Optimal Operation of an Industrial Dividing Wall Column through Multiparametric Programming
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Evaluation of chromatographic resins for high efficacy separation of radium from chemical analogues
The separation of Radium (Ra) from interfering chemical analogues is of major importance for both the accurate measurement of Ra-226 in environmental samples and the preparation of radium targets destined for medical isotope production. The adsorption behavior of Ra, Barium (Ba), and Strontium (Sr) was investigated on multiple crown-ether-based proprietary extraction chromatographic resins developed by TrisKem Int. Among these, the TK101 resin, characterized by a novel room-temperature ionic liquid (RTIL) dual extractant–solvent system, demonstrated enhanced affinity and selectivity, particularly at low acid concentrations, achieving a D w of 3477 ± 73 for Ra in 0.04 M HNO₃, whereas the maximum Ra D w obtained with the traditional Sr resin in 8 M HNO 3 was only 12.33 ± 0.4. In 0.04 M HNO 3 , a Ra distribution ratio (D w ) of 776 was achieved within 1 min, indicating rapid uptake kinetics. The adsorption capacities were estimated at 19.6 ± 0.1 mg/g for Ba and 12.0 ± 0.2 mg/g for Sr. However, competing alkali metals significantly reduced alkaline earth metal uptake, indicating that the TK101 resin is best suited for radium purification following a preconcentration step to minimize matrix effects in high salinity samples. Dynamic column studies confirmed the strong chromatographic performance of the TK101 resin, with no significant Ba or Sr breakthrough in the Ra fraction and a Ra recovery of 87 ± 2.8%. These results demonstrate the potential of the TK101 resin for selective radium separation in analytical and radiochemical applications.
and nuclear chemistry↗
Neutral hydrogen in the direction of the Small Magellatic Cloud and the limits of an extragalactic soft X-ray flux
Previously reported X-ray data from the vicinity of the Small Magellanic Cloud (SMC) have been reanalyzed using H I data from a more detailed and sensitive 21-cm survey of this region. The results support the previous conclusion: assuming that the interstellar material absorbs according to the cross sections of Brown and Gould (1970), at least 75 per cent of the observed 0.25-keV X-ray flux is of local origin. The corollary problem of placing a cosmologically useful upper limit on the extragalactic flux will be difficult to solve until the behavior of the local component is better understood; but if the local flux is isotropic, a 3-sigma upper limit of 240 photons per (sq cm s sr keV) at 0.25 keV may be placed on a flux originating beyond the SMC. Tables of H I column density are given for an area 30 deg by 30 deg about the SMC. The high-velocity component, presumably associated with the Magellanic Cloud system, and the galactic disk component are tabulated separately.
Mccammon, D.↗
Creeping flow of a conducting fluid past axisymmetric bodies in the presence of an aligned magnetic field
The use of strong magnetic fields for the control of particle settling in metallic systems is investigated by altering the fluid mechanics in the melt. The fluid mechanism of particle settling is analyzed for the motion around single, axisymmetric particles in the limit of creeping flow for a fluid with a large electrical conductivity. The drag is found to increase proportionately to the intensity of the magnetic field or the Hartmann number Ha. The flowfield forms boundary layers, which thin out with increasing Ha, along the surfaces parallel to the flow. For axisymmetric bodies, the boundary layer separates as the poles of the surface are approached and encloses regions of almost stagnant fluid. These regions spread upstream and downstream along the body with increasing Ha, thereby trapping the particle in a column of stagnant fluid.
Kyrlidis, A.↗
Theory of Metastable State Relaxation in a Gravitational Field for Non-Critical Binary Systems with Non-Conserved Order Parameter
A new mathematical ansatz is developed for solution of the time-dependent Ginzburg-Landau nonlinear partial differential equation describing metastable state relaxation in binary (solute+solvent) non-critical solutions with non-conserved scalar order parameter in presence of a gravitational field. It has been demonstrated analytically that in such systems metastability initiates heterogeneous solute redistribution which results in the formation of a non-equilibrium singly-periodic spatial solute structure in the new solute-rich phase. The critical radius of nucleation and the induction time in these systems are gravity-dependent. It has also been proved that metastable state relaxation in vertical columns of supersaturated non-critical binary solutions leads to formation of the solute concentration gradient. Analytical expression for this concentration gradient is found and analysed. It is concluded that gravity can initiate phase separation (nucleation or spinodal decomposition).
