This study demonstrates the use of NMR techniques coupled with chemometric analysis as a high throughput data mining method to identify and examine the efficiency of different disruption techniques tested on microalgae (Chlorella variabilis, Scenedesmus regularis and Ankistrodesmus gracilis). The yield and chemical diversity from the disruptions together with the effects of pre-oven and pre-freeze drying prior to disruption techniques were discussed. HCl extraction showed the highest recovery of oil compounds from the disrupted microalgae (up to 90%). In contrast, NMR analysis showed the highest intensity of bioactive metabolites obtained for homogenized extracts pre-treated with freeze-drying, indicating that homogenizing is a more favorable approach to recover bioactive substances from the disrupted microalgae. The results show the potential of NMR as a useful metabolic fingerprinting tool for assessing compound diversity in complex microalgae extracts.
Calcium contents of demineralised human cortical bone determined by titrimetric assay and atomic absorption spectrophotometry technique were verified by comparing to neutron activation analysis which has high recovery of more than 90%. Conversion factors determined from the comparison is necessary to correct the calcium content for each technique. Femurs from cadaveric donors were cut into cortical rings and demineralised in 0.5 M hydrochloric acid for varying immersion times. Initial calcium content in the cortical bone measured by titration was 4.57%, only 21% of the measurement by neutron activation analysis; while measured by atomic absorption spectrophotometer was 13.4%, only 61% of neutron activation analysis. By comparing more readings with the measurements by neutron activation analysis with 93% recovery, a conversion factor of 4.83 was verified and applied for the readings by titration and 1.45 for atomic absorption spectrophotometer in calculating the correct calcium contents. The residual calcium content started to reduce after the cortical bone was demineralised in hydrochloric acid for 8 h and reduced to 13% after 24 h. Using the linear relationship, the residual calcium content could be reduced to less than 8% after immersion in hydrochloric acid for 40 h. Atomic absorption spectrophotometry technique is the method of choice for calcium content determination as it is more reliable compared to titrimetric assay.
Extracts from plant materials have great potential as alternatives to inorganic corrosion inhibitors, which typically have harmful consequences. Experimental and theoretical methodologies studied the effectiveness of agricultural waste, namely, date palm seed extract as a green anti-corrosive agent in 0.5 M hydrochloric acid. Experimental results showed that immersion time and temperature are closely related to the effectivity of date palm seed as a corrosion inhibitor. The inhibition efficiency reduced from 95% to 91% at 1400 ppm when the immersion time was increased from 72 h to 168 h. The experimental results also indicated that the inhibition efficiency decreased as the temperature increased. The presence of a protective layer of organic matter was corroborated by scanning electron microscopy. The adsorption studies indicated that date palm seed obeyed Langmuir adsorption isotherm on the carbon steel surface, and Gibbs free energy values were in the range of -33.45 to -38.41 kJ·mol-1. These results suggested that the date palm seed molecules interacted with the carbon steel surface through mixture adsorption. Theoretical calculations using density functional theory showed that the capability to donate and accept electrons between the alloy surface and the date palm seed inhibitor molecules is critical for adsorption effectiveness. The HOMO and LUMO result indicated that the carboxyl (COOH) group and C=C bond were the most active sites for the electron donation-acceptance type of interaction and most auxiliary to the adsorption process over the Fe surface.
In the present study, microcrystalline cellulose (MCC) was isolated from oil palm fronds (OPF) using chemo-mechanical process. Wherein, alkaline hydrogen peroxide (AHP) was utilized to extract OPF fibre at different AHP concentrations. The OPF pulp fibre was then bleached with acidified sodium chlorite solution followed by the acid hydrolysis using hydrochloric acid. Several analytical methods were conducted to determine the influence of AHP concentration on thermal properties, morphological properties, microscopic and crystalline behaviour of isolated MCC. Results showed that the MCC extracted from OPF fibres had fibre diameters of 7.55-9.11nm. X-ray diffraction (XRD) analyses revealed that the obtained microcrystalline fibre had both celluloses I and cellulose II polymorphs structure, depending on the AHP concentrations. The Fourier transmission infrared (FTIR) analyses showed that the AHP pre-hydrolysis was successfully removed hemicelluloses and lignin from the OPF fibre. The crystallinity of the MCC was increased with the AHP concentrations. The degradation temperature of MCC was about 300°C. The finding of the present study showed that pre-treatment process potentially influenced the quality of the isolation of MCC from oil palm fronds.
