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1.
J Microsc ; 294(2): 225-232, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38558054

RESUMO

Both copper and lithium act as strong fluxes and lower the temperature of the clinker melt formation. Sulphur promotes the stabilisation of more hydraulically active modification of alite M1. It is expected that this combination could produce an alite clinker at significantly lower temperatures with high quality technological parameters. In this paper, the effect of combined oxides of copper, lithium and sulphur addition on the phase composition and clinker structure of Portland cement was investigated. The reference raw meal was prepared from common cement raw materials. Each of the mentioned oxides was added to the reference raw meal in two different concentrations, and 8 combinations were prepared. Chemically pure compounds (NH4)2SO4, CuO and Li2CO3 were used as a source of these oxides. The raw meals were burned to equilibrium at 1450°C. Their phase composition was determined by X-ray diffraction analysis, the microstructure was monitored by optical microscopy, and the microchemistry of the clinker phases was observed by electron microscopy with EDS analysis. It was found that in samples with high lithium or copper content, there is an increase in belite and free lime at the expense of alite. The combination of Cu + Li has the most negative effect, followed by Li alone and Cu alone. The higher SO3 content slightly offsets this negative effect.

2.
J Microsc ; 286(2): 108-113, 2022 05.
Artigo em Inglês | MEDLINE | ID: mdl-34820840

RESUMO

The effect of CuO addition on the phase composition of clinker and the Cu incorporation into the structure of clinker phases was monitored under laboratory conditions. Separate synthesized CuO-doped clinker phases as well as clinkers with different CuO content up to 4 wt.% were characterized by XRD, optical and electron microscopy with EDS analysis. It has been found that Cu tends to form a separate phase or a double oxide with Ca and incorporates in the clinker phases to a limited extent, except for C4 AF. With increasing CuO content in clinker, its phase composition changes, and the size of alite crystals increases.


Assuntos
Cobre , Cobre/química
3.
Solid State Nucl Magn Reson ; 105: 101637, 2020 02.
Artigo em Inglês | MEDLINE | ID: mdl-31830666

RESUMO

Phase composition and molecular mobility were studied using 1H NMR T2 relaxometry in isotactic polybutene-1 (iPB-1) with two polymorphs - form I and II crystals. Several types of NMR relaxation methods and data analysis were evaluated for determining the most reliable way for studying physical phases in iPB-1. Three-phase model provided the most appropriate description of the phase composition in iPB-1, i.e., a crystal-amorphous interface separates the crystalline and the amorphous phases. Due to complex molecular mobility in iPB-1, the amount of rigid fraction should be considered as NMR crystallinity number. Two types of chain segments are present in the amorphous phase: (1) chain segments with anisotropic mobility due to chain anchoring to crystals and chain entanglements; and (2) highly mobile chain end segments. The polymorphic phase II to I transition causes significant immobilization of polymer chains in the crystalline and the amorphous phases. Molecular weight of iPB-1 largely influences phase composition and molecular mobility in crystalline and amorphous phases.

4.
Entropy (Basel) ; 21(6)2019 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-33267296

RESUMO

In this study, the wear behaviour of a powder metallurgically produced AlCoCrFeNiTi0.5 high-entropy alloy (HEAs) is investigated at elevated temperatures. Spark plasma sintering (SPS) of inert gas atomised feedstock enables the production of dense bulk material. The microstructure evolution and phase formation are analysed. The high cooling rate in the atomisation process results in spherical powder with a microstructure comprising two finely distributed body-centred cubic phases. An additional phase with a complex crystal structure precipitates during SPS processing, while no coarsening of microstructural features occurs. The wear resistance under reciprocating wear conditions increases at elevated temperatures due to the formation of a protective oxide layer under atmospherical conditions. Additionally, the coefficient of friction (COF) slightly decreases with increasing temperature. SPS processing is suitable for the production of HEA bulk material. An increase in the wear resistance at elevated temperature enables high temperature applications of the HEA system AlCoCrFeNiTi0.5.

