Various pretreatments on Ceiba pentandra (L.) Gaertn. (kapok) fiber prior to enzymatic hydrolysis for sugar production were optimized in this study. The optimum conditions for water, acid, and alkaline pretreatments were 170°C for 45 min, 120°C for 45 min in 1.0% (v/v) H2SO4 solution and 120°C for 60 min in 2.0% (v/v) NaOH solution, respectively. Among the three pretreatments, the alkaline pretreatment achieved the highest total glucose yield (glucose yield calculated based on the untreated fiber) (38.5%), followed by the water (35.0%) and acid (32.8%) pretreatments. As a result, the relative effectiveness of the pretreatment methods for kapok fiber was verified as alkali>water>acid at the condition stated.
Oil palm empty fruit bunch (EFB) is abundantly available in Malaysia and it is a potential source of xylose for the production of high-value added products. This study aimed to optimize the hydrolysis of EFB using dilute sulfuric acid (H2SO4) and phosphoric acid (H3PO4) via response surface methodology for maximum xylose recovery. Hydrolysis was carried out in an autoclave. An optimum xylose yield of 91.2 % was obtained at 116 °C using 2.0 % (v/v) H2SO4, a solid/liquid ratio of 1:5 and a hydrolysis time of 20 min. A lower optimum xylose yield of 24.0 % was observed for dilute H3PO4 hydrolysis at 116 °C using 2.4 % (v/v) H3PO4, a solid/liquid ratio of 1:5 and a hydrolysis time of 20 min. The optimized hydrolysis conditions suggested that EFB hydrolysis by H2SO4 resulted in a higher xylose yield at a lower acid concentration as compared to H3PO4.
In this work, we successfully isolated microcrystalline cellulose (MCC) from oil palm empty fruit bunch (OPEFB) fiber-total chlorine free (TCF) pulp using acid hydrolysis method. TCF pulp bleaching carried out using an oxygen-ozone-hydrogen peroxide bleaching sequence. Fourier transform infrared (FT-IR) spectroscopy indicates that acid hydrolysis does not affect the chemical structure of the cellulosic fragments. The morphology of the hydrolyzed MCC was investigated using scanning electron microscopy (SEM), showing a compact structure and a rough surface. Furthermore, atomic force microscopy (AFM) image of the surface indicates the presence of spherical features. X-ray diffraction (XRD) shows that the MCC produced is a cellulose-I polymorph, with 87% crystallinity. The MCC obtained from OPEFB-pulp is shown to have a good thermal stability. The potential for a range of applications such as green nano biocomposites reinforced with this form of MCC and pharmaceutical tableting material is discussed.
A high concentration of phosphorus in wastewater may lead to excessive algae growth and deoxygenation of the water. In this work, nanofiltration (NF) of phosphorus-rich solutions is studied in order to investigate its potential in removing and recycling phosphorus. Wastewater samples from a pulp and paper plant were first analyzed. Commercial membranes (DK5, MPF34, NF90, NF270, NF200) were characterized and tested in permeability and phosphorus removal experiments. NF90 membranes offer the highest rejection of phosphorus; a rejection of more than 70% phosphorus was achieved for a feed containing 2.5 g/L of phosphorus at a pH <2. Additionally, NF90, NF200 and NF270 membranes show higher permeability than DK5 and MPF34 membranes. The separation performance of NF90 is slightly affected by phosphorus concentration and pressure, which may be due to concentration polarization and fouling. By adjusting the pH to 2 or adding sulfuric acid, the separation performance of NF90 was improved in removing phosphorus. However, the presence of acetic acid significantly impairs the rejection of phosphorus.
Oxygenated fuel additives can be produced by acetylation of glycerol. A 91% glycerol conversion with a selectivity of 38%, 28% and 34% for mono-, di- and triacetyl glyceride, respectively, was achieved at 120 °C and 3 h of reaction time in the presence of a catalyst derived from activated carbon (AC) treated with sulfuric acid at 85 °C for 4h to introduce acidic functionalities to its surface. The unique catalytic activity of the catalyst, AC-SA5, was attributed to the presence of sulfur containing functional groups on the AC surface, which enhanced the surface interaction between the glycerol molecule and acyl group of the acetic acid. The catalyst was reused in up to four consecutive batch runs and no significant decline of its initial activity was observed. The conversion and selectivity variation during the acetylation is attributed to the reaction time, reaction temperature, catalyst loading and glycerol to acetic acid molar ratio.
