DMF Solution Research Articles

Synthesis, And Characterization Of Five New Metal Transition Complexes Derived From The Schiff Base Ligand N' 1 ,N' 4 -Bis(2- Hydroxybenzylidene)Succinohydrazide (H4L)

Schiff base ligand N'1 ,N'4 -bis(2-hydroxybenzylidene)succinohydrazide (H4L) was synthesized via condensation of salicylaldehyde and succinohydrazide in ethanol. The complexes were obtained from 1:2:1 (H4L/LiOH/MCl2 .nH2O) molar ratio reactions, yielding compound formulated as [M2(H2L)2] .nH2O, where M=Mn(II, Fe(II), Co(II), Ni(II) and Cu(II). Elemental analysis, 1H and 13C NMR, FT-IR and UV-Visible spectroscopies were used for the characterization of the ligand. The complexes were structurally studied using FT-IR, UV-Visible spectroscopies, conductance, and magnetic susceptibility measurements. All complexes are non-electrolytes in DMF solutions. In each complex unit two ligand molecules acting in hexadentate fashion bridges two metal ions are present. Thus, each metal ion of the binuclear unit is coordinated to two azomethine nitrogen atoms, two phenolate oxygen atoms and two carbonyl oxygen atoms, resulting in a hexacoordinated metal ion. The environment around each metal ion is described as octahedral geometry owing to the results of the magnetic susceptibility measurement and the UV-visible spectra analyses.

Recovery of lead from perovskite solar cells using ion-exchange resin

Recent developments in perovskite solar cells (PSCs) yielded a power conversion efficiency of 26.56%, making them a practically viable technology. However, the end-of-life lead of (Pb)-based PSCs raises significant environmental concerns. In this study, we used ion-exchange resin to recover Pb from PSCs decomposed by immersion into chlorobenzene and N, N-dimethylformamide (DMF) solvents. We applied inductively coupled plasma atomic emission spectroscopy to the as-prepared pollutants and successfully recovered 100% of Pb from the chlorobenzene and 99.57% from the DMF solution. This study highlights the potential for developing green disposal and recycling methods for emerging PSC technology.

Using novel open-framework copper borovanadate as an effective catalyst in the conversion of cyclohexanol to cyclohexanone

A new open-framework copper borovanadate containing two oxidation states of V4+ and V5+ cations {[Cu5(1,2-dap)10][VV2VIV10B18O54(OH)6(H2O)]}·2H3BO3·9H2O (1,2-dap: 1, 2-propylene diamine) (1) using 1,2-dap as template agent has been successfully prepared. It is composed of five coordination cations [Cu(1,2-dap)2]2+and one borovanadate anion [VV2VIV10B18O54(OH)6(H2O)]10- constructed by one {B18O30(OH)6} and two {V6O18} subunits, as well as two isolated H3BO3 molecules and nine H2O molecules. The compound exhibits for the first time penta-coordinated copper cations, uncoordinated H3BO3 molecules and 1, 2-dap ligands in the series of open-framework borovanadates. Its UV diffuse-reflectance spectrum, Mott-Schottky curve, fluorescent emission, chromaticity and second-order lifetime were investigated in detail. The stable pH range (5.8–2.3) of the borovanadate anion in DMF solution was explored by means of fluorescence and UV spectra. In particular, it showed effective catalytic activity in the conversion of cyclohexanol to cyclohexanone (conversion: 86.8 %, selectivity: 97.4 %). The possible catalytic mechanism for the catalytic reaction had been also established. The studies revealed that the borovanadate could be used as a potential stable catalyst for the selective oxidation of cyclohexanol.

