In our previous paper, we reported that a dimeric Zn(2+) complex with a 2,2'-bipyridyl linker (Zn2L(1)), cyanuric acid (CA), and a Cu(2+) ion automatically assemble in aqueous solution to form 4:4:4 complex 3, which selectively catalyzes the hydrolysis of mono(4-nitrophenyl)phosphate (MNP) at neutral pH. Herein, we report that the use of barbital (Bar) instead of CA for the self-assembly with Zn2L(1) and Cu(2+) induces 2:2:2 complexation of these components, and not the 4:4:4 complex, to form supramolecular complex 6 a, the structure and equilibrium characteristics of which were studied by analytical and physical measurements. The finding show that 6 a also accelerates the hydrolysis of MNP, similarly to 3. Moreover, inspired by the crystal structure of 6 a, we prepared barbital units that contain functional groups on their side chains in an attempt to produce supramolecular phosphatases that possess functional groups near the Cu2(μ-OH)2 catalytic core so as to mimic the catalytic center of alkaline phosphatase (AP).
Coal combustion by-products (CCPs) (i.e. fly (FA) and bottom (BA) ashes) generated by power plants contain heavy metals. This research presents leaching properties of coal ashes (FA and BA) collected from Jimah coal-fired power station, Port Dickson, Negeri Sembilan using USEPA standard methods namely toxicity characteristic leaching procedure (TCLP), and synthetic precipitation leaching procedure (SPLP). Heavy metals like lead (Pb), zinc (Zn), copper (Cu) and arsenic (As) were quantified using atomic absorption spectrometer (AAS). The leached of heavy metals fluxes were Cu < Zn < Pb < As. As leached the most whilst indicating of possible contamination from As. Overall, the ranges of leached concentration were adhered to permissible limits of hazardous waste criteria for metal (Pb and As) and industrial effluent (Zn and Cu). The presented data has potential reuse as reference for the coal ash concrete mixed design application in construction industries.
Biobased polymers are useful materials in substituting conventional petroleum-derived polymers because of their good properties, ready availability, and abundance in nature. This study reports a new jatropha oil-based gel polymer electrolyte (GPE) for use in dye-sensitized solar cells (DSSCs). The GPE was prepared by mixing jatropha oil-based polyurethane acrylate (PUA) with different concentrations of lithium iodide (LiI). The GPE was characterized by infrared spectroscopy, thermal analysis, lithium nuclear magnetic resonance analysis, electrochemical analysis, and photocurrent conversion efficiency. The highest room-temperature ionic conductivity of 1.88 × 10-4 S cm-1 was obtained at 20 wt % of LiI salt. Additionally, the temperature-dependent ionic conductivity of the GPE exhibited Arrhenius behavior with an activation energy of 0.42 eV and a pre-exponential factor of 1.56 × 103 S cm-1. The electrochemical stability study showed that the PUA GPE was stable up to 2.35 V. The thermal stability of the gel electrolyte showed an improvement after the addition of the salt, suggesting a strong intermolecular interaction between PUA and Li, which leads to polymer-salt complexation, as proven by Fourier transform infrared spectroscopy analysis. A DSSC has been assembled using the optimum ionic conductivity gel electrolyte which indicated 1.2% efficiency under 1 sun condition. Thus, the jatropha oil-based GPE demonstrated favorable properties that make it a promising alternative to petroleum-derived polymer electrolytes in DSSCs.
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.
This study aimed to assess the concentrations of cadmium (Cd), nickel (Ni) and lead (Pb) in the tissues of fish collected from the lower reach of the Kelantan River, Malaysia. Fishes were collected using gill nets during the dry and wet seasons. A total of 78 individual fish were caught and comprised 6 families, 11 genera and 13 species. The dorsal muscle was analysed using a graphite furnace Atomic Absorption Spectrometer (AAS). The mean concentration of Cd in Chitala chitala (0.076 mg/kg) was above the critical limit values of the European Commission (EC), World Health Organization (WHO) and Food and Agriculture Organization (FAO). The mean concentrations of Cd in Barbonymus gonionatus and Tachysurus maculatus were already at the level of concern, whereas the other species were approaching the limits of permissible levels. No fish samples were found to have a Ni level higher than the permissible limit of 0.5-0.6 mg/kg set by the WHO (1985). Osteochilus hasseltii (0.169 mg/kg) and T. maculatus (0.156 mg/kg) showed high Pb concentrations. The concentrations of heavy metals were found to be elevated in the wet season (p<0.05). Omnivorous fish were detected with elevated concentrations of Cd and Ni, whereas carnivorous fish had the highest concentration of Pb. The concentrations of Cd and Pb in fish tissues were positively correlated with fish weight (p<0.05). This study determined that the fish species caught in the Kelantan River were contaminated with non-essential metals (Cd, Ni and Pb). Nevertheless, the heavy metal concentration in the fish tissues, with the exception of C. chitala, O. hasseltii and T. maculatus, did not exceed the EC, FAO, Malaysian Food Act (MFA) or WHO guidelines.
