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ANALYTICAL CHEMISTRY · 2024 · IF 6.7

Solid-Phase Microextraction Mediated Solid-Phase Dielectric Barrier Discharge Vapor Generation–Atomic Fluorescence Spectrometry for Sensitive Determination of Mercury in Seawater

Runyan Wang,Shanshan Chen,Qian He,Shengrui Xu

A novel method coupling solid-phase microextraction (SPME) to solid-phase dielectric barrier discharge (SPDBD) vapor generation was proposed and used for the sensitive detection of trace mercury (Hg) in seawater with atomic fluorescence spectrometry (AFS) in this work. The method proposed herein offers the unique advantages of integrating desorption and chemical vapor generation into one step, eliminating the use of elution reagents, and reducing the analysis time. SPME with multiwalled carbon nanotubes (MWCNTs) coated on the glass tube was used to extract Hg2+ in seawater. The Hg2+ was then desorbed and reduced to Hg0 vapor by SPDBD, which was detected by cold vapor AFS. The parameters affecting Hg2+ extraction, desorption, and vapor generation were studied. The detection limit of Hg2+ was 0.0003 μg L–1, and the relative standard deviation at a Hg2+ concentration of 0.05 μg L–1 was 4.4%. This method also has excellent antimatrix interference ability for Hg2+ determination with recoveries between 91.8% and 101.1% in the presence of extremely high concentrations (two million times excess) of coexisting ions. The practicality of this method was also evaluated by analyzing two different certified reference materials of Hg2+ in water and several seawater samples with good spike recoveries (94.0%–107.4%). Compared with solid-phase photothermo-induced vapor generation, this method has higher extraction efficiency and higher desorption efficiency without the assistance of heating as well as a lower detection limit of Hg2+, which is capable of performing trace Hg analysis in seawater.

CAS / MDL: 25014-41-9
研究领域: 分析化学 · 环境科学
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2019 · IF 2.931

Rapid determination of fumonisin (FB1) by syringe SPE coupled with solid-phase fluorescence spectrometry

Long Li,Wanchao Chen,Hui Li,Jibran Iqbal,Ying Zhu,Ting Wu,Yiping Du

Fumonisin B 1 is the most prevalent member of a family of toxins, known as fumonisins , which occurs mainly in maize, wheat and other cereals. Due to its hepatotoxic and nephrotoxic in all animal species, very strict regulations have been imposed on the levels of fumonisin B 1 in cereal and cereal-based foods worldwide. In this work, a rapid determination method of fumonisin B 1 by membrane solid phase extraction coupled with solid-phase fluorescence analysis is developed. A rhodamine based fluorescent probe was used for derivatization with fumonisin B 1 . After derivatization and extraction by nylon membrane, the enriched fumonisin B 1 can be detected directly on the membrane without further elution process that is placed in a designed spectra collection device. The established method showed a linear relationship in concentration range of 0.5–5.0 μg/L, with the R 2  = 0.991, and a limit of detection of 0.119 μg/L. Method accuracy was further confirmed using LC-MS method by comparing the detection results of 3 corn powder samples spiked with FB 1 , that demonstrated equivalent results. The results of this study indicated that the proposed method was simple, sensitive, reliable and suitable for trace fumonisins B 1 quantitation in corn-based feeds.

研究领域: 食品安全 · 分析化学 · 毒理学
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CRYSTENGCOMM · 2021 ·Vol. 23 ·期 39 ·6899-6908 · IF 3.545

Growth of MSe semiconductor nanowires on metal substrates through an Ag2Se-catalyzed solution–solid–solid mechanism (M = Zn, Cd and Mn)

Huimin Wang,Tingting Wang,Zibin Huang,Yizhuo Liu,Dehui Leng,Junli Wang

The growth of metal chalcogenide nanowires (NWs) on metal substrates is challenging work since the direct reactions taking place between the chalcogen (S, Se or Te) and zero-valent metal (M0) are frequently unable to regulate the crystallization of nanocrystals in an anisotropic one-dimensional (1D) manner. We here report the use of Ag2Se seeds as catalyst particles to realize the growth of metal selenide (MSe) NWs on their respective metal foil or flakes, including ZnSe/Zn, CdSe/Cd, and MnSe/Mn material systems. Metal foil or flakes (M = Zn, Cd and Mn) serve as a support substrate as well as a metal cation source during the NW synthesis. The preformed Ag2Se seeds play the roles of not only catalytic particles that initiate a so-called solution–solid–solid process to produce crystalline MSe NWs on metal substrates, but also inert impurities that promote an electrochemical anodic reaction of the metal to supply metal cations (M0 − 2e → M2+) for the NW formation. The microstructural studies by HRTEM reveal the polytypism and particularly the diameter-dependence of crystal phases and growth directions in the resulting MSe NWs, which can be rationalized from the viewpoints of the energetics and the catalyst/NW interfacial structures. These semiconductor NWs grown on metal foil or flakes may find wide use in photoelectric catalysis and devices without a transfer process of free-standing NWs onto a conductive support substrate.

