Spectrometer Research Articles

Determination of Hafnium in Zirconium by Spectrophotometry

Zirconium and hafnium have opposite nuclear properties and are used very differently in the nuclear industry. However, hafnium is a common metal impurity in zirconium, and the chemical properties of the two are very similar except for nuclear properties, and it is difficult to separate and detect them. At present, the detection of hafnium content in zirconium is usually achieved by using an inductively coupled plasma (ICP) spectrometer, but ICP equipment is expensive, and the detection cost is high. Therefore, it is necessary to develop a simple and low-cost method for the determination of hafnium content in zirconium. Based on this, this paper takes the spectrophotometric method as a starting point. Through a series of experiments on the influence of pH and concentrations of the color-developing agent xylenol orange sodium salt on the absorbance of zirconium and hafnium ions, the appropriate variables are selected to detect the content of hafnium in zirconium. Finally, according to the measured absorbance and total ion concentration, by comparing the working curve of zirconium and hafnium ions, the content of hafnium in zirconium is calculated based on the lever principle.

Evaluation of the Level of Soil Pollution by Metallic Trace Elements: Case of the Kachoma District of the City of Kipushi/Haut-Katanga (DR Congo)

The objective of this research was to assess the level of soil pollution in the Kachoma district located around the former discharge basin (dike 1) of the Générale desquarries et des mines/Kipushi (Gécamines/Kipushi). The samples were taken from two sites (OUA 1 and the cell five years) using a manual auger at a depth of 20 cm to 40 cm and packaged in a plastic bag before being analyzed in the laboratory. The Cu, Co, Ni, Pb, and Zn content was determined by an Inductively Coupled Plasma (ICP) spectrometer. The results showed that the soils sampled in the two cells were largely polluted by Cu, Zn, Pb, Mn, and Co. It is, therefore, imperative to see how to remedy the soil pollution of the Kachoma district.

Measurement report: The Fifth International Workshop on Ice Nucleation phase 1 (FIN-01): intercomparison of single-particle mass spectrometers

Abstract. Knowledge of the chemical composition and mixing state of aerosols at a single-particle level is critical for gaining insights into atmospheric processes. One common tool to make these measurements is single-particle mass spectrometry. There remains a need to compare the performance of different single-particle mass spectrometers (SPMSs). An intercomparison of SPMSs was conducted at the Aerosol Interaction and Dynamics in the Atmosphere (AIDA) chamber at the Karlsruhe Institute of Technology (KIT) in November 2014, as part of the first phase of the Fifth International Workshop on Ice Nucleation (FIN-01). In this paper we compare size distributions and mass spectra of atmospherically relevant particle types measured by five SPMSs. These include different minerals, desert and soil dusts, soot, bioaerosol (Snomax; protein granule), secondary organic aerosol (SOA), and SOA-coated mineral particles. Most SPMSs reported similar vacuum aerodynamic diameter (dva) within typical instrumental ranges from ∼100–200 nm (lower limit) to ∼2–3 µm (upper limit). In general, all SPMSs exhibited a wide dynamic range (up to ∼103) and high signal-to-noise ratio (up to ∼104) in mass spectra. Common spectral features with small diversities in mass spectra were found with high average Pearson's correlation coefficients, i.e., for average positive spectra ravg-pos=0.74 ± 0.12 and average negative spectra ravg-neg=0.67 ± 0.22. We found that instrument-specific detection efficiency (DE) was more dependent on particle size than particle type, and particle identification favored the use of bipolar, rather than monopolar, instruments. Particle classification from “blind experiments” showed that all instruments differentiated SOA, soot, and soil dust and detected subtle changes in the particle internal mixing but had difficulties differentiating among specific mineral types and dusts. This study helps to further understand the capabilities and limitations of the single-particle mass spectrometry technique in general and the specific performance of the instrument in characterizing atmospheric aerosol particles.

Silica Nanoparticles Tailored with a Molecularly Imprinted Copolymer Layer as a Highly Selective Biorecognition Element.