Izmailov, Alexander F.↗
Ultraviolet Broad Absorption Features and the Spectral Energy Distribution of the QSO PG 1351+64
We present a moderate-resolution (approximately 20 km s(exp -1) spectrum of the mini broad absorption line QSO PG 1351+64 between 915-1180 A, obtained with the Far Ultraviolet Spectroscopic Explorer (FUSE). Additional low-resolution spectra at longer wavelengths were also obtained with the Hubble Space Telescope (HST) and ground-based telescopes. Broad absorption is present on the blue wings of C III (lambda)977, Ly(beta), O VI (lambda)(lambda)1032,1038, Ly(alpha), N V (lambda)(lambda)1238,1242, Si IV (lambda)(lambda)1393,1402, and C IV (lambda)(lambda)1548,1450. The absorption profile can be fitted with five components at velocities of approximately -780, -1049, -1629, -1833, and -3054 km s(exp -1) with respect to the emission-line redshift of z = 0.088. All the absorption components cover a large fraction of the continuum source as well as the broad-line region. The O VI emission feature is very weak, and the O VI/Ly(alpha) flux ratio is 0.08, one of the lowest among low-redshift active galaxies and QSOs. The UV (ultraviolet) continuum shows a significant change in slope near 1050 A in the restframe. The steeper continuum shortward of the Lyman limit extrapolates well to the observed weak X-ray flux level. The absorbers' properties are similar to those of high-redshift broad absorption-line QSOs. The derived total column density of the UV absorbers is on the order of 10(exp 21) cm(exp -2), unlikely to produce significant opacity above 1 keV in the X-ray. Unless there is a separate, high-ionization X-ray absorber, the QSO's weak X-ray flux may be intrinsic. The ionization level of the absorbing components is comparable to that anticipated in the broad-line region, therefore the absorbers may be related to broad-line clouds along the line of sight.
Zheng, W.↗
Enabling Microliquid Chromatography by Microbead Packing of Microchannels
The microbead packing is the critical element required in the success of on-chip microfabrication of critical microfluidic components for in-situ analysis and detection of chiral amino acids. In order for microliquid chromatography to occur, there must be a stationary phase medium within the microchannel that interacts with the analytes present within flowing fluid. The stationary phase media are the microbeads packed by the process discussed in this work. The purpose of the microliquid chromatography is to provide a lightweight, low-volume, and low-power element to separate amino acids and their chiral partners efficiently to understand better the origin of life. In order to densely pack microbeads into the microchannels, a liquid slurry of microbeads was created. Microbeads were extracted from a commercially available high-performance liquid chromatography column. The silica beads extracted were 5 microns in diameter, and had surface coating of phenyl-hexyl. These microbeads were mixed with a 200- proof ethanol solution to create a microbead slurry with the right viscosity for packing. A microfilter is placed at the outlet via of the microchannel and the slurry is injected, then withdrawn across a filter using modified syringes. After each injection, the channel is flushed with ethanol to enhance packing. This cycle is repeated numerous times to allow for a tightly packed channel of microbeads. Typical microbead packing occurs in the macroscale into tubes or channels by using highly pressurized systems. Moreover, these channels are typically long and straight without any turns or curves. On the other hand, this method of microbead packing is completed within a microchannel 75 micrometers in diameter. Moreover, the microbead packing is completed into a serpentine type microchannel, such that it maximizes microchannel length within a microchip. Doing so enhances the interactions of the analytes with the microbeads to separate efficiently amino acids and amino acid enantiomers.