5.
Entropy (Basel) ; 20(7)2018 Jul 02.
Artigo em Inglês | MEDLINE | ID: mdl-33265595

RESUMO

The novel alloying concept of high-entropy alloys (HEAs) has been the focus of many recent investigations revealing an interesting combination of properties. Alloying with aluminium and titanium showed strong influence on microstructure and phase composition. However, detailed investigations on the influence of titanium are lacking. In this study, the influence of titanium in the alloy system AlCoCrFeNiTix was studied in a wide range (molar ratios x = 0.0; 0.2; 0.5; 0.8; 1.0; 1.5). Detailed studies investigating the microstructure, chemical composition, phase composition, solidification behaviour, and wear behaviour were carried out. Alloying with titanium showed strong influence on the resulting microstructure and lead to an increase of microstructural heterogeneity. Phase analyses revealed the formation of one body-centred cubic (bcc) phase for the alloy without titanium, whereas alloying with titanium caused the formation of two different bcc phases as main phases. Additional phases were detected for alloys with increased titanium content. For x ≥ 0.5, a minor phase with face-centred cubic (fcc) structure was formed. Further addition of titanium led to the formation of complex phases. Investigation of wear behaviour revealed a superior wear resistance of the alloy AlCoCrFeNiTi0.5 as compared to a bearing steel sample.

6.
Electrophoresis ; 38(15): 1948-1955, 2017 08.
Artigo em Inglês | MEDLINE | ID: mdl-28432770

RESUMO

We used a permethyl-ß-cyclodextrin chiral stationary phase under reversed-phase conditions for the chiral separation of four aryloxyphenoxy-propionate herbicides (fenoxaprop-p-ethyl, quizalofop-p-ethyl and tefuryl, and haloxyfop-p-methyl) with mixtures of methanol, ethanol, 2-propanol, n-propanol, tert-butanol, or acetonitrile and water as mobile phases and investigated the influence of mobile phase composition and column temperature (from 0 to 50°C) on the separation. The retention factors (k) and selectivity factors (α) of all the herbicides investigated decreased with increasing temperature. The lnα versus 1/T and lnk versus 1/T plots for the enantiomers of the chiral pesticides were linear within the range of 0-50°C with all alcohol/water mixtures constituting the mobile phase, but the lnk versus 1/T plots were nonlinear for all the enantiomers chromatographed in acetonitrile/water mixtures. The thermodynamic parameters based on linear van't Hoff plots were calculated. The influence of temperature and mobile phase composition on the enantioseparation of the solutes has rarely been considered simultaneously. The temperature and the solvents used in the mobile phase, however, were found to have a profound effect on the enantioseparation of these herbicides.


Assuntos
Cromatografia de Fase Reversa/métodos , Herbicidas/análise , Propionatos/análise , Propionatos/isolamento & purificação , beta-Ciclodextrinas/química , Cromatografia de Fase Reversa/instrumentação , Herbicidas/química , Herbicidas/isolamento & purificação , Modelos Lineares , Propionatos/química , Estereoisomerismo , Temperatura
7.
Heliyon ; 10(8): e29665, 2024 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-38644889

RESUMO

In this study, the interplay between the structural complexity, microstructure, and mechanical properties of calcium phosphates (CaPs) derived from fish bones, prepared at various calcination temperatures, and their corresponding sintered ceramics was explored. Fourier-transform infrared analysis revealed that the calcined powders primarily consisted of hydroxyapatite (HAp) and carbonated calcium hydroxyapatite, with an increasing concentration of Mg-substituted ß-tricalcium phosphate (ß-TCP) as the calcination temperature was increased. X-ray diffraction patterns showed enhanced sharpness of the peaks at higher temperatures, indicating a larger crystallite size and improved crystallinity. The ceramics exhibited a significantly larger crystallite size and an increased concentration of the ß-TCP phase. Rietveld analysis revealed a larger volume of the ß-TCP phase in the ceramics than in their calcined powders; this could be attributed to a newly formed ß-TCP phase due to the decomposition of HAp. Extended X-ray absorption fine structure analysis revealed the incorporation of Mg in the Ca2 site of HAp, Ca2 site of ß-TCP, and Ca5 site of ß-TCP, with a higher substitution of Mg in the Ca5 site of ß-TCP at elevated temperatures. The mechanical properties of HAp ceramics can be improved by increasing the calcination temperature because of their improved relative density and dense porous structure at elevated temperatures. This comprehensive investigation sheds light on the phase evolution, microstructural changes, and consequential impact on the mechanical properties of CaPs derived from fish bones, thereby facilitating the development of tailored CaP ceramics for biomedical applications.