Molecularly imprinted silica nanoparticles (SP-MIP) are synthesized for the real-time optical detection of low-molecular-weight compounds. Azo-initiator-modified silica beads are functionalized through reversible addition-fragmentation chain transfer (RAFT) polymerization, which leads to efficient control of the grafted layer. The copolymerization of methacrylic acid (MAA) and ethylene glycol dimethacrylate (EDMA) on azo initiator-coated silica particles (≈100nm) using chain transfer agent (2-phenylprop-2-yl-dithiobenzoate) is carried out in the presence of a target analyte molecule (l-Boc-phenylalanine anilide, l-BFA). The chemical and morphological properties of SP-MIP are characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface analysis, and thermogravimetric analysis. Finally, SP-MIP is located on the gold surface to be used as a biorecognition layer on the surface plasmon resonance spectrometer (SPR). The sensitivity, response time, and selectivity of SP-MIP are investigated by three similar analogous molecules (l-Boc-Tryptophan, l-Boc-Tyrosine, and l-Boc-Phenylalanine) and the imprinted particle surface showed excellent relative selectivity toward l-Boc-Phenylalanine (l-BFA) (k=61), while the sensitivity is recorded as limit of detection=1.72×10-4m.

Surface Functionalization of Bamboo via Photo-Grafting Tannic Acid for Enhanced Silver Ion Loading Properties.

Photo-grafting is a gentle, simple, and precise approach to incorporating specific functional molecules for the surface functionalization of substrates. In this work, ultraviolet (UV)-induced tannic acid (TA) grafting onto the surface of bamboo was proposed as a viable strategy for functionalizing bamboo. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) clearly indicated that TA was successfully introduced to the bamboo's surface. The optimal conditions for the grafting reaction were determined to be 15 mM Methyl-2-benzoylbenzoate (BB), 30 mM TA, 20 min, and a pH = 8. Under these conditions, the amount of TA grafted onto the bamboo's surface was measured to be 19.98 μg/cm2. Results from Inductively Coupled Plasma (ICP) and Energy Dispersive Spectrometer (EDS) analyses showed that the silver ion loading capacity of tannic acid-grafted bamboo was significantly improved compared to that of raw bamboo and tannic acid-impregnated bamboo. Furthermore, the presence of TA grafted on the bamboo's surface exhibited a positive correlation with the loading of silver ions, indicating that grafted TA plays an important role in the surface functionalization of bamboo. We believe that photo-grafted TA may help generate multifunctional bamboo with diverse properties.

Technical note: Determining chemical composition of atmospheric single particles by a standard-free mass calibration algorithm

Abstract. The chemical composition of individual particles can be revealed by single-particle mass spectrometers (SPMSs). With higher accuracy in the ratio of mass to charge (m/z), more detailed chemical information could be obtained. In SPMSs, the conventional standard-based calibration methods (internal/external) are constrained by the inhomogeneity of ionization lasers and the finite focusing ability of the inlet system, etc.; therefore, the mass accuracy is restricted. In this study, we obtained the detailed and reliable chemical composition of single particles utilizing a standard-free mass calibration algorithm. In the algorithm, the characteristic distributions of hundreds of ions were concluded and collected in a database denoted as prototype. Each single-particle mass spectrum was initially calibrated by a function with specific coefficients. The range of coefficients was constrained by the magnitude of mass deviation to a finite vector space. To find the optimal coefficient vector, the conformity of each initially calibrated spectrum to the prototype dataset was assessed. The optimum calibrated spectrum was obtained with maximum conformity. For more than 98 % ambient particles, a 20-fold improvement in mass accuracy, from ∼ 10 000 ppm (integer) to ∼ 500 ppm (two decimal places), was achieved. The improved mass accuracy validated the determination of adjacent ions with a m/z difference ∼ 0.05 Th. Furthermore, atmospheric particulate trace elements that were poorly studied before are specified. The obtained detailed single-particle-level chemical information could help explain the source apportionment, reaction mechanism, and mixing state of atmospheric particles.

A simple spacecraft – vector intersection methodology and applications

Abstract Observations with spacecraft-mounted instruments are usually limited by their field-of-view and are often affected by the spacecraft's shadow or wake. Their extent though can be derived from the spacecraft's geometry. In this work we present a robust method for calculating the field-of-view as well as the extent of a spacecraft shadow and wake from readily available spacecraft CAD models. We demonstrate these principles on Cassini, where we give examples of vector-spacecraft intersection for the Cassini Langmuir Probe, as well the field-of-view of the Langmuir Probe and the Cassini Plasma Spectrometer.