Novel pervaporation separation of PVA/CS blend membranes for the removal of DMF from industrial wastewater

AbstractAchieving satisfactory separation of N, N‐Dimethylformamide (DMF)/water is still challenging in industrial wastewater treatment. To address this issue, a novel method involving pervaporation (PV) separation using polyvinyl alcohol/chitosan (PVA/CS) blend films is proposed. Various characterization methods confirmed the strong compatibility between PVA and CS, and the blending improved their mechanical properties and thermal stability. Heat treatment significantly reduced the swelling degree of the membranes. In a binary aqueous system with low concentrations of DMF, controlled separation can be achieved by adjusting the blending ratio of PVA to CS. The membranes exhibited preferential selectivity for DMF when the CS content is 40–75 wt%, which allowed for the concentration and recovery of DMF. At 20 °C with a feed of 10 wt% DMF solution, 2 h heat‐treated PVA/CS‐50 membrane exhibited the best performance, which could be attributed to its strong hydrogen bonding force, with a total flux of 484.09 g m−2 h−1 and a separation factor of 5.41 for DMF. The PVA/CS blend membranes exhibit excellent acid and alkali resistant and are promising candidates for the separation and recovery of DMF from industrial wastewater by membrane technology.

Synergistic Electronic and Carbonyl Proximity Effects in Electrochemical Hydrogen Evolution Catalyzed by Tetrakis(ethoxycarbonyl)porphyrin Metal Complexes

Electrocatalytic properties of a series of tetrakis(ethoxycarbonyl)porphyrin (TECP) 3d-metal complexes, and the influence of ester groups on the hydrogen evolution reaction (HER), were investigated using trifluoroacetic acid in a 0.1 M [Bu4N]PF6 DMF solution. [Co(TECP)], [Ni(TECP)], and [Cu(TECP)] exhibited three redox couples, with reversibility decreasing at more negative potentials. The third reduction couple was predominantly ligand-centered. Upon addition of TFA, the second reduction waves became catalytic, increasing proportionally with TFA concentration, indicating that the molecular nature of the [M(TECP)] complexes plays a role in facilitating HER. Electrochemical and catalytic studies revealed that [Cu(TECP)] demonstrated the highest Faradaic efficiency (FE) of 98% and the lowest overpotential (0.7 V) while maintaining strong acid tolerance. [Co(TECP)] became effective at overpotentials exceeding 800 mV, suggesting the predominance of EECC pathway at more negative potential. The roles of the ester groups extended beyond a simple inductive effect, as confirmed by controlled potential electrolysis and spectroelectrochemical analyses. The superior HER activity of [Cu(TECP)] compared to [Cu(TPrP)] and [Cu(TPP)] highlights the contribution of the carbonyl groups to catalytic performance. This work underscores the importance of ester groups placement within the porphyrin framework and suggests that meso-ester groups can influence both the stability and catalytic performance, paving the way for further investigations.

The nitrogen heterocyclic dithione rare earth complexes as a multi-response high-efficiency detection sensor for the detection of Cu2+, Co2+, Cr3+, Fe3+, Bi3+ cations and its magnetic study

In this paper, eight novel rare earth complexes Ln(H3L2)(DMA)3(H2O), (Ln = Sm (1), Tb(2), Dy(3), Gd(4), Ho(5), Tm(6), Er(H3L2)(DMA)2(H2O)2 (7), [(μ3-OH)(μ2OH2)3Eu3(H4/3L1)3]n (8)), have been successfully synthesized by solvothermal method. Herein, H4L1 is 1,4,1′,4′-Tetrahydro-[3,3′]bi[[1,2,4] triazolyl]-5,5′-dithione, H6L2 is 5-((5-thioxo-4,5-dihydro-1H,4′H-[3,3′-bi(1,2,4-triazol)]-5′-yl)thio)-1′,4′- dihydro-1H,5′H-[3,3′-bi(1,2,4-triazole)]-5′-thione which was synthesized through in situ condensation reaction of two H4L1. The complexes 1–7 are mononuclear zero-dimensional structures of SmIII, TbIII, DyIII, GdIII, HoIII, TmIII, and ErIII, respectively, and complex 8 is a trinuclear EuIII coordinational polymer. Complexes 1–8 were characterized by the single-crystal X-ray diffraction, powder XRD, infrared spectroscopy and elemental analysis. The luminescence sensing and basic magnetic properties will be studied further. It was found that complexes 2 and 3 could specifically recognize Cu2+, Fe3+, Co2+, Cr3+, and Bi3+ in DMF solution. In 2, the limit of detection (LOD) are 2.33 × 10–5 M, 1.10 × 10–5 M, 2.14 × 10–5 M, 2.15 × 10–5 M for Cu2+, Fe3+, Co2+, Cr3+, respectively, while in 3, the LOD is 7.98 × 10–6 M for Bi3+. Magnetic studies revealed that 3 and 5 exhibit dominant antiferromagnetic interactions.

