Search Results (23)

The development and validation of a sensitive, rapid, and specific gas chromatography method for the evaluation of 19 common Class 2 and Class 3 solvents frequently used in nanomedicine formulation is described. Method validation was performed using PerkinElmer’s headspace gas chromatograph system with flame ionization detection and an Elite 624 Crossbond 6% cyanopropylphenyl-94% dimethylpolysiloxane or DB-Fatwax-Ultra Inert column with helium as the carrier gas. Validation characteristics such as linearity, spike recovery, method precision, specificity, sensitivity, limit of detection/quantitation, and analyte stability were evaluated. The validated methods showed excellent linearity, with a correlation coefficient > 0.99, and good precision, with intra-day precision < 7.4% for all tested analytes. The percent recoveries ranged 83–104% within the method’s quantitation range. In comparison to previously reported methods, the current method has a much shorter equilibration time, higher sensitivity, better separation for many solvents, and a wide concentration detection range. The current method is also perfectly suitable to analyze short chain fatty acids such as formic acid, acetic acid, butyric acid, and valeric acid without requiring additional extraction or derivatization steps. Notably, the method was found to be suitable for analysis of formic acid—a common solvent in certain nanoformulations and one in which there is no prior gas chromatography method available which does not require this additional sample manipulation—down to approximately 75 ppm. Herein, the method is demonstrated using various nanoformulations, including the commercial Doxil formulation as well as several research nanoformulations, including polymeric, cross-linked polymeric, and dendrimer platforms. Full article

Residual volatile organic compounds (VOCs) and non-intentionally added substances (NIASs) limit the reuse of post-consumer recycled high-density polyethylene (rHDPE) in high-value applications because they generate persistent odors and may compromise product quality and regulatory acceptance. This work comparatively assesses five deodorization and purification routes for rHDPE: agitation washing, ultrasound-assisted washing, reflux heating, Soxhlet extraction, and dissolution/precipitation, by combining VOC removal performance, material characterization, and techno-economic evaluation. Ultrasound-assisted washing with SDS achieved ~96% total VOC removal, while reflux heating resulted in near-complete removal (~98%), approaching the analytical detection limit. Soxhlet extraction with ethanol reached 94% after 1 h, and the dissolution/precipitation method provided near-complete purification and removed additional impurities, but at the expense of substantially higher process complexity and cost. Mechanical and physicochemical characterization indicated that the evaluated treatments did not appreciably compromise the measured properties of the recycled polymer. In addition, equilibrium screening with representative analytes in ethanol provided qualitative support for the solvent–polymer interaction discussion. A plant-scale techno-economic assessment identified ultrasound-assisted SDS washing as the most attractive option, offering the best balance between deodorization efficiency, process simplicity, and cost. Overall, the results provide a practical basis for selecting scalable decontamination strategies to upgrade rHDPE quality and expand its use in circular plastic applications. Full article

L-thyroxine (T4) is an important hormone for diagnosing and evaluating thyroid function disorders. As outlined in ISO17511, having a certified reference material (CRM) is crucial for ensuring that the results of clinical tests are traceable to the SI-unit. This study employed two principal methods to evaluate the purity of T4, mass balance (MB) and quantitative nuclear magnetic resonance (qNMR), both of which are SI-traceable (International System of Units) approaches. The MB method involved a detailed analysis of impurities, including water, structurally related compounds, and volatile and non-volatile substances. A variety of techniques were employed to characterize T4 and its impurities, including liquid-phase tandem high-resolution mass spectrometry, ultraviolet spectrophotometry, infrared spectroscopy, and both ¹H-NMR and ¹³C-NMR. Additionally, impurities were quantified using Karl Fischer coulometric titration, ion chromatography, gas chromatography–mass spectrometry, and inductively coupled plasma–mass spectrometry. In qNMR, ethylparaben was used as the internal standard for direct value assignment. The results showed T4 purities of 94.92% and 94.88% for the MB and qNMR methods, respectively. The water content was determined to be 3.563% (n = 6), representing the highest impurity content. Ten structurally related organic impurities were successfully separated, and five of them were quantified. Ultimately, a purity of 94.90% was assigned to T4 CRM, with an expanded uncertainty of 0.34% (k = 2). Full article