Various pre-treatment techniques change the physical and chemical structure of the lignocellulosic biomass and improve hydrolysis rates. The effect of ultrasonic pre-treatment on oil palm empty fruit bunch (OPEFB) fibre prior to acid hydrolysis has been evaluated. The main objective of this study was to determine if ultrasonic pre-treatment could function as a pre-treatment method for the acid hydrolysis of OPEFB fibre at a low temperature and pressure. Hydrolysis at a low temperature was studied using 2% sulphuric acid; 1:25 solid liquid ratio and 100 degrees C operating temperature. A maximum xylose yield of 58% was achieved when the OPEFB fibre was ultrasonicated at 90% amplitude for 45min. In the absence of ultrasonic pre-treatment only 22% of xylose was obtained. However, no substantial increase of xylose formation was observed for acid hydrolysis at higher temperatures of 120 and 140 degrees C on ultrasonicated OPEFB fibre. The samples were then analysed using a scanning electron microscope (SEM) to describe the morphological changes of the OPEFB fibre. The SEM observations show interesting morphological changes within the OPEFB fibre for different acid hydrolysis conditions.
The kitchen waste fraction in municipal solid waste contains high organic matter particularly carbohydrate that can contribute to fermentable sugar production for subsequent conversion to bioethanol. This study was carried out to evaluate the influence of single and combination pretreatments of kitchen waste by liquid hot water, mild acid pretreatment of hydrochloric acid (HCl) and sulphuric acid (H2SO4) and enzymatic hydrolysis (glucoamylase). The maximum total fermentable sugar produced after combination pretreatment by 1.5% HCl and glucoamylase consisted of 93.25 g/L glucose, 0.542 g/L sucrose, 0.348 g/L maltose, and 0.321 g/L fructose. The glucose released by the combination pretreatment method was 0.79 g glucose/g KW equivalent to 79% of glucose conversion. The effects of the pre-treatment on kitchen waste indicated that the highest solubilization was 40% by the combination method of 1.5% HCl and glucoamylase. The best combination pre-treatment gave concentrations of lactic acid, acetic acid, and propionic acid of 11.74 g/L, 6.77 g/L, and 1.02 g/L, respectively. The decrease of aliphatic absorbance bands of polysaccharides at 2851 and 2923 cm(-1) and the increase on structures of carbonyl absorbance bands at 1600 cm(-1) reflects the progress of the kitchen waste hydrolysis to fermentable sugars. Overall, 1.5% HCl and glucoamylase treatment was the most profitable process as the minimum selling price of glucose was USD 0.101/g kitchen waste. Therefore, the combination pretreatment method was proposed to enhance the production of fermentable sugar, particularly glucose from kitchen waste as the feedstock for bioethanol production.
Bleached kenaf core pulps (BKC) were hydrolyzed in H2SO4 (0.5M) at different time (0min to 90min) at room temperature. After the hydrolysis process, the viscosity average molecular weight (Mŋ) for BKC sample has reduced from 14.5×10(4) to 2.55×10(4). The hydrolyzed BKC was then dissolved in NaOH:urea:water and in LiOH:urea:water mixed solvent at the ratio of 7:12:81 and 4.6:15:80.4, respectively. The increased in hydrolysis time has decreased Mŋ of cellulose leading to easy dissolution process. Higher porosity and transparency with lower crystallinity index (CrI) of regenerated membrane produced can be achieved as the Mŋ reduced. The properties of membrane were observed through FESEM, UV-vis spectrophotometer and XRD. This study has proven that acid hydrolysis has reduced the Mŋ of cellulose, thus, enhanced the properties of regenerated membrane produced with assisted by alkaline/urea system.
The kinetic and thermodynamic adsorption and adsorption isotherms of Pb(II) and Cu(II) ions onto H(2)SO(4) modified chitosan were studied in a batch adsorption system. The experimental results were fitted using Freundlich, Langmuir and Dubinin-Radushkevich isotherms; the Langmuir isotherm showed the best conformity to the equilibrium data. The pseudo-first order, pseudo-second order and intraparticle diffusion kinetic models were employed to analyze the kinetic data. The adsorption behavior of Pb(II) and Cu(II) was best described by the pseudo-second order model. Thermodynamic parameters such as free energy change (DeltaG degrees ), enthalpy change (DeltaH degrees ) and entropy change (DeltaS degrees ) were determined; the adsorption process was found to be both spontaneous and exothermic. No physical damage to the adsorbents was observed after three cycles of adsorption/desorption using EDTA and HCl as eluents. The mechanistic pathway of the Pb(II) and Cu(II) uptake was examined by means of Fourier transform infrared (FTIR) and Energy dispersive X-ray (EDX) spectroscopy. The equilibrium parameter (R(L)) indicated that chitosan-H(2)SO(4) was favorable for Pb(II) and Cu(II) adsorption.
