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Cellulose Supported Pd(II) Complex Catalyzed Carbon-Carbon Bonds Formation

Sarkar SM, Rashid SS, Karim KMR, Mustapha SNH, Lian YM, Zamri N, et al.

J Nanosci Nanotechnol, 2019 05 01;19(5):2856-2861.
PMID: 30501791 DOI: 10.1166/jnn.2019.16289

Corn-cobs are an agro-industrial waste and composed of cellulose mostly. In this study cellulose was isolated from the waste corn-cobs and modified to polymeric hydroxamic acid palladium complex 1 and characterized by using a variety of spectroscopic methods such as field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The complex 1 exhibited high catalytic activity towards Suzuki and Heck coupling reactions of activated and deactivated aryl halides to give the respective coupling products with high yield. Moreover, the complex 1 was recovered and recycled five times with no considerable loss of catalytic overall performance.

Matched MeSH terms: Photoelectron Spectroscopy
High-performance interactive analysis of split aptamer and HIV-1 Tat on multiwall carbon nanotube-modified field-effect transistor

Fatin MF, Rahim Ruslinda A, Gopinath SCB, Arshad MKM

Int J Biol Macromol, 2019 Mar 15;125:414-422.
PMID: 30529550 DOI: 10.1016/j.ijbiomac.2018.12.066

Interaction between split RNA aptamer and the clinically important target, HIV-1 Tat was investigated on a biosensing surface transduced by functionally choreographed multiwall carbon nanotubes (MWCNTs). Acid oxidation was performed to functionalize MWCNTs with carboxyl functional groups. X-ray photoelectron spectroscopy analysis had profound ~2.91% increment in overall oxygen group and ~1% increment was noticed with a specific carboxyl content owing to CO and OCO bonding. The interaction between split RNA aptamer and HIV-1 Tat protein was quantified by electrical measurements with the current signal (Ids) over a gate voltage (Vgs). Initially, 34.4 mV gate voltage shift was observed by the immobilization of aptamer on MWCNT. With aptamer and HIV-1 Tat interaction, the current flow was decreased with the concomitant gate voltage shift of 23.5 mV. The attainment of sensitivity with split aptamer and HIV-1 Tat interaction on the fabricated device was 600 pM. To ensure the genuine interaction of aptamer with HIV-1 Tat, other HIV-1 proteins, Nef and p24 were interacted with aptamer and they displayed the negligible interferences with gate voltage shift of 3.5 mV and 5.7 mV, which shows 4 and 2.5 folds lesser than HIV-1 Tat interaction, respectively.

Matched MeSH terms: Photoelectron Spectroscopy/methods
Fulltext Photochemical Synthesis of Nanosheet Tin Di/Sulfide with Sunlight Response on Water Pollutant Degradation

Matmin J, Jalani MA, Osman H, Omar Q, Ab'lah N, Elong K, et al.

Nanomaterials (Basel), 2019 Feb 14;9(2).
PMID: 30769911 DOI: 10.3390/nano9020264

The photochemical synthesis of two-dimensional (2D) nanostructured from semiconductor materials is unique and challenging. We report, for the first time, the photochemical synthesis of 2D tin di/sulfide (PS-SnS₂-x, x = 0 or 1) from thioacetamide (TAA) and tin (IV) chloride in an aqueous system. The synthesized PS-SnS₂-x were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), a particle size distribution analyzer, X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FTIR), thermal analysis, UV⁻Vis diffuse reflectance spectroscopy (DR UV⁻Vis), and photoluminescence (PL) spectroscopy. In this study, the PS-SnS₂-x showed hexagonally closed-packed crystals having nanosheets morphology with the average size of 870 nm. Furthermore, the nanosheets PS-SnS₂-x demonstrated reusable photo-degradation of methylene blue (MB) dye as a water pollutant, owing to the stable electronic conducting properties with estimated bandgap (Eg) at ~2.5 eV. Importantly, the study provides a green protocol by using photochemical synthesis to produce 2D nanosheets of semiconductor materials showing photo-degradation activity under sunlight response.