The widespread use of alcohol-based hand sanitizers (ABHS) during and after the COVID-19 pandemic has raised concerns about potential exposure to harmful volatile organic compounds (VOCs), such as benzene, acetaldehyde, and other impurities, which may pose health risks. This study investigated the concentrations of ethanol, isopropanol, and 12 impurities, including benzene, acetaldehyde, and methanol, in 85 commercially available ABHS products in Taiwan using gas chromatography-mass spectrometry (GC-MS). The results revealed that 12 samples contained alcohol concentrations below the recommended 60% (v/v) threshold. Benzene and acetaldehyde were identified as the primary impurities, with mean concentrations of 0.84 μg/g and 22.39 μg/g, respectively, exceeding the US FDA interim limits. For frequent ABHS users, the average dermal exposure doses (DEDs) to benzene ranged from 3.17 × 10⁻² to 15.5 μg/kg-bw/day, with children aged 2–11 years showing the highest non-carcinogenic risk (Hazard Quotient > 1) and cancer risk (6.37 × 10⁻⁵ to 9.33 × 10⁻⁴). The findings emphasize the need for stringent quality control of ABHS products and caution in their selection and use. This study provides critical insights into the health risks associated with ABHS in Taiwan, underscoring the importance of regulatory oversight to ensure consumer safety. Full article

The management of municipal solid waste remains a critical environmental and energy challenge across the European Union (EU), where a significant portion of waste still ends up in landfills, generating landfill gas (LFG) rich in methane and harmful impurities. In Latvia, despite national strategies to enhance circularity, untreated LFG is underutilized due to inadequate purification infrastructure, particularly in meeting biomethane standards. This study addressed this gap by proposing and evaluating an innovative, multistep LFG purification system tailored to Latvian conditions, with the aim of enabling the broader use of LFG for energy cogeneration and potentially biomethane injection. The research objective was to design, describe, and preliminarily assess a pilot-scale LFG purification prototype suitable for deployment at Latvia’s largest landfill facility—Landfill A. The methodological approach combined chemical composition analysis of LFG, technical site assessments, and engineering modelling of a five-step purification system, including desulfurization, cooling and moisture removal, siloxane filtration, pumping stabilization, and activated carbon treatment. The system was designed for a nominal gas flow rate of 1500 m³/h and developed with modular scalability in mind. The results showed that raw LFG from Landfill A contains high concentrations of hydrogen sulfide, siloxanes, and volatile organic compounds (VOCs), far exceeding permissible thresholds for biomethane applications. The designed prototype demonstrated the technical feasibility of reducing hydrogen sulfide (H₂S) concentrations to <7 mg/m³ and siloxanes to ≤0.3 mg/m³, thus aligning the purified gas with EU biomethane quality requirements. Infrastructure assessments confirmed that existing electricity, water, and sewage capacities at Landfill A are sufficient to support the system’s operation. The implications of this research suggest that properly engineered LFG purification systems can transform landfills from passive waste sinks into active energy resources, aligning with the EU Green Deal goals and enhancing local energy resilience. It is recommended that further validation be carried out through long-term pilot operation, economic analysis of gas recovery profitability, and adaptation of the system for integration with national gas grids. The prototype provides a transferable model for other Baltic and Eastern European contexts, where LFG remains an underexploited asset for sustainable energy transitions. Full article

Volatile organic compounds (VOCs) from petrochemical, pharmaceutical, and other industries have serious damage to human health and the environment. Catalytic oxidation is a promising method to eliminate air pollution due to its high efficiency, wide application range, and environmental friendliness. However, in the actual industrial environment, the composition of industrial exhaust gases is complex, including VOCs, water vapour, chloride, sulfide and so on. The impurities would have competitive adsorption with reactants or react with the active sites, leading to the decline of catalytic activity, even the deactivation of catalysts. Therefore, this review summarises the recent research on the anti-poisoning ability of catalysts in the catalytic oxidation of VOCs, primarily focusing on the effect of water vapour, chloride, and sulfide. The catalytic oxidation mechanism manifested that the adsorption and activation of reactants are significant in VOCs degradation. On this basis, the mechanism of catalyst poisoning was analysed, and the inhibitory effect of impurities on the oxidation reaction was elucidated. According to the research status, three anti-poisoning strategies are proposed, including building a bimetallic system, modifying supports, and establishing the protected coating. This work provides a theoretical foundation and reference point for the rational construction of anti-poisoning catalysts in VOCs elimination. Full article