Pretreatments with different types of alkali and acid were compared to determine their effects on gelatin extraction from African catfish (Clarias gariepinus) skin. The study was divided into three parts. In the first part, the skins were only treated with alkaline (Ca(OH)2 or NaOH) solution or pretreated with acetic acid solution. For second part, combination of alkali and acid pretreatment was carried out. For the third part, the skins were first treated with NaOH solution, followed by the treatment with acetic acid, citric acid or sulfuric acid solution. Functional properties including the yield of protein recovery, gel strength, viscosity, pH and viscoelastic properties were determined on gelatins obtained with different pretreatment conditions. Pretreatment with alkali removed noncollagenous proteins effectively, whilst acid pretreatment induced some loss of collagenous proteins. Combination of alkali and acid pretreatment not only removed the noncollagenous proteins and caused a significant amount of swelling, but also provided the proper pH condition for extraction, during which some cross-linkages could be further destroyed but with less breakage of intramolecular peptide chains. Pretreatment of catfish skins with 0.2 N NaOH followed by 0.05 M acetic acid improved yield of protein recovery, gel strength, viscosity, melting temperature and gelling temperature of gelatin extract.
Hermetia illucens larvae by nature are a decomposer which fed on organic wastes. This study explores the potential of producing biodiesel using lipids from H. illucens larvae. Three types of organic wastes (sewage sludge, fruit waste and palm decanter cake from oil palm mill) were selected based on considerable generation and disposal concern in the area of study as well as lack of investigations as feed for Hermetia illucens larvae in current literatures. Growth rate of the larvae was determined with studying the changes in the biomass per day. H. illucens larvae fed with fruit waste and palm decanter cake have shown growth rates of 0.52±0.02 and 0.23±0.09 g d(-1), respectively. No positive sign of growth were observed in the larvae fed with treated sewage sludge (-0.04±0.01 g d(-1)). Biodiesel as fatty acid methyl ester (FAME) was synthesized by transesterification of the larvae lipid using sulphuric acid as catalyst in methanol. FAME produced was ascertained using ATR-FTIR spectroscopy and GC-MS. The main compositions of fatty acid were found to be C12:0, C16:0 and C18:1n9c. Fatty acid composition of C12:0 fed with fruit waste, sewage sludge and palm decanter was found to be most abundant in the larvae lipid. The amount of C12:0 obtained was 76.13%, 58.31% and 48.06%, respectively. In addition, fatty acid of C16:0 was attained at 16.48% and 25.48% fed with sewage sludge and palm decanter, respectively. Based on the findings, FAME derived from larvae lipids is feasible to be used for biodiesel production.
Treatment of vanadium(V) oxide with an ethanol-concentrated sulfuric acid mixture, followed by the addition of an equimolar amount of beta-alanine and sodium hydroxide, and finally raising the pH to 3.9 with sodium carbonate solution, under continuous heating in a water bath and in the presence of air, leads to the polyionic sodium cyclo-[mu(6)-(sulfato-O,O',O'')tris[mu-(beta-alanine-O,O')-mu-oxo]tris(mu-hydroxo-mu-oxo)hexa[oxovanadium(V)]] sulfate tridecahydrate which crystallizes in the monoclinic P2(1)/n space group [a = 9.5192(4), b = 20.1185(9), c = 22.6174(9) A, beta = 97.011(1) degrees; Z = 4]. The crown-shaped polyoxovanadium(V) cluster cation, with carboxylate-bridging amino acid ligands, has an Anderson structure with two unique capping sulfato ligands. Its structural analysis, together with IR, UV-vis, and preliminary data on its solution properties, is presented.
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.
The aim was to explore the utilization of tea leaf waste fibers (TLWF) as a source for the production of cellulose nanocrystals (CNC). TLWF was first treated with alkaline, followed by bleaching before being hydrolyzed with concentrated sulfuric acid. The materials attained after each step of chemical treatments were characterized and their chemical compositions were studied. The structure analysis was examined by Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). From FTIR analysis, two peaks at 1716 and 1207 cm-1-which represent C=O stretching and C⁻O stretching, respectively-disappeared in the spectra after the alkaline and bleaching treatments indicated that hemicellulose and lignin were almost entirely discarded from the fiber. The surface morphology of TLWF before and after chemical treatments was investigated by scanning electron microscopy (SEM) while the dimension of CNC was determined by transmission electron microscopy (TEM). The extraction of CNC increased the surface roughness and the crystallinity index of fiber from 41.5% to 83.1%. Morphological characterization from TEM revealed the appearance of needle-like shaped CNCs with average diameter of 7.97 nm. The promising results from all the analyses justify TLWF as a principal source of natural materials which can produce CNC.