8.
Foods ; 13(12)2024 Jun 20.
Artigo em Inglês | MEDLINE | ID: mdl-38928884

RESUMO

To decrease the lipid content in water-in-oil (W/O) emulsions, high internal phase Pickering W/O emulsions (HIPPE) were fabricated using magnetic stirring using a combination of monoglyceride (MAG) oleogel and polyglycerol polyacrylate oleate (PGPR) as stabilizers. Effects of MAGs (glyceryl monostearate-GMS, glycerol monolaurate-GML and glycerol monocaprylate-GMC) and internal phase components on the formation and properties of HIPPEs were investigated. The results showed that milky-white stabilized W/O HIPPE with up to 85 wt% aqueous phase content was successfully prepared, and the droplet interfaces presented a network of MAG crystals, independent of the MAG type. All HIPPEs exhibited great stability under freeze-thaw cycles but were less plastic. Meanwhile, GML-oleogel-based HIPPEs had larger particle size and were less thermal stable than GMS and GMC-based HIPPEs. Compared to guar gum, the internal phase components of sodium chloride and sucrose were more effective in reducing the particle size of HIPPEs, improving their stability and plasticity, and stabilizing them during 100-day storage. HIPPEs presented great spreadability, ductility and plasticity after whipping treatment. This knowledge provides a new perspective on the use of oleogels as co-stabilizers for the formation of W/O HIPPEs, which can be used as a potential substitute for creams.

9.
Materials (Basel) ; 17(3)2024 Jan 26.
Artigo em Inglês | MEDLINE | ID: mdl-38591481

RESUMO

The main strengthening mechanism for Inconel 718 (IN718), a Ni-based superalloy, is precipitation hardening by γ' and γ″ particles. It is thus essential, for good alloy performance, that precipitates with the desired chemical composition have adequate size and dispersion. The distribution of the γ' and γ″ phases and their chemical composition were investigated in the nickel-based Inconel 718 superalloy by taking advantage of the new capabilities of scanning transmission electron microscopy and energy-dispersive X-ray spectrometry using a windowless multiple detector, a high-brightness Schottky electron gun, and a spherical aberration corrector in the illumination probe optics. A small routine was developed to deconvolute the respective compositions of γ' and γ″ nanoprecipitates embedded in the γ matrix. Keeping the electron probe current low enough-a few hundred pA-prevented excessive irradiation damage during the acquisition of element maps and brought their spatial resolution down to the atomic column level to track their element compositions. The present results agree with and complement atomic probe tomography observations and Thermo-Calc predictions from the literature. The presence of an Al enrichment at the γ'/γ″ interface-which may control the γ″ phase coarsening-is observed in the last row of Al-Nb-Ti columns along this interface. In addition, a few columns with similar composition changes are found randomly distributed in the γ' phase.

10.
J Chromatogr A ; 1714: 464551, 2024 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-38065026

RESUMO

The chromatographic retention of carbohydrates on chelating stationary phase loaded with different metal ions was studied under conditions of hydrophilic interaction chromatography (HILIC). The chelating stationary phases represented silica microparticles with immobilized 2-hydroxyethyliminodiacetic acid (HEIDA) groups in loose form and saturated with Ca2+, Pb2+, and La3+form. The role of loaded metal ion, the acetonitrile and methanol content in the mobile phase, buffer pH and column temperature on the retention of l-(+)-arabinose, d-(+)-maltose, l-(+)-rhamnose, d-(+)-lactose, d-(+)-xylose, glucose, fructose, sucrose, mannose, maltotriose and d-(+) raffinose was studied. The investigation was mainly focused on possible contribution of the complexation in the stationary phase on retention of carbohydrates as well as on effect of the presence metal ion in HEIDA-silica on resulting HILIC behavior of. It is shown that adsorbents with immobilized metal complexes have a good potential for the separation of organic ligands under HILIC mode.