Matched MeSH terms: Photoelectron Spectroscopy
Measuring the Ultrafast Correlation Dynamics between the Q x and Q y Bands in Chlorophyll Molecules

Khyasudeen MF, Nowakowski PJ, Tan HS

J Phys Chem B, 2019 02 14;123(6):1359-1364.
PMID: 30657672 DOI: 10.1021/acs.jpcb.9b00099

We use two-dimensional electronic spectroscopy to measure the ultrafast correlation dynamics between the Q x and Q y transitions in chlorophyll molecules. We derive a variation to the center line slope method to quantify the frequency fluctuation cross-correlation function, C xy( Tw). Compared with the frequency fluctuation correlation function of the Q y transition, we observe that there is only a minimal correlation between the Q x and Q y transition, even at the ultrashort timescale of ∼100 fs, which then decays to zero in a time scale of ∼2 ps.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Ultraviolet A and Ultraviolet C Light-Induced Reduction of Surface Hydrocarbons on Titanium Implants

Naauman Z, Rajion ZAB, Maliha S, Hariy P, Muhammad QS, Noor HAR

Eur J Dent, 2019 Feb;13(1):114-118.
PMID: 31170762 DOI: 10.1055/s-0039-1688741

OBJECTIVE: The carbon, titanium, and oxygen levels on titanium implant surfaces with or without ultraviolet (UV) pretreatment were evaluated at different wavelengths through X-ray photoelectron spectroscopy (XPS).
MATERIALS AND METHODS: This interventional experimental study was conducted on nine Dio UFII implants with hybrid sandblasted and acid-etched (SLA) surface treatments, divided equally into three groups. Control group A samples were not given UV irradiation, while groups B and C samples were given UVA (382 nm, 25 mWcm2) and UVC (260 nm, 15 mWcm2) irradiation, respectively. The atomic ratio of carbon, titanium, and oxygen was compared through XPS.
RESULTS: Mean carbon-to-titanium ratio and C1 peaks considerably increased in Group A compared to those in experimental Groups B and C. The intensity of Ti2p and O1s peaks was more pronounced for group C compared to that for groups A and B.
CONCLUSIONS: Although the decrease in surface hydrocarbons was the same in both UV-treated groups, the peak intensity of oxygen increased in the UVC-treated group. Thus, it can be concluded that compared with UVA irradiation, UVC irradiation has the potential to induce more hydrophilicity on SLA-coated implants.

Matched MeSH terms: Photoelectron Spectroscopy
Physicochemical characteristics of microbial content in a modified anaerobic inclining-baffled reactor (MAI-BR) treating recycled paper mill effluent (RPME)

Zwain HM, Chang SM, Dahlan I

Prep Biochem Biotechnol, 2019;49(4):344-351.
PMID: 30712465 DOI: 10.1080/10826068.2019.1566144

Microbial content formed in bioreactors plays a significant role in the anaerobic process. Therefore, the physicochemical characteristics of microbial content in a modified anaerobic inclining-baffled reactor (MAI-BR) treating recycled paper mill effluent (RPME) were investigated using Fourier transform infrared (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric (TG), and derivative thermogravimetric (DTG) analyses, scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), Brunauer-Emmett-Teller (BET), and surface area analyzer. FTIR spectra revealed that the microbial content had stronger characteristic peaks corresponding to alcohols, water, lipids carbohydrates, proteins, and mineral compounds. Calcite, muscovite, and lepidolite were the prevalent mineral phases found by XRD analysis. The elemental of these minerals like C, Ca, N, O, and Si was confirmed by XPS results. The microbial content samples from each compartment showed similar thermal behavior. SEM images showed that straight rod-shaped and Methanosaeta-like microorganisms were predominant, whereas C, O, and Ca were noticed by EDS on the surface of granules. The BET surface areas and pores of granules are found to decline throughout the reactor's compartment, where Compartment 1 had the largest values. Thus, the findings of this study establish further understanding of the physicochemical properties of microbial content formed in MAI-BR during the RPME treatment.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Application of Biochar Derived From Pyrolysis of Waste Fiberboard on Tetracycline Adsorption in Aqueous Solution

Xu D, Gao Y, Lin Z, Gao W, Zhang H, Karnowo K, et al.

