Linear Calibration Research Articles

An Innovative Vortex-Assisted Liquid-Liquid Microextraction Approach Using Deep Eutectic Solvent: Application for the Spectrofluorometric Determination of Rhodamine B in Water, Food and Cosmetic Samples.

A new green and highly sensitive method for the determination of rhodamine B (RhB) by deep eutectic solvent-based vortex-assisted liquid-liquid microextraction with fluorescence detection (DES-VALLME-FLD) was developed. The extraction efficiency of conventional solvents and different deep eutectic solvent (DES) systems composed of tetrabutylammonium bromide (TBAB) and an alcohol (hexanol, octanol, or decanol) in different ratios were compared. DFT calculations of intermolecular electrostatic and non-covalent interactions of the most stable RhB forms with DES and water explain the experimental DESs' extraction efficiency. Semiempirical PM7 computations were used to obtain Hansen solubility parameters, which supported the good solubility of the monocationic RhB form in selected DESs. The dependence of the linear calibration of microextraction into 100 µL DES was observed in the RhB calibration range from 0.2 to 10.0 µg L-1 with a correlation coefficient of R2 = 0.9991. The LOD value was calculated to be 0.023 µg L-1. The accuracy and precision of the proposed method were verified over two days with RSD values of 2.9 to 4.1% and recovery of 94.6 to 103.7%. The developed method was applied to the determination of RhB in real samples (tap water, energy drink, and lipstick).

Development of a Disposable, Amperometric Glycerol Biosensor Based on a Screen-Printed Carbon Electrode, Modified with the Electrocatalyst Meldolas Blue, Coated with Glycerol Dehydrogenase and NAD+: Application to the Analysis of Wine Quality

This paper describes the design and development of a novel electrochemical biosensor for measuring glycerol in wine. Our initial detailed studies were aimed at deducing the optimum conditions for biosensor operation by conducting hydrodynamic voltammetric and amperometric studies. The resulting voltammograms revealed a maximum electrocatalytic current at 0.0 V vs. Ag/AgCl, which we used for all further studies. We also examined the effect of pH (8–10) on the amperometric responses of different glycerol concentrations over a range of 0.04 to 0.20 mM. Based on our findings, we propose that pH 9 would be suitable as the supporting electrolyte for further studies with the amperometric biosensor. The biosensor was constructed by immobilising 10 units of GLDH and 660 μg NAD+ onto the MB-SPCE surface using glutaraldehyde (GLA) as a cross-linking agent. Calibration studies were performed with glycerol over the 1.0–7.5 mM concentration range. Chronoamperometry was the electrochemical technique chosen for this purpose as it is convenient and can be performed with only 100 μL of sample directly deposited onto the biosensor’s surface. In the current study, we observed linear calibration plots with the above standard solutions using current measurements at a selection of sampling times along the chronoamperograms (30–340 s). We have evaluated the glycerol biosensor by carrying out an analysis of commercially available red wine. Overall, these findings will form a platform for the development of novel rapid technology for point-of-test evaluation of glycerol in the production and quality control of wine.

Central Composite Design Expert-Supported RP-HPLC Optimization and Quantitative Evaluation of Efonidipine Hydrochloride Ethanolate & Chlorthalidone in Tablet.

Central composite design based RP-HPLC method optimization for the synchronized analysis of Efonidipine Hydrochloride Ethanolate (EFE) and Chlorthalidone (CHL) in tablet. The effective separation was performed using Inertsil ODS C18 column (250 × 4.6mm, 5μm), PDA detector with 0.05M KH2PO4 Buffer (pH4.5): Acetonitrile (40:60%v/v) mobile phase. Independent variables were investigated include the concentration of KH2PO4 (X1) and flow rate of mobile phase (X2). Based on responses obtained (retention time, resolution and tailing factor), the optimum condition selected was X1 = 40% and X2 = 1ml/min. Optimized HPLC condition was validated by assessing validation parameters and it meets the acceptance criteria set by ICH. The linear calibration curve was found to be in the quantity range 6.25-18.75 and 20-60μg/ml Assay of drugs was 100.94 and 100.06% for CHL and EFE. The validated RP-HPLC-PDA method can be used for routine analysis of EFE and CHL in tablet.

