Solid Samples Research Articles

Ensuring the Quality of the Analytical Process in a Research Laboratory

This paper discusses approaches for verification of methods of measurements of chemical and physical characteristics of specific samples. The limitations of well-known approaches are discussed. Some examples of alternatives are given to demonstrate specific issues encountered in the research laboratory analyzing new materials or characterizing new properties of materials. Application of sequential procedure using lower quantities of samples and reagents is presented. A standard addition to solid samples is discussed. The approach of control charts for estimation of method uncertainty for determination of plant available phosphorus is presented. The method comparison is applied as an approach to verification of alkaline reactivity by inductively coupled plasma–optical emission spectroscopy (ICP-OES) measurement, as well as density of newly synthesized chalcogenide glass materials. The presented examples demonstrated that alternative approaches are needed in order to verify the methods applied due to the great variety of activities and corresponding tasks in a research laboratory.

A novel 5,10,15,20-tetrakis-(4-(triazol-1-yl)phenyl)porphyridine compound: Crystal structure, photophysical properties and TDDFT calculations

A novel 5,10,15,20-tetrakis-(4-(triazol-1-yl)phenyl)porphyridine compound, namely, Zn[5,10,15,20-tetrakis-(4-(triazol-1-yl)phenyl)porphyridine] (hereafter tagged as 1) was synthesized through a solvothermal reaction with mixed solvents at 413 K. The X-ray single-crystal structure of compound 1 is featured as a two-dimensional (2D) layer-like structure with the zinc ion located at the center of the 5,10,15,20-tetrakis-(4-(triazol-1-yl)phenyl)porphyridine. The macrocycle of the 5,10,15,20-tetrakis-(4-(triazol-1-yl)phenyl)porphyridine is coplanar. The zinc ion has six coordination and coordinates with three porphyridines. The photoluminescence spectra of compound 1 with DMF solution reveal that it shows upconversion red photoluminescence. The time-dependent density functional theory (TDDFT) calculation confirms that this upconversion red photoluminescence originated from the MLCT process (metal to ligand charge transfer). The CCT (Correlated Color Temperature) is 2200 K and the CIE (Commission Internationale de I’Éclairage) chromaticity coordinate is (0.6311, 0.3595) for compound 1. The UV-vis diffuse reflectance curve measured with a solid state sample reveals that compound 1 possesses a 2.75 eV band gap.

Comparison of laser-induced breakdown spectroscopy (LIBS) and ICP analysis results for measuring Pb and Zn in soil

Context Laser-induced breakdown spectroscopy (LIBS) is a rapid, multielement analytical technique. It is particularly suitable for the qualitative and quantitative analyses of heavy metals in solid samples. Aims To validate the technique, the LIBS data were compared with the data obtained via conventional inductively coupled plasma (ICP) spectroscopy for the same soil samples. Methods In this study, standard and unknown soil samples from contaminated areas were prepared and fixed to an adhesive tape for LIBS analysis. The soils were also digested with acids for ICP analysis. The emission intensity of one selected line for each of the two analytes, i.e. lead (Pb) and zinc (Zn), was normalised to the background signal and plotted as a function of the concentration values previously determined via ICP analysis. Key results The data demonstrated good linearity for the calibration lines drawn, and the correlation between the ICP and LIBS data was confirmed by the satisfactory agreement between the corresponding values. Conclusions The concentration coefficient of determination (R2) between LIBS and ICP-aqua regia digestion analysis or ICP-total digestion analysis were >0.86 and >0.89 for Pb and Zn, respectively. The total analysis time for the LIBS method was 310 min, which was 54.40% shorter than that for the ICP method (680 min). Implications Consequently, LIBS can be used to measure Pb and Zn in soils without any chemical preparation.