Influence of ionic radius on the degree of extraction of rare earth metals during sorption by the interpolymer system AMBERLITE IR-120 –AВ-17-8

Studies have been carried out on the sorption of rare earth metal ions in solution using the interpolymer system Amberlite IR-120:AB-17-8. The purpose of the work is to search for conditions for maximum sorption of rare earth elements (Dy, Tb, Gd, Eu and Sm) from aqueous solutions using the effect of remote interaction of ion exchange resins. Methodology. The residual concentrations of rare earth ions were determined using an Optima 8300DV Duo inductively coupled plasma spectrometer. Results. The best sorption characteristics were determined by the interpolymer system at a ratio of 3:3. The residual concentration of rare earth elements in the solution was: Dy – 4.64 mg/l, Tb – 4.16 mg/l, Gd – 4.21 mg/l, Eu – 4.16 mg/l, Sm – 4.56 mg/l. The variations in the ionic radius of the ions chosen for the study are Dy3+<Tb3+<Gd3+<Eu3+<Sm3+. The degree of sorption of interpolymer system increased with increasing ionic radius of the metals. For dysprosium with the smallest ionic radius, the degree of sorption was η – 52%, and for terbium, gadolinium and europium it increased to η – 58%. For individual Amberlite IR-120 (6:0), the degree of sorption of terbium ions was 47%. Conclusion. The results of the study showed that the interpolymer system with a ratio of 3:3 has the best sorption activity. It has been established that the degree of sorption of interpolymer pairs increases with increasing order of the ionic radius of metals (Tb3+< Gd3+< Eu3+).

Biochemical and allelopathic features of Adonis vernalis, Allium ursinum, and Leucojum vernum in the M.M. Gryshko National Botanical Garden of the NAS of Ukraine

The article presents the results of a study on the content and dynamics of the accumulation of biogenic elements and brassinolides in plants of Adonis vernalis, Allium ursinum, and Leucojum vernum in Kyiv, Ukraine. Data is provided on allelopathic activity, content of macro- and microelements, phenolic compounds, and laccase activity in plants and the rhizosphere soil under the conditions of the M.M. Gryshko National Botanical Garden of the National Academy of Sciences of Ukraine (NBG). The plants from the collection of the NBG were used as objects of study in field experiments. The content of biogenic elements in plant tissues and soil was analyzed using an inductively coupled plasma spectrometer. The allelopathic analysis of soil was conducted using a direct bioassay method with Lepidium sativum seedlings as the test object. Phenolic compounds were extracted from the soil using the ion exchange (desorption) method. The content of brassinosteroids was measured spectrophotometrically at a wavelength of 450 nm. The content of laccase was measured spectrophotometrically at a wavelength of 530 nm.The results demonstrate that model plant species employ a wide range of physiological mechanisms throughout the vegetation period to enhance their resistance to abiotic factors. These mechanisms include maintaining potassium and calcium balance and utilizing hormonal compounds. Plants have been proven to have compensatory mechanisms in response to stress factors, substituting one biochemical marker of resistance with another. Both, brassinosteroids and silicon, contribute to the adaptive capacity of organisms.

Statistical Analysis of Mercury's Magnetotail Lobe Field Using MESSENGER Observations