Front Chem, 2019;7:943.
PMID: 32117859 DOI: 10.3389/fchem.2019.00943

In this study, biochars derived from waste fiberboard biomass were applied in tetracycline (TC) removal in aqueous solution. Biochar samples were prepared by slow pyrolysis at 300, 500, and 800°C, and were characterized by ultimate analysis, Fourier transform infrared (FTIR), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET), etc. The effects of ionic strength (0-1.0 mol/L of NaCl), initial TC concentration (2.5-60 ppm), biochar dosage (1.5-2.5 g/L), and initial pH (2-10) were systemically determined. The results present that biochar prepared at 800°C (BC800) generally possesses the highest aromatization degree and surface area with abundant pyridinic N (N-6) and accordingly shows a better removal efficiency (68.6%) than the other two biochar samples. Adsorption isotherm data were better fitted by the Freundlich model (R2 is 0.94) than the Langmuir model (R2 is 0.85). Thermodynamic study showed that the adsorption process is endothermic and mainly physical in nature with the values of ΔH0 being 48.0 kJ/mol, ΔS0 being 157.1 J/mol/K, and ΔG0 varying from 1.02 to -2.14 kJ/mol. The graphite-like structure in biochar enables the π-π interactions with a ring structure in the TC molecule, which, together with the N-6 acting as electron donor, is the main driving force of the adsorption process.

Matched MeSH terms: Photoelectron Spectroscopy
Equilibrium, kinetic and mechanism studies of Cu(II) and Cd(II) ions adsorption by modified chitosan beads

Sutirman ZA, Sanagi MM, Abd Karim KJ, Wan Ibrahim WA, Jume BH

Int J Biol Macromol, 2018 Sep;116:255-263.
PMID: 29746971 DOI: 10.1016/j.ijbiomac.2018.05.031

In this study, the Cu(II) and Cd(II) ions removal behavior of crosslinked chitosan beads grafted poly(methacrylamide) (abbreviated as crosslinked chitosan-g-PMAm) from single metal ion solutions was investigated. The modified chitosan beads presented a remarkable improvement in acid resistance. The batch experiments demonstrated that pH of solution played a significant role in adsorption. It was found that the adsorption of Cu(II) and Cd(II) were optimum at pH 4 and pH 5, respectively. The maximum adsorption capacities for Cu(II) and Cd(II) based on Langmuir equation were 140.9 mg g-1 and 178.6 mg g-1, respectively. Pseudo-second order gave a better fit for adsorption data with respect to linearity coefficients than pseudo-first order suggesting that chemisorption or electron transfer is the dominant mechanism of the metal ions onto crosslinked chitosan-g-PMAm. In addition, X-ray photoelectron spectroscopy (XPS) investigations revealed that adsorption of both metal ions took place on the surfaces of crosslinked chitosan-g-PMAm by chelation through CNH2, CO and CO groups. Overall, the modified chitosan has proved a promising adsorbent for removal of metal ions.

Matched MeSH terms: Photoelectron Spectroscopy/methods
Thermal Calcination-Based Production of SnO₂ Nanopowder: An Analysis of SnO₂ Nanoparticle Characteristics and Antibacterial Activities

