obtained as the 1st rank in up to 60% of the search results when retrieved with (on average) 2.2 'unknown' and 6.2 reference replicates per compound. With two or more replicates of both 'unknown' and reference spectra (the average numbers of replicates were 4.0 and 7.8, respectively), the fraction of correct answers in the 1st rank increased to 77%. This value is close to the performance of established electron ionization mass spectra libraries (up to 79%) found by other workers. The hypothesis that MS2 spectra better match reference spectra acquired using the same type of tandem mass spectrometer (IT or QqQ) was neither strongly proved nor rejected here. The present work shows that MS2 spectral libraries containing sufficiently numerous different entries for each compound are sufficiently efficient for identification of unknowns and suitable for use with different tandem mass spectrometers.     

Recovery of 177Lu from Irradiated HfO2 Targets for Nuclear Medicine Purposes

A new method of production of one of the most widely used isotopes in nuclear medicine, ¹⁷⁷Lu, with high chemical purity was developed; this method includes irradiation of the HfO₂ target with bremsstrahlung photons. The irradiated target was dissolved in HF and then diluted and placed onto a column filled with LN resin. Quantitative sorption of ¹⁷⁷Lu could be observed during this process. The column later was rinsed with the mixture of 0.1 M HF and 1 M HNO₃ and then 2 M HNO₃ to remove impurities. Quantitative desorption of ¹⁷⁷Lu was achieved by using 6 M HNO₃. The developed method of ¹⁷⁷Lu production ensures high purification of this isotope from macroquantities of hafnium and zirconium and radioactive impurities of carrier-free yttrium. The content of ^177mLu in ¹⁷⁷Lu in photonuclear production was determined. Due to high chemical and radionuclide purity, ¹⁷⁷Lu obtained by the developed method can be used in nuclear medicine.     

330 GHz FMCW Image Sensor for Homeland Security Applications

A single-pixel imaging remote sensor operating at 330 GHz is described. It is based on a frequency modulated continuous wave (FMCW) and aimed at detection of concealed objects for ranges up to 40 m. The system consists of 2 horn-lens antennas integrated with a homodyne transceiver. The synthesized linear FMCW signal at X-band is multiplied by a factor of 32 to generate the transmitted signal. An intermediate frequency (IF) signal obtained in the output port of the 2-nd harmonic mixer is employed for image processing. Distance measurements were made by performing data acquisition unit based on LabView interface and resulting in a range resolution about 1 cm. Examples of 2D and 3D images reconstructed with this sensor are presented.     

Influence of Multiple Binding Sites on the Supramolecular Assembly of N-[(3-pyridinylamino) Thioxomethyl] Carbamates

In this study, we investigated how the presence of multiple intermolecular interaction sites influences the heteromeric supramolecular assembly of N-[(3-pyridinylamino) thioxomethyl] carbamates with fluoroiodobenzenes. Three targets—R-N-[(3-pyridinylamino) thioxomethyl] carbamate (R = methyl, ethyl, and isobutyl)—were selected and crystallized, resulting in three parent structures, five co-crystals, and one co-crystal solvate. Three hydrogen-bonded parent crystal structures were stabilized by N-H···N hydrogen bonding and assembled into layers that stacked on top of one another. Molecular electrostatic potential surfaces were employed to rank binding sites (Npyr > C=S > C=O) in order to predict the dominant interactions. The N-H⋯H hydrogen bond was replaced by I⋯Npyr in 3/6 cases, I⋯C=S in 4/6 cases, and I⋯O=C in 1 case. Interestingly, the I⋯C=S halogen bond coexisted twice with I⋯Npyr and I⋯O=C. Overall, the MEPs were fairly reliable for predicting co-crystallization outcomes; however, it is crucial to also consider factors such as molecular flexibility. Finally, halogen-bond donors are capable of competing for acceptor sites, even in the presence of strong hydrogen-bond donors.     

Rapid determination of 90Sr in urine samples using AnaLig® Sr-01

This paper describes the use of IBC’s AnaLig^® Sr-01 molecular recognition technology product to effectively and selectively pre-concentrate, separate, and recover strontium from urine samples. This method uses two-stage columns separation consisting of two different commercial products Eichrom’s Pre-filter Material and AnaLig^® Sr-01 column from IBC Advanced Technologies. This method does not involve co-precipitation of strontium as phosphates and oxalates from urine samples. The new rapid method separates strontium-90 with high chemical recovery.     

Stability bands for moving solitons in uniform and inhomogeneous damped ac-driven circular Toda lattices

By means of systematic simulations, we study the motion of discrete solitons in weakly dissipative Toda lattices (TLs) with periodic boundary conditions, resonantly driven by a spatially staggered time-periodic (ac) force. A complex set of alternating stability bands and instability gaps, including scattered isolated stability points, is revealed in the parametric plane of the soliton’s velocity and forcing amplitude for a given size of the circular lattice. The analysis is also reported for the circular TL including a single light- or heavymass defect. The stability chart as a whole shrinks and eventually disappears with the increase of the lattice’s size and strength of the mass defect. Qualitative explanations to these findings are proposed. We also report the dependence of the stability area on the initial position of the soliton, finding that the area is largest for some intersite position. For a pair of solitons traveling in opposite directions, there exist regimes where both solitons survive periodic collisions in small-size lattices.     

激光辐射下的固体双基推进剂的燃烧特性

燃速与辐射通量之间的关系可以由两支相交直线构成的线性方程进行描述,其中折点(交点)是外界辐射能作用下固体双基推进剂燃烧的一个重要特征。包括折点附近在内的燃烧特性可以采用Fourier方程进行分析。考虑到辐射在燃烧表面上形成的碳化层对辐射传递的阻碍作用,本文分析了1040,1041,N-5和N型推进剂的燃烧特性。导致两段函数和折点形成的主要原因是在辐射能到达凝聚相表面之前部分辐射能已经发生了损失。     

On the Capacity of IEEE 802.11 DCF with Capture in Multipath-Faded Channels

In this paper, we estimated the influence of capture effect over the capacity of IEEE 802.11b DCF within a single picocell. The channel utilization is examined analytically by introducing two capture models based on Rayleigh-distributed envelopes of the captured and the interfering frames divided into two local-mean power classes. Simulations in a pure Rician-faded channel depict the conditions under which both Rayleigh-faded capture models can be used to accurately predict the peak network capacity. Unlike the RTS/CTS handshake access mode, Basic access mode is significantly sensitive to the capture ratio, i.e., the receiver design. The packet size threshold over which it is convenient to switch from Basic to RTS/CTS handshake access scheme is also sensitive to the capture effect.     

Aging of the over-voltage protection elements caused by over-voltages

The aim of this work is examining the influence of the number of the activation––over-voltage pulses to the aging of over-voltage protection elements. Both non-linear (gas-filled surge arresters (GFSA), varistors, over-voltage diodes) and linear (capacitors––constituents of filters) over-voltage protection elements were tested. The instruments employed allow reliable measurements, 1000 consecutive activation were tested. The double-exponential current pulse (amplitude I₁^max=13 A, I₂^max=16 A, rise time T₁=8 μs, fall time T₂=20 μs) for non-linear elements and a double-exponential over-voltage pulse (rise time T₁=1.2 μs, fall time T₂=50 μs) of the amplitude U₁^max=320 V, U₂^max=480 V and U₃^max=640 V for capacitors were used. The experimental results show that the over-voltage diodes are the most reliable elements in view of characteristic modifications that are consequence of aging. However, it was observed that varistors, GFSA and capacitors undergo noticeable changes in characteristics.