Mass-Based Environmental Factor and Energy Assessment of Microwave-Assisted Synthesized Transition Metal Nanostructures

This paper describes mass-based energy phase-space projection of microwave-assisted synthesis of transition metals (zinc oxide, palladium, silver, platinum, and gold) nanostructures. The projection uses process energy budget (measured in kJ) on the horizontal axes and process density (measured in kJg−1) on the vertical axes. These two axes allow both mass usage efficiency (Environmental-Factor) and energy efficiency to be evaluated for a range of microwave applicator and metal synthesis. The metrics are allied to the: second, sixth and eleventh principle of the twelve principle of Green Chemistry. This analytical approach to microwave synthesis (widely considered as a useful Green Chemistry energy source) allows a quantified dynamic environmental quotient to be given to renewable plant-based biomass associated with the reduction of the metal precursors. Thus allowing a degree of quantification of claimed “eco-friendly” and “sustainable” synthesis with regard to waste production and energy usage.

Microwave-assisted Synthesis of Al_(4)SiC_(4) and Its Effect on Properties of MgO-C Refractories

Al_(4)SiC_(4) was synthesized from Al powder, silicon carbide, and graphite by microwave sintering, and characterized by XRD and SEM. Then the synthesized material was added to the magnesia carbon refractory brick to study its effect on the oxidation resistance, apparent porosity, bulk density, elastic modulus, and modulus of rupture. It is found that Al_(4)SiC_(4) can be synthesized by microwave sintering at 1 300 ℃ and the addition of Al_(4)SiC_(4)-containing material as an antioxidant can enhance the oxidation resistance of the magnesia carbon refractory brick.

Effect of microwave-assisted acidification on the microstructure of coal:XRD,^(1)H-NMR, and SEM studies

Microwave heating contributes to coal fracturing and gas desorption. However, problems of low penetration depth, local overheating and fracture closure exist. Coal demineralisation by acids has advantages in coal unblocking and permeability improvement, while it is difficult for acid to enter microcracks.Microwave-asisted acidification may offer an alternative. In this work, XRD,^(1)H-NMR, and SEM were used to evaluate the effect of microwave-assisted acidification on the microstructure of coal. Results show that kaolinite, calcite, and dolomite can be dissolved by acid. After microwave irradiation, the graphitization of microcrystalline structure of carbon improves. Microwave-assisted acidification erodes minerals in coal and enhances the graphitization degree of microcrystalline structure. Compared to individual microwave irradiation or acidification, the pore volume and pore connectivity can be greatly enhanced by microwave-assisted acidification. The NMR permeability of coal increased by 28.05%. This study demonstrates the potential of microwave-assisted acidification for coalbed methane recovery.

Gradient Si-and Ti-doped Fe_(2)O_(3) hierarchical homojunction photoanode for efficient solar water splitting:Effect of facile microwave-assisted growth of Si-FeOOH on Ti-FeOOH nanocorals

The construction of a homojunction is an effective approach for addressing issues such as slow charge separation and charge-transfer kinetics in photoanodes.In the present work,we designed a gradient Si-and Ti-doped Fe_(2)O_(3) homojunction photoanode to improve the photoelectrochemical(PEC)performance of a Ti-doped Fe_(2)O_(3) photoanode.Ti-FeOOH nanocorals were synthesized using a hydrothermal process,and Si-FeOOH was grown on Ti-FeOOH nanocorals using a rapid and facile microwaveassisted(MW)technique.By varying the MW irradiation time,the thickness of the Si/Ti:Fe_(2)O_(3) photoanode was adjusted and an optimized 3-Si/Ti:Fe_(2)O_(3) photoelectrode was achieved with a significantly enhanced photocurrent density(1.37 mA cm^(-2) at 1.23 V vs.RHE)and a cathodic shift of the onset potential(150 mV)compared with that of bare Ti-Fe_(2)O_(3).This enhanced PEC performance can be ascribed to homojunction formation and Si gradient doping.The Si dopant increased the donor concentration and the formation of a homojunction improved the intrinsic built-in electric field,thereby promoting charge separation and charge transfer.Furthermore,the as-formed homojunction passivated the surfacetrapping states,consequently improving the charge transfer efficiency(60%at 1.23 VRHE)at the photoanode/electrolyte interface.These findings could pave the way for the microwave-assisted fabrication of diverse efficient homojunction photoanodes for PEC water splitting applications.