Differential metamaterial based sensor for solid dielectric characterization with improved sensitivity

Purpose The purpose of this study is to introduce a new type of sensor which uses microwave metamaterials and direct-coupled split-ring resonators (DC-SRRs) to measure the dielectric properties of solid materials in real time. The sensor uses a transmission line with a bridge-type structure to measure the differential frequency, which can be used to calculate the dielectric constant of the material being tested. The study aims to establish an empirical relationship between the dielectric properties of the material and the frequency measurements obtained from the sensor. Design/methodology/approach In the proposed design, the opposite arm of the bridge transmission line is loaded by DC-SRRs, and the distance between DC-SRRs is optimized to minimize the mutual coupling between them. The DC-SRRs are loaded with the material under test (MUT) to perform differential permittivity sensing. When identical MUT is placed on both resonators, a single transmission zero (notch) is obtained, but non-identical MUTs exhibit two split notches. For the design of differential sensors and comparators based on symmetry disruption, frequency splitting is highly useful. Findings The proposed structure is demonstrated using electromagnetic simulation, and a prototype of the proposed sensor is fabricated and experimentally validated to prove the differential sensing principle. Here, the sensor is analyzed for sensitivity by using different MUTs with relative permittivity ranges from 1.006 to 10 and with a fixed dimension of 9 mm × 10 mm ×1.2 mm. It shows a very good average frequency deviation per unit change in permittivity of the MUTs, which is around 743 MHz, and it also exhibits a very high average relative sensitivity and quality factor of around 11.5% and 323, respectively. Originality/value The proposed sensor can be used for differential characterization of permittivity and also as a comparator to test the purity of solid dielectric samples. This sensor most importantly strengthens robustness to environmental conditions that cause cross-sensitivity or miscalibration. The accuracy of the measurement is enhanced as compared to conventional single- and double-notch metamaterial-based sensors.

Microbial induced wettability alteration with implications for Underground Hydrogen Storage

Characterization of the microbial activity impacts on transport and storage of hydrogen is a crucial aspect of successful Underground Hydrogen Storage (UHS). Microbes can use hydrogen for their metabolism, which can then lead to formation of biofilms. Biofilms can potentially alter the wettability of the system and, consequently, impact the flow dynamics and trapping mechanisms in the reservoir. In this study, we investigate the impact of microbial activity on wettability of the hydrogen/brine/rock system, using the captive-bubble cell experimental approach. Apparent contact angles are measured for bubbles of pure hydrogen in contact with a solid surface inside a cell filled with living brine which contains sulphate reducing microbes. To investigate the impact of surface roughness, two different solid samples are used: a “rough” Bentheimer Sandstone sample and a “smooth” pure Quartz sample. It is found that, in systems where buoyancy and interfacial forces are the main acting forces, the impact of biofilm formation on the apparent contact angle highly depends on the surface roughness. For the “rough” Bentheimer sandstone, the apparent contact angle was unchanged by biofilm formation, while for the smooth pure Quartz sample the apparent contact angle decreased significantly, making the system more water-wet. This decrease in apparent contact angle is in contrast with an earlier study present in the literature where a significant increase in contact angle due to microbial activity was reported. The wettability of the biofilm is mainly determined by the consistency of the Extracellular Polymeric Substances (EPS) which depends on the growth conditions in the system. Therefore, to determine the impact of microbial activity on the wettability during UHS will require accurate replication of the reservoir conditions including surface roughness, chemical composition of the brine, the microbial community, as well as temperature, pressure and pH-value conditions.

The value of contrast-enhanced ultrasound in percutaneous biopsy of retroperitoneal masses.

To evaluate the diagnostic yield of contrast-enhanced ultrasound (CEUS)-guided biopsy of retroperitoneal masses (RMs). Between 2006 and 2023, 87 patients presented at our US center for biopsy of an RM. In all biopsies, CEUS was performed prior to the intervention. The technical success rate of biopsy, the presence of diagnostic tissue in solid tumor biopsy samples, the accuracy of the biopsy and the occurrence of post-interventional complications were evaluated. A US-guided biopsy could be conducted in 84/87 cases (96.6%). In 3/87 cases (3.4%), US-guided biopsy was impossible because the planned needle path was obstructed by vital structures. Of 84 lesions, 80 (95.2%) were solid lesions, and 4 (4.8%) were lesions containing fluid. In all solid tumors, 80/80 (100%), diagnostic vital tissue was successfully obtained. CEUS-guided biopsy showed a sensitivity of 93.2%, a specificity of 100%, a positive predictive value of 100%, a negative predictive value of 72.2%, and a diagnostic accuracy of 94.2% for the differentiation between malignant and benign RMs. In one of the 84 cases (1.2%), there was a complication of postinterventional abdominal pain. Percutaneous CEUS-guided biopsy is a safe procedure with a high diagnostic yield and a low complication rate.