1,5-Dimethyl-4-((2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-one (DMPO) was synthesized to be evaluated as a corrosion inhibitor. The corrosion inhibitory effects of DMPO on mild steel in 1.0 M HCl were investigated using electrochemical impedance spectroscopy (EIS), potentiodynamic polarization, open circuit potential (OCP) and electrochemical frequency modulation (EFM). The results showed that DMPO inhibited mild steel corrosion in acid solution and indicated that the inhibition efficiency increased with increasing inhibitor concentration. Changes in the impedance parameters suggested an adsorption of DMPO onto the mild steel surface, leading to the formation of protective films. The novel synthesized corrosion inhibitor was characterized using UV-Vis, FT-IR and NMR spectral analyses. Electronic properties such as highest occupied molecular orbital energy, lowest unoccupied molecular orbital energy (EHOMO and ELUMO, respectively) and dipole moment (μ) were calculated and discussed. The results showed that the corrosion inhibition efficiency increased with an increase in the EHOMO values but with a decrease in the ELUMO value.
A new, effective one-pot synthesis of the 6, N2-diaryl-1,3,5-triazine-2,4-diamines under microwave irradiation was developed. The method involved an initial three-component condensation of cyanoguanidine, aromatic aldehydes, and arylamines in the presence of hydrochloric acid. Without isolation, the resulting 1,6-diaryl-1,6-dihydro-1,3,5-triazine-2,4-diamines were treated with a base to initiate Dimroth rearrangement and spontaneous dehydrogenative aromatization, affording the desired compounds. The developed method was found to be sufficiently general in scope, tolerating various aromatic aldehydes and amines; by using their combinations in the first step, a representative library of 110 compounds was successfully prepared and screened for anticancer properties.
Chemical etching, which is the most sensitive method to recover obliterated serial numbers on metal surfaces, has been practised quite successfully in forensic science laboratories all over the world. A large number of etchants suitable for particular metal surfaces based on empirical studies is available in the literature. This article reviews the sensitivity and efficacy of some popular etchants for recovering obliterated marks on medium carbon steel (0.31% C with ferrite-pearlite microstructure) used in automobile parts. The experiments involved engraving these carbon steel plates with some alphanumeric characters using a computer controlled machine "Gravograph" and erasing them to several depths below the bottom of their engraving depth. Seven metallographic reagents of which most of them were copper containing compounds were chosen for etching. The erased plates were etched with every one of these etchants using swabbing method. The results have revealed that Fry's reagent comprising cupric chloride 90 g, hydrochloric acid 120 mL and water 100mL provided the necessary contrast and was concluded to be the most sensitive. The same reagent was recommended by earlier workers for revealing strain lines in steel surfaces. Earlier, another reagent containing 5 g copper sulphate, 60 mL water, 30 mL (conc.) ammonium hydroxide, and 60 mL (conc.) hydrochloric acid was proved to be more sensitive to restore erased marks on low carbon steel (0.1% C with ferrite-pearlite structure) [M.A.M. Zaili, R. Kuppuswamy, H. Harun, Restoration of engraved marks on steel surfaces by etching technique, Forensic Sci. Int. 171 (2007) 27-32]. Thus the sensitivity of the etching reagent on steel surfaces appeared to be dependent on the content of carbon in the steel.
It is known that restoration of erased engraved identification marks on the engine and the chassis of a car or on a firearm has low success rate. Unlike stamping, engraving on a metal surface leaves no pronounced, permanent subsurface deformation in the crystalline structure, also called dislocation that can be revealed by suitable methods. Hence, the current research work investigated whether metallographic reagents used in the restoration of stamp (compression) marks could be applied to recover engraved marks on steel surfaces and also to establish the sensitivity and effectiveness of some of these reagents for the restoration of the marks. Experiments were conducted by mechanically engraving alphanumeric characters on several steel plates using a computer controlled engraving machine called Gravograph. The markings were later erased from the above steel plates by removing the metal in stages of 0.01 mm through 0.04 mm below the bottom of the engraving. Several plates were thus prepared wherein each one had been abraded to a specific depth. Then eight metallographic reagents were tested on each one of the above erased plates using a swabbing technique. The results had shown that while most of the reagents were able to restore marks up to certain levels of erasure, the reagent 5 g copper sulphate, 60 ml water, 30 ml concentrated ammonium hydroxide and 60 ml concentrated hydrochloric acid restored marks erased to a depth of 0.04 mm below the engraving depth, thus presenting itself the most sensitive reagent. Quite significantly, the above reagent was also able to decipher successfully the original engraved marks that had been erased and engraved with a new number, or obliterated by centre punching. The results of this research work should benefit the forensic practitioners engaged in the serial number recovery on vehicles, firearms and other objects.
