Drug crystallization on and in the skin has been reported following application of topical or transdermal formulations. This study explored novel probe-based approaches including localized nanothermal analysis (nano-TA) and photothermal microspectroscopy (PTMS) to investigate and locate drug crystals in the stratum corneum (SC) of porcine skin following application of simple ibuprofen (IBU) formulations. We also conducted in vitro skin permeation studies and tape stripping. The detection of drug crystals in the SC on tape strips was confirmed using localized nano-TA, based on the melting temperature of IBU. The melting of IBU was also evident as indicated by a double transition and confirmed the presence of drug crystals in the SC. The single point scans of PTMS on the tape strips allowed collection of the photothermal FTIR spectra of IBU, confirming the existence of drug crystals in the skin. The combined methods also indicated that drug crystallized in the SC at a depth of ∼4-7 μm. Future studies will examine the potential of these techniques to probe crystallization of other commonly used actives in topical and transdermal formulations.
Pectin is an anionic, water-soluble polymer predominantly consisting of covalently 1,4-linked α-d-galacturonic acid units. This naturally occurring, renewable and biodegradable polymer is underutilized in polymer science due to its insolubility in organic solvents, which renders conventional polymerization methods impractical. To circumvent this problem, cerium-initiated radical polymerization was utilized to graft methoxy-poly(ethylene glycol) methacrylate (mPEGMA) onto pectin in water. The copolymers were characterized by ¹H nuclear magnetic resonance (NMR), Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA), and used in the formation of supramolecular hydrogels through the addition of α-cyclodextrin (α-CD) to induce crosslinking. These hydrogels possessed thixotropic properties; shear-thinning to liquid upon agitation but settling into gels at rest. In contrast to most of the other hydrogels produced through the use of poly(ethylene glycol) (PEG)-grafted polymers, the pectin-PEGMA/α-CD hydrogels were unaffected by temperature changes.
Nanocomposite polymer electrolyte membranes (NCPEMs) based on poly(acrylic acid)(PAA) and titania (TiO₂) are prepared by a solution casting technique. The ionic conductivity of NCPEMs increases with the weight ratio of TiO₂.The highest ionic conductivity of (8.36 ± 0.01) × 10-4 S·cm-1 is obtained with addition of 6 wt % of TiO₂ at ambient temperature. The complexation between PAA, LiTFSI and TiO₂ is discussed in Attenuated total reflectance-Fourier Transform Infrared (ATR-FTIR) studies. Electrical double layer capacitors (EDLCs) are fabricated using the filler-free polymer electrolyte or the most conducting NCPEM and carbon-based electrodes. The electrochemical performances of fabricated EDLCs are studied through cyclic voltammetry (CV) and galvanostatic charge-discharge studies. EDLC comprising NCPEM shows the specific capacitance of 28.56 F·g-1 (or equivalent to 29.54 mF·cm-2) with excellent electrochemical stability.
Cadmium oxide semiconductor nanoparticles were produced using a water based mixture, incorporating cadmium nitrates, polyvinyl pyrrolidone (PVP), and calcination temperature. An X-ray diffraction (XRD) evaluation was conducted to determine the degree of crystallization of the semiconductor nanoparticles. In addition, scanning electron microscopy (SEM) was conducted to identify the morphological features of the nanoparticles. The typical particle sizes and particle dispersal were analyzed via the use of transmission electron microscopy (TEM). The findings provided further support for the XRD outcomes. To determine the composition phase, Fourier transform infrared spectroscopy (FT-IR) was conducted, as it indicated the existence of not only metal oxide ionic band in the selection of samples, but also the efficient removal of organic compounds following calcinations. The optical characteristics were demonstrated, so as to analyze the energy band gap via the use of a UV⁻Vis spectrophotometer. A reduced particle size resulted in diminution of the intensity of photoluminescence, was demonstrated by PL spectra. Plus, the magnetic characteristics were examined using an electron spin resonance (ESR) spectroscopy, which affirmed the existence of unpaired electrons.