Balvin, Manuel↗
Enabling Microliquid Chromatography by Microbead Packing of Microchannels
The microbead packing is the critical element required in the success of on-chip microfabrication of critical microfluidic components for in-situ analysis and detection of chiral amino acids. In order for microliquid chromatography to occur, there must be a stationary phase medium within the microchannel that interacts with the analytes present within flowing fluid. The stationary phase media are the microbeads packed by the process discussed in this work. The purpose of the microliquid chromatography is to provide a lightweight, low-volume, and low-power element to separate amino acids and their chiral partners efficiently to understand better the origin of life. In order to densely pack microbeads into the microchannels, a liquid slurry of microbeads was created. Microbeads were extracted from a commercially available high-performance liquid chromatography column. The silica beads extracted were 5 microns in diameter, and had surface coating of phenyl-hexyl. These microbeads were mixed with a 200- proof ethanol solution to create a microbead slurry with the right viscosity for packing. A microfilter is placed at the outlet via of the microchannel and the slurry is injected, then withdrawn across a filter using modified syringes. After each injection, the channel is flushed with ethanol to enhance packing. This cycle is repeated numerous times to allow for a tightly packed channel of microbeads. Typical microbead packing occurs in the macroscale into tubes or channels by using highly pressurized systems. Moreover, these channels are typically long and straight without any turns or curves. On the other hand, this method of microbead packing is completed within a microchannel 75 micrometers in diameter. Moreover, the microbead packing is completed into a serpentine type microchannel, such that it maximizes microchannel length within a microchip. Doing so enhances the interactions of the analytes with the microbeads to separate efficiently amino acids and amino acid enantiomers.
Balvin, Manuel↗
PHOTCAL: The IRAF photometric calibration package
The IRAF photmetric calibration package PHOTCAL is discussed. PHOTCAL is a set of tasks designed to derive the transformation from the instrumental photometric system to the standard photometric system, and apply the transformation to the observations. The PHOTCAL package contains tasks for: (1) creating and/or editing standard star catalogs and observations catalogs, (2) creating, checking and editing the configuration file which specifies the format of the standard star and observations catalogs and the form of the transformation equations, (3) solving the transformation equations interactively or non-iteractively using non-linear least squares fitting routines, and (4) applying the transformation to the observations. PHOTCAL standard star and observations catalogs are simple text files, whose columns are delimited by whitespace, and whose first column contains the star names. This format makes it relatively easy to interface the output of non-IRAF photometry programs as well as the output of the IRAF APPHOT and DAOPHOT photometry packages to PHOTCAL. PHOTCAL maintains a standard star catalog directory for the convenience of the user, but users can easily create their own standard star catalogs and/or define their own standard star catalog directory. Separate observations files produced by APPHOT, DAOPHOT or a user program containing data for stellar fields taken through different filters, can be combined into observations catalogs using one of the PHOTCAL preprocessor tasks. The input configuration file required by PHOTCAL is a text file, consisting of a series of instructions written by the user in a mini-language understood by the PHOTCAL parser. These instructions: (1) assign names to the input data columns in the standard star and observations catalogs, (2) assign names and initial values to the parameters to be fit, (3) define and describe how to solve the transformation equations. The mini-language approach permits great flexibility in the format of the input catalogs and the form of the transformation equations.
Davis, L. E.↗
An ab initio study of core-valence correlation
Especially in the cases of the first two columns of the periodic table, the inclusion of core-valence correlation in ab initio CI calculations yields a contraction of the atomic valence shell and improves both calculated atomic ionization potentials and atomic energy separations. For the alkali dimers Na2, K2, and Rb2, the presently calculated bond lengths are in excellent agreement with experiments when core-valence is included. In addition, the valence dissociation energies are accurate.
Partridge, H.↗
Influences of Local Sea-Surface Temperatures and Large-scale Dynamics on Monthly Precipitation Inferred from Two 10-year GCM-Simulations
Two parallel sets of 10-year long: January 1, 1982 to December 31, 1991, simulations were made with the finite volume General Circulation Model (fvGCM) in which the model integrations were forced with prescribed sea-surface temperature fields (SSTs) available as two separate SST-datasets. One dataset contained naturally varying monthly SSTs for the chosen period, and the oth& had the 12-monthly mean SSTs for the same period. Plots of evaporation, precipitation, and atmosphere-column moisture convergence, binned by l C SST intervals show that except for the tropics, the precipitation is more strongly constrained by large-scale dynamics as opposed to local SST. Binning data by SST naturally provided an ensemble average of data contributed from disparate locations with same SST; such averages could be expected to mitigate all location related influences. However, the plots revealed: i) evaporation, vertical velocity, and precipitation are very robust and remarkably similar for each of the two simulations and even for the data from 1987-ENSO-year simulation; ii) while the evaporation increased monotonically with SST up to about 27 C, the precipitation did not; iii) precipitation correlated much better with the column vertical velocity as opposed to SST suggesting that the influence of dynamical circulation including non-local SSTs is stronger than local-SSTs. The precipitation fields were doubly binned with respect to SST and boundary-layer mass and/or moisture convergence. The analysis discerned the rate of change of precipitation with local SST as a sum of partial derivative of precipitation with local SST plus partial derivative of precipitation with boundary layer moisture convergence multiplied by the rate of change of boundary-layer moisture convergence with SST (see Eqn. 3 of Section 4.5). This analysis is mathematically rigorous as well as provides a quantitative measure of the influence of local SST on the local precipitation. The results were recast to examine the dependence of local rainfall on local SSTs; it was discernible only in the tropics. Our methodology can be used for computing relationship between any forcing function and its effect(s) on a chosen field.