High temperature nanoindentation of (U,Ce)O2 compounds

Continuing to refine our knowledge of the evolving mechanical properties of nuclear fuel over the entire fuel service cycle is necessary to understand the pellet-clad mechanical interaction that occurs in the fuel rods during the operation. A challenge with measuring the mechanical properties of irradiated fuels is their high levels of radioactivity that usually require the use of hot cells making testing time consuming and expensive. Nanoindentation based techniques can be employed on minute volumes of material to measure mechanical properties, including Young’s modulus, hardness, and creep stress exponents. Increasing the mixed oxide fuels mechanical properties database through a variety of testing techniques should enhance modelers’ abilities to predict failure mechanisms in the fuel/clad interface. A current challenge to testing mixed oxide fuels is the plutonium component in the fuel. Mixed fluorite type oxides with ceria (CeO2) can be used as a surrogate for mixed oxide fuels. In this study, (U,Ce)O2 solid solutions samples are used to develop elevated temperature nanoindentation and nanoindentation creep testing methods for use on mixed oxide fuels. Nanoindentation testing was performed on 3 separate (Ux-1,Cex)O2 compounds ranging from x equals 0.1 to 0.3 in equal steps at temperatures up to 800 °C: their Young’s modulus, hardness, and creep stress exponents were evaluated. The Young’s modulus decreases in the expected linear manner while the hardness decreases in the expected exponential manner. The nanoindentation creep experiments at 800 °C give stress exponent values, n = 4.7–6.9, that suggests dislocation motion as the deformation mechanism.

Development of magnetic matrix solid phase dispersion method for the extraction of crystal violet and rhodamine B from sediments based on magnetic ZIF-8 and a deep eutectic solvent

A magnetic matrix solid phase dispersion (MSPD) method based on magnetic ZIF-8 (SDS@MZIF-8) and a deep eutectic solvent was developed and used to the extraction of crystal violet and rhodamine B in lake sediments. SDS@MZIF-8 was prepared and used as the extraction sorbent and dispersant in MSPD. The magnetic property of MZIF-8 facilitated the recovery of the extraction sorbent after the blending step. Hydrophilic deep eutectic solvents were prepared and used as efficient green dispersing solvents in MSPD. The use of magnetic sorbent in MSPD is simple and fast, eliminating some additional steps commonly used in the classical MSPD and shortening the extraction time. The parameters influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, the intra- and inter-day relative standard deviations were less than 4.9 %. The linearity ranged from 2-400 µg g−1 with coefficients of determination higher than 0.9943. The detection and quantification limits of RB and CV varied between 0.3–0.5 μg g−1 and 1.0–1.8 μg g−1, respectively. Finally, the developed method was applied to the analysis of RB and CV in the sediment samples. The recoveries ranged from 93.2 to 107.3 % and the relative standard deviations ranged from 0.8 to 4.9 %. The results suggest a high potential use of the proposed method to determine the organic pollutants in solid samples. Compared with the conventional MSPD extraction technique, the developed method considerably reduced the sample and solvent consumption, offering important environmental benefits.

Quantification of Quaternary Ammonium Compounds by Liquid Chromatography-Mass Spectrometry: Minimizing Losses from the Field to the Laboratory

Quaternary Ammonium Compounds (QACs) are widely used in household, medical and industrial settings. As a consequence, they are ubiquitously found in the environment. Although significant efforts have been put into the development of sensitive and reproducible analytical methods, much less effort has been dedicated to the monitoring of QACs upon sample storage and sample preparation. Here we studied the effect of storage, concentration, and extraction procedures on the concentrations of QACs in samples. Thirteen QACs selected amongst benzalkonium compounds (BACs), dialkyldimethylammonium compounds (DADMACs) and alkyltrimethylammonium compounds (ATMACs) were quantified in aqueous and solid samples using LC-MS/MS. Most QACs adsorbed on container walls could be recovered using a short washing step with MeOH containing 2% v/v formic acid. Concentrations of QACs from aqueous solutions using solid phase extraction (SPE) with Strata-X cartridges and elution with acidified MeOH utilized to wash the emptied containers gave highly satisfactory recoveries (101-111%). Good recoveries (89-116%) were also obtained when extracting a spiked organic-rich synthetic soil using accelerated solvent extraction (ASE) with acidified MeOH at low solid/solvent ratio (0.4 g/20 mL). Applying the recommended methodologies to real samples collected from a Canadian wastewater treatment plant (WWTP) gave QAC concentrations in the ranges of 0.01-30 µg/L, < 1.2 µg/L, and 0.05-27 mg/kg for the influent, effluent and biosolids samples, respectively.