AbstractThe magnetotail lobe region at Mercury is characterized by low plasma density and low magnetic field variability compared to the nightside magnetosheath and central plasma sheet. At Mercury, as well as other planets, lobe magnetic fields play a crucial role in storing and releasing magnetic flux in response to changing upstream solar wind conditions such as interplanetary magnetic field (IMF) orientation and solar wind dynamic pressure (Pdyn). This makes the region significant for studying the magnetospheric interaction with the intense solar wind conditions at Mercury's orbit. Here, we identify and analyze magnetotail lobe observations made by the Mercury Surface, Space Environment, Geochemistry and Ranging (MESSENGER) spacecraft during its 4 years orbital phase. We empirically determined a set of criteria using magnetometer (MAG) and the Fast Imaging Plasma Spectrometer instruments onboard MESSENGER to identify lobe magnetic field intervals. From 3,332 MESSENGER orbits, we identify 1,242 lobe field intervals. We derive an expression for the average lobe magnetic field strength in nanotesla with respect to radial distance downtail: Blobe(r) = (135 ± 8) * r(−2.1±0.3) + (31 ± 8). The lobe magnetic field exhibits both small‐scale (∼3 min) and orbit‐to‐orbit (∼8–12 hr) variability in magnetic field strength compared to this averaged field strength expression. The orbit‐to‐orbit variability in lobe field strength is not significantly correlated with estimated IMF orientation, but is directly correlated with Pdyn. Thus, our findings provide evidence for the pressure balance between the inward facing Pdyn on the nightside magnetopause and the outward facing magnetic pressure supplied by the lobes.

Spectroscopic Diagnostics of Radiation Reabsorption in Dense He Arc Plasmas

Observing the light emission from plasmas spectroscopically allows for the determination of key plasma parameters like electron temperature, density and external field. This method, known as plasma spectroscopy, serves as a non-intrusive diagnostic tool to study plasma dynamics. However, overlooking the impact of radiation reabsorption in the typical analytic model may compromise the accuracy of observed plasma behavior. This study addresses the influence of radiation reabsorption on plasma spectroscopic diagnosis, focusing on linear divertor simulators and plasma spectrometers designed for high-density Large Helical Device (LHD) plasmas, where optical thickness cannot be disregarded. The discussion delves into understanding the effects of radiation reabsorption in these observations.

Demonstration of a Multi‐Layer, Lithographically Manufactured Plasma Spectrometer

AbstractDevelopment of new plasma instruments is needed to enable constellation‐ and small satellite‐based missions. Key steps in the development pathway of ultra‐compact plasma instruments employing lithographically patterned wafers are the implementation of layer‐to‐layer electrical interconnects and demonstration of massively parallel measurements, that is, simultaneous measurements through multiple identical plasma analyzer structures. Here we present energy resolved measurements of electron beams using a 5‐layer stack of wafer‐based, energy‐per‐charge, electrostatic analyzers. Each layer has eight distinct analyzer groups that are comprised of multiple micron scale energy‐per‐charge analyzers. The process of fabricating the electrical interconnects between the layers is described and the measured energy resolution and the angular resolution compared to theoretical predictions. The measurements demonstrate successful operation of 400 micron scale analyzers operating in parallel.

Study on the preparation of ceramic membrane support and its Fe migration rule by high‐aluminum fly ash as raw material

AbstractIn order to reduce the cost of ceramic membrane support, ceramic membrane support was prepared using high‐aluminum fly ash as raw material, and its Fe migration rules during the preparation process are studied. The effects of sintering temperature, pore forming agent content, and binder content on the properties of support, such as porosity, pore size, bending strength and water flux have been investigated. The optimum contents of high‐aluminum fly ash, pore forming agent and binder in the ceramic membrane support are 95%, 4%, and 1% respectively, and its sintering temperature is 1300°C. The porosity, bending strength, pore size, and water flux of the prepared support are 37%, 22 MPa, 665 nm, and 2800 L/h·m2·MPa, respectively. X‐ray powder diffractometer, X‐ray fluorescence spectrometer, X‐ray photoelectron spectrometer, inductively coupled plasma spectrometer, transmission electron microscope, spherical aberration corrected transmission electron microscopy, and laser Raman spectroscopy were used to characterize the support and Fe existing morphology in it. The results show that the main phases of sintered support are mullite, corundum, and silica. Massive mullite is produced when the sintering temperature reaches 1200°C. The content of mullite increases with increasing sintering temperature. About 7.7 % content of total Fe in the support exists in the form of Fe2O3. About 92.3% content of total Fe is dissolved into mullite. Fe is evenly distributed in mullite, and it is enriched at the grain boundary by element segregation. Fe in mullite is difficult to dissolve under strong acid conditions, so its stability is very strong.