Synthesis, antimicrobial activity, molecular docking and MD simulation studies, in silico ADME investigations and thermo-acoustic studies of heterocyclic dihydropyrimidine substituted 1,3,4-thiadiazole scaffolds

The connections between the chemical structures and antibacterial properties of different functional groups including organic molecules were examined in this study. we have synthesized a novel series of 1,3,4-thiadiazole hybrids (5a-o) based on 3,4-dihydropyrimidines. After an effective synthesis, the compounds' structure was confirmed by using spectrum techniques like IR, 1H NMR, 13C NMR, and mass spectrometry. Elemental analyses were performed on a Perkin-Elmer 2400 CHN analyzer and the resulting data were within the accepted range (± 0.40) of the calculated values. The in vitro antimicrobial activity of the compounds against a range of bacterial and fungal species. Compound 5i showed potent inhibitory effects against P. aeruginosa with MIC values of 12.5 μg/ml S. aureus and A.niger were positively affected by compound 5k with MIC values of 12.5 μg/ml and 50 μg/ml, respectively. Based on the results, compounds 5a and 5o have moderate activity against C.albicans and E. coli with MIC values of 50 μg/ml and 62.5 μg/ml respectively. Furthermore, molecular docking and molecular dynamics simulations were used to identify the most stable conformation of newly discovered inhibitors. Thermo-acoustical properties of derivatives 5k and 5l in DMSO and DMF solvent have been determined at three different atmospheric pressure temperatures (298.15, 308.15, and 318.15)K. The components of the liquid mixture's molecular interactions have been taken into account to explain these results. The acquired results are interpreted in terms of interactions between solutes and solvents, providing insight into the compounds' potential to form or disrupt structures in DMSO and DMF solutions.

Stability and photophysical study of bright day light fluorescent material and its fabrication in laser patterning and LED application

Developing aggregation-induced emission (AIE) active highly visible fluorescent dyes is of great importance because of its numerous applications. We have successfully developed and synthesized two novel napthalimide based molecules PU1 and PU2, that exhibit bright greenish yellow in day light and vivid green emission when exposed to UV light. Compounds PU1 and PU2 exhibit variable emission behavior at different solvent polarities. Upon raising the solvent polarity from ether to DMF, emission maxima of PU1 and PU2 underwent a bathochromic shift. Additionally, compounds PU1 and PU2 show signs of AIE, which cause a restriction in intramolecular mobility. A distinct self-assembled structure was generated at 30 % aqueous DMF solution following aggregation, as demonstrated by experiments using dynamic light scattering and field emission scanning electron microscopy. Compounds PU1 and PU2 have been blended with poly(urethane) to develop a polymeric film. Tensile strain studies, and TGA, DSC analyses were used to examine the thermal/mechanical stability of PU films. The photostability of PU1 and PU2 in both solution and polymeric film was examined using a 5-h UV-beam irradiation. Furthermore, in the presence of trifluoroacetic acid, the blended polymeric film and 365 nm LED light coated material exhibits distinct colorimetric and fluorimetric transformations. Finally, laser-induced periodic surface structure (LIPSS) pattern processing on PU1 coated substrates can be extended for optical applications.