Depth profile analysis and high-resolution surface mapping of lithium isotopes in solids using laser-induced breakdown spectroscopy (LIBS)

Lithium isotopic analysis is of interest in various fields from biology to energy. In addition to analytical methods commonly used for that purpose, a new complementary method for determining the spatial resolution of isotopic ratio in solid samples was previously developed: laser induced self-reversal isotopic spectrometry (LIBRIS), derived from laser-induced breakdown spectroscopy (LIBS). In this paper, we present a proof of concept of fast spatially-resolved quantitative isotopic analysis of lithium by LIBS both in depth (z resolution) and in configuration of high-resolution surface mapping (x and y resolution). First, a depth profile measurement where a 9% relative uncertainty on the 6Li isotopic ratio and 0.74 μm depth resolution is obtained. Then, we introduce the first high-resolution lithium isotopic mapping obtained by LIBS with a 3.3 μm lateral resolution and a typical 40% relative uncertainty on the 6Li isotopic ratio is obtained. Those results could be applied in the future to a large number of solid samples where fast information on the lithium isotopic distribution are needed, for instance in solid-state batteries development.

Study on the grain evolution of austenitic steel for nuclear power during hot working based on large area EBSD mapping

To address the issue of non-standard grain sizes and difficult control of uniformity in the manufacturing of large, complex-shaped nuclear power pipelines. In this paper, double wedge-shaped samples of X2 CrNiMo 18.12 (CN) austenitic stainless steel were hot deformed at 1000 °C, 1100 °C, and 1180 °C to obtain deformation samples with a gradient strain, and the deformation sample at 1180 °C was subjected to solid solution treatment at 1060 °C × 4 h (water quenching; the measured cooling rate of water cooling was approximately 4400 °C/min). Large-area electron backscattered diffraction mapping technology was used to characterize the 80 mm × 5 mm full-area range of samples. The initiation sequence of various dynamic recrystallization mechanisms and the grain evolution under continuous effective strain conditions at a hot deformation temperature of 1000–1180 °C were investigated. The influence of the hot deformation process parameters on the grains after solid solution treatment was examined, the process interval for the generation of severe mixed grains was determined. The results show that the recrystallization behavior of X2 CrNiMo 18.12 (CN) austenitic stainless steel is mainly determined by a combination of recrystallization mechanisms dominated by discontinuous dynamic recrystallization, supplemented by continuous dynamic recrystallization, twinning-induced dynamic recrystallization, and geometrical dynamic recrystallization during the hot deformation process at 1000–1180 °C. The effective strain intervals of the solid solution sample that produces severely mixed grains are in the range of 0.11–0.22 mm/mm, with the probability of producing severely mixed grains with an effective strain in the range of 0.13–0.14 mm/mm reaching 74%.

Combined leaching and steam explosion pretreatment of lignocellulosic biomass for high quality feedstock for thermochemical applications