Head-on collision of ion-acoustic (modified) Korteweg–de Vries solitons in Saturn's magnetosphere plasmas with two temperature superthermal electrons

In view of the recent observations by plasma science-spacecraft-voyager and Cassini plasma spectrometer of Saturn's magnetosphere, the interaction between two counter-propagating ion-acoustic (IA) solitons is studied in an unmagnetized plasma consisting of warm adiabatic ions in addition to hot and cold electrons following kappa distribution. The head-on collision of the IA solitons is investigated using the extended Poincare–Lighthill–Kuo technique. Since this model supports both compressive and rarefactive solitons, therefore, the soliton collisions for both Korteweg–de Vries (KdV) and the modified KdV (mKdV) equations are investigated. The corresponding phase shifts after the collision for both these equations are also derived and examined. Furthermore, the effects of different plasma parameters (corresponding to Saturn's magnetosphere), including superthermality, density, and temperature on the colliding soliton profiles and their phase shifts, are examined. It is concluded that the phase shift is smaller when both hot and cold electrons are Maxwellian by comparison with the superthermal case.

Mineral Bioaccessibility and Antioxidant Capacity of Protein Hydrolysates from Salmon (Salmo salar) and Mackerel (Scomber scombrus) Backbones and Heads

Information on the bioaccessibility of minerals is essential to consider a food ingredient as a potential mineral fortifier. In this study, the mineral bioaccessibility of protein hydrolysates from salmon (Salmo salar) and mackerel (Scomber scombrus) backbones and heads was evaluated. For this purpose, the hydrolysates were submitted to simulated gastrointestinal digestion (INFOGEST method), and the mineral content was analyzed before and after the digestive process. Ca, Mg, P, Fe, Zn, and Se were then determined using an inductively coupled plasma spectrometer mass detector (ICP-MS). The highest bioaccessibility of minerals was found in salmon and mackerel head hydrolysates for Fe (≥100%), followed by Se in salmon backbone hydrolysates (95%). The antioxidant capacity of all protein hydrolysate samples, which was measured by Trolox Equivalent Antioxidant Capacity (TEAC), increased (10-46%) after in vitro digestion. The heavy metals As, Hg, Cd, and Pb were determined (ICP-MS) in the raw hydrolysates to confirm the harmlessness of these products. Except for Cd in mackerel hydrolysates, all toxic elements were below the legislation levels for fish commodities. These results suggest the possibility of using protein hydrolysates from salmon and mackerel backbones and heads for food mineral fortification, as well as the need to verify their safety.

Antibacterial activity of multi-metallic (Ag–Cu–Li) nanorods with different metallic combination ratios against Staphylococcus aureus

ObjectiveBecause of the need to extensively study the synergistic activity of metallic nanoparticles, this study aimed to evaluate the antibacterial activity of mixed metallic nanoparticles, made by differing the weight mixing ratio. We prepared multi-metallic nanorods (NRs) by chemical reduction method, with different ratio combinations of silver Ag and copper Cu, two main batches of nanorods were produced: bimetallic mix made only of Ag–Cu, and trimetallic mix made of Ag–Cu and lithium Li, AgCu NRs and AgCuLi NRs respectively. NaOH was used in the synthesis for the co-reduction of salt precursors. Ag percentage was varied from 10 to 90% in bimetallic NRs but in the trimetallic NRs, which has a fixed ratio of Li (10%), the percentage of silver precursor was from 10 to 80%. The presence of metals was confirmed by energy dispersive X-rays (EDX) analysis. Ion release was detected using inductively coupled plasma spectrometer (ICP) and the values showed that NRs are effective source for ion supply for up to 24 h. The antibacterial activity of metallic NRs was tested against Staphylococcus aureus using Bauer Kirby method.ResultsThe bi-synergistic mix of Ag and Cu generates more ions than the tri-synergistic mix of Ag, Cu, and Li. Nevertheless, the later was more efficient and showed higher antibacterial activity at lower concentrations. This effect is less likely to be attributed to modality of ion release. Indeed, the results of our work suggest that besides ion release, alloyed nanorods themselves are toxic and the trimetallic mix exhibited more biocidal activity, specifically at Ag salt concentrations of 30%, 50% and 70%.