An analytical method using salting-out assisted liquid-liquid extraction to quantify ceftriaxone from micro volumes of human serum.

Ceftriaxone (CTRX) is a commonly used cephalosporin antibiotic. It is suggested that monitoring plasma/serum concentrations is helpful for its safe use. This study aimed to develop and validate an analytical method for measuring CTRX concentrations in human serum according to International Conference on Harmonization guideline M10. Ten microliters of serum sample was purified using a salting-out assisted liquid-liquid extraction procedure with magnesium sulfate. The upper layer was then diluted threefold and analyzed using a liquid chromatography-tandem mass spectrometry-based method with a total run time of 12 min. The linear calibration curve was obtained over the concentration range 5-500 μg/ml. The within-run accuracy varied from 0.2 to 6.5%, and the precision was ≤8.0%. The between-run accuracy and precision ranged from 0.7% to 5.6% and ≤6.4%, respectively. Significant carryover was resolved by injecting four blanks after high-concentration CTRX samples. The recovery rates from spiked serum at low and high concentrations were 44.4 and 43.4%, respectively. Other factors, including selectivity, matrix effects, stability, dilution integrity and reinjection reproducibility also met the acceptance criteria. Serum concentrations in 14 samples obtained from two participants receiving 2 g/day of CTRX were successfully determined using this method.

Mechanism, thermochemistry, and kinetics of formation of PhC(O)H and HOPhC(O)H during unimolecular decomposition of P-PhC(O2•)HPhOH.

Bisphenols are one of the main components of bio-oil, produced during the pyrolysis of lignin-containing biomass. Synthetic bisphenols are used in polycarbonate plastics, epoxy resins, and thermal papers. Their mechanism of oxidation is important for the determination of the fire safety of these materials and the possibility of using them as additives in fuels for the decrease and description of ignition delays, as well as for the determination of their health risk assessment in medicine. One representative of bisphenols is p-benzylphenol (p-PhCH2PhOH), which is formed during the fast pyrolysis of lignine-containing biomass. Its thermochemistry of oxidation has been partially studied previously. It is shown that the reaction of chain oxidation of p-PhCH2PhOH is thermochemically favorable at low temperatures. However, these studies consider only two pathways of this reaction: (1) the chain oxidation of RH by RO2• and (2) the tautomerization of R'HO2• to R'O2H with following production of R'O• and OH radicals. At the same time, the reactions of intramolecular rearrangement of RO2•, produced PhC(O)H and •PhOH or HOPhC(O)H and •Ph, are not reported but can be an important part of its oxidation mechanism. The five DFT (M06-2X (i = 1), B3LYP (i = 2), wB97XD (i = 3), M08HX (i = 4), MN15 (i = 5)) approaches with 6-311 + + G(d,p) basis set are used for the determination of standard enthalpies of atomization (ΔraH°(Xi)) of considered compounds (molecules, radicals, and transition states). These values of ΔraH°(Xi) are corrected using the empirical linear calibration dependencies, reported previously. The different calibration dependencies are used for the hydrocarbons (including the aromatics and simple oxygenated derivatives) and for the peroxides. The corrected values of ΔraH°(Xi, CORR) are used according to Hess's law for the determination of ΔfH°(Xi, CORR). The most consistent values of ΔfH°(X, MEAN) are derived from the coordination of the values of ΔfH°(Xi,CORR) using the intersection of their values of standard deviations (3SDi). These values of ΔfH°(X, MEAN), as well as the B3LYP values of S°(X), which are accounting the frequencies correction and internal rotations, as well as their temperature dependencies, are used for the determination of thermochemistry of considered reactions and of the calculation, within transition state theory (TST), of the values of high pressure limits of the rate constant. The values of H°(Xi), S°(Xi), and G°(Xi) are calculated using the Gaussian 16w program. The considered mechanism is prepared using ISIS/Draw package. The temperature dependencies of thermochemical properties and the values of rate constants are determined using the ChemRate program (v.1.5). The optimized structures are visualized using the Chemcraft package.

Electrocatalysis Using Cobalt Porphyrin Covalently Linked with Multi-Walled Carbon Nanotubes: Hydrazine Sensing and Hydrazine-Assisted Green Hydrogen Synthesis.