A simple atomic-absorption spectrophotometry method is described for the determination of silver, bismuth, cadmium, copper, iron, nickel and zinc in lead- and tin-base solders and white-metal bearing alloys, with use of a single sample solution. The sample is dissolved in a mixture of hydrobromic acid and bromine, then fumed with sulphuric acid. The lead sulphate is dissolved in concentrated hydrochloric acid. The method is particularly suitable for the determination of silver and bismuth, which are co-precipitated with lead sulphate. The other elements can also be determined after removal of the lead sulphate by filtration.
Chlorine radical plays an important role in the formation of ozone and secondary aerosols in the troposphere. It is hence important to develop comprehensive emissions inventory of chlorine precursors in order to enhance our understanding of the role of chlorine chemistry in ozone and secondary pollution issues. Based on a bottom-up methodology, this study presents a comprehensive emission inventory for major atomic chlorine precursors in the Yangtze River Delta (YRD) region of China for the year 2017. Four primary chlorine precursors are considered in this study: hydrogen chloride (HCl), fine particulate chloride (Cl-) (Cl- in PM2.5), chlorine gas (Cl2), and hypochlorous acid (HClO) with emissions estimated for twelve source categories. The total emissions of these four species in the YRD region are estimated to be 20,424 t, 15,719 t, 1556 and 9331 t, respectively. The emissions of HCl are substantial, with major emissions from biomass burning and coal combustion, together accounting for 68% of the total HCl emissions. Fine particulate Cl- is mainly emitted from industrial processing, biomass burning and waste incineration. The emissions of Cl2 and HClO are mainly associated with usage of chlorine-containing disinfectants, for example, water treatment, wastewater treatment, and swimming pools. Emissions of each chlorine precursor are spatially allocated based on the characteristics of individual source category. This study provides important basic dataset for further studies with respect to the effects of chlorine chemistry on the formation of air pollution complex in the YRD region.
Danio rerio or commonly known as zebrafish are a very popular fish among scientists and also a well-known vertebrate model species widely used in research. Zebrafish, are also a popular species among aquarists and have been put in aquariums all around the world as ornamental fish. The acid rain phenomenon has lowered the pH level of the wild habitat of zebrafish by shifting it to a more acidic pH level. This study was carried out to observe the effect of low pH level on the reproductive performance of zebrafish. The zebrafish were quarantined for a week to make sure they were healthy to be used in the experiment. The zebrafish were reared continuously for 14 days in three different pH treatments T1 (pH 2-4), T2 (pH 4-6), T3 (pH 6-8)). T3 (pH 6-8) was used as the control treatment. Hydrochloric acid (HCl) was used to control the pH level of treatments T1 (pH 2-4), T2 (pH 4-6), T3 (pH 6-8) with three replicates of each treatment. The male chasing female frequency was significant (p: 0.0001) and the data showed the highest frequency (2568.000±140.6272) at treatment 3 (pH 6-8). For the spawning frequency of zebrafish, treatment 3 (pH 6-8) showed the highest value (4.000±0.5774) followed by treatment 2 and treatment 1 and the data was significant (p: 0.0004). The fertilisation rate of the zebrafish was significant (p: 0.0001) and the highest was shown at T2 (pH 4-6) with 89.8018±0.3782, followed by T3 and treatment T1. For the hatching rate of the zebrafish, the data collected were significant (p: 0.0002) and the highest value of 2.9350±0.4070 was shown at T3 (pH 6-8), followed by T2 (pH 4-6) and T1 (pH 2-4). The overall result showed that pH 2-4 had the worst effect on the reproductive performance of zebrafish. Therefore, low pH has a significant effect on reducing the reproductive performance of zebrafish. The local fish population can be affected by the decrease of pH level due to acid rains and chemical waste pollution.