Profiling the effects of microwave-assisted and soxhlet extraction techniques on the physicochemical attributes of Moringa oleifera seed oil and proteins

There is a constant search for biomaterials from natural products like plants for food and industrial applications.The work embodied in this report aimed at investigating the effects of microwave-assisted and soxhlet extraction(MAE and SE) techniques on the functional physicochemical quality characteristics of Moringa oleifera seed oil and proteins extracts. M. oleifera seeds were ground to fine powders and oil was extracted by microwave-assisted and soxhlet extraction techniques using petroleum ether. Quality attributes including yield percent, moisture content,iodine, saponification, specific gravity, viscosity, p H, thiobarbituric acid, acid and peroxide values were measured. Mineral and vitamin contents, chemical/functional groups, fatty acid(FA) composition, and reducing power of the oil were evaluated. Metabolomics of protein extracted from the defatted powders were analyzed by nuclear magnetic resonance(NMR). M. oleifera oil from MAE and SE methods had good yield(34.25 ± 0.0%,28.75 ± 0.0%), low moisture content(0.008 ± 0.0%, 0.011 ± 0.0%), non-drying and unsaturated, moderately saponified, less dense(0.91 ± 0.01, 0.92 ± 0.02 g m L^(-1)), had Newtonian flow, were weakly acidic, showed good content of FAs, recorded strong potential for long shelf-life, showed stability against oxidative rancidity and enzymatic hydrolysis, had very rich deposits of micro-and macro-nutrients as well as water-soluble and lipidsoluble vitamins, and functional groups in the oil were reflective of its content of long-and medium-chain triglycerides(LCT and MCT). Monounsaturated and saturated fatty acids(MUFA and SFA) were detected and the oil has excellent ferric ion reducing power. NMR metabolomic assay revealed the presence of nine essential amino acids(EAAs) in the protein extract. MAE technique is a feasible and acceptable alternative for high throughput extraction of M. oleifera oil with high yield and excellent quality attributes. The study revealed that MAE did not impart any remarkable advantage(s) on the physicochemical properties of M. oleifera seed oil and protein compared to SE technique.

Microwave-Assisted Au and Ag Nanoparticle Synthesis: An Energy Phase-Space Projection Analysis

Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commercial temperature controlled microwave chemistry ovens (TCMC), digesters, and axial field helical antennae. For each of these microwave applicators the process energy budget where estimated (Watts multiplied by process time = kJ) and energy density (applied energy divided by suspension volume = kJ·ml-1) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml-1, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m-1 per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml-1 per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m-1 per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m-1 per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R2 = 0.7923) four orders of magnitude. The paper provides a discussion on the Au and Ag nanoparticle chemistry and bio-chemistry synthesis aspects of the microwave applicator energy datasets and variation within each dataset. The visual and analytical approach within the energy phase-space projection enables a nanoparticle synthesis route to be systematically characterized, and where changes to the synthesis are to be mapped and compared directly with historical datasets. In order to help identify lower cost nanoparticle synthesis, in addition to potentially reduce synthesis energy to routes informed changes to potentially reduce synthesis energy budget, along with nanoparticle morphology and yield.

Green Chemistry Allometry Test of Microwave-Assisted Synthesis of Transition Metal Nanostructures

Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rather than hours when compared to conventional thermal heating. This works describes a dual allometry test for the discrimination between the solvents and reagents used in the microwave-assisted synthesis of transition metal (zinc oxide, palladium silver, platinum, and gold) nanostructures. The test is performed in log-log process energy phase-space projection, where the synthesis data (kJ against kJ·mol-1) has a power-law signature. The test is shown to discriminate between recommended Green Chemistry, problematic Green Chemistry, and Green Chemistry hazardous solvents. Typically, recommended Green chemistry exhibits a broad y-axes distribution within an upper exponent = 1 and lower exponent = 0.5. Problematic Green Chemistry exhibits a y-axes narrower distribution with an upper exponent = 0.94 and lower exponent = 0.64. Non-Green Chemistry hazardous data exhibits a further narrowing of the y-axes distribution within upper exponent = 0.87 and lower exponent = 0.66. In all three cases, the y-axes is aligned to original database power-law signature. It is also shown that in the x-axes direction (process energy budget) the grouped order of magnitude decreases from four orders for recommended Green Chemistry solvent and reagent data, through two orders for non-Green Chemistry hazardous material and down to one order for problematic Green Chemistry.

Microwave-Assisted Transition Metal Nanostructure Synthesis: Power-Law Signature Verification

A power-law (y = cxn) signature between process energy budget (kJ) and process energy density (kJ·ml-1) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml-1. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml-1. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml-1 at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.