Acid-treated multi-walled carbon nanotube (MWCNT) covalently functionalized with cobalt triphenothiazine porphyrin (CoTriPTZ-OH) A3B type porphyrin, containing three phenothiazine moieties (represented as MWCNT-CoTriPTZ) is synthesized and characterized by various spectroscopic and microscopic techniques. The nanoconjugate, MWCNT-CoTriPTZ, exhibits a pair of distinct redox peaks due to the Co2+/Co3+ redox process in 0.1M pH 7.0 phosphate buffer. Further, it electrocatalytically oxidizes hydrazine at a low overpotential with a high current. This property is advantageously utilized for the sensitive determination of hydrazine. The developed electrochemical sensor exhibits high sensitivity (0.99 µAµM-1cm-2), a low limit of detection (4.5 ppb), and a broad linear calibration range (0.1µM to 3.0mM) for the determination of hydrazine. Further, MWCNT-CoTriPTZ is exploited for hydrazine-assisted green hydrogen synthesis. The high efficiency of hydrazine oxidation is confirmed by the low onset potential (0.45V (vs RHE)) and 0.60V (vs RHE) at the current density of 10mA.cm-2. MWCNT-CoTriPTZ displays a high current density (77.29mA.cm-2) at 1.45V (vs RHE).

Exploitation of erythrosine B as a fluorometric marker for lurasidone determination through electrostatic attraction; application to content uniformity test.

A recently developed antipsychotic drug, lurasidone, was determined using a simple, sensitive, and eco-friendly spectrofluorimetric approach. The suggested approach was based on the quantifiable quenching impact of lurasidone on the inherent fluorescence of erythrosine B in an acidic environment employing a Teorell-Stenhagen buffer (pH4). Following excitation at 530 nm, the quenching of erythrosine B fluorescence was monitored at 552 nm. The system variables were systematically optimized to enhance the formation of the lurasidone-erythrosine B ion pair for analytical purposes. A linear calibration graph was built in the range of 20-600 ng mL-1 with 0.9998 as a coefficient of correlation. The quantitation and detection limits were 13.5 and 4.5ng/mL, respectively. The analytical validity of the designed approach was assessed with respect to International Council on Harmonization (ICH) guiding principles. The proposed methodology was employed with high recoveries for assessing lurasidone in bulk powder and its therapeutic tablet dosage form. Additionally, the uniformity of tablet formulations was tested using the developed approach. Finally, the established approach was assessed for its greenness using various tools.

Pharmacokinetics of Anti-rheumatic Drugs Methotrexate and Tofacitinib with its Metabolite M9 in Rats by UPLC-MS/MS.

Tofacitinib is an oral JAK inhibitor for the treatment of rheumatoid arthritis (RA). The clinical efficacy and safety of an administered tofacitinib, either monotherapy or in combination with conventional synthetic disease-modifying anti-rheumatic drugs, mainly methotrexate (MTX), have been evaluated. The high plasma concentration with delayed medicine clearance may affect the liver and/or kidney functions. In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC- MS/MS) method for the quantitative analysis of methotrexate, tofacitinib, and metabolite M9 in plasma of Sprague Dawley (SD) rats was developed, and its effectiveness was validated as well. Methotrexate, tofacitinib, M9 and fedratinib (internal standard, IS) were separated by gradient elution. The chromatography was performed on an Acquity BEH C18 (2.1 mm × 50 mm, 1.7 μm) column with the mobile phases of acetonitrile and 0.1% formic acid aqueous solution with different proportions at the flow rate of 0.30 mL/min. In the positive ionization mode, the analyzes were detected using a Xevo TQ-S triple quadrupole tandem mass spectrometer, with the following mass transition pairs: m/z 313.12 → 148.97 for tofacitinib, m/z 329.10 → 165.00 for M9 and m/z 455.12 → 308.05 for methotrexate. The obtained results manifested good calibration linearity over the ranges of tofacitinib at 0.1-100 ng/mL, M9 at 0.05-100 ng/mL, and methotrexate at 0.05-100 ng/mL. The lower limit of quantifications (LLOQs) of methotrexate, tofacitinib and M9 were 0.05 ng/mL, 0.1 ng/mL and 0.05 ng/mL, respectively. Intra-day and inter-day accuracy values were confirmed with a range of -6.3% to 12.7%, while intra-day and inter-- day precision values were ≤14.4%. Additionally, recoveries were greater than 86.5% for each compound without significant matrix effects. The currently established analytical method exhibited great potential for the evaluation of plasma concentrations of methotrexate, tofacitinib and M9 simultaneously, greatly reducing the detection time, which would serve as a supplementary role in formulating dose decisions to achieve personalized treatment, identify drugs that cause adverse reactions and finally, to assess drug-drug interactions on clinical studies.