One of the approaches to prolong the service lifespan of polymeric material is the development of self-healing ability by means of embedded microcapsules containing a healing agent. In this work, poly(melamine-urea-formaldehyde) (PMUF) microcapsules containing a palm oil-based alkyd were produced by polymerization of melamine resin, urea and formaldehyde that encapsulated droplets of the suspended alkyd particles. A series of spherical and free-flowing microcapsules were obtained. The chemical properties of core and shell materials were characterized by Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) and proton nuclear magnetic resonance spectroscopy (¹H-NMR). Differential scanning calorimetry (DSC) analysis showed a glass transition around -15 °C due to the alkyd, and a melting temperature at around 200 °C due to the shell. Thermogravimetric analysis (TGA) results showed that the core and shell thermally degraded within the temperature range of 200⁻600 °C. Field emission scanning electron microscope (FESEM) examination of the ruptured microcapsule showed smooth inner and rough outer surfaces of the shell. Flexural strength and microhardness (Vickers) of the cured epoxy compound were not affected with the incorporation of 1%⁻3% of the microcapsules. The viability of the healing reactions was demonstrated by blending small amounts of alkyd with epoxy and hardener at different ratios. The blends could readily cure to non-sticky hard solids at room temperature and the reactions could be verified by ATR-FTIR.
To evaluate the possibilities for biofuel and bioenergy production Acacia Holosericea, which is an invasive plant available in Brunei Darussalam, was investigated. Proximate analysis of Acacia Holosericea shows that the moisture content, volatile matters, fixed carbon, and ash contents were 9.56%, 65.12%, 21.21%, and 3.91%, respectively. Ultimate analysis shows carbon, hydrogen, and nitrogen as 44.03%, 5.67%, and 0.25%, respectively. The thermogravimetric analysis (TGA) results have shown that maximum weight loss occurred for this biomass at 357 °C for pyrolysis and 287 °C for combustion conditions. Low moisture content (<10%), high hydrogen content, and higher heating value (about 18.13 MJ/kg) makes this species a potential biomass. The production of bio-char, bio-oil, and biogas from Acacia Holosericea was found 34.45%, 32.56%, 33.09% for 500 °C with a heating rate 5 °C/min and 25.81%, 37.61%, 36.58% with a heating rate 10 °C/min, respectively, in this research. From Fourier transform infrared (FTIR) spectroscopy it was shown that a strong C-H, C-O, and C=C bond exists in the bio-char of the sample.
Graphene oxide/Cuprous oxide (GO/Cu₂O) composite is a visible light photocatalyst for the degradation of dyes. A simple and efficient approach for preparing GO/Cu₂O composite adopted in this study involves reducing cuprous oxide precursors in the presence of graphene oxide using an aqueous solution of pulp derived from banana fruit. The GO/Cu₂O composite was characterized by Fourier transform infrared spectroscopy (FT-IR), Diffused reflectance Ultraviolet visible spectroscopy (DRS UV-Vis), Raman spectroscopy and Field Emission Scanning electron microscopy (FE-SEM). Cu₂O particles were distributed randomly on the graphene oxide sheets due to the template effect of GO. The results showed higher photocatalytic activity for the composite (band gap 2.13 eV), for the degradation of the organic dyes (Methylene blue and Rhodamine-B). The enhanced photocatalytic activity is due to effective charge transfer from GO to Cu₂O, and high specific surface area which improves the effective separation of the generated electron-hole pairs. Our present study is inspired by a facile, low cost, green production of (GO/Cu₂O) composite whose photocatalytic activity can be extended to degradation of all other water-born textile dyes.