Mild steel plays an essential part in many construction industries due to its low cost and excellent mechanical properties. However, the use of strong acid in pickling, construction, and oil refining processes adds to a serious corrosion problem for mild steel. Two Cu(II) dithiocarbamate (DTC) complexes were successfully synthesised, namely Cu(II) ethyl-benzyl DTC (Cu[EtBenzdtc]2) and Cu(II) butyl-methyl DTC (Cu[BuMedtc]2) complexes, by a condensation reaction and subsequently used to scrutinise the corrosion resistance activity towards mild steel in acidic media. The proposed structures of complexes were characterised by using the Fourier transform infrared (FTIR) and ultraviolet-visible (UV-Vis) spectroscopies. The melting point for Cu[EtBenzdtc]2 was found around 362–375°C, and 389–392°C for Cu[BuMedtc]2. The percentages of Cu(II) found in Cu[EtBenzdtc]2 and Cu[BuMedtc]2 were 7.6% and 7.5%, respectively. Both complexes were non-electrolyte based on the molar conductivity analysis. Their corrosion inhibition performances were tested by using a weight loss measurement. Cu[BuMedtc]2 showed a good result as a corrosion inhibitor compared to Cu[EtBenzdtc]2. The complexes showed good effectiveness in sulfuric acid (H2SO4) compared to hydrochloric acid (HCl) solution. Furthermore, Cu[BuMedtc]2 showed a good result as a corrosion inhibitor compared to Cu[EtBenzdtc]2 with the highest percentage of corrosion inhibition recorded at 91.8%. Meanwhile, the highest percentage of corrosion inhibition shown by Cu[EtBenzdtc]2 was only 86.9%. The lowest corrosion rate shown for Cu[BuMedtc]2 was 8.1944×10-4 cm-1 h-1. Meanwhile, the Cu[EtBenzdtc]2 showed the lowest corrosion rate only at 1.3194×10-3 cm-1 h-1. This implies that Cu[BuMedtc]2 showed lower corrosion rate but higher inhibition efficiency compared to Cu[EtBenzdtc]2.
The hydrochloride, sulphate and ethylcarbonate salts of quinine were given in single oral doses (600 mg base equivalent) to nine healthy male subjects according to a cross-over design. No statistically significant differences were noted in the plasma drug concentration-time profiles although inter- and intra-subject variation in AUC, Cmax and tmax values was appreciable. The ethylcarbonate salt may be preferred for use in paediatric patients because of its neutral taste.
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.
Acanthamoeba is a free living protozoa that can cause keratitis and granulomatous amoebic encephalitis. Physiological characteristics of this amoeba are found to have a medical importance in which it can be related to the pathogenicity potential of the organism. This study was carried out to investigate the physiological characteristics of survivability during axenization. Six Acanthamoeba strains from three clinical isolates (HSB 1, HKL 48 and HKL 95) and three environmental isolates (PHS 2, PHS 11 and PHS 15) were used in this study. Axenization test was done by treating cysts with hydrochloric acid (3%) and Page saline containing Gentamicin (100 µg/ml). Cysts were then cultured into PYG enrich media, incubated at 30oC and the presence and proliferation of trophozoites of Acanthamoeba were observed. This study showed that PHS 15, HSB 1, HKL 48 and HKL 95 could be axenized but they have poor proliferation rate in PYG enrich media. The result showed that the difference between both clinical and environmental isolates was observed in two strains; PHS 2 and PHS 11. This indicates that there is a possibility that the physiological traits of strains from both isolates are the same and strains from the environment are able to show the pathogenic potential and capable of causing infection to human.
This research investigated the removal of lead (Pb(2+)) by a novel biochar derived from palm oil sludge (POS-char) by slow pyrolysis. Multistage optimizations with central composite design were carried out to firstly optimize pyrolysis parameters to produce the best POS-char for Pb(2+) removal and secondly to optimize adsorption conditions for the highest removal of Pb(2+). The optimum pyrolysis parameters were nitrogen flowrateof30mLmin(-1), heating rateof10°Cmin(-1), temperatureof500°C and timeof30min. The optimum Pb(2+) adsorption conditions were concentrationof200mgL(-1), timeof60min, dosageof0.3g and pH of 3.02. The various functional groups within POS-char played a vital role in Pb(2+) uptake. Regeneration was demonstrated to be feasible using hydrochloric acid. Adsorption equilibrium was best described by Freundlich model. At low concentration range, adsorption kinetic obeyed pseudo-first-order model, but at high concentration range, it followed pseudo-second-order model. Overall, the results highlighted that POS-char is an effective adsorbent for Pb(2+) removal.
An acidic solution containing mercury chelating agents to eliminate mercury in raw fish (mackerel) fillet was developed. The solution contained hydrochloric acid, sodium hydroxide, cysteine, EDTA, and NaCl. The optimum conditions for mercury reduction were achieved using response surface methodology (RSM) at cysteine concentration of 1.25%, EDTA of 275 mg/L, NaCl of 0.5%, pH of 3.75, and exposure time of 18 min. The optimized conditions produced a solution which can remove up to 91% mercury from raw fish fillet. Cysteine and EDTA were identified as potential chelating agents with the greatest potential for use. The solution can be employed in fish industries to reduce mercury in highly contaminated fish.