A novel pretreatment approach was developed in the present study to simultaneously reduce the content of inorganic troubling elements (TEs) and improve biomass energy density, i.e., combined leaching and steam explosion (SE) pretreatment with mechanical pressing. Three different high-ash-containing biomass feedstocks were studied – wheat straw (WS), spruce bark (SB), and empty fruit bunches of oil palm (EFB). Before studying the combined pretreatment, the impact of individual pretreatment was determined in-depth on biomass composition and ash-transformation behaviour. In leaching pretreatment, the effect of leaching with steam explosion condensate (SEC), dilute acetic acid and water was studied comprehensively. The solid (raw and treated) and liquid samples (leachate, SEC, hydrolysate) were characterized for a detailed comparative analysis. The ash-fusion and −transformation behaviour of raw and pretreated biomass was studied in-depth using advanced multicomponent thermodynamic equilibrium modelling (TEM) and push-rod dilatometry. After combined pretreatment, a considerably high reduction in TEs content was noted: 82–98 % K, 93–99 % Na, 80–99 % Cl, 34–90 % S, 3–77 % Mg, ash 43–63 %, 26–67 % P, and 19–63 % Ca. Simultaneously, heating values of all three feedstocks increased by 1.3–2.3 MJ/kg, reaching up to 20–22 MJ/kg. TEM results reveal that much lesser amounts of molten slag and volatile inorganic compounds were formed in pretreated samples compared to raw and SE biomass, such as K2Si5MgO12, KCl, KPMgO4, K2Si2O5, CaSiO3, and MgSiO3 in WS; Na2CO3, K2CO3, K2CaC2O6, KPMgO4, and CaCO3 in SB. Due to higher energy density and lower propensity towards ash-related issues, combined pretreated WS and SB have a high potential to be used in large-scale thermochemical applications.

UBE2C: A pan-cancer diagnostic and prognostic biomarker revealed through bioinformatics analysis.

The diverse and complex attributes of cancer have made it a daunting challenge to overcome globally and remains to endanger human life. Detection of critical cancer-related gene alterations in solid tumor samples better defines patient diagnosis and prognosis, and indicates what targeted therapies must be administered to improve cancer patients' outcome. To identify genes that have aberrant expression across different cancer types, differential expressed genes were detected within the TCGA datasets. Subsequently, the DEGs common to all pan cancers were determined. Furthermore, various methods were employed to gain genetic alterations, co-expression genes network and protein-protein interaction (PPI) network, pathway enrichment analysis of common genes. Finally, the gene regulatory network was constructed. Intersectional analysis identified UBE2C as a common DEG between all 28 types of studied cancers. Upregulated UBE2C expression was significantly correlated with OS and DFS of 10 and 9 types of cancer patients. Also, UBE2C can be a diagnostic factor in CESC, CHOL, GBM, and UCS with AUC = 100% and diagnose 19 cancer types with AUC ≥90%. A ceRNA network constructed including UBE2C, 41 TFs, 10 shared miRNAs, and 21 circRNAs and 128 lncRNAs. In summary, UBE2C can be a theranostic gene, which may serve as a reliable biomarker in diagnosing cancers, improving treatment responses and increasing the overall survival of cancer patients and can be a promising gene to be target by cancer drugs in the future.

Effect of volatile compounds produced by Weissella cibaria BWL4 on Botrytis cinerea infection in fruit and complete genome sequence analysis of BWL4

Botrytis cinerea, one of the most harmful pathogenic fungi, causes significant postharvest decay in fruit. In this study, the effects of Weissella cibaria BWL4 on B. cinerea and the gray mold in grape and kiwifruit were evaluated. Additionally, the genome of an antagonistic bacterium BWL4 was sequenced. Results showed that the application of BWL4 inhibited B. cinerea infection in grape and kiwifruit. BWL4 produced antifungal volatile substances against B. cinerea. A gas chromatography–mass spectrometry of solid phase microextraction samples (SPME-GC-MS) analysis showed that BWL4 produced 54 volatiles. Among these volatiles, furfural, 2,6-dimethyl-pyrazine, dimethyl trisulfide, 2-pentyl furan, 2-ethyl hexanol, hexamethyl-cyclotrisiloxane, dodecamethyl-cyclohexasiloxane, 2,4-di-tert-butylphenol, and butylated hydroxytoluene, exhibited antifungal activity against B. cinerea, with MICs of 0.8 g L−1, 0.2 g L−1, 0.9 g L−1, 5 g L−1, 0.4 g L−1, 8 g L−1, 8 g L−1, 80 mg L−1, and 2 g L−1, respectively. In vivo assay showed that these compounds inhibited the disease development in kiwifruit. These compounds except dimethyl trisulfide can also inhibit gray mold in grape. The genome of W. cibaria BWL4 consists of a circular chromosome of 2.42 Mb and 6 plasmids. The genome size is 2.53 Mb, encoding 2327 putative genes. Several genes involved in the biosynthesis of some antifungal volatiles and 17 genes associated with biocontrol were identified. These results suggested that W. cibaria BWL4 can be considered as an effective biological control agent for the postharvest management of B. cinerea infection.