Assuntos
Carboidratos , Dióxido de Silício , Cromatografia Líquida/métodos , Carboidratos/química , Dióxido de Silício/química , Temperatura , Interações Hidrofóbicas e Hidrofílicas
11.
Materials (Basel) ; 16(5)2023 Feb 27.
Artigo em Inglês | MEDLINE | ID: mdl-36903076

RESUMO

The aim of this paper is to study the effect of variation in the component ratio of (1-x)Si3N4-xAl2O3 ceramics on the phase composition, strength and thermal properties of ceramics. To obtain ceramics and their further study, the solid-phase synthesis method combined with thermal annealing of samples at a temperature of 1500 °C typical for the initialization of phase transformation processes was used. The relevance and novelty of this study lies in obtaining new data on the processes of phase transformations with a variation in the composition of ceramics, as well as determining the effect of the phase composition on the resistance of ceramics to external influences. According to X-ray phase analysis data, it was found that an increase in the Si3N4 concentration in the composition of ceramics leads to a partial displacement of the tetragonal phase of SiO2 and Al2(SiO4)O and an increase in the contribution of Si3N4. Evaluation of the optical properties of the synthesized ceramics depending on the ratio of the components showed that the formation of the Si3N4 phase leads to an increase in the band gap and the absorbing ability of the ceramics due to the formation of additional absorption bands from 3.7-3.8 eV. Analysis of the strength dependences showed that an increase in the contribution of the Si3N4 phase with subsequent displacement of the oxide phases leads to a strengthening of the ceramic by more than 15-20%. At the same time, it was found that a change in the phase ratio leads to the hardening of ceramics, as well as an increase in crack resistance.

12.
Materials (Basel) ; 16(5)2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36903148

RESUMO

Cenospheres are hollow particles in fly ash, a by-product of coal burning, and are widely used as a reinforcement when developing low-density composites called syntactic foams. This study has investigated the physical, chemical, and thermal properties of cenospheres obtained from three different sources, designated as CS1, CS2, and CS3, for the development of syntactic foams. Cenospheres with particle sizes ranging from 40 to 500 µm were studied. Different particle distribution by size was observed, and the most uniform distribution of CS particles was in the case of CS2: above 74% with dimensions from 100 to 150 µm. The CS bulk had a similar density for all samples and amounted to around 0.4 g·cm-3, with a particle shell material density of 2.1 g·cm-3. Post-heat-treatment samples showed the development of a SiO2 phase in the cenospheres, which was not present in the as-received product. CS3 had the highest quantity of Si compared to the other two, showing the difference in source quality. Energy-dispersive X-ray spectrometry and a chemical analysis of the CS revealed that the main components of the studied CS were SiO2 and Al2O3. In the case of CS1 and CS2, the sum of these components was on average from 93 to 95%. In the case of CS3, the sum of SiO2 and Al2O3 did not exceed 86%, and Fe2O3 and K2O were present in appreciable quantities in CS3. Cenospheres CS1 and CS2 did not sinter during heat treatment up to 1200 °C, while sample CS3 was already subjected to sintering at 1100 °C because of the presence of a quartz phase, Fe2O3 and K2O. For the application of a metallic layer and subsequent consolidation via spark plasma sintering, CS2 can be deemed the most physically, thermally, and chemically suitable.