As cobalt (Co) represents an effective transition metal for activating Oxone to degrade contaminants, tricobalt tetraoxide (Co3O4) is extensively employed as a heterogeneous phase of Co for Oxone activation. Since Co3O4 can be manipulated to exhibit various shapes, 2-dimensional plate-like morphology of Co3O4 can offer large contact surfaces. If the large plate-like surfaces can be even porous, forming porous nanoplate Co3O4 (PNC), such a PNC should be a promising catalyst for Oxone activation. Therefore, a facile but straightforward method is proposed to prepare such a PNC for activating Oxone to degrade pollutants. In particular, a cobaltic coordination polymer with a morphology of hexagonal nanoplate, which is synthesized through coordination between Co2+ and thiocyanuric acid (TCA), is adopted as a precursor. Through calcination, CoTCA could be transformed into hexagonal nanoplate-like Co3O4 with pores to become PNC. This PNC also shows different characteristics from the commercial Co3O4 nanoparticle (NP) in terms of surficial reactivity and textural properties. Thus, PNC exhibits a much higher catalytic activity than the commercial Co3O4 NP towards activation of Oxone to degrade a model contaminant, salicylic acid (SA). Specifically, SA was 100% degraded by PNC activating Oxone within 120 min, and the Ea of SA degradation by PNC-activated Oxone is 70.2 kJ/mol. PNC can also remain stable and effective for SA degradation even in the presence of other anions, and PNC could be reused over multiple cycles without significant loss of catalytic activity. These features validate that PNC is a promising and useful Co-based catalyst for Oxone activation.
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.
Palm oil-based Trimethylolpropane ester (TMP ester), with an iodine value of 66.4 g/100g, was epoxidizedto produce epoxidized TMP esters. In situ epoxidation method was used with peracetic acid to eliminatefatty acid double bonds in palm oil-based TMP ester and change it into oxirane ring. This was done toimprove the oxidative stability of trimethylolpropane ester which is a key concern limiting the usefulservice life in lubricants. The epoxidation was performed by reacting acetic acid as active oxygen carrierwith concentrated hydrogen peroxide as oxygen donor and a small amount of homogeneous catalyst(sulphuric acid). The effects of various parameters on the rate of epoxidation (such as the ratio of moleacetic acid to ethylenic unsaturation, hydrogen peroxide to ethylenic unsaturation and acetic acid moleratio, and amount of catalyst) were studied. The rate of oxidation was investigated by the percentageof oxirane oxygen analysis and iodine value.
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.
Waste water treatment reservoirs are contaminated with many hazardous chemicals and acids. Reservoirs typically comprise concrete and reinforcement steel bars, and the main elements responsible for their deterioration are hazardous chemicals, acids, and ozone. Currently, a variety of techniques are being used to protect reservoirs from exposure to these elements. The most widely used techniques are stainless steel plating and polymeric coating. In this study, a technique known as arc thermal spraying was used. It is a more convenient and economical method for protecting both concrete and reinforcement steel bar from deterioration in waste water treatment reservoirs. In this study, 316L stainless steel coating was applied to a concrete surface, and different electrochemical experiments were performed to evaluate the performance of coatings in different acidic pH solutions. The coating generated from the arc thermal spraying process significantly protected the concrete surface from corrosion in acidic pH solutions, owing to the formation of a double layer capacitance-a mixture of Cr3+ enriched with Cr₂O₃ and Cr-hydroxide in inner and Fe3+ oxide on the outer layer of the coating. The formation of this passive film is defective owing to the non-homogeneous 316L stainless steel coating surface. In the pH 5 solution, the growth of a passive film is adequate due to the presence of un-dissociated water molecules in the aqueous sulfuric acid solution. The coated surface is sealed with alkyl epoxide, which acts as a barrier against the penetration of acidic solutions. This coating exhibits higher impedance values among the three studied acidic pH solutions.
The efficiency of Schiff base derived from 4-aminoantipyrine, namely 2-(1,5-dimethyl-4-(2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-ylidene) hydrazinecarbothioamide as a corrosion inhibitor on mild steel in 1.0 M H2SO4 was investigated using electrochemical impedance spectroscopy (EIS), potentiodynamic polarization (PD) and electrochemical frequently modulation (EFM) in addition to the adsorption isotherm, corrosion kinetic parameters and scanning electron microscopy (SEM). The results showed that this inhibitor behaved as a good corrosion inhibitor, even at low concentration, with a mean efficiency of 93% and, also, a reduction of the inhibition efficiency as the solution temperature increases. A polarization technique and EIS were tested for different concentrations and different temperatures to reveal that this compound is adsorbed on the mild steel, therefore blocking the active sites, and the adsorption follows the Langmuir adsorption isotherm model. The excellent inhibition effectiveness of 2-(1,5-dimethyl-4-(2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-ylidene)hydrazinecarbothioamide was also verified by scanning electron microscope (SEM).