The crystal engineering of 3d-metal with two tetrazole-phenyl-carboxylate linkers and multiple post-synthetic metal exchange

Ligand with mixed-groups contributes to the construction of special structure motif with novel properties, yet it is challenging to understand and regulate the competitive coordination of different functional groups toward metal ions. Herein, the crystal engineering for MOF construction from two linear di-topic linkers of 4-(1H-tetrazol-5-yl)benzoic acid (H2tzba) and the longer 4′-(1H-tetrazol-5-yl)-[1,1′-biphenyl]-4-carboxylic acid (H2tzbba) featuring dual groups of phenyl-carboxylate and tetrazole, with three typical 3d metal ions (Mn2+, Fe2+ and Zn2+) were investigated. A series of five new MOFs, that are [Mn3(tzba)3(dmf)4]·11dmf (1, dmf = N,N-Dimethylformamide), [Mn(tzba)(H2O)] (2), [Zn2(tzba)2(dmf)]·0.5dmf (3), [Fe2(tzba)2(dmf)]·0.5dmf (4) and [Zn2(tzbbz)(gac)(dmf)2]·1.5dmf (5), were synthesized under solvothermal reactions. The modified solvent template and temperature effects lead to 3D framework of 1 (dmf solution under 433 K) with [Mn3(tz)3(COO)3] nodes and 1D hexagonal channels, while the 2 (water solution under 373 K) posssesses compact pillared-layer motif from [Mn2(tz)2] nodes. Under changed metal salt reactents but same solvent of dmf, the generated 3 and 4 have isoreticular and porous pillared-layer structure constituted of [M2(COO)2] nodes. The use of tzbba coupled with a crucial auxiliary ligand of glycollic acid, leads to 5 as porous pillared-layer MOFs with 1D rounded channels. The porous flexible skeleton of 1 constructed from [Mn3] node with four coordinated dmf facilitates post-synthetic metal exchange of the Mn2+ by radius similar metal ions following priority of Cu2+ < Zn2+ < Ni2+< Co2+, with maximum exchange percentage ranging from 17 % to 69 %. Time dependent ICP-AES analysis revealed the quite wide feasible solvents for post-synthetic metal exchange, as well as the fine control on substituting degree based on soaking temperature and time. Particularly, the compatible introduce of four different metal ions support the potential of preparing bi-, tri-, tetra- and penta- metal MOF crystals, that can not be obtained by traditional solvothermal reactions.

Slowdown of solvent structural dynamics in aqueous DMF solutions

This study presents a comprehensive investigation into the molecular dynamics of solvation environments through an integrated approach combining Fourier-transform infrared (FTIR) spectroscopy, molecular dynamics (MD) simulations, and two-dimensional infrared (2D IR) spectroscopy. We explore the solvation of an ionic solute (ammonium thiocyanate) in various solvent systems, including N,N-dimethylformamide (DMF), water, and a 0.5 mole fraction of DMF in water, aiming to unravel the intricate interplay between solute-solvent interactions and solvent dynamics across diverse solvation environments. By integrating FTIR spectral analysis with radial distribution functions and coordination numbers obtained from MD simulations, we decipher the solvent composition around the solute molecule. Analysis of 2D IR spectra and hydrogen bond, as well as dipolar autocorrelation function from MD simulations, further elucidates the nuances of solute-solvent interactions, highlighting the impact of solvent dynamics on solvation structures. Our results reveal a significant slowdown of the solvent structural dynamics in the equimolar binary solvent mixture compared to the neat solvents. This slowdown underscores the complex relationship between solute-solvent interactions and solvent dynamics. The integration of FTIR, MD simulations, and 2D IR spectroscopy provides a unified framework for obtaining a holistic understanding of solvation dynamics, offering valuable insights into the underlying molecular mechanisms governing solute-solvent interactions in complex systems. These results pave the way for future studies to delve deeper into the molecular intricacies of solvation phenomena.