13.
Biomimetics (Basel) ; 8(7)2023 Nov 14.
Artigo em Inglês | MEDLINE | ID: mdl-37999188

RESUMO

This study aimed to explore the effects of the full-scale replacement (up to 100%) of Ca2+ ions with Ag1+ ions in the structure of brushite (CaHPO4·2H2O). This substitution has potential benefits for producing monophasic and biphasic Ca1-xAgxHPO4·nH2O compounds. To prepare the starting solutions, (NH4)2HPO4, Ca(NO3)2·4H2O, and AgNO3 at different concentrations were used. The results showed that when the Ag/Ca molar ratio was below 0.25, partial substitution of Ca with Ag reduced the size of the unit cell of brushite. As the Ag/Ca molar ratio increased to 4, a compound with both monoclinic CaHPO4·2H2O and cubic nanostructured Ag3PO4 phases formed. There was a nearly linear relationship between the Ag ion ratio in the starting solutions and the wt% precipitation of the Ag3PO4 phase in the resulting compound. Moreover, when the Ag/Ca molar ratio exceeded 4, a single-phase Ag3PO4 compound formed. Hence, adjusting the Ag/Ca ratio in the starting solution allows the production of biomaterials with customized properties. In summary, this study introduces a novel synthesis method for the mono- and biphasic Ca1-xAgxHPO4·nH2O compounds brushite and silver phosphate. The preparation of these phases in a one-pot synthesis with controlled phase composition resulted in the enhancement of existing bone cement formulations by allowing better mixing of the starting ingredients.

14.
Materials (Basel) ; 16(23)2023 Nov 24.
Artigo em Inglês | MEDLINE | ID: mdl-38068057

RESUMO

The article reveals for the first time the features of nanoparticle morphology, phase compositions, and their changes when heating FePt and CoPt nanoalloys. Nanoparticles were obtained by co-reduction of precursor solution mixtures with hydrazine hydrate. The features were found by a complex of methods of X-ray diffraction (in situ XRD and X-ray scattering), TEM HR, and cyclic voltammetry. In addition, adsorbometry results were obtained, and the stability of different nanocluster structures was calculated by the molecular dynamics method. There were only FCC solid solutions in the X-ray patterns of the FePt and CoPt nanoalloys. According to XRD, in the case of nanoparticle synthesis with Fe and Co content less than 10 at. %, the composition of solid solutions was close to or practically equal to the composition of the as-synthesized nanoparticles quantified by inductively coupled plasma optical emission spectrometry. For systems synthesis with Fe and Co content greater than the above, the solubility limits (SLs) of Fe and Co in Pt were set 11.4 ± 0.7 at. % and 17.5 ± 0.6 at. %, respectively. Therefore, there were non-registered XRD extra-phases (XRNDPh-1) in the systems when CFe,Co ≥ SL. This statement was supported by the results of TEM HR and X-ray scattering: the smallest nanocrystals (1-2 nm) and amorphous particles were found, which qualitatively agreed with the sorbometry and SAXS results. Molecular dynamics calculations of stability for FePt and CoPt alloys claimed the structures of the most stable phase corresponded to phase diagrams (A1 and L12). Specific peculiarities of the morphology and compositions of the solid solutions of nanoalloys were established: structural blockiness (domain) and composition heterogeneity, namely, platinum enrichment of internal (deep) layers and homogenization of the nanoalloy compositions at relatively low temperatures (130-200 °C). The suggested model of the formation of nanoalloys during the synthesis, qualitatively, was compliant with the results of electrochemical deposition of FePt films on the surface of various electrodes. When nanocrystals of solid solutions (C(Fe, Co) < SL) were heated above specific temperatures, there were phase transformations with the formation of two-phase regions, with solid solutions enriched with platinum or iron (non-registered XRD phase XRNDPh-2). The newly formed phase was most likely intermetallic compounds, FePt3, CoPt3. As a result of the study, the model was developed, taking into account the nanoscale of the particles: XRDPh (A1, FeaPt1-a) → XRDPh (A1, Fem×a-xPtm-m×a+x) + XRNDPh-2 (Fen×a+yPtn-n×a-y) (here, m + n = 1, m ≤ 1, n ≤ 1).