Monitoring residual solvents in pharmaceutical products using a portable pre-concentration GC-PID

Pharmaceutical manufacturing utilizes solvents at different stages of production. Some of the harmful solvent residuals may be retained in the final product; therefore, they need to be monitored for quality control and to meet the regulation requirement. Here, a novel method capable of rapidly analyzing residual solvents in pharmaceutical products was developed using a compact-portable gas chromatography with a photoionization detector (GC-PID). The method consists of modified Tedlar® bag sampling, online pre-concentration, separation of volatiles by miniaturized GC, and micro-PID detection. The method detection limits of selected residual solvents were in the range of 26.00 – 52.03 pg/mL which is much lower than the pharmaceutical compliance concentration limits. Limits of detection > 520 pg of analyte per grams of sample was also determined for the over-the-counter drugs. The method performance showed rapid speed (5 min), linear calibration (r2 < 0.99), and repeatable retention time (RSD < 0.4 %). Direct analysis of residual solvents in solid samples was conducted without the need for complex sample preparation. The method validation using over-the-counter pharmaceutical products yielded excellent accuracy (recovery > 91.2 %) and precision (RSD < 6.5 %) for the selected residual solvents, including 1,4-dioxane, benzene, chlorobenzene, cyclohexane, xylenes, and toluene. This portable and rapid method could be deployed during the pharmaceutical drug manufacturing processes for quality control.

Sequential thin film microextraction and overcoated thin film microextraction devices for characterization of sparkling wine aroma profiles and partitioning equilibria

Solid Phase Microextraction (SPME) is a commonly used, robust method for characterization of aroma profiles in food matrices. However, challenges such as saturation, swelling, and competition can occur when sampling such complex matrices, resulting in decreased accuracy in the quantitation of polar compounds. In this study, sequential thin film micro-extraction (TFME) was employed to study the aroma profile of sparkling wine, with a focus to evaluate the displacement of polar analytes at extraction times longer than their corresponding equilibrium time. This investigation also describes advancements in the production of TFME devices, specifically the overcoating of hydrophilic-lipophilic balance/polydimethylsiloxane (HLB/PDMS) thin films to increase their matrix compatibility. Sequential thin film micro-extraction and overcoated HLB/PDMS thin films were evaluated for characterization of sparkling wine samples. The results were encouraging, showing that these advancements can decrease competition phenomena and increase the calibration linearity range compared to traditional micro-extraction approaches more commonly used for the characterization of such samples. In addition, multiphase equilibria investigation involving micellar systems enabled by the microextraction technology provides better understanding between wine aroma and its composition.

Investigation of on-line electrokinetic enrichment strategies for capillary electrophoresis of extracellular vesicles

This work explores strategies for electrokinetic preconcentration of extracellular vesicles (EVs) that are potential source of biomarkers for different diseases. The first approach that led to successful preconcentration of EVs is based on large volume sample stacking (LVSS), allowing an enrichment factor of 7 for CE of EVs with long-end injection (using a capillary with an effective length of 50 cm). Attempts were also made to perform multiple cycles of LVSS, field amplified sample stacking (FASS) and field amplified sample injection (FASI), to improve EVs preconcentration performance. The focus was then put on development of capillary isotachophoresis under high ionic strengths (IS) for electrokinetic enrichment of slow migrating EVs having heterogeneous mobilities. This approach relies on the use of extremely high concentrations of the terminating electrolyte (TE) to slow down the mobility of TE co-ions, rendering them slower than those of EVs. The limit of detection for intact EVs using the developed ITP-UV method reached 8.3 × 108 EVs/mL, allowing an enrichment of 25 folds and a linear calibration up to 4 × 1010 EVs/mL. The ITP-UV and ITP-LIF approaches were applied to provide the electrokinetic signature of EVs of bovine milk and human plasma as well as to visualize more specifically intravesicular fluorescently labelled EVs. The investigation of these strategies shredded light into the challenges still encountered with electrokinetic preconcentration and separation of heterogeneous EVs sub-populations which are discussed herein based on our results and other attempts reported in the literature.