Al-Hada NM, Kamari HM, Baqer AA, Shaari AH, Saion E

Nanomaterials (Basel), 2018 Apr 17;8(4).
PMID: 29673195 DOI: 10.3390/nano8040250

SnO₂ nanoparticle production using thermal treatment with tin(II) chloride dihydrate and polyvinylpyrrolidone capping agent precursor materials for calcination was investigated. Samples were analyzed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse UV-vis reflectance spectra, photoluminescence (PL) spectra and the electron spin resonance (ESR). XRD analysis found tetragonal crystalline structures in the SnO₂ nanoparticles generated through calcination. EDX and FT-IR spectroscopy phase analysis verified the derivation of the Sn and O in the SnO₂ nanoparticle samples from the precursor materials. An average nanoparticle size of 4–15.5 nm was achieved by increasing calcination temperature from 500 °C to 800 °C, as confirmed through TEM. The valence state and surface composition of the resulting nanoparticle were analyzed using XPS. Diffuse UV-vis reflectance spectra were used to evaluate the optical energy gap using the Kubelka-Munk equation. Greater calcination temperature resulted in the energy band gap falling from 3.90 eV to 3.64 eV. PL spectra indicated a positive relationship between particle size and photoluminescence. Magnetic features were investigated through ESR, which revealed the presence of unpaired electrons. The magnetic field resonance decreases along with an increase of the g-factor value as the calcination temperature increased from 500 °C to 800 °C. Finally, Escherichia coli ATCC 25922 Gram (–ve) and Bacillus subtilis UPMC 1175 Gram (+ve) were used for in vitro evaluation of the tin oxide nanoparticle’s antibacterial activity. This work indicated that the zone of inhibition of 22 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Two-Dimensional, Hierarchical Ag-Doped TiO2 Nanocatalysts: Effect of the Metal Oxidation State on the Photocatalytic Properties

Md Saad SK, Ali Umar A, Ali Umar MI, Tomitori M, Abd Rahman MY, Mat Salleh M, et al.

ACS Omega, 2018 Mar 31;3(3):2579-2587.
PMID: 31458546 DOI: 10.1021/acsomega.8b00109

This paper reports the synthesis of two-dimensional, hierarchical, porous, and (001)-faceted metal (Ag, Zn, and Al)-doped TiO2 nanostructures (TNSs) and the study of their photocatalytic activity. Two-dimensional metal-doped TNSs were synthesized using the hydrolysis of ammonium hexafluorotitanate in the presence of hexamethylenetetramine and metal precursors. Typical morphology of metal-doped TNSs is a hierarchical nanosheet that is composed of randomly stacked nanocubes (dimensions of up to 5 μm and 200 nm in edge length and thickness, respectively) and has dominant (001) facets exposed. Raman analysis and X-ray photoelectron spectroscopy results indicated that the Ag doping, compared to Zn and Al, much improves the crystallinity degree and at the same time dramatically lowers the valence state binding energy of the TNS and provides an additional dopant oxidation state into the system for an enhanced electron-transfer process and surface reaction. These are assumed to enhance the photocatalytic of the TNS. In a model of photocatalytic reaction, that is, rhodamine B degradation, the AgTNS demonstrates a high photocatalytic activity by converting approximately 91% of rhodamine B within only 120 min, equivalent to a rate constant of 0.018 m-1 and ToN and ToF of 94 and 1.57 min-1, respectively, or 91.1 mmol mg-1 W-1 degradation when normalized to used light source intensity, which is approximately 2 times higher than the pristine TNS and several order higher when compared to Zn- and Al-doped TNSs. Improvement of the crystallinity degree, decrease in the defect density and the photogenerated electron and hole recombination, and increase of the oxygen vacancy in the AgTNS are found to be the key factors for the enhancement of the photocatalytic properties. This work provides a straightforward strategy for the preparation of high-energy (001) faceted, two-dimensional, hierarchical, and porous Ag-doped TNSs for potential use in photocatalysis and photoelectrochemical application.

Matched MeSH terms: Photoelectron Spectroscopy
A facile, bio-based, novel approach for synthesis of covalently functionalized graphene nanoplatelet nano-coolants toward improved thermo-physical and heat transfer properties

Sadri R, Hosseini M, Kazi SN, Bagheri S, Abdelrazek AH, Ahmadi G, et al.