In recent years, the use of biogas as a natural gas substitute has gained great attention. Typically, in addition to methane (CH₄), biogas contains carbon dioxide (CO₂), as well as small amounts of impurities, e.g., hydrogen sulfide (H₂S), nitrogen (N₂), oxygen (O₂) and volatile organic compounds (VOCs). One of the latest trends in biogas purification is the application of membrane processes. However, literature reports are ambiguous regarding the specific requirement for biogas pretreatment prior to its upgrading using membranes. Therefore, the main aim of the present study was to comprehensively examine and discuss the most recent achievements in the use of single-membrane separation units for biogas upgrading. Performing a literature review allowed to indicate that, in recent years, considerable progress has been made on the use of polymeric membranes for this purpose. For instance, it has been documented that the application of thin-film composite (TFC) membranes with a swollen polyamide (PA) layer ensures the successful upgrading of raw biogas and eliminates the need for its pretreatment. The importance of the performed literature review is the inference drawn that biogas enrichment performed in a single step allows to obtain upgraded biogas that could be employed for household uses. Nevertheless, this solution may not be sufficient for obtaining high-purity gas at high recovery efficiency. Hence, in order to obtain biogas that could be used for applications designed for natural gas, a membrane cascade may be required. Moreover, it has been documented that a significant number of experimental studies have been focused on the upgrading of synthetic biogas; meanwhile, the data on the raw biogas are very limited. In addition, it has been noted that, although ceramic membranes demonstrate several advantages, experimental studies on their applications in single-membrane systems have been neglected. Summarizing the literature data, it can be concluded that, in order to thoroughly evaluate the presented issue, the long-term experimental studies on the upgrading of raw biogas with the use of polymeric and ceramic membranes in pilot-scale systems are required. The presented literature review has practical implications as it would be beneficial in supporting the development of membrane processes used for biogas upgrading. Full article

Analytical methods based on the mass balance approach were developed for the purity evaluation of tetracycline hydrochloride, a representative salt compound used in pure veterinary drug analysis. The purity assignment method was used to quantify individual classes of impurities via independent analytical techniques. The mass fraction of the free base or salt form contained in a high-purity organic compound with a hydrochloride salt can be determined. The chloride content by ion chromatography-conductivity detector (IC-CD) and general classes of impurities, including structurally related impurities by liquid chromatography–ultraviolet (LC-UV) detector, water by Karl Fischer (KF) coulometric titration, residual solvents by headspace sampler gas chromatography/mass spectrometry (HS-GC/MS), and non-volatiles by thermogravimetric analyzer (TGA), were considered to calculate the purity of the mass fraction. The chloride content of the salt compound can be considered the main impurity in the mass fraction of the free base in the salt compound. A purity assay using quantitative nuclear magnetic resonance (q-NMR) as a direct determination method was performed to confirm the results of the mass balance method. The assigned purities of the tetracycline free form and its salt form in mass fraction were (898.80 ± 1.60) mg/g and (972.65 ± 1.58) mg/g, respectively, which are traceable to the international system of units (SI). Thus, the procedure for evaluating the purity of the free base and salt forms in the salt compound is newly demonstrated in this study. Full article

The characteristics of the surface and interface of nanocomposites are important for exerting multi-functional properties and widening interdisciplinary applications. These properties are mainly depending on the electronic structures of materials. Some key factors, such as the surface, interface, grain boundaries, and defects take vital roles in the contribution of desired properties. Due to the excellent sensitivity of the QCM (quartz crystal microbalance) device, the surface and interface features of the nanocomposite were studied with the aid of the gas-response of the sensors (Sensor’s Gas-Sensitivity) in this work. To make full use of the visible light and part of NIR, a ZnO/MnS_x nanocomposite was constructed using hydrothermal synthesis for narrowing the bandgap width of wide bandgap materials. The results indicated that the absorbance of the resulting nanocomposite was extended to part of the NIR range due to the introduction of impurity level or defect level, although ZnO and MnS belonged to wide bandgap semiconductor materials. To explore the physical mechanism of light activities, the photoconductive responses to weak visible light (650 nm, etc.) and NIR (near-infrared) (808 nm, 980 nm, and 1064 nm, etc.) were studied based on interdigital electrodes of Au on flexible PET (polyethylene terephthalate) film substrate with the casting method. The results showed that the on/off ratio of ZnO/MnS_x nanocomposite to weak visible light and part of NIR light were changed by about one to five orders of magnitude, with changes varying with the amount of MnS_x nanoparticle loading due to defect-assisted photoconductive behavior. It illustrated that the ZnO/MnS_x nanocomposite easily produced photo-induced free charges, effectively avoiding the recombination of electrons/holes because of the formation of strong built-in electrical fields. To examine the surface and interface properties of nanocomposites, chemical prototype sensor arrays were constructed based on ZnO, ZnO/MnS_x nanocomposite, and QCM arrays. The adsorption response behaviors of the sensor arrays to some typical volatile compounds were examined under a similar micro-environment. The results exhibited that in comparison to ZnO nanosheets, the ZnO nanosheets/MnS_x nanocomposite increased adsorption properties to some typical organic volatile compounds significantly. It would have good potential applications in photo-catalysts, self-cleaning films, multi-functional coatings, and organic pollutants treatment (VOCs) of environmental fields for sustainable development. It provided some reference value to explore the physical mechanism of materials physics and photophysics for photo-active functional nanocomposites. Full article