研究领域: 材料科学 · 纳米技术 · 半导体物理
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Nano Research · 2021 ·Vol. 14 ·期 10 ·3386-3394 · IF 8.897

Unconventionally anisotropic growth of PbSe nanorods: Controllable fabrication under solution-solid-solid regime over Ag2Se catalysis for broadband photodetection

You Su,Zhang Li,Yang Qing

Broadband optoelectronic devices intrigue enormous interests on account of their promising potential in optical communications, sensors and environmental monitoring. PbSe nanocrystals are promising candidates for the construction of next-generation photodetectors due to their fascinating intrinsic properties and solution-processed compatibility with varied substrates. Here, we report the fabrication of a broadband photodetector on the basis of high-quality solution-processed PbSe nanorods in rock-salt phase grown along unconventionally anisotropic growth direction of <112> zone axis. The rock-salt PbSe nanorods are synthesized in solution phase over the catalysis of Ag 2 Se with relatively high-temperature body-centered cubic phase via a solution-solid-solid growth regime using oleylamine and oleic acid as solvents and stabilizer surfactants, from which the PbSe nanorods with the unconventionally anisotropic growth direction are controllably grown in size and shape in the synthetic procedure typically with about 17 nm in diameter and 58 nm in length on average. Meanwhile, the PbSe nanorods-based photodetector exhibits a broadband response from 405 to 1,064 nm with a high responsivity of 0.78 A·W −1 and a fast response time of 17.5 µs. The response time is much faster in comparison with most of the PbSe-based photodetectors with response time in millisecond level.

研究领域: 材料科学 · 光电探测器领域
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International Journal of Environmental Research and Public Health · 2023 ·Vol. 20 ·期 2 ·1393 · IF 4.614

The Preparation of Covalent Bonding COF-TpBD Coating in Arrayed Nanopores of Stainless Steel Fiber for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons in Water

Zihan Li,Mengqi Yang,Xuetong Shen,Hongtao Zhu,Baohui Li

Covalent organic framework (COF)-TpBD was grafted on the arrayed nanopores of stainless steel fiber (SSF) with (3-aminopropyl) triethoxysilane as the cross-linking agent. The prepared SSF bonded with COF-TpBD showed high thermal and chemical stability and excellent repeatability. The prepared SSF bonded with COF-TpBD was also used for the solid-phase microextraction (SPME) of seven kinds of polycyclic aromatic hydrocarbons (PAHs) in actual water samples, followed by gas chromatography with flame ionization detection (GC-FID) determination, which exhibited low limits of detection (LODs), good relative standard deviation (RSD) and high recoveries.Keywords:solid-phase microextraction;COF-TpBD;polycyclic aromatic hydrocarbons

研究领域: 分析化学 · 环境科学
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MICROCHIMICA ACTA · 2014 ·Vol. 182 ·期 3 ·737-744 · IF 3.719

Synthesis of a graphitic carbon nitride nanocomposite with magnetite as a sorbent for solid phase extraction of phenolic acids

Yang Jing,Si Ling,Cui Shihai,Bi Wentao

We have developed a facile in-situ growth method for the deposition of magnetite (Fe 3 O 4 ) particles on the surface of a graphitic carbon nitride (g-C 3 N 4 ) nanosheet. The material was characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The high affinity of g-C 3 N 4 for phenolic acids in combination with the magnetism of Fe 3 O 4 provides an efficient means for magnetic solid phase extraction. The adsorption, desorption and recoveries were examined. Under optimized conditions, the method has limits of detection in the range from 17.5–42.6 ng mL −1 (at an S/N of 3), and precisions from 2.8–3.8 % (for n  = 5). The method was successfully applied to the determination of protocatechuic, caffeic, and ferulic acids in Salicornia herbacea L . plant extracts. Recoveries ranged from 92.4–99.5 %. The high affinity of g-C 3 N 4 toward the phenolic acids as well as the magnetic behavior of Fe 3 O 4 were combined in this nanocomposite material to provide an efficient and simple magnetic solid phase extraction (MSPE) approach.