3D-printed ultra-small Brownian viscometers

Measuring viscosity in volumes smaller than a microliter is a challenging endeavor. A new type of microscopic viscometers is presented to assess the viscosity of Newtonian liquids. Micron-sized flexible polymer cantilevers are created by two-photon polymerization direct laser writing. Because of the low stiffness and high elasticity of the polymer material the microcantilevers exhibit pronounced Brownian motion when submerged in a liquid medium. By imaging the cantilever’s spherically shaped end, these fluctuations can be tracked with high accuracy. The hydrodynamic resistance of the microviscometer is determined by fitting the power spectral density of the measured fluctuations with a theoretical frequency dependence. Validation measurements in water-glycerol mixtures with known viscosities reveal excellent linearity of the hydrodynamic resistance to viscosity, allowing for a simple linear calibration. The stand-alone viscometer structures have a characteristic size of a few tens of microns and only require a very basic external instrumentation in the form of microscopic imaging at moderate framerates (~ 100 fps). Thus, our results point to a practical and simple to use ultra-low volume viscometer that can be integrated into lab-on-a-chip devices.

Embroidered textile-based electrochemical sensors towards urinary nitrite measurement

Wearable biochemical sensors enable the real-time measurement of health parameters in non-invasive manner. In this work, we have developed polyaniline (PANI)/COOH-functionalized multiwalled carbon nanotubes (MWCNTs)/sodium copper chlorophyllin (CuCP) coated conductive thread as a novel wearable platform for monitoring nitrite (NO2–) levels. The linear calibration plots for NO2– were obtained over the concentration range of 0.05 µM–10 mM with detection limit of 0.35 nM. The sensor platform was also tested for measuring NO2– levels in artificial urine samples.

Green analytical chemistry-based spectrophotometric techniques for ternary component analysis of pain relievers

BackgroundThe management of pain presents a significant challenge in healthcare, particularly in cases where conventional therapies prove inadequate. In response to this need, this study aims to devise two innovative UV spectrophotometric techniques rooted in the principles of green analytical chemistry for the analysis of Aceclofenac (ACE), Paracetamol (PAR), and Tramadol (TRM) in both bulk and tablet forms.ResultsUtilizing advanced mathematical methodologies such as the double divisor ratio spectra method and area under the curve, the concentrations of these drugs were accurately determined. Validation of the developed methods adhered to the guidelines outlined by the International Council for Harmonisation in the Q2 (R1), revealing linear calibration curves for ACE (8–12 µg/mL), PAR (22.75–35.75 µg/mL), and TRM (2.62–4.12 µg/mL). Furthermore, statistical analyses employing Student’s t test and F test were conducted to ensure the robustness of the proposed method. The evaluation of environmental impact through green metric tools confirmed the eco-friendliness of the proposed methodologies.ConclusionThe assessment performed utilizing green metric tools has substantiated the environmental sustainability of the proposed approach. Thus, this methodology offers accurate and reliable outcomes for the determination of three drugs, as indicated by the complete overlap observed in the zero-order spectra.

Determination of Inorganic Arsenic Species in Drinking Water by Cloud Point Extraction Coupled with Ultraviolet-Visible Spectrophotometry

A novel method has been developed for accurately quantifying arsenic species, including As(III), As(V), and total inorganic arsenic, in drinking water. The technique combines ultraviolet-visible spectrophotometry with cloud point extraction (UV/CPE), ensuring high sensitivity and selectivity. The methodology relies on complex formation between As(III) and Pyronin B in the presence of tartaric acid. The resulting complex is efficiently extracted into the surfactant-rich phase consisting of 5.0% (v/v) Triton X-114. Under optimized conditions, a linear calibration relationship from 3 to 500 µg/L is obtained. The method offers low detection and quantification limits of 1.04 and 3.48 µg/L, respectively, with a corresponding relative standard deviation below 5% for 11 replicates. Furthermore, spiked samples demonstrated excellent recovery values from 95.1% to 102.3%. The accuracy was verified by the analysis of the standard reference material SRM 1643e (trace elements in water), revealing no significant differences at the 95% confidence level. The approach was successfully utilized for the quantification of As(III), As(V), and total inorganic arsenic in commercial and domestic drinking water.