Sud, Y. C.↗
A Simple and Sensitive LC-MS/MS Method for the Determination of Free 8-Hydroxy-2'-Deoxyguanosine in Human Urine
Urinary free 8-hydroxy-2'-deoxyguanosine (8OHdG), an oxidized product of DNA, and is frequently chosen as a biomarker of oxidative stress in humans, including studies of oxidative DNA damage during space flight. It is challenging to accurately and efficiently quantify urinary free 8OHdG in large scale human studies. LC-MS/MS is emerging as a preferable analytical technique owing its high sensitivity, selectivity and efficiency, compared to some traditional methods such as ELISA and HPLC. A simple and sensitive LC-MS/MS method has been developed for the determination of free 8OHdG in human urine. Sample preparation was done by solid phase extraction with a Waters Oasis HLB 96 well plate. A Waters Alliance 2795 HT Separation Module combined with a Quattro Micro tandem mass spectrometer was used as the LC-MS/MS system. The runtime of one injection can be less than 5 minutes using a reversed phase C18 column and an isocratic flow of methanol/water. ESI positive ions were quantified in the multiple reaction modes (MRM) using m/z 284 yields 168 for 8OHdG and m/z 289 yields173 for stable isotope labeled internal standard [(15)N5] 8OHdG. With this method for 8OHdG, a lower limit of quantitation of 1.0 nM (0.28 ng/mL) has been achieved using 100 microliter urine sample. The analytical range is between 1.0 and 100 nM with a correlation coefficient greater than or equal to 0.99. Good reproducibility can be obtained with intra-assay and inter-assay CVs less than or equal to 10% for 8OHdG spiked urine QC samples. This method can be used in high-throughput routine analysis of free 8OHdG in human urine.
Wang, Zuwei↗
NuSTAR Observations of Four Mid-IR-Selected Dual AGN Candidates in Galaxy Mergers
Mergers of galaxies are a ubiquitous phenomenon in the universe and represent a natural consequence of the “bottom-up” mass accumulation and galaxy evolution cosmological paradigm. It is generally accepted that the peak of active galactic nucleus (AGN) accretion activity occurs at nuclear separations of ≲10 kpc for major mergers. Here we present new NuSTAR and XMM-Newton observations for a subsample of mid-IR preselected dual AGN candidates in an effort to better constrain the column densities along the line of sight (LOS) for each system. Only one dual AGN candidate, J0841+0101, is detected as a single, unresolved source in the XMMNewton and NuSTAR imaging, while the remaining three dual AGN candidates, J0122+0100, J1221+1137, and J1306+0735, are not detected with NuSTAR; if these nondetections are due to obscuration alone, these systems are consistent with being absorbed by column densities of log ( N H /cm −2 ) ≽ 24.9, 24.6, and 24.3, which are roughly consistent with previously inferred column densities in these merging systems. In the case of J0841+0101, the analysis of the 0.3–30 keV spectra reveal an LOS column density of N H ≳ 10 24 cm −2 , significantly larger than the column densities previously reported for this system and demonstrating the importance of the higher signal-to-noise ratio XMM-Newton spectra and access to the >10 keV energies via NuSTAR. Though it is unclear if J0841+0101 truly hosts a dual AGN, these results are in agreement with the high obscuring columns expected in AGNs in late-stage mergers.
