Isolation and structural studies of porcine, ovine and murine thymosin beta 4 by high-performance liquid chromatography

Rapid high-performance liquid chromatographic (HPLC) procedures have been used to isolate and characterize thymosin beta 4 from different species. Crude extracts termed thymosin fraction 5A were prepared from porcine and ovine thymus glands as well as murine spleen. Each fraction 5A preparation was then fractionated by HPLC on a muBondapak C18 reversed-phase column. Porcine and ovine thymus fraction 5A, and murine spleen 5A, each yields a predominant peak at a retention time similar to that of bovine thymosin beta 4. Amino acid analysis as well as HPLC tryptic peptide mapping of these peaks indicate that they have homologous sequences to bovine thymosin beta 4. Chromatographic analysis of fresh murine thymus and spleen tissues also revealed protein peaks at the position of bovine beta 4, suggesting that thymosin beta 4 is the native protein present in the animal tissues.     

Carboxylation and Mitsunobu reaction of amines to give carbamates: retention vs inversion of configuration is substituent-dependent

A mild method for the synthesis of carbamates from amino alcohols involves sequential carboxylation with carbon dioxide, followed by a Mitsunobu reaction. Unexpectedly, the stereochemical course of the Mitsunobu reaction is dependent on whether the carbamic acid intermediate is N-substituted with hydrogen (retention) or carbon (inversion).     

A multiresidue pesticide monitoring procedure using gas chromatography/mass spectrometry and selected ion monitoring for the determination of pesticides containing nitrogen, sulfur, and/or oxygen in fruits and vegetables

A procedure for the analysis of over 100 pesticides that only contain combinations of carbon, hydrogen, nitrogen, sulfur, and oxygen (i.e., no phosphorous or halogen atoms) has been developed. The procedure employs gas chromatography with a mass selective detector (GC/MSD), electron impact ionization, and selected ion monitoring. This GC/MSD procedure provided lower limits of quantitation and increased confirmational data compared to the traditional element-selective GC procedures that are commonly used for the detection of this "class" of pesticides. These analytical improvements were demonstrated by 26 pesticides that were detected at ng/g levels in a variety of fruit and vegetable matrixes using this procedure; these pesticides were missed by the traditional element-selective GC procedures. Validation of the procedure was performed using acetone extraction with solid-phase extraction cleanup. Twenty representative target pesticides were used to demonstrate repeatability and linearity of the chromatographic response and recovery from fruit and vegetable matrixes.     

The determination of radium-226 and radium-228 in soils and plants,using radium-225 as a yield tracer

Recovery of²²⁶Ra in analysis is determined using²²⁵Ra separated by anion exchange from²²⁹Th and²³³U. Radium is coprecipitated with barium, and purified by ion exchange.²²⁶Ra and²¹⁷At (decay product of²²⁵Ra) are measured by α-spectrometry.²²⁸Ra is determined both by β-counting²²⁸Ac and²²⁵Ac separated from²²⁸Ra and²²⁵Ra, and by α-counting its daughters after the decay of²²⁵Ra. Sources for α-spectrometry are prepared by electrodeposition (molecular plating).     

An Interwoven Metal‐Organic Framework Combining Mechanically Interlocked Linkers and Interpenetrated Networks

New dibenzo[24]crown‐8 ether derivatives were prepared that contain appendages with thioether donors that can coordinate to a metal ion. These macrocycles were then combined with 1,2‐bis(pyridinium) ethane axles to create two types of [2]rotaxane ligands; those with the four thioether donors on the crown ether and those with six donor groups, four from the crown ether and two more attached to the stoppering groups of the dumbbell. The crown ethers and both types of [2]rotaxane ligands were allowed to react with Ag^I ions to form metal‐organic rotaxane framework (MORF) style coordination polymers. The interlocked hexadentate ligand forms the first example of a new type of lattice containing interwoven frameworks resulting from both interpenetration of frameworks due to the presence of an interlocked ligand and more classical interpenetration of independent frameworks.     

Sodiation Of Hard Carbon: How Separating Enthalpy And Entropy Contributions Can Find Transitions Hidden In The Voltage Profile

Sodium-ion batteries (NIBs) utilize cheaper materials than lithium-ion batteries (LIBs) and can thus be used in larger scale applications. The preferred anode material is hard carbon, because sodium cannot be inserted into graphite. We apply experimental entropy profiling (EP), where the cell temperature is changed under open circuit conditions. EP has been used to characterize LIBs; here, we demonstrate the first application of EP to any NIB material. The voltage versus sodiation fraction curves (voltage profiles) of hard carbon lack clear features, consisting only of a slope and a plateau, making it difficult to clarify the structural features of hard carbon that could optimize cell performance. We find additional features through EP that are masked in the voltage profiles. We fit lattice gas models of hard carbon sodiation to experimental EP and system enthalpy, obtaining: 1. a theoretical maximum capacity, 2. interlayer versus pore filled sodium with state of charge.     

Physics-based generation of gamma-ray response functions for CdZnTe detectors

A physics-based approach to gamma-ray response-function generation is presented in which the response of CdZnTe detectors is modeled from first principles. Numerical modeling is used to generate response functions needed for spectrum analysis for general detector configurations (e.g., electrode design, detector materials and geometry, and operating conditions). With numerical modeling, requirements for calibration and characterization are significantly reduced. Elements of the physics-based model, including gamma-ray transport, charge carrier drift and diffusion, and circuit response, are presented. Calculated and experimental gamma-ray spectra are compared for a coplanar-grid CdZnTe detector.     

Hadamard's inequality and Trapezoid Rules for the Riemann-Stieltjes integral

We obtain Midpoint and Trapezoid Rules for the Riemann-Stieltjes integral which engender a natural generalization of Hadamard's integral inequality. Error terms are then obtained for this Riemann-Stieltjes Trapezoid Rule and other related quadrature rules.     

A spatially dependent model for washing wool

We analytically model the transport of dirt in the industrial washing of wool using the advection–diffusion equation in two dimensions. Separation of variables leads to a Sturm–Liouville problem where the analytic solution reveals how contamination is distributed both along and down the wool and indicates the operating parameter regimes that optimise the cleaning efficiency.