Blood compatibility of metallocene polyethylene (mPE) was investigated after modifying the surface using hydrochloric acid. Contact angle of the mPE exposed to HCl poses a decrease in its value which indicates increasing wettability and better blood compatibility. Surface of mPE analyzed by using FTIR revealed no significant changes in its functional groups after treatment. Furthermore, scanning electron microscope images supported the increasing wettability through the modifications like pit formations and etching on the acid rendered surface. To evaluate the effect of acid treatment on the coagulation cascade, prothrombin time (PT) and activated partial thromboplastin time (APTT) were measured. Both PT and APTT were delayed significantly (P < 0.05) after 60 min exposure implying improved blood compatibility of the surfaces. Hemolysis assay of the treated surface showed a remarkable decrease in the percentage of lysis of red blood cells when compared with untreated surface. Moreover, platelet adhesion assay demonstrated that HCl exposed surfaces deter the attachment of platelets and thereby reduce the chances of activation of blood coagulation cascade. These results confirmed the enhanced blood compatibility of mPE after HCl exposure which can be utilized for cardiovascular implants like artificial vascular prostheses, implants, and various blood contacting devices.
A dynamic supported liquid membrane tip extraction (SLMTE) procedure for the effective extraction and preconcentration of glyphosate (GLYP) and its metabolite aminomethylphosphonic acid (AMPA) in water has been investigated. The SLMTE procedure was performed in a semi-automated dynamic mode and demonstrated a greater performance against a static extraction. Several important extraction parameters such as donor phase pH, cationic carrier concentration, type of membrane solvent, type of acceptor stripping phase, agitation and extraction time were comprehensively optimized. A solution of Aliquat-336, a cationic carrier, in dihexyl ether was selected as the supported liquid incorporated into the membrane phase. Quantification of GLYP and AMPA was carried out using capillary electrophoresis with contactless conductivity detection. An electrolyte solution consisting of 12 mM histidine (His), 8 mM 2-(N-morpholino)ethanesulfonic acid (MES), 75 microM cetyltrimethylammonium bromide (CTAB), 3% methanol, pH 6.3, was used as running buffer. Under the optimum extraction conditions, the method showed good linearity in the range of 0.01-200 microg/L (GLYP) and 0.1-400 microg/L (AMPA), acceptable reproducibility (RSD 5-7%, n=5), low limits of detection of 0.005 microg/L for GLYP and 0.06 microg/L for AMPA, and satisfactory relative recoveries (90-94%). Due to the low cost, the SLMTE device was disposed after each run which additionally eliminated the possibility of carry-over between runs. The validated method was tested for the analysis of both analytes in spiked tap water and river water with good success.
The efficiency of sodium hydroxide treated rubber (Hevea brasiliensis) leaves powder (NHBL) for removing copper ions from aqueous solutions has been investigated. The effects of physicochemical parameters on biosorption capacities such as stirring speed, pH, biosorbent dose, initial concentrations of copper, and ionic strength were studied. The biosorption capacities of NHBL increased with increase in pH, stirring speed and copper concentration but decreased with increase in biosorbent dose and ionic strength. The isotherm study indicated that NHBL fitted well with Langmuir model compared to Freundlich and Dubinin-Radushkevich models. The maximum biosorption capacity determined from Langmuir isotherm was 14.97 mg/g at 27 degrees C. The kinetic study revealed that pseudosecond order model fitted well the kinetic data, while Boyd kinetic model indicated that film diffusion was the main rate determining step in biosorption process. Based on surface area analysis, NHBL has low surface area and categorized as macroporous. Fourier transform infrared (FT-IR) analyses revealed that hydroxyl, carboxyl, and amino are the main functional groups involved in the binding of copper ions. Complexation was one of the main mechanisms for the removal of copper ions as indicated by FT-IR spectra. Ion exchange was another possible mechanism since the ratio of adsorbed cations (Cu2+ and H+) to the released cations (Na+, Ca2+, and Mg2+) from NHBL was almost unity. Copper ions bound on NHBL were able to be desorbed at > 99% using 0.05 mol/L HCl, 0.01 mol/L HNO3, and 0.01 mol/L EDTA solutions.