Achieving Inkjet‐Printed 2D Tin Iodide Perovskites: Excitonic and Electro‐Optical Properties

AbstractCurrently, there is a great demand for non‐toxic lead‐free halide perovskites as active materials for solar cells, light‐emitting diodes and other optoelectronic devices. Although an essential progress has been made using tin(II) halide perovskites, still greater efforts are needed to improve their stability and manufacture films and devices under a scalable technology. The first goal of the work is to achieve suitable physical properties of 2D Sn(II) polycrystalline perovskite films obtained by the industrially scalable inkjet printing deposition technique. In the present work, inks of 2D tin(II) halide perovskite 2‐thiopheneethylammonium tin(II) iodide, TEA2SnI4, have been successfully formulated in DMF (toxic) and DMSO (non‐toxic) solutions and using appropriate additives (SnF2 and reducing agents) for improving the stability of the inks and the resulting films. Room‐ and low‐temperature excitonic photoluminescence (PL), charge carrier recombination dynamics and µ‐PL is used to explain the observed two excitonic bands, which are associated to the bulk and edges of perovskite grains nanoplatelet‐like composing the polycrystalline films. Promising electro‐optical properties are also obtained in the TEA2SnI4 films inkjet‐printed from DMSO formulations onto ITO‐interdigitated electrodes, such as low dark currents, ≈10 – 20 nA at 10 V of bias voltage, and high responsivities ≈1–20 A/W.

THE EFFECT OF CHEMICAL STRUCTURE OF VINYL CHLORIDE BASED POLYMERS ON ITS THE COMPATIBILITY WITH POLYURETHANEUREA ELASTOMER

The effect of the chemical structure of vinyl chloride-based polymers, such as poly(vinyl chloride) (PVC), chlorinated PVC (cPVC), vinyl chloride/vinylidene chloride copolymer VCVD-40TM, vinyl chloride/vinyl acetate copolymer А-15TM on its compatibility with poly(ether-urethane)urea elastomer (PUU) was studied by DSC and FTIR spectroscopy. The segmented PUU was synthesized by prepolymer approach in N,N-dimethylformamide (DMF) solution using poly(propylene glycol) of number-averaged molecular weight (Mn) of 1000 Da, 2,4-tolylenediisocyanate and tolylene 2,4-diamine as a chain extender at a molar ratio of 1:2:1. PUU/vinyl chloride-based polymer blends was prepared by solution casting technique vie DMF solution. It was found a compatibility of PUU based blends containing 30 % PVC (PUU/30PVC blend) or cPVC (PUU/30cPVC) were initiated by strong hydrogen bonding. As a result, the blends are characterized by single wide relaxation transition. A glass transition temperature (Тс) of PUU/30PVC composite is similar to the theoretical one (ТFс), which is calculated using the Flory-Fox equation, whereas Тс value of PUU/30cPVC composite is higher than ТFс. Introducing polar vinyl acetate or vinylidene chloride fragments into vinyl chloride-based polymer macrochains suppresses the compatibility of components of the polymer blends and initiates the formation of a biphase microheterogeneous structure. The formation of intermolecular hydrogen bonding network at the interface in polymer-polymer blends is confirmed by FTIR spectroscopy. Comparative analysis of experimental and theoretically calculated (additive) tensile characteristics of polymer blends demonstrates their substantial dependence on interface interactions between the constituents. The highest strengthening effect was observed for cPVC or PVC-containing nanocomposites.

A new 3D Zn(II)‐based MOF with gra topological network as a photocatalyst for antibiotic degradation