J Colloid Interface Sci, 2018 Jan 01;509:140-152.
PMID: 28898734 DOI: 10.1016/j.jcis.2017.07.052

In this study, we synthesized covalently functionalized graphene nanoplatelet (GNP) aqueous suspensions that are highly stable and environmentally friendly for use as coolants in heat transfer systems. We evaluated the heat transfer and hydrodynamic properties of these nano-coolants flowing through a horizontal stainless steel tube subjected to a uniform heat flux at its outer surface. The GNPs functionalized with clove buds using the one-pot technique. We characterized the clove-treated GNPs (CGNPs) using X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). We then dispersed the CGNPs in distilled water at three particle concentrations (0.025, 0.075 and 0.1wt%) in order to prepare the CGNP-water nanofluids (nano-coolants). We used ultraviolet-visible (UV-vis) spectroscopy to examine the stability and solubility of the CGNPs in the distilled water. There is significant enhancement in thermo-physical properties of CGNPs nanofluids relative those for distilled water. We validated our experimental set-up by comparing the friction factor and Nusselt number for distilled water obtained from experiments with those determined from empirical correlations, indeed, our experimental set-up is reliable and produces results with reasonable accuracy. We conducted heat transfer experiments for the CGNP-water nano-coolants flowing through the horizontal heated tube in fully developed turbulent condition. Our results are indeed promising since there is a significant enhancement in the Nusselt number and convective heat transfer coefficient for the CGNP-water nanofluids, with only a negligible increase in the friction factor and pumping power. More importantly, we found that there is a significant increase in the performance index, which is a positive indicator that our nanofluids have potential to substitute conventional coolants in heat transfer systems because of their overall thermal performance and energy savings benefits.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Antimicrobial quaternary ammonium organosilane cross-linked nanofibrous collagen scaffolds for tissue engineering

Dhand C, Balakrishnan Y, Ong ST, Dwivedi N, Venugopal JR, Harini S, et al.

Int J Nanomedicine, 2018;13:4473-4492.
PMID: 30122921 DOI: 10.2147/IJN.S159770

Introduction: In search for cross-linkers with multifunctional characteristics, the present work investigated the utility of quaternary ammonium organosilane (QOS) as a potential cross-linker for electrospun collagen nanofibers. We hypothesized that the quaternary ammonium ions improve the electrospinnability by reducing the surface tension and confer antimicrobial properties, while the formation of siloxane after alkaline hydrolysis could cross-link collagen and stimulate cell proliferation.
Materials and methods: QOS collagen nanofibers were electrospun by incorporating various concentrations of QOS (0.1%-10% w/w) and were cross-linked in situ after exposure to ammonium carbonate. The QOS cross-linked scaffolds were characterized and their biological properties were evaluated in terms of their biocompatibility, cellular adhesion and metabolic activity for primary human dermal fibroblasts and human fetal osteoblasts.
Results and discussion: The study revealed that 1) QOS cross-linking increased the flexibility of otherwise rigid collagen nanofibers and improved the thermal stability; 2) QOS cross-linked mats displayed potent antibacterial activity and 3) the biocompatibility of the composite mats depended on the amount of QOS present in dope solution - at low QOS concentrations (0.1% w/w), the mats promoted mammalian cell proliferation and growth, whereas at higher QOS concentrations, cytotoxic effect was observed.
Conclusion: This study demonstrates that QOS cross-linked mats possess anti-infective properties and confer niches for cellular growth and proliferation, thus offering a useful approach, which is important for hard and soft tissue engineering and regenerative medicine.

Matched MeSH terms: Photoelectron Spectroscopy
Acanthamoebicidal activity of periglaucine A and betulinic acid from Pericampylus glaucus (Lam.) Merr. in vitro

Mahboob T, Azlan AM, Shipton FN, Boonroumkaew P, Nor Azman NS, Sekaran SD, et al.