AGN host galaxies↗
Adaptable SEC‐SAXS data collection for higher quality structure analysis in solution
Abstract The two major challenges in synchrotron size‐exclusion chromatography coupled in‐line with small‐angle x‐ray scattering (SEC‐SAXS) experiments are the overlapping peaks in the elution profile and the fouling of radiation‐damaged materials on the walls of the sample cell. In recent years, many post‐experimental analyses techniques have been developed and applied to extract scattering profiles from these problematic SEC‐SAXS data. Here, we present three modes of data collection at the BioSAXS Beamline 4–2 of the Stanford Synchrotron Radiation Lightsource (SSRL BL4‐2). The first mode, the High‐Resolution mode, enables SEC‐SAXS data collection with excellent sample separation and virtually no additional peak broadening from the UHPLC UV detector to the x‐ray position by taking advantage of the low system dispersion of the UHPLC. The small bed volume of the analytical SEC column minimizes sample dilution in the column and facilitates data collection at higher sample concentrations with excellent sample economy equal to or even less than that of the conventional equilibrium SAXS method. Radiation damage problems during SEC‐SAXS data collection are evaded by additional cleaning of the sample cell after buffer data collection and avoidance of unnecessary exposures through the use of the x‐ray shutter control options, allowing sample data collection with a clean sample cell. Therefore, accurate background subtraction can be performed at a level equivalent to the conventional equilibrium SAXS method without requiring baseline correction, thereby leading to more reliable downstream structural analysis and quicker access to new science. The two other data collection modes, the High‐Throughput mode and the Co‐Flow mode, add agility to the planning and execution of experiments to efficiently achieve the user's scientific objectives at the SSRL BL4‐2.
Matsui, Tsutomu↗
Participation in TOMS missions
In the past year we have been investigating a new algorithm for the derivation of column sulfur dioxide, column ozone, and aerosol optical depth from the Total Ozone Mapping Spectrometer (TOMS) High Density TOMS (HDT) archived albedos. Simulations of the measured albedos were made using a radiative transfer model, and a technique developed to separate the effects of the aerosol optical depth from the absorption optical depth. The retrieval adopted obtained values from the three parameters with high accuracy. This retrieval was then applied to the TOMS data.
Hudson, Robert D.↗
Highly crosslinked silicon polymers for gas chromatography columns
A new highly crosslinked silicone polymer particle for gas chromatography application and a process for synthesizing such copolymer are described. The new copolymer comprises vinyltriethoxysilane and octadecyltrichlorosilane. The copolymer has a high degree of crosslinking and a cool balance of polar to nonpolar sites in the porous silicon polymer assuring fast separation of compounds of variable polarity.
Shen, Thomas C.↗
Near-Real-Time Material Tracking: Combining Vis–NIR Spectroscopy with Flow Sensing for Accurate Nd(III) Quantification
A fiber-optic visible–near-infrared (vis–NIR) absorption spectroscopy and flow sensor system has been developed for near-real-time tracking of Nd mass in the effluent stream from a column in a fume hood. The approach leverages two unique data streams and a partial least-squares regression (PLSR) model trained on vis–NIR absorption spectra of Nd(III) (0–1.5 M) in 1 M HNO 3 . In-line volumetric flow rate and vis–NIR spectra are measured in sequence after a chromatography column. The time stamps from each data stream are then synchronized, which allows integrated volumes to be combined with Nd(III) molarities predicted by a PLSR model to accurately calculate the Nd mass flowing through the column. This integrated measurement provides instantaneous mass flow and accumulates these data over time to obtain the total mass processed. The methodology developed in this study contributes critical technical infrastructure to improve monitoring capabilities to support chemical separations and the production of strategic materials and isotopes.
Irvine, Sawyer B. [Oak Ridge National Laboratory (↗
Applications of space-electrophoresis in medicine
The nature of electrophoresis is reviewed and potential advances realizable in the field of biology and medicine from a space electrophoresis facility are examined. The ground-based applications of electrophoresis: (1) characterization of an ionized species; (2) determination of the quantitative composition of a complex mixture; and (3) isolation of the components of a mixture, separation achieved on the basis of the difference in transport rates is reviewed. The electrophoresis of living cells is considered, touching upon the following areas: the separation of T and B lymphocytes; the genetic influence on mouse lymphocyte mobilities; the abnormal production of specific and monoclonal immunoproteins; and the study of cancer. Schematic diagrams are presented of three types of electrophoresis apparatus: the column assembly for the static electrophoresis experiment on the Apollo-Soyuz mission, the continuous flow apparatus used in the same mission and a miniaturized electrophoresis apparatus.
Bier, M.↗