15.
Materials (Basel) ; 16(22)2023 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-38005101

RESUMO

The alloying compound FeTe2 is a semi-metallic material with low thermal conductivity and has the potential to become a thermoelectric material. Single-phase FeTe2 compounds are synthesized using a two-step sintering method, and the effects of the optimal sintering temperature, holding temperature, and holding time on the thermoelectric properties of the alloy compound FeTe2 are investigated. The phase composition, microstructure, and electrical transport properties of the FeTe2 compound are systematically analyzed. The results show that single-phase FeTe2 compounds can be synthesized within the range of a sintering temperature of 823 K and holding time of 10~60 min, and the thermoelectric properties gradually deteriorate with the prolongation of the holding time. Microstructural analysis reveals that the sample of the alloy compound FeTe2 exhibits a three-dimensional network structure with numerous fine pores, which can impede thermal conduction and thus reduce the overall thermal conductivity of the material. When the sintering temperature is 823 K and the holding time is 30 min, the sample achieves the minimum electrical resistivity of 6.9 mΩ·cm. The maximum Seebeck coefficient of 65.48 µV/K is obtained when the sample is held at 823 K for 10 min; and under this condition, the maximum power factor of 59.54 µW/(m·K2) is achieved. In the whole test temperature range of 323~573 K, when the test temperature of the sample is 375 K, the minimum thermal conductivity is 1.46 W/(m·K), and the maximum ZT is 1.57 × 10-2.

16.
J Colloid Interface Sci ; 640: 270-280, 2023 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-36863183

RESUMO

The phase composition of photocatalyst has a substantial effect on its photocatalytic activity. In this work, the rhombohedral phase ZnIn2S4 was synthesized by a one-step hydrothermal method by using inexpensive Na2S as a sulfur source with the assistance of NaCl. The Na2S as the S source can promote the generation of rhombohedral ZnIn2S4, and the addition of NaCl enhances the crystallinity of the as-prepared rhombohedral ZnIn2S4. The rhombohedral ZnIn2S4 nanosheets had a narrower energy gap, more negative conductive band potential, and higher separation efficiency of photogenerated carriers relative to the hexagonal ZnIn2S4. The as-synthesized rhombohedral ZnIn2S4 exhibited high visible photocatalytic activity with removal efficiencies of 96.7% in 80 min for the methyl orange, 86.3% in 120 min for ciprofloxacin hydrochloride and nearly 100% in 40 min for Cr(VI).

17.
Jpn Dent Sci Rev ; 59: 28-37, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-36819742

RESUMO

Binary titanium-zirconium alloys have been studied as promising alternatives for Ti implants. The commercial Ti-15Zr alloy (Roxolid, Straumann) has been the major subject of numerous binary Ti-Zr alloys-related studies and has gained wide recognition in laboratory studies and clinical practices. However, binary Ti-Zr alloys of other composition ratios are still being investigated by researchers. This review aims to provide information on the potential of binary Ti-Zr alloys other than Ti-15Zr as implant materials in terms of mechanical strengths, chemical or electrochemical corrosion resistance capabilities, and biological performances. In addition, in this review, the Ti-15Zr alloy is discussed only when compared with other binary Ti-Zr alloys. From the included 26 studies, it is confirmed that the mechanical, chemical, electrochemical, and biological properties of Ti-Zr alloys are related to the Ti and Zr composition ratio in the alloy, phase, manufacturing process, and surface treatment. Among the studied alloys, α-or α' phase-Ti-5 wt, 45 wt/30at, and 50 wt. %Zr exhibited relatively more promising results for further investigation. More research is necessary to evaluate the potential for future use of these materials for implants.