Sumatran pit viper (Trimeresurus sumatranus sumatranus) venom was fractionated by DEAE-Sephacel ion exchange chromatography into seven fractions. Fractions 4, 5 and 6 were lethal to mice and exhibited strong hemorrhagic activity, as well as some enzymatic activities. Fraction 6 also exhibited potent anticoagulant and thrombin-like activities. Analysis of the biological and enzymatic properties of the three lethal fractions suggests that the major lethal component of fractions 4 and 5 may be the hemorrhagic principle, and that the lethality of fraction 6 may be due to the hemorrhagic principle and/or the anticoagulant principle.
A simple high-performance liquid chromatographic method using fluorescence detection was developed for the determination of vitamin E especially delta-, gamma- and alpha-tocotrienols in human plasma. The method entailed direct injection of plasma sample after deproteinization using a 3:2 mixture of acetonitrile-tetrahydrofuran. The mobile phase comprised 0.5% (v/v) of distilled water in methanol. Analyses were run at a flow-rate of 1.5 ml/min with the detector operating at an excitation wavelength of 296 nm and emission wavelength of 330 nm. This method is specific and sensitive, with a quantification limit of approximately 40, 34 and 16 ng/ml for alpha-, gamma- and delta-tocotrienol, respectively. The mean absolute recovery values were about 98% while the within-day and between-day relative standard deviation and percent error values of the assay method were all less than 12.0% for alpha-, gamma- and delta-tocotrienol. The calibration curve was linear over a concentration range of 40-2500, 30-4000 and 16-1000 ng/ml for alpha-, gamma- and delta-tocotrienol, respectively. Application of the method in a bioavailability study for determination of the above compounds was also demonstrated.
Side effects such as abrasion of the dental hard tissue have been frequently observed following the extensive use of mechanical cleansing. As promising antiseptics like chlorhexidine produces extrinsic dental staining on long term usage, there has been increasing interest and research generated towards chemically based stain removing agents. This invitro studyexamined whether some commercial oral hygiene products could inhibit chlorhexidine derived stain independent of any mechanical cleansing action. Perspex blocks were soaked in triplicate in chlorhexidine solution for 2 minutesand stain inhibition by these products was determined by further soaking the blocks in productl water slurries for 2 minutes and finally in tea solution for I hourly periods. The optical density (OD) of each specimen was determined at each hourly interval by spectrophotometry at 395 nm and the mean values obtained. At the end of the study, most of the products inhibited stain compared to water control and there was a variation in the stain inhibitingefficacyof the products. It is thus concluded that oral hygiene products like dentifricesand mouthrinses can inhibit chlorhexidine derived extrinsic dental stain to a variable degree through a chemical action by contained ingredients.
Fractional factorial design was utilized to evaluate the effect of combinations of nitric acid, hydrogen peroxide, hydrochloric acid and water for microwave digestion of fish muscle. Upon digestion, copper, iron and zinc were determined by flame atomic absorption spectroscopy. H2O2 and HCl volumes were found to be the most significant parameters which resulted in good metal recoveries. This is especially so for the effect of HCl on Fe recovery. The results indicated that the combination of 4 mL 65% HNO3, 2 mL 30% H2O2 and 2 mL 30% HCl gave the most satisfactory percentage recovery. There was good agreement between measured and certified values for all metals with respect to the DORM-3 fish protein.
As consumption of stingless bee honey has been gaining popularity in many countries including Malaysia, ability to identify accurately its geographical origin proves pertinent for investigating fraudulent activities for consumer protection. Because a chemical signature can be location-specific, multi-element distribution patterns may prove useful for provenancing such product. Using the inductively coupled-plasma optical emission spectrometer as well as principal component analysis (PCA) and linear discriminant analysis (LDA), the distributions of multi-elements in stingless bee honey collected at four different geographical locations (North, West, East, and South) in Johor, Malaysia, were investigated. While cross-validation using PCA demonstrated 87.0% correct classification rate, the same was improved (96.2%) with the use of LDA, indicating that discrimination was possible for the different geographical regions. Therefore, utilization of multi-element analysis coupled with chemometrics techniques for assigning the provenance of stingless bee honeys for forensic applications is supported.