Exp Parasitol, 2017 Dec;183:160-166.
PMID: 28916456 DOI: 10.1016/j.exppara.2017.09.002

Acanthamoeba species are pathogenic protozoa which account for amoebic keratitis, conjunctivitis and granulomatous amoebic encephalitis. These amoebae form cysts which resist drugs and more effective acanthamoebicidal agents are needed. Medicinal plants could be useful in improving the current treatment strategies for Acanthamoeba infections. In the present study, we examined the amoebicidal effects of Pericampylus glaucus (Lam.) Merr., a medicinal plant used for the treatment of conjunctivitis in Malaysia. Pathogenic Acanthamoeba triangularis were isolated from environmental water samples and treated with different concentrations of fractions obtained from Pericampylus glaucus (Lam.) Merr. as well as main constituents for 24-72 h. Chlorhexidine was used as a reference drug. Ethanol fraction of stem showed significant (p

Matched MeSH terms: Photoelectron Spectroscopy
Polyelectrolyte multi-layers assembly of SiCHA nanopowders and collagen type I on aminolysed PLA films to enhance cell-material interactions

Baba Ismail YM, Ferreira AM, Bretcanu O, Dalgarno K, El Haj AJ

Colloids Surf B Biointerfaces, 2017 Nov 01;159:445-453.
PMID: 28837894 DOI: 10.1016/j.colsurfb.2017.07.086

This paper presents a new approach in assembling bone extracellular matrix components onto PLA films, and investigates the most favourable environment which can be created using the technique for cell-material interactions. Poly (lactic acid) (PLA) films were chemically modified by covalently binding the poly(ethylene imine) (PEI) as to prepare the substrate for immobilization of polyelectrolyte multilayers (PEMs) coating. Negatively charged polyelectrolyte consists of well-dispersed silicon-carbonated hydroxyapatite (SiCHA) nanopowders in hyaluronic acid (Hya) was deposited onto the modified PLA films followed by SiCHA in collagen type I as the positively charged polyelectrolyte. The outermost layer was finally cross-linked by 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrocholoride and N-hydroxysulfosuccinimide sodium salt (EDC/NHS) solutions. The physicochemical features of the coated PLA films were monitored via X-ray Photoelectron Spectroscopy (XPS) and Atomic Force Microscope (AFM). The amounts of calcium and collagen deposited on the surface were qualitatively and quantitatively determined. The surface characterizations suggested that 5-BL has the optimum surface roughness and highest amounts of calcium and collagen depositions among tested films. In vitro human mesenchymal stem cells (hMSCs) cultured on the coated PLA films confirmed that the coating materials greatly improved cell attachment and survival compared to unmodified PLA films. The cell viability, cell proliferation and Alkaline Phosphatase (ALP) expression on 5-BL were found to be the most favourable of the tested films. Hence, this newly developed coating materials assembly could contribute to the improvement of the bioactivity of polymeric materials and structures aimed to bone tissue engineering applications.

Matched MeSH terms: Photoelectron Spectroscopy
A bio-based, facile approach for the preparation of covalently functionalized carbon nanotubes aqueous suspensions and their potential as heat transfer fluids

Sadri R, Hosseini M, Kazi SN, Bagheri S, Zubir N, Solangi KH, et al.

J Colloid Interface Sci, 2017 Oct 15;504:115-123.
PMID: 28531649 DOI: 10.1016/j.jcis.2017.03.051

In this study, we propose an innovative, bio-based, environmentally friendly approach for the covalent functionalization of multi-walled carbon nanotubes using clove buds. This approach is innovative because we do not use toxic and hazardous acids which are typically used in common carbon nanomaterial functionalization procedures. The MWCNTs are functionalized in one pot using a free radical grafting reaction. The clove-functionalized MWCNTs (CMWCNTs) are then dispersed in distilled water (DI water), producing a highly stable CMWCNT aqueous suspension. The CMWCNTs are characterized using Raman spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy. The electrostatic interactions between the CMWCNT colloidal particles in DI water are verified via zeta potential measurements. UV-vis spectroscopy is also used to examine the stability of the CMWCNTs in the base fluid. The thermo-physical properties of the CMWCNT nano-fluids are examined experimentally and indeed, this nano-fluid shows remarkably improved thermo-physical properties, indicating its superb potential for various thermal applications.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext The Development of Non-Enzymatic Glucose Biosensors Based on Electrochemically Prepared Polypyrrole-Chitosan-Titanium Dioxide Nanocomposite Films