The purpose of this study was to produce a novel pH sensitive hydrogel with superior thermal stability, composed of
poly(acrylic acid) (PAA) and cellulose nanocrystal (CNC). CNC was extracted from kenaf fiber through a series of alkali
and bleaching treatments followed by acid hydrolysis. PAA was then subjected to chemical cross-linking using the crosslinking
agent (N,N-methylenebisacrylamide) in CNC suspension. The mixture was casted onto petri dish to obtain disc
shape hydrogel. PAA/cellulose hydrogel with the same composition ratio were also prepared as control. The effect of
reaction conditions such as the ratio of PAA and CNC on the swelling behavior of the hydrogel obtained towards pH
was studied. The obtained hydrogel was further subjected to different tests such as thermogravimetric analysis (TGA) to
study the thermal behavior, Fourier transform infrared for functional group identification and swelling test for swelling
behavior at different pH. The cross-linking of PAA was verified with FTIR with the absence of C=C double bond. In TGA
test, PAA/CNC hydrogel showed significantly higher thermal stability compared with pure PAA hydrogel. The hydrogel
obtained showed excellent pH sensitivity and experienced maximum swelling at pH7. The PAA/CNC hydrogel can be
developed further as drug carrier
Cellulose nanocrystals (CNC) from mengkuang leaves (Pandanus tectorius) were investigated as potential reinforcement
in poly(vinyl chloride) (PVC) matrix. The surface of CNC was modified with silane coupling agent to improve fillermatrix
adhesion. Solution casting method was used to prepare PVC nanocomposites with various amounts of modified
(SCNC) and unmodified (CNC) nanocrystals. Both SCNC and CNC were examined by Fourier transform infrared (FTIR)
spectroscopy and X-ray diffraction (XRD) which showed that surface chemical modification has occurred. An increase
in tensile strength was observed with the addition of SCNC compared to the CNC. However, the elongation at break of the
nanocomposites was found to decrease with the increase of both fillers loading. An increasing trend was observed in the
tensile modulus with the addition of CNC to the PVC matrix, but decreasing with the addition of SCNC. The morphology
of a fractured surface of nanocomposites showed silane modification reduced the number of voids in the structure of
PVC. The observation indicated the adhesion between the fiber and the matrix had improved upon surface modification
of the nanocrystals with silane.
Recent developments have found the viability of chitosan as a new alternative additive in the pulp and paper technology.
This study was carried out to investigate the effect of chitosan as a paper coating which were prepared by dissolution in
acetic acid solution. The mechanical properties of coated paper were improved significantly compared with non-coated
paper. The FT-IR spectra showed peak evolution at 1558 cm-1 for coated paper due to the existence of amine group. Since
FT-IR spectra for the coated paper was almost identical to the chitosan spectrum, it is assumed that there is an obvious
physical interaction rather than the chemical interaction. The SEM micrographs showed that some of the chitosan has
occupied the pores and some of them adhered only on the surface. This may be due to the chemical similarities between
cellulose and chitosan which enhanced the strength of fiber matrixes via hydrogen bonding. The antibacterial property
of coated paper showed that chitosan in dried form has no significant effect but effective when applied as wet solution.
In this study, cellulose nanocrystals (CNC) were produced using acid hydrolysis method. Kenaf core was pretreated with 4
wt. % sodium hydroxide (NaOH), followed by bleaching using 1.7 wt. % sodium chlorite (NaClO2
) in acetate buffer. The
bleached fiber was acid hydrolyzed for 45 and 55 min using 64 wt. % sulfuric acid (H2
SO4
). The size distribution of the
CNC segregated via differential centrifugation with different speed was also investigated. The CNC suspension obtained
was centrifuged at 3000, 6000, 9000 and 12000 rpm. The resultant CNC suspension collected was characterized using
Fourier transform infrared (FTIR) analysis, X-ray diffraction (XRD) and transmission electron microscopy (TEM). FTIR
results showed the progressive removal of non-cellulosic constituents for each subsequent treatment. It also showed that
the CNC produced after hydrolysing for 55 min has the highest degree of crystallinity (81.15%). CNC produced from acid
hydrolysis process of 45 min have lengths between 50 and 270 nm while CNC produced from acid hydrolysis process of
55 min have length around 40 to 370 nm.
The development of natural fiber polymer composites is increasing worldwide and in some applications, these composites
are used at outdoor rendering them exposed to ultra-violet (UV) radiation. The paper investigates the degradation behavior
of linear low density polyethylene/poly (vinyl alcohol)/kenaf (LLDPE/PVOH/KNF) composites after exposure to different
natural weathering durations. The composites with KNF loadings of 10, 20 and 40 parts per hundred resin (phr) were
exposed to natural weathering for 3 months and 6 months, respectively. The weathered composites were characterized by
Fourier transform infrared (FTIR) spectroscopy, universal testing machine, field emission scanning electron microscopy
(FESEM) and differential scanning calorimetry (DSC). The FTIR analysis showed an obvious carbonyl peak in composites
after weathering as an evidence of oxidation. The weight loss percentage of composites increased with respect to exposure
duration due to higher absorption of UV irradiation. The tensile properties of weathered composites were lower than
that of control composites and these properties also decreased with increasing exposure duration. FESEM micrographs
illustrated that composites with longer exposure duration suffered more surface damaged. The crystallinity percentage
was found to increase with increasing exposure duration.