A novel zinc‐based metal–organic framework (Zn‐MOF), designated as [Zn3(L)(bpyp)2(HCOO)3·2DMF·H2O] (1), was synthesized using 2,5‐bis(pyrid‐4‐yl)pyridine (bpyp), 1,3,5‐benzenetricarboxylic acid (H3L), and Zn(CH3COO)2·2H2O in a DMF solution. Single‐crystal X‐ray diffraction analysis revealed that MOF 1 crystallizes in the monoclinic system with a C2/c space group, featuring a (3,5)‐connected binodal network. The structural integrity and characteristics of MOF 1 were confirmed by Fourier transform infrared (FT‐IR), thermal gravimetric analysis (TGA), powder X‐ray diffraction (PXRD), and Brunauer–Emmett–Teller (BET) analyses, showing type IV isotherms indicative of microporous structures. The photocatalytic efficiency of MOF 1 was evaluated for the degradation of various antibiotics under UV light, with nitrofurantoin (NFT) demonstrating the highest degradation rate of 83.9% at an optimal concentration of 40 ppm and catalyst loading of 5 mg. The degradation process followed a pseudo‐first‐order kinetic model with a rate constant of 0.02492 min−1. Radical trapping experiments identified superoxide radicals (O2˙−) and holes (h+) as the predominant reactive species, while hydroxyl radicals (˙OH) played a negligible role. Reusability tests over four cycles confirmed the stability and durability of MOF 1, with consistent photocatalytic performance and unchanged structural morphology as evidenced by PXRD and SEM analyses. The proposed mechanism involves photoinduced electron–hole pair generation, with subsequent formation of reactive oxygen species (ROS) facilitating NFT degradation. This study highlights MOF 1 as a promising photocatalyst for environmental remediation, specifically for the efficient degradation of pharmaceutical contaminants in aquatic systems, providing insights into its structural properties, photocatalytic activity, and underlying degradation mechanisms.

Cd-Ln (Ln = Pr, Sm, Yb and Nd) heteronuclear complexes based on the linear chain ether Schiff base: Structural regulation and fluorescence properties

Four structurally different Cd-Ln heteronuclear complexes based on the linear chain ether Schiff base ligand (bis(3-methoxysalicylidene)-3-oxapentane-1,5-diamine (H2L) and the co-ligands 4,4′-bipyridine (bipy) or isonicotinate (IN), with composition [PrCd2L2(CH3COO)2](NO3)·CH2Cl2 (1), {[SmCdL(bipy)(NO3)3]·CH2Cl2·CH3CH2OH}n (2), [YbCdL(IN)(NO3)(CH3COO)]n (3) and {[Nd2Cd2L2(IN)2(NO3)2(CH3OH)2(CH3COO)](NO3)}n (4), have been synthesized by interfacial diffusion methods. Structural regulation is achieved by changes in the co-ligands or Ln(III) ions of different radii: Single crystal X-ray analysis determined that 1 is a trinuclear cluster with the Pr(III) ion as a joint bridging of two CdL coordination units; 2 and 3 are both infinite one-dimensional zigzag coordination polymers consisting of CdLnL secondary units through coordination bridging bipy or IN; 4 is a two-dimensional graphene laminate structure formed by two types of CdNdL secondary units bridged by both IN and acetate simultaneously. In the solid state, the complexes 1–4 all exhibit fluorescence peaks based on H2L with blue shift and enhancement. The order of fluorescence peaks intensity of the complexes in N,N-dimethylformamide (DMF) solution is consistent with that in the solid state. Moreover, the corresponding characteristic emissions of Sm(III) ion in complex 2 can be observed in the fluorescence spectra in either solid state and DMF solution, indicating that [CdL] unit is suitable for the sensitization of Sm(III) ion.

Ultrahigh proton conductivity of four ionic hydrogen-bonded organic frameworks based on functionalized terephthalates