The status ofhve l1eavy metals: cadmium, lead copper, zinc and mercury were determined in seafood and its products imported_ti·om Thailand via Bukit Kayu Hiram, Kedah, Flame Atomic Absorption Spectrophotometer was used to determine the level of these heary metals except for mercury, where the cold vapor technique was used, Randomized sampling was done according to a predetermined sampling plan based on the previous years consignments. Data collected were compared with the maximum permitted level of -metal contaminants in fish and fish products- ofthe Fourteenth Schedule (Regulation 38) of Food Act I983 and Food Regulations I 985 to ascertain compliance. lt was noted form this study, that the level of metals detected in seafood and its products had a very wide range, The levels detected for cadmium was at a range of 0. 00] - 3.9/2, 0.07 — 0.29, 0,04 - 4,4 mg/kg in fish, shellfish and cuttlefish respectivelv. In general, cadmium level in some samples was notably higher particularly in shellfish. All samples had lead level less than the permitted value except for fish where the highest value detected was 3.28 mg/kg. The level of copper and zinc was higher than the permitted value in octopus, prawn and crab, Mercury level in all samples analvzed was found to be below the detection level. As for fish samples, zinc level was found to be higher whereas copper was within the limit. However, it was also noted that the level of all the heavy metals in jiozen jish was within the permitted limit.
A cross-sectional study was conducted on 83 female electronics factory workers. The respondents comprised 50 exposed workers who use lead alloy solder and 33 unexposed workers. The objective of this study was to assess the lead exposure of these workers. Breathing zone were sampled using air sampling pumps. Dust samples were collected by wipe method. Venous blood collected and blood pressure were measured. All lead analyses were carried out with Graphite Furnace Atomic Absorption Spectrophotometer. The mean air lead for exposed workers (57 0. ± 0.93 μg/m³) was significantly higher than the unexposed workers (0.0067 ± 0.0045μg/m³) (p
A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient (R2 ) in the range of 0.991-0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l-1 (atrazine) and 1.22 µg l-1 (propazine), and the limit of quantitation was 3.54 µg l-1 (atrazine) and 4.07 µg l-1 (propazine). Satisfactory recoveries in the range of 81-108% were determined in milk samples at 5 and 1000 µg l-1, respectively, with low relative standard deviation, n = 3 of 0.301-7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.
The combination of compounds with different classes (hydrophobic and hydrophilic characters) in single chitosan carrier is a challenge due to the hydrophilicity of chitosan. Utilization of l-ascorbic acid (LAA) and thymoquinone (TQ) compounds as effective antioxidants is marred by poor bioavailability and uptake. Nanoparticles (NPs) solved the problem by functioning as a carrier for them because they have high surface areas for more efficient delivery and uptake by cells. This research, therefore, synthesized chitosan NPs (CNPs) containing LAA and TQ, CNP-LAA-TQ via ionic gelation routes as the preparation is non-toxic. They were characterized using electron microscopy, zetasizer, UV⁻VIS spectrophotometry, and infrared spectroscopy. The optimum CNP-LAA-TQ size produced was 141.5 ± 7.8 nm, with a polydispersity index (PDI) of 0.207 ± 0.013. The encapsulation efficiency of CNP-LAA-TQ was 22.8 ± 3.2% for LAA and 35.6 ± 3.6% for TQ. Combined hydrophilic LAA and hydrophobic TQ proved that a myriad of highly efficacious compounds with poor systemic uptake could be encapsulated together in NP systems to increase their pharmaceutical efficiency, indirectly contributing to the advancement of medical and pharmaceutical sectors.
There are various approaches to enhancing the catalytic properties of TiO₂, including modifying its morphology by altering the surface reactivity and surface area of the catalyst. In this study, the primary aim is to enhance the photocatalytic activity by changing the TiO₂ nanotubes' architecture. The highly ordered infrastructure is favorable for a better charge carrier transfer. It is well known that anodization affects TiO₂ nanotubes' structure by increasing the anodization duration which in turn influence the photocatalytic activity. The characterizations were conducted by FE-SEM (fiend emission scanning electron microscopy), XRD (X-ray diffraction), RAMAN (Raman spectroscopy), EDX (Energy dispersive X-ray spectroscopy), UV-Vis (Ultraviolet visible spectroscopy) and LCMS/MS/MS (liquid chromatography mass spectroscopy). We found that the morphological structure is affected by the anodization duration according to FE-SEM. The photocatalytic degradation shows a photodegradation rate of k = 0.0104 min-1. It is also found that a mineralization of Simazine by our prepared TiO₂ nanotubes leads to the formation of cyanuric acid. We propose three Simazine photodegradation pathways with several intermediates identified.