Occurrence and abundance of microplastics and plasticizers in landfill leachate from open dumpsites in Sri Lanka

Occurrence and abundance of microplastics and plasticizers in landfill leachate from open dumpsites in Sri Lanka

Physicochemical characteristics of grease-trap wastewater with different potential mechanisms of FOG solid formation, separation, and accumulation inside grease traps

This work investigates the physicochemical characteristics of grease-trap wastewater discharged from a large community market. It proposes potential mechanisms of fat, oil, and grease (FOG) solid formation, separation, and accumulation inside grease traps. Sixty-four samples, i.e., the floated scum, suspended solid-liquid wastewater, and settled sludge, were collected from the grease-trap inlet and outlet chambers. A lower pH of 5-6 at 25-29°C inside the grease trap than those reported under the sewer conditions (pH 6-7) was revealed. A significant difference in solid and dissolved constituents was also discovered between the inlet and outlet chambers, indicating that the baffle wall could affect the separation mechanism. The sludge samples had 1.5 times higher total solids (TS) than the scum samples, i.e., 0.225 vs. 0.149 g g−1 TS, revealing that the sludge amount impacted more significantly the grease trap capacity and operation and maintenance. In contrast, the scum samples had 1.4 times higher volatile solids (VS) than the sludge samples, i.e., 0.134 vs. 0.096 g g−1 VS, matching with the 64.2 vs. 29.7% of carbon content from CHN analysis. About 2/3 of the free fatty acids (FFAs) with palmitic acids were the primary saturated FFAs, while the remaining 1/3 of unsaturated FFAs were found in the solid and liquid samples. Although up to 0.511 g g−1 FOG can be extracted from the scum samples, none from the sludge samples. More diverse minerals/metals other than Na, Cl, and Ca were found in the sludge samples than in the scum samples. Grease-trap FOG solids and open drain samples exhibited similar physicochemical properties to those reported in the literature. Four potential mechanisms (crystallization, emulsification, saponification, and baffling) were presented. This work offers insights into the physicochemical properties of grease-trap wastewater that can help explore its FOG solid formation, separation, and accumulation mechanisms inside a grease trap.

Experimental study on the micro-mechanical parameters of Ni-based single-crystal superalloys using nanoindentation and element distribution analysis

Ni-based single-crystal superalloys are normally prepared by directional solidification. Due to different solidification sequences, Ni-based single-crystal superalloys exhibit a typical dendritic arm structure, and the element segregation in the dendritic arm can affect the high temperature mechanical properties of the alloy. Solid solution treatment has a certain extent to reduce the inter-dendritic and dendritic arm between the concentrations of the elements, thereby changing the alloy micro-nano view parameters to improve the high temperature mechanical properties of the alloy. In this study, nanoindentation experiments were carried out on the inter-dendritic and dendritic arm of the cast and solid solution samples. The micromechanical parameters were calculated. The amounts of changes in elemental concentration were discussed with the results of the energy dispersive spectroscopy and electron probe microanalysis, so as to analyse the relationship between the micromechanical parameters and the changes in elemental concentration. The results show that solid solution treatment has a significant impact on the elastic modulus, with an increase of 114.7% of the inter-dendritic region and an increase of 142.7% of the dendritic arm. However, solid solution treatment has little effect on the hardness, with no significant change in the hardness of the inter-dendritic region and an increase of 43.86% of the dendritic arm. Solid solution treatment has a more significant effect on improving the segregation behavior of Al and Co elements, with the segregation coefficients of Al and Co elements in the inter-dendritic region decreasing and increasing by 36% and 19%, and the segregation coefficients of Al and Co elements in the dendritic arm region decreasing and increasing by 29% and 34%.

A mass balance approach for quantifying the role of natural decay and fate mechanisms on SARS-CoV-2 genetic marker removal during water reclamation.