Al-Mokaram AMAAA, Yahya R, Abdi MM, Mahmud HNME

Nanomaterials (Basel), 2017 May 31;7(6).
PMID: 28561760 DOI: 10.3390/nano7060129

The performance of a modified electrode of nanocomposite films consisting of polypyrrole-chitosan-titanium dioxide (Ppy-CS-TiO₂) has been explored for the developing a non-enzymatic glucose biosensors. The synergy effect of TiO₂ nanoparticles (NPs) and conducting polymer on the current responses of the electrode resulted in greater sensitivity. The incorporation of TiO₂ NPs in the nanocomposite films was confirmed by X-ray photoelectron spectroscopy (XPS) spectra. FE-SEM and HR-TEM provided more evidence for the presence of TiO₂ in the Ppy-CS structure. Glucose biosensing properties were determined by amperommetry and cyclic voltammetry (CV). The interfacial properties of nanocomposite electrodes were studied by electrochemical impedance spectroscopy (EIS). The developed biosensors showed good sensitivity over a linear range of 1-14 mM with a detection limit of 614 μM for glucose. The modified electrode with Ppy-CS nanocomposite also exhibited good selectivity and long-term stability with no interference effect. The Ppy-CS-TiO₂ nanocomposites films presented high electron transfer kinetics. This work shows the role of nanomaterials in electrochemical biosensors and describes the process of their homogeneous distribution in composite films by a one-step electrochemical process, where all components are taken in a single solution in the electrochemical cell.

Matched MeSH terms: Photoelectron Spectroscopy
Synthesis, Structural, Thermal, and Electronic Properties of Palmierite-Related Double Molybdate α-Cs2Pb(MoO4)2

Solodovnikov SF, Atuchin VV, Solodovnikova ZA, Khyzhun OY, Danylenko MI, Pishchur DP, et al.

Inorg Chem, 2017 Mar 20;56(6):3276-3286.
PMID: 28266857 DOI: 10.1021/acs.inorgchem.6b02653

Cs2Pb(MoO4)2crystals were prepared by crystallization from their own melt, and the crystal structure has been studied in detail. At 296 K, the molybdate crystallizes in the low-temperature α-form and has a monoclinic palmierite-related superstructure (space group C2/m, a = 2.13755(13) nm, b = 1.23123(8) nm, c = 1.68024(10) nm, β = 115.037(2)°, Z = 16) possessing the largest unit cell volume, 4.0066(4) nm3, among lead-containing palmierites. The compound undergoes a distortive phase transition at 635 K and incongruently melts at 943 K. The electronic structure of α-Cs2Pb(MoO4)2was explored by using X-ray emission spectroscopy (XES) and X-ray photoelectron spectroscopy methods. For α-Cs2Pb(MoO4)2, the photoelectron core-level and valence-band spectra and the XES band representing the energy distribution of Mo 4d and O 2p states were recorded. Our results allow one to conclude that the Mo 4d and O 2p states contribute mainly to the central part and at the top of the valence band, respectively, with also significant contributions throughout the whole valence-band region of the molybdate under consideration.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Down-top nanofabrication of binary (CdO)x (ZnO)1-x nanoparticles and their antibacterial activity

Al-Hada NM, Mohamed Kamari H, Abdullah CAC, Saion E, Shaari AH, Talib ZA, et al.