The magnetic adsorbents i.e. oil palm frond-magnetic particles (OPF-MP) and oil palm frond activated carbon-magnetic particles (OPFAC-MP) have been prepared by impregnation of iron oxide via co-precipitation method. The magnetic adsorbents and their parent materials were characterized using Fourier transform infrared (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), Brunauer Emmett Teller (BET), Barrett, Joyner & Halenda (BJH) and t-plot method, x-ray diffraction (XRD) and also using vibrating sample magnetometry (VSM) to study their properties and surface chemistry. The activated carbon magnetic adsorbent confers high surface area of 700 m2/g with amorphous structure and magnetic properties of 2.76 emu/g. The OPF-MP and OPFAC-MP were then applied in adsorption study for ions removal of Pb(II), Zn(II) and Cu(II). OPFAC-MP has shown high removal efficiency of 100 % with adsorption capacity up to 15 mg/g of Pb(II), Zn(II) and Cu(II) ions compared to OPF-MP. In addition, the magnetic adsorbents were also compared with their parent materials to observe the effect of magnetic particles. Accordingly, the impregnation of magnetic particles enhances the metal ions adsorption comparing to their parent materials.
Liquid natural rubber (LNR) was functionalized into liquid epoxidized natural rubber (LENR) and hydroxylated LNR (LNROH)
via oxidation using a Na2
WO4
/CH3
COOH/H2
O2
catalytic system. Microstructures of LNR and functionalized LNRs
were characterized using Fourier Transform Infrared (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopies. The
effect of CH3
COOH, H2
O2
, Na2
WO4
, reaction time and temperature. reaction time and temperature on epoxy content were
investigated. LNR-OH was obtained when oxidation reaction was conducted at a longer reaction time, higher temperature
or excess amount of catalyst. Thermogravimetric analysis (TGA) reported the thermal behavior of functionalized LNRs.
Molecular weight and polydispersity index (PDI) were determined using gel permeation chromatography (GPC).
In this study, the adsorption efficiency of methyl violet (MV) dye onto Ce0.3Al0.7 and Ce0.3Al0.7Agx (x = 0.1, 0.3 & 0.5) mixed oxides was investigated. The properties of mixed oxide were determined by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), N2 adsorption-desorption isotherm, diffuse reflectance UV-vis spectroscopy (UV-vis DRS) and X-ray absorption near edge structure (XANES). Characterization showed that synthesized mixed oxide with fluorite has a pure cubic structure of a mesoporous nature and a small grain size with rough surface. Batch adsorption experiments were used to study parameters including contact time and initial dye concentration. The results showed that these parameters affected the degree of MV dye adsorption. The dye adsorption of mixed oxides attained equilibrium at 120 min. The equilibrium adsorption data were analyzed using Langmuir, Freundlich and Temkin isotherms. The adsorption behavior of MV dye onto Ce0.3Al0.7 was found to follow the Langmuir isotherm (R2 = 0.9951), providing a maximum monolayer adsorptive capacity of 2.35 mg/g. Alternatively, the adsorption of MV dye onto Ce0.3Al0.7Ag0.1 (R2 = 0.7839), Ce0.3Al0.7Ag0.3 (R2 = 0.9301) and Ce0.3Al0.7Ag0.5 (R2 = 0.9396) followed the Freundlich isotherm. The possible adsorption mechanisms of MV dyes onto the Ce0.3Al0.7 and Ce0.3Al0.7Agx were also discussed.
This paper reports the post-processing ageing phenomena of thermoplastic sago starch (TPS) and plasticised sago pith waste (SPW), which were processed using twin-screw extrusion and compression moulding techniques. Wide angle X-ray diffraction (XRD) analyses showed that after processing, starch molecules rearranged into VH-type (which was formed rapidly right post processing and concluded within 4 days) and B-type (which was formed slowly over a period of months) crystallites. Evidence from Fourier transform infrared spectroscopy (FTIR) analyses corroborated the 2-stage crystallisation process, which observed changes in peak styles and peak intensities (at 1043 and 1026 cm-1) and bandnarrowing. Thermogravimetric analysis (TGA) studies showed that the thermal stability of plasticised SPW declined continuously for 90 days before gradual increments ensued. For all formulations tested, post-processing ageing led to drastic changes in the tensile strength (increased) and elongation at break (decreased). Glycerol and fibres restrained the retrogradation of starch molecules in TPS and SPW.