Vinyl acetate is a restricted substance in food products. The quantification of the organic impurities in vinyl acetate is a major problem due to its activity, instability, and volatility. In this paper, while using the mass balance method to determine the purity of vinyl acetate, an improved method was established for the determination of the content of three impurities in vinyl acetate reference material, and the GC-FID peak area normalization for vinyl acetate was calibrated. The three trace organic impurities were identified by gas chromatography tandem high-resolution mass spectrometry to be methyl acetate, ethyl acetate, and vinyl propionate. The content and relative correction factors for the three organic impurities were measured. The purity of vinyl acetate determined by the mass balance method was 99.90% with an expanded uncertainty of 0.30%, and the total content of organic impurities was 0.08% with a relative correction factor of 1.23%. The vinyl acetate reference material has been approved as a national certified reference material in China as GBW (E) 062710. Full article

Procedures for determination of the residual solvent and volatile impurity content in pharmaceutical products usually rely on dissolution in a solvent, followed by headspace-gas chromatography (HS-GC) analysis. Whereas chromatographic systems can utilize a wide variety of solvents, direct-injection mass spectrometry (DIMS) techniques have fewer solvent options, because elimination of the chromatographic column means that the instrument is more susceptible to saturation. Since water has the lowest impact, it has almost always been the default solvent for DIMS. In this study, selected ion flow tube mass spectrometry (SIFT-MS)—a DIMS technique—was applied to the systematic evaluation of the proportion of solvent that can be utilized (with aqueous diluent) without causing instrument saturation and while maintaining satisfactory analytical performance. The solvents evaluated were N,N-dimethylacetamide (DMAC), N,N-dimethylformamide (DMF), 1,3-dimethyl-2-imidazolidinone (DMI), dimethyl sulfoxide (DMSO), methanol, and triacetin. All solvents are compatible with headspace-SIFT-MS analysis at 5% (min) in water, while DMI, DMAC, and DMSO can be used at higher concentrations (50, 100, and 25%, respectively), though suffering substantial diminution of the limit of quantitation for non-polar analytes at higher proportions of non-aqueous solvent. Analytical performance was also evaluated using linearity, repeatability, and recovery measurements. This work demonstrates that organic solvents diluted in water can be utilized with headspace-SIFT-MS and provide an approach for evaluation of additional diluent solvents. Full article

Graphitic carbon is a valuable material that can be utilized in many fields, such as electronics, energy storage and wastewater filtration. Due to the high demand for commercial graphite, an alternative raw material with lower costs that is environmentally friendly has been explored. Amongst these, an agricultural bio-waste material has become an option due to its highly bioactive properties, such as bioavailability, antioxidant, antimicrobial, in vitro and anti-inflammatory properties. In addition, biomass wastes usually have high organic carbon content, which has been discovered by many researchers as an alternative carbon material to produce graphite. However, there are several challenges associated with the graphite production process from biomass waste materials, such as impurities, the processing conditions and production costs. Agricultural bio-waste materials typically contain many volatiles and impurities, which can interfere with the synthesis process and reduce the quality of the graphitic carbon produced. Moreover, the processing conditions required for the synthesis of graphitic carbon from agricultural biomass waste materials are quite challenging to optimize. The temperature, pressure, catalyst used and other parameters must be carefully controlled to ensure that the desired product is obtained. Nevertheless, the use of agricultural biomass waste materials as a raw material for graphitic carbon synthesis can reduce the production costs. Improving the overall cost-effectiveness of this approach depends on many factors, including the availability and cost of the feedstock, the processing costs and the market demand for the final product. Therefore, in this review, the importance of biomass waste utilization is discussed. Various methods of synthesizing graphitic carbon are also reviewed. The discussion ranges from the conversion of biomass waste into carbon-rich feedstocks with different recent advances to the method of synthesis of graphitic carbon. The importance of utilizing agricultural biomass waste and the types of potential biomass waste carbon precursors and their pre-treatment methods are also reviewed. Finally, the gaps found in the previous research are proposed as a future research suggestion. Overall, the synthesis of graphite from agricultural bio-waste materials is a promising area of research, but more work is needed to address the challenges associated with this process and to demonstrate its viability at scale. Full article