CAS / MDL: 108-78-1 99-50-3
研究领域: 材料科学 · 分析化学 · 环境科学
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Nanomaterials · 2024 ·Vol. 14 ·期 19 ·1613 · IF 4.4

Modulating Near-Infrared Persistent Luminescence via Diverse Preparation Approaches

Xiaomeng Wang,Hengli Zhu,Yan Liu,Jingyuan Li,Lejia Cao,Jiaren Du,Hengwei Lin

Near-infrared (NIR) persistent luminescence (PersL) materials have attracted extensive attention due to their great promise in medical diagnostics, bio-imaging, night vision surveillance, multi-level anticounterfeiting, and information encryption. To achieve NIR PersL (micro/nano-) materials with the desired properties, a variety of synthesis methods have been employed, including solid-phase reaction and liquid-phase synthesis. Different synthesis methods have different but important effects on the micro/nano-structure, luminescence, and PersL properties of the materials. Moreover, the influence of various synthesis methods on the properties of NIR PersL materials determines the selection of preparation approaches for other new material systems. Taking the representative NIR PersL ZnGa 2 O 4 :Cr 3+ material as an example, four synthesis procedures are applied, namely, high-temperature solid-state reaction (SSR), high-temperature molten salt method (MSM), hydrothermal method (HM), and microwave-assisted solid-state (MASS) method. The structural and luminescent properties of samples made by SSR, MSM, HM, and MASS are compared. Notably, it is revealed that the MASS method can create additional trapping energy levels, which is of great significance for emerging applications. This work demonstrates the different effects of synthesis methods on PersL performance and provides a good guideline for the rapid and reasonable selection of preparation methods for diverse applications.

研究领域: 材料科学 · 纳米技术 · 生物医学工程 · 光学材料
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POWDER METALLURGY AND METAL CERAMICS · 2022 ·Vol. 60 ·期 11 ·738-747 · IF 0.913

Solid-State Reactions of SiC–TiO2–MgO System and Phase Relations in SiC–SiO2–TiC–TiO2–MgO System

Sun W.Z.,Huang Z.K.,Lu Y.J.,Liu L.M.,Xiao Z.

Preliminary experiments revealed solid-state reactions in the SiC–TiO 2 –MgO system that resulted in forming TiC compound, providing, thus, a new reaction system for the formation of TiC–SiC ceramic matrix composites. This system’s high-temperature physicochemical reaction and the phase equilibrium relations of TiC–SiC with salt compounds in the SiC–TiO 2 –MgO system will be examined in this paper. The obtained findings may significantly contribute to the composition of TiC–SiC ceramic composites. Solid-state reactions in the SiC–TiO 2 –MgO system were investigated during experimental procedures employing thermodynamic computing. Chemical kinetics of some reactions were highlighted and discussed, including mutual displacement reaction of SiC + TiO 2 = = TiC + SiO 2 to form TiC, the acid-based reaction of MgO with SiO 2 or TiO 2 to form Mg-silicates (Mg 2 SiO 4 , MgSiO 3 ) or Mg-titanates (Mg 2 TiO 4 , MgTiO 3 , MgTi 2 O 5 ), the reduction reaction of 2TiO 2 + C = Ti 2 O 3 + CO (g) with the involvement of excessive TiO 2 . The appearance of Ti 2 O 3 may also be due to significant surface defects of rutile TiO 2 (110) derived from its bulk Ti 3+ defects. However, Mg-silicates and Mg-titanates were not found in the design of the current SiC–TiO 2 –MgO system but the oxide design of the MgO–TiO 2 –SiO 2 system. As the SiC–TiO 2 –MgO ternary system was extended to the SiC–SiO 2 –TiC–TiO 2 –MgO quinary system, the phase relations form a combination of the TiC–SiC phase relations with all salts of the TiO 2 –MgO–SiO 2 system. Experiments confirmed the formation of TiC and its coexistence with SiC and all binary compounds of the TiO 2 –MgO–SiO 2 system, specifying an interaction in the SiC–SiO 2 –MgO–TiO 2 –TiC system. The phase relations of the quinary system were established, followed by constructing its phase diagram relations at 1400°C, which would be beneficial for the compositional design of TiC–SiC, TiC–ceramic, and SiC–ceramic composites.

研究领域: 材料科学 · 化学工程
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CONSTRUCTION AND BUILDING MATERIALS · 2025 · IF 8

Development of PTMEG/MDI-based solid-solid phase change materials for asphalt pavements deicing