18.
Materials (Basel) ; 16(3)2023 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-36770181

RESUMO

Recent trends to improve the aesthetic properties-tooth-like color and translucency-of ceramic dental crowns have led to the development of yttria-stabilized zirconia (Y-TZP) materials with higher stabilizer content. These 5Y-TZP materials contain more cubic or t' phase, which boosts translucency. The tradeoff as a consequence of a less transformable tetragonal phase is a significant reduction of strength and toughness compared to the standard 3Y-TZP composition. This study aims at determining the durability of such 5Y-TZP crowns under lab conditions simulating the conditions in the oral cavity during mastication and consumption of different nutrients. The test included up to 10,000 thermal cycles from 5 °C to 55 °C "from ice cream to coffee" and a chewing simulation representing 5 years of use applying typical loads. The investigation of the stress-affected zone at the surface indicates only a very moderate phase transformation from tetragonal to monoclinic after different varieties of testing cycles. The surface showed no indication of crack formation after testing. It can, therefore, be assumed that over the simulated period, dental crowns of 5Y-TZP are not prone to fatigue failure.

19.
J Chromatogr A ; 1705: 464163, 2023 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-37348226

RESUMO

The present paper illustrates the versatility of the supercritical fluid chromatography (SFC) since, for the first time, four spirooxindole alkaloids (SOAs) including two pairs of isomers were separated by using two types of reversed-phase/ ion chromatography (RP/IC) mixed-mode stationary phases. Two mixed-mode stationary phases (C8SAX and C8SCX) was simultaneously provided dispersive and electrostatic interactions, which were suitable for the separation of such alkaloids. This study tried to provide an in-depth understanding of the SFC separation mechanism of the mixed-mode stationary phase through investigation of the impact of changes in mobile phase composition on alkaloids' retention behavior. On C8SAX, due to the strong electrostatic repulsion, there was a very narrow elution window of the alkaloids, of which behaviors were hardly affected by adding diethylamine in mobile phase. When adding formic acid or acidic ammonium formate, the prolonged retention time of alkaloids was presented because of the shielded effect of formate anions on the electrostatic repulsion. In particular, better peak shape and improved resolution were obtained by using acidic ammonium formate due to the deactivation of silanol groups by ammonium cations. On the other hand, both formic acid and acidic ammonium formate can strengthen the electrostatic attraction of C8SCX, causing difficult elution of the alkaloids. Ammonium cations from either the protonated diethylamine or the ionized ammonium formate, were considered as counter ions to effectively mask the electrostatic attraction of C8SCX, to significantly reduce the retention of alkaloids, but improve the resolution. Finally, utilizing two developed SFC methods, i.e., C8SAX with EtOH+ 10 mM acidic ammonium formate in CO2, or C8SCX with EtOH+0.1% diethylamine in CO2, the baseline separation of corynoxeine and isocorynoxeine, rhynchophylline and isorhynchophylline was achieved within 5 min.


Assuntos
Alcaloides , Compostos de Amônio , Cromatografia com Fluido Supercrítico , Cromatografia com Fluido Supercrítico/métodos , Dióxido de Carbono , Ânions/química , Cátions/química , Alcaloides/análise
20.
Nanomaterials (Basel) ; 13(4)2023 Feb 16.
Artigo em Inglês | MEDLINE | ID: mdl-36839115

RESUMO

A Zr-doped CaO sorbent for high-temperature CO2 capture was fabricated using electrospinning. The nanofiber sorbent with an average filament diameter of about 160 nm is characterized by an initial CO2 uptake capacity of 12.1 mmol/g, a specific surface area of 79 m2/g, an indentation Young's modulus of 520 MPa, and a hardness of 1.6 MPa. After 50 carbonation/decarbonation cycles, the sorbent has a decent CO2 uptake capacity of 9.7 mmol/g due to the uniform distribution of CaZrO3 in the CaO nanofibers to prevent CaO grain growth caused by CaCO3 sintering. It is revealed that the sorbent CO2 uptake capacity decreases both with an increase in the decarbonation temperature and with an increase in the CO2 concentration in the gas flow upon carbonation, where the sorbent CO2 uptake capacity is more sensitive to the decarbonation temperature than to the CO2 concentration in the gaseous stream during carbonation. It is assumed that the electrospun regenerable Zr-doped CaO sorbent is effective for removing CO2 from flue gases.

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