Soil contamination with organic contaminants and various heavy metals has become a global environmental concern. Biochar application for the remediation of polluted soils may render a novel solution to soil contamination issues. However, the complexity of the decontaminating mechanisms and the real environment significantly influences the preparation and large-scale application of biochar for soil ramification. This review paper highlights the utilization of biochar in immobilizing and eliminating the heavy metals and organic pollutants from contaminated soils and factors affecting the remediation efficacy of biochar. Furthermore, the risks related to biochar application in unpolluted agricultural soils are also debated. Biochar production conditions (pyrolysis temperature, feedstock type, and residence time) and the application rate greatly influence the biochar performance in remediating the contaminated soils. Biochars prepared at high temperatures (800 °C) contained more porosity and specific surface area, thus offering more adsorption potential. The redox and electrostatic adsorption contributed more to the adsorption of oxyanions, whereas ion exchange, complexation, and precipitation were mainly involved in the adsorption of cations. Volatile organic compounds (VOCs), dioxins, and polycyclic aromatic hydrocarbons (PAHs) produced during biochar pyrolysis induce negative impacts on soil alga, microbes, and plants. A careful selection of unpolluted feedstock and its compatibility with carbonization technology having suitable operating conditions is essential to avoid these impurities. It would help to prepare a specific biochar with desired features to target a particular pollutant at a specific site. This review provided explicit knowledge for developing a cost-effective, environment-friendly specific biochar, which could be used to decontaminate targeted polluted soils at a large scale. Furthermore, future study directions are also described to ensure a sustainable and safe application of biochar as a soil improver for the reclamation of polluted soils. Full article

In this paper, we present the work of designing and fabricating a new generation of microelectromechanical systems (MEMS) based microfluidic preconcentrators (MFP) for volatile organic compounds (VOCs) quantification. The main objective of this work is to quantify the n-pentane impurities using MFP for sample preparation. The MFP was analyzed using Hewlett-Packard 5890 gas chromatography, having a flame ionization detector under isothermal conditions. The proposed MFP system includes two-microfluidic preconcentrators for continuous action and a system of four 3/2 solenoid valves with a control unit. Microfluidic preconcentrators were placed on metal plates and have circular channels filled with Al₂O₃ (50 μm), n-octane ResSil-C (80/100 mesh) sorbents of one nature and are hyphenated with the Peltier elements to regulate the temperature of sorption and desorption. The n-pentane quantitative determination was carried out using a calibration plot of gas mixtures on a successive dilution with the nitrogen. This study shows that the microfluidic preconcentrator system with Al₂O₃ and n-Octane ResSil-C sorbent concentrates the n-pentane traces up to 41 to 47 times from the gas mixture with the standard deviation of ≤5%. It has been observed that the n-octane ResSil-C based MFC shows very fast response (<5 min) and stability up to 300 cycles. Full article

The measurement of air quality parameters for indoor environments is of increasing importance to provide sufficient safety conditions for workers, especially in places including dangerous chemicals and materials such as laboratories, factories, and industrial locations. Indoor air quality index (IAQ-index) and total volatile organic Compounds (TVOC) are two important parameters to measure air impurities or air pollution. Both parameters are widely used in gases sensing applications. In this paper, the IAQ-index and TVOCs have been investigated to identify the best and most flexible solution for air quality threshold selection of hazardous/toxic gases detection and alarming systems. The TVOCs from the SGP30 gas sensor and the IAQ-index from the SGP40 gas sensor were tested with 12 different organic solvents. The two gas sensors are combined with an IoT-based microcontroller for data acquisition and data transfer to an IoT-cloud for further processing, storing, and monitoring purposes. Extensive tests of both sensors were carried out to determine the minimum detectable volume depending on the distance between the sensor node and the leakage source. The test scenarios included static tests in a classical chemical hood, as well as tests with a mobile robot in an automated sample preparation laboratory with different positions. Full article