Optimization of SLIPI–polarization ratio imaging for droplets sizing in dense sprays

In this article, structured laser illumination planar imaging and polarization ratio techniques are successfully combined to size droplets in various optically dense sprays. The polarization ratio approach is based on the acquisition of the perpendicular and parallel polarized components of Lorenz–Mie scattered light, for which the ratio is proportional to the surface mean diameter, D21. One of the main advantages of this technique, compared to some other laser imaging techniques for particle sizing, is that no fluorescent dye is required. This makes the technique suitable for characterizing sprays under evaporation conditions, such as combustion or spray drying applications. In addition, the SLIPI technique aims at suppressing the detection of multiple light scattering and at extracting the desirable single-light scattering signal. To test the reliability of this novel approach, an industrial hollow-cone nozzle is used, injecting at 50 bar water mixed with Glycerol (in the range of 0–60%). The first aim of this work is to study the experimental parameters that influence the reliability of the technique, such as the polarization orientation of the incident light, the refractive index of the injected liquid and the variation of the droplet size distribution. Using Phase Doppler Anemometry, the results show that a linear calibration is obtained for droplets ranging between 10 and 70 μm, when the incident illumination has a polarization set to 10° and 20°. In addition, this article demonstrates the feasibility of the technique for the measurement of liquids having a refractive index reaching 1.41. In the last stage of this work, after rotating the nozzle every 5°, a 3D tomographic reconstruction of D21 is performed. This demonstrates the robustness and efficiency of the technique for droplet sizing in 3D, under challenging conditions.

Preparation of graphene oxide and multi-walled carbon nanotubes, and they are used to modify the glassy carbon electrode for sensing Enalapril Maleate

In this study, the graphene oxide and multi-walled carbon nanotubes fabrication was evaluated using (SEM), (FTIR), Raman spectroscopy and (XRD). The results showed promising accuracy for the graphene oxide and multi-walled carbon nanotubes voltammetric sensor. The direct voltammetric determination of Enalapril Maleate in pharmaceutical samples, urine, and serum is detailed using a straightforward and extremely sensitive technique. Graphene oxide-multiwall carbon nanotubes are added to glassy carbon electrodes in an efficient manner to activate the GO-MWNT structures, which then electrocatalyzes the reduction of Enalapril Maleate. The results of the cyclic voltammetric (CV) experiment showed that the electrocatalytic activity of GO-MWNTs to reduce Enalapril Maleate was significantly improved, leading to a much higher cathodic peak current for EM. This finding opens the door to the possibility of creating a very sensitive voltammetric sensor to detect EM in biological and pharmaceutical fluid samples. A linear calibration curve in the 2.5–12.5 ppm concentration range, a detection limit of 0.2 ppm, and a relative standard deviation (R.S.D.%) lower than 1.0 % (n = 5) were all indicative of ideal conditions. Lastly, EM is a diffusion-controlled process that proceeds through a two-electron-two-proton change, which provides a mechanism for the reduction of EM.. The GO-MWCNTs/GCE sensor had a good repeatability and excellent reproducibility, R.S.D.% =1.77 and 1.82.

Responsiveness and Precision of Digital IMUs under Linear and Curvilinear Motion Conditions for Local Navigation and Positioning in Advanced Smart Mobility.