On Current Sheets and Associated Density Spikes in Titan’s Ionosphere as Seen From Cassini

AbstractThe Cassini spacecraft made in‐situ measurements of Titan's plasma environment during 126 close encounters between 2004 and 2017. Here we report on observations from the Radio and Plasma Waves System/Langmuir probe instrument (RPWS/LP) from which we have observed, primarily on the outbound leg, a localized increase of the electron density by up to 150 cm−3 with respect to the background. This feature, appearing as an electron density spike in the data, is found during 28 of the 126 flybys. The data from RPWS/LP, the electron spectrometer from the Cassini Plasma Spectrometer package , and the magnetometer is used to calculate electron densities and magnetic field characteristics. The location of these structures around Titan with respect to the nominal corotation direction and the sun direction is investigated. We find that the electron density spikes are primarily observed on the dayside and ramside of Titan. We also observe magnetic field signatures that could suggest the presence of current sheets in most cases. The density spikes are extended along the trajectory of the spacecraft with the horizontal scale of ∼537 ± 160 km and vertical scale ∼399 ± 163 km. We suggest that the density spikes are formed as a result of the current sheet formation.

Characterization of Foreshock Plasma Populations at Mercury

AbstractObservations of foreshock plasma populations at Mercury are presented utilizing measurements from the Fast Imaging Plasma Spectrometer aboard the Mercury Surface, Space Environment, Geochemistry, and Ranging spacecraft. The magnetosphere and foreshock system at Mercury exists in a unique parameter space, due to the planet's relatively weak magnetic dipole and the proximity of its orbit to the Sun. Previous investigations have therefore questioned whether there is sufficient free energy at Mercury to generate foreshock populations, due to the small spatial scale of its bow shock. The observations presented in this work show that field‐aligned beam and diffuse populations similar to those seen in the terrestrial foreshock are able to form upstream of the Hermean bow shock. The observed populations are organized by the bow shock geometry, and are associated with magnetic wave activity previously detected in Mercury's foreshock with corollaries to the terrestrial foreshock.

A review of instrument techniques to measure magnetospheric cold electrons and ions

A review of the instruments and techniques to directly measure the full distributions of the cold-ion and cold-electron populations in the magnetosphere is presented. Relatively few studies have focused on the cold plasma populations of the magnetosphere due to difficulties associated with obtaining measurements. The cold particle populations are defined here as those with total energy approximately <100 eV which is an energy range for which measurements are difficult (regardless of species), but which often make up the bulk of the plasma density. These populations have known and suspected impacts on the structure and dynamics of the magnetosphere but to date have not yet been measured adequately. The lack of accurate measurements cold ion and electron populations through the magnetosphere makes closure of these science questions extremely difficult if not impossible. Reaching closure will require innovations in plasma spectrometers and associated techniques required to obtain high-fidelity measurements of the cold ion and electron populations in the magnetosphere. This paper seeks to review the instruments and techniques that have been used to date and present possible options for future missions.

The neutron dose equivalent rate measurements by R3DR/R2 sp ectrometers on the international space station

The data from two Bulgarian-German instruments with the basic name “Radiation Risk Radiometer-Dosimeter” (R3D) are discussed. The R3DR instrument worked inside the ESA EXPOSE-R facility (2009–2010), while R3DR2 worked inside the ESA EXPOSE-R2 facility (2014–2016). Both were outside the Russian Zvezda module on the International Space Station (ISS). The data from both instruments were used for calculation of the neutron dose equivalent rate. Similar data, obtained by the Russian “BTNNEUTRON” instrument on the ISS are used to benchmark the R3DR/R2 neutron dose equivalent rate. The analisys reveals that the “BTNNEUTRON” and R3DR/R2 values are comparable both in the equatorial and in the South Atlantic Anomaly (SAA) regions. The R3DR/R2 values are smaller than the “BTNNEUTRON” values in the high latitude regions. The comparison with the Monte Carlo simulations of the secondary galactic cosmic rays (GCR) neutron ambient dose equivalent rates (El-Jaby and Richardson, 2015, 2016) also shows a good coincidence with the R3DR/R2 spectrometer data obtained in the equatorial and high latitude regions.