Int J Nanomedicine, 2017;12:8309-8323.
PMID: 29200844 DOI: 10.2147/IJN.S150405

In the present study, binary oxide (cadmium oxide [CdO])x (zinc oxide [ZnO])1-x nanoparticles (NPs) at different concentrations of precursor in calcination temperature were prepared using thermal treatment technique. Cadmium and zinc nitrates (source of cadmium and zinc) with polyvinylpyrrolidone (capping agent) have been used to prepare (CdO)x (ZnO)1-x NPs samples. The sample was characterized by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. XRD patterns analysis revealed that NPs were formed after calcination, which showed a cubic and hexagonal crystalline structure of (CdO)x (ZnO)1-x NPs. The phase analysis using EDX spectroscopy and FTIR spectroscopy confirmed the presence of Cd and Zn as the original compounds of prepared (CdO)x (ZnO)1-x NP samples. The average particle size of the samples increased from 14 to 33 nm as the concentration of precursor increased from x=0.20 to x=0.80, as observed by TEM results. The surface composition and valance state of the prepared product NPs were determined by X-ray photoelectron spectroscopy (XPS) analyses. Diffuse UV-visible reflectance spectra were used to determine the optical band gap through the Kubelka-Munk equation; the energy band gap was found to decrease for CdO from 2.92 to 2.82 eV and for ZnO from 3.22 to 3.11 eV with increasing x value. Additionally, photoluminescence (PL) spectra revealed that the intensity in PL increased with an increase in particle size. In addition, the antibacterial activity of binary oxide NP was carried out in vitro against Escherichia coli ATCC 25922 Gram (-ve), Salmonella choleraesuis ATCC 10708, and Bacillus subtilis UPMC 1175 Gram (+ve). This study indicated that the zone of inhibition of 21 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.

Matched MeSH terms: Photoelectron Spectroscopy
Fulltext Patterned Array of Poly(ethylene glycol) Silane Monolayer for Label-Free Detection of Dengue

Rosly NZ, Ahmad SA, Abdullah J, Yusof NA

Sensors (Basel), 2016 Aug 25;16(9).
PMID: 27571080 DOI: 10.3390/s16091365

In the present study, the construction of arrays on silicon for naked-eye detection of DNA dengue was demonstrated. The array was created by exposing a polyethylene glycol (PEG) silane monolayer to 254 nm ultraviolet (UV) light through a photomask. Formation of the PEG silane monolayer and photomodifed surface properties was thoroughly characterized by using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements. The results of XPS confirmed that irradiation of ultraviolet (UV) light generates an aldehyde functional group that offers conjugation sites of amino DNA probe for detection of a specific dengue virus target DNA. Employing a gold enhancement process after inducing the electrostatic interaction between positively charged gold nanoparticles and the negatively charged target DNA hybridized to the DNA capture probe allowed to visualize the array with naked eye. The developed arrays demonstrated excellent performance in diagnosis of dengue with a detection limit as low as 10 pM. The selectivity of DNA arrays was also examined using a single base mismatch and noncomplementary target DNA.

Matched MeSH terms: Photoelectron Spectroscopy
Fabrication of CoTiO3-TiO2 composite films from a heterobimetallic single source precursor for electrochemical sensing of dopamine

Ehsan MA, Naeem R, Khaledi H, Sohail M, Hakeem Saeed A, Mazhar M

Dalton Trans, 2016 Jun 21;45(25):10222-32.
PMID: 27230711 DOI: 10.1039/c6dt01016d

Cobalt titanate-titania composite oxide films have been grown on FTO-coated glass substrates using a single-source heterometallic complex [Co2Ti4(μ-O)6(TFA)8(THF)6]·THF () which was obtained in quantitative yield from the reaction of diacetatocobalt(ii) tetrahydrate, tetraisopropoxytitanium(iv), and trifluoroacetic acid from a tetrahydrofuran solution. Physicochemical investigations of complex have been carried out by melting point, FT-IR, thermogravimetric and single-crystal X-ray diffraction analyses. CoTiO3-TiO2 films composed of spherical objects of various sizes have been grown from by aerosol-assisted chemical vapor deposition at different temperatures of 500, 550 and 600 °C. Thin films characterized by XRD, Raman and X-ray photoelectron spectroscopy, scanning electron microscopy, energy-dispersive X-ray analysis have been explored for electrochemical detection of dopamine (DA). The cyclic voltammetry with the CoTiO3-TiO2 electrode showed a DA oxidation peak at +0.215 V while linear sweep voltammetry displayed a detection limit (LoD) of 0.083 μM and a linear concentration range of 20-300 μM for DA. Thus, the CoTiO3-TiO2 electrode is a potential candidate for the sensitive and selective detection of DA.

Matched MeSH terms: Photoelectron Spectroscopy

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