Sensors based on MEMS technology, in particular Inertial Measurement Units (IMUs), when installed on vehicles, provide a real-time full estimation of vehicles' state vector (e.g., position, velocity, yaw angle, angular rate, acceleration), which is required for the planning and control of cars' trajectories, as well as managing the in-car local navigation and positioning tasks. Moreover, data provided by the IMUs, integrated with the data of multiple inputs from other sensing systems (such as Lidar, cameras, and GPS) within the vehicle, and with the surrounding information exchanged in real time (vehicle to vehicle, vehicle to infrastructure, or vehicle to other entities), can be exploited to actualize the full implementation of "smart mobility" on a large scale. On the other hand, "smart mobility" (which is expected to improve road safety, reduce traffic congestion and environmental burden, and enhance the sustainability of mobility as a whole), to be safe and functional on a large scale, should be supported by highly accurate and trustworthy technologies based on precise and reliable sensors and systems. It is known that the accuracy and precision of data supplied by appropriately in-lab-calibrated IMUs (with respect to the primary or secondary standard in order to provide traceability to the International System of Units) allow guaranteeing high quality, reliable information managed by processing systems, since they are reproducible, repeatable, and traceable. In this work, the effective responsiveness and the related precision of digital IMUs, under sinusoidal linear and curvilinear motion conditions at 5 Hz, 10 Hz, and 20 Hz, are investigated on the basis of metrological approaches in laboratory standard conditions only. As a first step, in-lab calibrations allow one to reduce the variables of uncontrolled boundary conditions (e.g., occurring in vehicles in on-site tests) in order to identify the IMUs' sensitivity in a stable and reproducible environment. For this purpose, a new calibration system, based on an oscillating rotating table was developed to reproduce the dynamic conditions of use in the field, and the results are compared with calibration data obtained on linear calibration benches.

Eco-friendly optical sensor for precise detection of gold ions in diverse matrices through the integration of β-2-hydroxybenzyl-3-methoxy-2-hydroxyazastyrene in a PVC membrane

An environmentally conscious methodology is investigated for the precise and discerning identification of trace concentrations of gold ions in diverse matrices. A novel optical sensor membrane is proposed for the determination of Au3+ ions, utilizing the immobilization of β-2-hydroxybenzyl-3-methoxy-2-hydroxyazastyrene (HMHS) entrapped in polyvinyl chloride (PVC). The sensor incorporates sodium tetraphenylborate (Na-TPB) as the ionic additive and dibutyl phthalate (DBP) as a plasticizer. Under optimal conditions, the suggested sensor exhibits a linear calibration response to Au3+ ions within a concentration range of 5.0 to 165 ng mL−1. Detection and quantification limits are specified as 1.5 and 4.8 ng mL−1, respectively, with a rapid response time of 5.0 min. Upon presentation, this optical sensor not only affirms high reproducibility, stability, and an extended operational lifespan but also showcases exceptional selectivity for Au3+ ions. Notably, no discernible interference is observed when assessing the potential influence of other cations and anions on Au3+ ion detection. The adaptability of this optical sensor is validated through its successful application in determining Au3+ ion concentrations across various sample types, including water, environmental, cosmetics, and soil matrices.Graphical

A series of triphenylamine-derived fluorophores attached to a Cu-based MOF for gaseous CO optical sensing: synthesis, performance, and mechanism.

A series of triphenylamine-derived fluorescent dyes were attached to a Cu2+-containing MOF (metal-organic framework), denoted as Pm@CuMOF. The molecular structures of these dyes were discussed by the single crystal structures. Their major absorption bands peaked at 410-450 nm, showing emission bands ranging from 556 to 586 nm with emission quantum yields ranging from 8.0 to 15.1%. It was found that the [-N(C2H5)2] group generally improved sensing performance, and the -OH group in the dyes helped the Cu2+ quenching effect. Pm@CuMOF was observed by SEM as nanorods with a width of ~100 nm and a length of 300 nm. Their XRD patterns and N2 adsorption/desorption isotherms were recorded to confirm their porous structure. A low probe loading level of ~4% was determined by TGA result. The CO sensing mechanism was revealed as a Cu2+/Cu+-involved sensing mechanism based on the result of NMR titration, IR, XPS, and EPR. The fluorescence of these triphenylamine-derived dyes was firstly quenched by CuMOF. In contact with CO, Cu2+ was reduced to Cu+, accompanied by the release and fluorescence recovery of the fluorescent dyes, showing emission turn-on effect towards CO gas. Pm@CuMOF showed increased emission intensity at CO level of 0.005% (versus N2), with response times ranging from 123 s to 280 s (depending on various temperatures). Good selectivity was observed over competing alkane gases, with stable emission for at least 5 days, but no linear calibration plots were observed.