Absorption is one of the effective, simple and economical methods to remove oil from oily wastewater. The most widely
used approach is to utilize lignocellulosic biomass as oil absorbent. However, the hygroscopic of cellulose have limited
the oil-water separation capability of lignocellulosic fibers. In this study, the surface functionality of oil palm empty
fruit bunch (EFB) fibers was slightly altered by grafting reduced graphene oxide (rGO). The modified EFB fibers show
a distinct morphological and chemical characteristics changes as the surface of fibers has been coated with rGO. This
was supported by FTIR analysis with the diminishing peak of hydroxyl group region of EFB fibers. While the surface
modification on EFB fibers shows a diminution of a hydrophilic characteristic of 131.6% water absorption in comparison
with 268.9% of untreated EFB fibers. Moreover, modified fibers demonstrated an oil-water separation increment as well,
as it shows 89% of oil uptake and improved ~17 times of oil selectivity in oil-water emulsion than untreated EFB fibers.
[BMIM]OTf and alcohol-based DES combination with a selected organic solvent (acetone and acetonitrile) have
been proven to efficiently extracting rotenone (isoflavonoid biopesticide) compound compared to individual organic
solvents. Their efficiency builds up interest to study the solvent-solute interaction that occurs between both selected
solvent systems with rotenone. The interaction study was analyzed using FTIR, 1D-NMR and 2D- NMR (NOESY, HMBC).
Correlation portrayed by NOESY and HMBC of [BMIM]OTf - standard rotenone mixture predicted probable hydrogen
bonding between the oxygen of rotenone with acidic proton C2-H of [BMIM]OTf. While for the alcohol-based DESrotenone
mixture, the correlation shows probable interaction to occur between methyl and methoxy group rotenone
with the hydroxyl group of 1,4-butanediol. In conclusion, potential hydrogen bonding that occurs between solvent
and solute aid towards the solvent efficiency in extracting rotenone compound while emphasizing on the low cost and
green mediated solvent systems.
Epoxidized natural rubber/polyvinyl chloride/microcrystalline cellulose (ENR/PVC/MCC) composite membranes were
prepared and used to treat palm oil mill effluent (POME). The loadings of MCC were varied at 0, 5, 10 and 15 w/w%. The
increment of MCC loads has intensified the hydroxyl peak of the membranes in FTIR spectrum, indicating the increase
in membrane hydrophilicity. MCC acted as a pore forming agent since the ENR/PVC/10% MCC gave the highest water
flux and well-distributed pores. After first treatment of POME, the levels of chemical oxygen demand (COD), biochemical
oxygen demand (BOD) and total suspended solid (TSS) were reduced to 99.9%, 70.3%, and 16.9%, respectively. These
data showed that ENR/PVC/MCC membrane has the potential to treat POME.
A series of amorphous carbon nitride (a-CNx) thin films were deposited on silicon (111) substrates using a home-built
radio frequency plasma enhanced chemical vapor deposition (RF-PECVD) system. The a-CNx thin films were deposited
from a mixture of a fixed flow-rate of ethane (C2
H6
, 20 sccm) and nitrogen (N2
, 47 sccm) gases with varying RF power. A
higher ratio of C to H (C to H ratio is 1:3) atoms in C2
H6
as compared to the ratio in methane (CH4
) gas (C to H ratio is
1:4) is expected to produce an interesting effect to the film properties as humidity sensor. The characterization techniques
used to determine the morphology and chemical bonding of the thin films are field emission scanning electron microscopy
(FESEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The variation of morphology and the existence
of nitrile band in these samples are correlated with the electrical properties of a-CNx thin films. Using humidity sensing
system, the sensing performance of the samples was examined. It was found that the response of sensors towards the
percentage of relative humidity (% RH) change is good resistive responses and good repeatability. The sensitivity of the
prepared a-CNx thin films is significantly higher (up to 79%) as compared to previous studies using CH4
or acetylene as
precursor gas. Based on these results, the properties and the sensitivity of the a-CNx thin films towards humidity can be
tailored by using an appropriate precursor gases and deposition parameters.