Recently, the utilization of hydrogen-bonded organic frameworks (HOFs) with high crystallinity and inherent well-defined H-bonding networks in the field of proton conduction has received increasing attention, but obtaining HOFs with excellent water stability and prominent proton conductivity (σ) remains challenging. Herein, by employing functionalized terephthalic acids, 2,5-dihydroxyterephthalic acid, 2-hydroxyterephthalic acid, 2-nitro terephthalic acid, and terephthalic acid, respectively, four highly water-stable ionic HOFs (iHOFs), [(C8H5O6)(Me2NH2)]∙2H2O (iHOF 1), [(C8H5O5)(Me2NH2)] (iHOF 2), [(C8H4NO6)(Me2NH2)] (iHOF 3) and [(C8H5O4)(Me2NH2)] (iHOF 4) were efficiently prepared by a straightforward synthesis approach in DMF and H2O solutions. The alternating-current (AC) impedance testing in humid conditions revealed that all four iHOFs were temperature- and humidity-dependent σ, with the greatest value reaching 10-2 S·cm−1. As expected, the high density of free carboxylic acid groups, crystallization water, and protonated [Me2NH2]+ units offer adequate protons and hydrophilic environments for effective proton transport. Furthermore, the σ values of these iHOFs with different functional groups were compared. It was discovered that it dropped in the following order under 100 °C and 98 % relative humidity (RH): σ iHOF 1 (1.72 × 10−2 S·cm−1) > σ iHOF 2 (4.03 × 10−3 S·cm−1) > σ iHOF 3 (1.46 × 10−3 S·cm−1) > σ iHOF 4 (4.86 × 10−4 S·cm−1). Finally, we investigated the causes of the above differences and the proton transport mechanism inside the framework using crystal structure data, water contact angle tests, and activation energy values. This study provides new motivation to develop highly proton-conductive materials.

Fabrication and regulation of self-assembled nanostructures of benzene-1,3,5-tricarboxamide derivatives

A variety of supramolecular structures of benzene-1,3,5-tricarboxamide derivatives (BTAs), such as helixes and nanosheets, have been fabricated. However, how to regulate the self-assembly behavior through molecular design and control of experimental conditions, and thus to form supramolecular structures with different morphologies is still a topic that needs to be further explored. In this paper, two kinds of BTAs with different end groups, i.e. terpyridine and carboxyl were synthesized, which are referred to as L and A, respectively. Their self-assembly behaviors in DMF/aqueous solution were investigated by adding the DMF solution of BTAs into the aqueous solution dropwise. It was found that the two BTAs exhibited different self-assembly behaviors. L self-assembled into helical nanowires and nanosheets in the mixed media at lower and higher metal ion concentrations. However, A formed multilayer vesicles and nanotubes at lower and higher concentrations of A molecules. Such a difference was ascribed to their different molecular structures and therefore the different amphiphilicity. The more hydrophobic L molecules could escape from DMF droplets and self-assembled with the help of supramolecular interactions. The more amphiphilic A molecules were prone to adsorb at the oil/water interface to form layered films. The relative strength of coordination interaction determined the self-assembly behavior of L and the formation of helical nanowires and nanosheets, and the packing mode of A molecules at the oil/water interface determined the formation of vesicles and nanotubes. In addition, the formed vesicles of A were responsive to pH.

Integration of UV Spectrophotometry Method For Simultaneous Estimation of Fluconazole and Efinaconazole in Nanoparticle Loaded Hydrogel

The goal of this study was to create and validate a UV spectrophotometric method for fluconazole and efinaconazole. Ultraviolet spectroscopy was employed at 255 nm for fluconazole and 268 nm for efinaconazole, using samples prepared in a DMF and phosphate buffer solution with a pH of 4.9. The method demonstrated strong linearity with a correlation coefficient of 0.999. Following ICH guidelines, the validity of the method was assessed for various parameters, including accuracy, precision, limit of detection (LoD), limit of quantification (LoQ), recovery study, and range. The simplicity, time efficiency, and cost-effectiveness of UV spectroscopy were key factors in its selection over HPLC technique, which is known for being expensive and time-consuming with potential susceptibility to various factors affecting determination. Through repeated experiments and meticulous sampling, the method exhibited linearity, accuracy, repeatability, and lack of errors. It was also found to be selective, specific, and cost-effective, affirming its reliability. Moreover, the use of a consistent solvent throughout the experimental work ensured that the method was free from interference by any excipients. Overall, the proposed UV spectrophotometric method was deemed simple, rapid, precise, accurate, and sensitive, making it suitable for routine analysis of fluconazole in both single and combined forms

Synthesis, characterization, photoluminescence properties, cytotoxic activities, molecular docking, and thermogravimetric analysis of a novel bis-N-carboxamide ligand and its Cu(II) binuclear complex