Wenxiu Jiao,Jiaxing Zhang,Zhiyong Zhang,Aimin Sha,Meng Jia

Adding phase change materials (PCMs) to asphalt pavements can effectively reduce temperature sensitivity and delay snow and ice accumulation. This study aims to develop solid-solid phase change materials (SSPCMs) for asphalt pavements, with a focus on winter road de-icing. First, the suitability of polyethylene glycol (PEG) and polytetramethylene ether glycol (PTMEG) with varying molecular weights as soft segments was systematically evaluated based on phase change performance, thermal stability, phase change cycling stability, and specific heat capacity. SSPCMs were synthesized using a two-step solution polymerization method, with successful synthesis confirmed by FTIR analysis. The influence of different soft-to-hard segment ratios on phase change performance was also examined. PTMEG2000 exhibited excellent performance, with an exothermic phase change temperature range from 8.5°C to -1.2°C and an enthalpy of 94.3 J/g. Its thermal decomposition onset temperature was 266.05°C, and its performance remained stable after 20 thermal cycles. The incorporation of hard segments led to a reduction in both phase change enthalpy and the initial phase change temperature. At a molar ratio of 4,4′-diphenylmethane diisocyanate (MDI) to PTMEG2000 of 2.4:1, the phase change temperature range was 4.1°C to -5.1°C, with an enthalpy of 37.1 J/g, demonstrating great potential as a de-icing material for roads in cold climates.

研究领域: 材料科学 · 土木工程
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ISIJ INTERNATIONAL · 2017 ·Vol. 57 ·期 1 ·62-67 · IF 1.11

Reaction between CaO and Fe3O4 under CO–CO2 Atmosphere at 800°C–1100°C

Zijian Su,Yuanbo Zhang,Yingming Chen,Guanghui Li,Tao Jiang

A considerable amount of works were focused on the formation mechanism of calcium ferrite phases during the iron ore sintering process, especially under various O2 content atmospheres at temperatures higher than 1100°C. But little attention has been paid on reactions between CaO and iron oxides in CO–CO2 atmospheres at lower temperatures. In this study, the solid state reaction mechanisms between CaO and Fe3O4 under CO–CO2 atmospheres at 800°C–1100°C were revealed by using XRD, VSM, etc. The results indicated that Ca2Fe2O5 was easily formed under 5–50 vol% CO/(CO+CO2) atmosphere above 850°C via the reaction of 6CaO + 2Fe3O4 +CO2 = 3Ca2Fe2O5 + CO and the reaction would be promoted with increasing the roasting temperature. In the CO–CO2 atmosphere, Fe3O4 is easily oxidized to Fe2O3 in the presence of CaO because CO2 components act as oxidative medium for the oxidation of Fe2+ to Fe3+.

CAS / MDL: 1305-78-8 1317-61-9
研究领域: 冶金学 · 材料科学
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ANALYTICAL SCIENCES · 2022 ·Vol. 38 ·期 1 ·105-112 · IF 1.967

Nanofibers comprising polystyrene and zinc acetate for extraction of salivary histidine prior to its determination by HPLC–DAD

Wu Xiaoxiao,Huang Jingjing,Zhang Chi,Kang Xuejun

A novel nanofiber-based solid phase extraction (NFSPE) coupled with HPLC–DAD was developed for the determination of salivary histidine, a new potential index of physiological events. The treatment of the sample was based on a coupling reaction of histidine with the diazotization products of sulfanilic acid and sodium nitrite in a slightly alkaline medium, followed by NFSPE. Nanofibers comprising polystyrene and zinc acetate were used as a novel solid-phase sorbent to extract derived histidine via the chelation of Zn 2+  with the imidazole group in the analyte. The eluted target compound was analyzed by HPLC–DAD. Good linearity was achieved with the concentrations of histidine ranging from 0.645 to 64.5 µM; the detection limit was 0.193 µM. The intra-day and inter-day coefficients of variation were less than 8.0%. The method was successfully applied to the determination of salivary histidine in the subjects exposed to a public speaking stress. Graphical abstract

CAS / MDL: 71-00-1
研究领域: 分析化学 · 生物医学 · 材料科学
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THERMOCHIMICA ACTA · 2021 · IF 3.115

Study on properties and phase transformation mechanism of oil-based solid-solid phase change materials

Yakun Wu,Nana Pan,Xinghui Li,Zhenping You,Miao Tang,Yue Dong,Xiaoyan Zhou,Minzhi Chen

Polymeric solid-solid phase change materials (PSSPCMs) can essentially solve the leakage problem of physically composited solid-solid phase change materials, but the phase change enthalpies, which are usually far lower than the theoretical values, limit their applications. In this work, three PSSPCMs were prepared by co-esterification and polymerization with different amount of stearic acid (SA). The PSSPCMs suffered from lower crystallinities and activation energies at transition than pure SA, indicating that confinement of polymeric network on crystalline domains may lead to the decrease of enthalpy. According to analysis from generalized two-dimensional correlation Fourier transform infrared, the polymer network confinement in PSSPCMs mainly restricted the vibrations of ν as CH 3 , νCH , and ν s CH 3 . In-depth understanding of the interaction between the crystalline chains and the polymeric networks would be beneficial for molecule design of novel PSSPCMs with high enthalpy.

研究领域: 材料科学 · 化学工程 · 聚合物化学
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