The recent SARS-CoV-2 outbreak yielded substantial data regarding virus fate and prevalence at water reclamation facilities (WRFs), identifying influential factors as natural decay, adsorption, light, pH, salinity, and antagonistic microorganisms. However, no studies have quantified the impact of these factors in full scale WRFs. Utilizing a mass balance approach, we assessed the impact of natural decay and other fate mechanisms on genetic marker removal during water reclamation, through the use of sludge and wastewater genetic marker loading estimates. Results indicated negligible removal of genetic markers during P/PT (primary effluent (PE) p value: 0.267; preliminary and primary treatment(P/PT) accumulation p value: 0.904; and thickened primary sludge (TPS) p value: 0.076) indicating no contribution of natural decay and other fate mechanisms toward removal in P/PT. Comparably, adsorption and decomposition was found to be the dominant pathway for genetic marker removal (thickened waste activated sludge (TWAS) log loading 9.75 log10 GC/day); however, no estimation of log genetic marker accumulation could be carried out due to high detections in TWAS. PRACTITIONER POINTS: The mass balance approach suggested that the contribution of natural decay and other fate mechanisms to virus removal during wastewater treatment are negligible compared with adsorption and decomposition in P/PT (p value: 0.904). During (P/PT), a higher viral load remained in the (PE) (14.16 log10 GC/day) compared with TPS (13.83 log10 GC/day); however, no statistical difference was observed (p value: 0.280) indicting that adsorption/decomposition most probably did not occur. In secondary treatment (ST), viral genetic markers in TWAS were consistently detected (13.41 log10 GC/day) compared with secondary effluent (SE), indicating that longer HRT and the potential presence of extracellular polymeric substance-containing enriched biomass enabled adsorption/decomposition. Estimations of total solids and volatile solids for TPS and TWAS indicated that adsorption affinity was different between solids sampling locations (p value: <0.0001).

A Univariate Optimization Strategy for Pre-concentration of Cobalt(II) in Various Matrixes by a DLLME before Analysis Using FAAS

A procedure based on dispersive liquid-liquid microextraction (DLLME) for cobalt (Co) quantification in an Iraqi environmental matrix by flame atomic absorption spectroscopy (FAAS) was applied in this work. A case-study approach was chosen to obtain further in-depth information on the Co levels and to evaluate the effectiveness of N-salicylideneaniline (SAN) as a complexing agent for pre-concentration and extraction of Co. An univariate strategy was utilized to achieve the optimum extraction conditions. The estimated limits of detection (LOD) and quantification (LOQ) under optimum conditions were 1.04 and 3.47 µg L−1, respectively. The results achieved by the proposed system were compared with those using the microwave digestion/graphite furnace atomic absorption spectrometer (MWD/GF-AAS) for digest samples and also for some water samples (Direct GF-AAS). The proposed procedure was applied for analyzing eleven environmental samples. The detectable Co levels for water samples ranged from 0.72 to 4.30 µg L−1 with a relative standard deviation of 3.7–8.8%, while the concentration for solid samples ranged from 0.17–4.51 µg g−1 (2.4–11.8 RSD %). DLLME/FAAS proposed procedure is effective, simple, and has the benefit of minimizing the organic solvent consumption by a few microliters, which results in little waste.

Refractory High‐Entropy Alloys Produced from Elemental Powders by Severe Plastic Deformation

A comparative investigation of two fundamentally different approaches for the synthesis, microstructure evolution, and mechanical properties of the refractory high‐entropy alloys (RHEA) HfNbTaTiZr and HfNbTiZr is performed. The two methods comprises conventional arc (button) melting and a powder route based on mechanical alloying and consolidation via severe plastic deformation. In particular, blended elemental powder is pre‐compacted and subjected to one or four passes of equal channel angular pressing (ECAP) at 500 °C and then 10 revolutions of high pressure torsion (HPT) at room temperature to an effective strain between 4 and 40. Some samples are then annealed at 500 °C for 1 h to investigate the thermal stability of the phases. The four ECAP passes at 500 °C do not result in the formation of the body‐centered cubic (BCC) phase typical for the program RHEAs despite the presence of interfacial zones between particles and defect‐driven diffusion. Nevertheless, a single ECAP pass is sufficient to create a solid bulk sample for subsequent HPT. After 10 HPT revolutions, in contrast to melting route resulting in a single BCC phase alloy, both alloys form new phases comprising a Nb‐rich BCC phase and a ZrHf‐rich HCP phase in both alloys.