A new bis-N-carboxamide ligand (H2L) was synthesized from reaction of dibenzoylaceticacid- N-carboxyethylamide with p-phenylenediamine. The binuclear metal complex of the new ligand was prepared from Cu(II) salt. The structures of the synthesized compounds were confirmed using elemental analysis, UV–Vis, IR, 1H NMR, 13C NMR, TGA, and LC-MS/MS spectroscopy. The stoichiometric ratio of H2L-Cu2+ was found to be 2:2 (L:M) by the use of Job’s graph. The photoluminescence properties of the ligand and Cu(II) complex was investigated in DMF solution. The ligand is highly emissive upon excitation at 291 nm. The coordination of the ligand to the Cu(II) ion caused quenching of the emission band along with the red shift. The Cu complex did not affect healthy cells at the dose administered, but showed toxic effects at concentrations close to the ligand, suggesting that the Cu complex may be a potential anticancer drug. In addition, molecular docking results indicate that amino acids Asp776 and Met742 generated π-Anionic and π-Sulfur interactions with the phenolic portions of the molecule. There was a π-sigma connection between the ligand and the amino acid Leu820, and a π-alkyl interaction between the ligand and the amino acids Val702 and Ala719.

Core-Shell Double Gyroids Directed by Selective Solvation for ABC Triblock Terpolymers.

The formation of ABC triblock terpolymers through solution casting is still challenging. In this study, core-shell double gyroid network structures are fabricated via solution casting using poly(2,2,2-trifluoroethyl methacrylate) (PTFEMA) (F)-b-[poly(4-vinylpyridine) (P4VP) (P)]-b-[polystyrene (PS) (S)] (FPS) triblock terpolymers in N,N-dimethylformamide (DMF). Upon heat treatment, the polymer tends to form a sphere-in-lamellar structure at the F/S interface. Given the solubility properties of each component in DMF, it is anticipated that the effective volume fraction of F relative to P would increase in concentrated solutions and the effective volume fraction of S would decrease. The microphase-separated structure derived from the DMF solution consistently results in the formation of a network structure composed of a core-shell double gyroid, with F as the matrix, P as the shell, and S as the core, and their periodic lengths gradually increase to 110.8, 131.8, and 162.7nm as increase molecular weights of PS blocks to 13.8, 20.7, and 28.8kg mol-1. Based on the solubility properties of the polymer components highlighted in this study, the solvent selection strategy is broadly applicable to ABC triblock terpolymers featuring various polymer components, offering a more efficient avenue for fabricating core-shell double gyroid structures.

Composition engineering of antimony selenosulfide films using hydrothermal method for efficient solar cells

In this work, Sb2SeyS3-y films were prepared by hydrothermal method at 135 °C for 135 min. The influence of the growth solution volume, the mixing S source, the selenourea concentration and the etching by the N-butyldithiocarbamic acid (BDCA) solution in DMF on the thickness, the content of Sb–O, Se, S and the Se distribution in Sb2SeyS3-y films and the power conversion efficiency (PCE) of solar cells was systematically investigated. When the growth solution volume was 30 mL and the chemical composition of the growth solution was 25 mM antimony potassium tartrate (KSbC4H4O7·0.5H2O), 75 mM Na2S2O3, 5 mM thioacetamide, 10.5 mM selenourea, the PCE of Sb2SeyS3-y solar cells were 9.56 % and 9.41 ± 0.10 %. When Sb2SeyS3-y films were etching by BDCA for 10 min, the PCE of Sb2SeyS3-y solar cells were 10.13 % and 9.95 ± 0.16 %. The result revealed that the homogeneous extent of the Se distribution in Sb2SeyS3-y films can be improved by changing the hydrothermal process parameters and the chemical composition of the growth solution. And the etching by BDCA should be an efficient strategy for eliminating the surface defects and decreasing the gradient of the Se distribution in Sb2SeyS3-y films.