A feasible production of poly (methyl methacrylate)@alloy (gold-silver) core shell has
been presented as candidate in enhanced detection of surface enhanced Raman scattering
(SERS). Free emulsifier- emulsion synthesised PMMA sphere with average size of 419 nm in
diameter were used as core material for incorporation of alloy nanoparticles (6 nm) resulting
a core-shell structure. The fabrication of PMMA@alloy SERS substrate was successfully
done via self-assembly thus the produced SERS substrate that comprise of unique optical
properties combination arising from periodic core arrangement and plasmonic activity of
alloy nanoparticles. Alloy is bimetallic nanoparticles in which the combination of silver
(Ag) and gold (Au) present an absolutely improved light resistance as compared to single
metal alone with great surface plasmon resonance. Morphology and elemental analysis was
performed through scanning electron microscope (SEM) and the analysis showing species of
both Au and Ag in single alloy nanoparticles. The alloy nanoparticles were also observed to
homogenously coating the PMMA sphere. Surface plasmon resonance activity was maximum
at 476 nm obtained from UV-Visible spectroscopy. High surface production was observed
to have periodically arranged PMMA@alloy core -shell and potentially to be used as SERS
substrate.
In this work, TiO2/SiO2 composite photocatalysts were prepared using biogenic silica extracted from bamboo leaves and titanium tetraisopropoxide as a titania precursor via a sol-gel mechanism. A study of the physicochemical properties of materials as a function of their titanium dioxide content was conducted using Fourier transform infrared spectroscopy, a scanning electron microscope, a diffuse reflectance ultraviolet-visible (UV-vis) spectrophotometer, and a gas sorption analyzer. The relationship between physicochemical parameters and photocatalytic performance was evaluated using the methylene blue (MB) photocatalytic degradation process under UV irradiation with and without the addition of H2O2 as an oxidant. The results demonstrated that increasing the TiO2 helps enhance the parameters of specific surface area, the pore volume, and the particle size of titanium dioxide, while the band gap energy reaches a maximum of 3.21 eV for 40% and 60% Ti content. The composites exhibit photocatalytic activity with the MB degradation with increasing photocatalytic efficiency since the composites with 40 and 60% wt. of TiO2 demonstrated the higher degradation rate compared with TiO2 in the presence and absence of H2O2. This higher rate is correlated with the higher specific surface area and band gap energy compared with those of TiO2.
Over the years, ethylene-diamine-tetra-acetate (EDTA) has been widely used for many purposes. However, there are inadequate phytoassessment studies conducted using EDTA in Vetiver grass. Hence, this study evaluates the phytoassessment (growth performance, accumulation trends, and proficiency of metal uptake) of Vetiver grass, Vetiveria zizanioides (Linn.) Nash in both single and mixed heavy metal (Cd, Pb, Cu, and Zn)-disodium EDTA-enhanced contaminated soil. The plant growth, metal accumulation, and overall efficiency of metal uptake by different plant parts (lower root, upper root, lower tiller, and upper tiller) were thoroughly examined. The relative growth performance, metal tolerance, and phytoassessment of heavy metal in roots and tillers of Vetiver grass were examined. Metals in plants were measured using the flame atomic absorption spectrometry (F-AAS) after acid digestion. The root-tiller (R/T) ratio, biological concentration factor (BCF), biological accumulation coefficient (BAC), tolerance index (TI), translocation factor (TF), and metal uptake efficacy were used to estimate the potential of metal accumulation and translocation in Vetiver grass. All accumulation of heavy metals were significantly higher (p < 0.05) in both lower and upper roots and tillers of Vetiver grass for Cd + Pb + Cu + Zn + EDTA treatments as compared with the control. The single Zn + EDTA treatment accumulated the highest overall total amount of Zn (8068 ± 407 mg/kg) while the highest accumulation for Cu (1977 ± 293 mg/kg) and Pb (1096 ± 75 mg/kg) were recorded in the mixed Cd + Pb + Cu + Zn + EDTA treatment, respectively. Generally, the overall heavy metal accumulation trends of Vetiver grass were in the order of Zn > Cu > Pb > Cd for all treatments. Furthermore, both upper roots and tillers of Vetiver grass recorded high tendency of accumulation for appreciably greater amounts of all heavy metals, regardless of single and/or mixed metal treatments. Thus, Vetiver grass can be recommended as a potential phytoextractor for all types of heavy metals, whereby its tillers will act as the sink for heavy metal accumulation in the presence of EDTA for all treatments.
This paper presents the results of mercury analysis on 786 abiotic (surface sediments) and biotic (plant and animal tissues) samples collected from 10 sites at Matang Mangrove Forest Reserve in Peninsular Malaysia. Sediment samples were collected at the surface level from both river bank and forest understory. Whereas plant tissues obtained from Rhizophora apiculata Blume and Rhizophora mucronata L. consisted of leaves (in four stages namely young, mature, senescent and decomposing), bark and roots (divided into xylem, cortex and epidermis), the animal samples were represented by muscle tissue of the gastropod Cassidula aurisfelis Bruguière and the cockle Tegillarca granosa L. The mercury concentration measurements were obtained through a cold vapor atomic absorption spectrometer. The core data have been analysed and interpreted in the paper "Distribution of mercury in sediments, plant and animal tissues in Matang Mangrove Forest Reserve, Malaysia" [1].