Optimization of Microwave-assisted Extraction Technology of Polyphenols from Loropetalum chinense(R. Br.) Oliv

In order to optimize the microwave-assisted extraction technology of polyphenols from Loropetalum chinense （R. Br.） Oliv., the effects of microwave power, ethanol concentration, solid to liquid ratio and extraction time on polyphenols extraction rate were investigated. On the basis of single-factor test, a four-factor and three-level orthogonal test was designed by response surface method to establish a mathematical model between the response value and various factors. The results showed that the intensity of effect of different influencing factor on polyphenols ex- traction rate ranked as microwave power＇s〉solid to liquid ratio＇s〉extraction time＇s〉 ethanol concentration＇s. The optimum microwave-assisted extraction conditions for polyphenols from L. chinense were as follows： extraction power 254 W, ethanol concentration 60%, extraction time 12.5 rain and solid to liquid ratio 1：17. Under the optimum extraction conditions, the extraction rate of polyphenols from L. chinense was 19.17%.

MICROWAVE-ASSISTED EXTRACTION OF GLYCYRRHIZIC ACID FROM LICORICE ROOT-EFFECT OF THE PROPERTY OF SOLUTION ON EXTRACTION OF GA

The property of extraction solution is an important factor influencing the extraction efficiency. In the present work, the effect of the property of solution on extraction of GA was studied, which including the concentration of ethanol, ammonia and cation (M+), pH of extraction solution, different kinds of organic solvent etc. The results show that 50%-60%(v/v) ethanol can reach high percentage extraction of GA. If 1% (v/v) ammonia solution was added into 60%(v/v) ethanol, the percentage extraction can be increased from 2.0% to 2.31%. Without ammonia, 50mmol/L [M+] (M+ = K+, NH4+) was added into 60%(v/v) ethanol, percentage extraction of GA can reach about 2.26%. If pH of solution (60% ethanol) was adjust to pH=4.0, it can reach high percentage extraction. If pH of solution (60% ethanol + 50mmol [M+], pH=6.1) was adjust tO PH=4.0, especially M+ is K+ or NH4+, it can reach almost same extraction efficiency as that of 1% ammonia solution + 60% ethanol, and the operation environment can be greatly improved.

Microwave-assisted extraction of polysaccharides from solanum nigrum

The microwave-assisted method was used to extract polysaccharides from solanum nigrum. The optimum experimental parameters, mechanism of the extraction and the effect of microwave-assisted extraction process on the structures of polysaccharides were investigated. The extract was analyzed by the modified phenol-sulfuric acid method at 490nm. The optimum experimental parameters were obtained by orthogonal experiments as follows: extraction time 15min, microwave radiation power 455W and the process ratio of materials mass to solvent volume 1∶20. The results show that compared with the conventional reflux extraction, the microwave-assisted extraction has a higher yield in shorter time, with no effect on the finally obtained polysaccharides as seen from the FT-IR spectra. The scanning electron microscopy images reveal that the mechanism of the extraction is related to the structural changes of the plant cells in different extracting conditions.

Low temperature microwave-assisted vs conventional pyrolysis of various biomass feedstocks

A comparison between conventional pyrolysis and a novel developed low-temperature microwave-assisted pyrolysis methodology has been performed for the valorisation of a range of biomass feedstocks including waste residues. Microwave pyrolysis was found to efficiently deliver comparable evolution of bio-gases in the system as compared with conventional pyrolysis at significantly reduced temperatures （120-180 ℃vs 250-400 ℃）. The gas obtained from microwave-assisted pyrolysis was found to contain CO2, CH4 and CO as major components as well

Microwave-assisted Extraction of Isoflavones from Belamcanda chinensis

Microwave-assisted extraction （MAE） of isoflavones from Belamcanda chinensis was studied using ethanol as the solvent. The single factor experiment and the orthogonal method were used to optimize the MAE condition. It was concluded that two doses of intermittent microwave power radiation, 300 W each for 4 rain, were needed for extraction. The mass ratio of solvent to material was 8：1 and the alcohol mass fraction was 80%. The extracted liquor was then concentrated under vacuum and degreased with petroleum ether. The yield of total isofiavones was about 8.8% and the contents of tectoridin and iridin were 67.6% and 16.3% respectively. Compared with direct-heating extraction （DHE）, MAE may shorten extracting duration, reduce solvent consumption, and improve yield and purity of isoflavones from Belamcanda chinensis.

Microwave-assisted Extraction of Effective Compounds from Traditional Chinese Herbal Medicine Ciwujia

Microwave-assisted extraction (MAE) for active ingredients in Ciwujia was studied by using ethanol as the extractant. Comparing MAE with conventional methods, the former can save the extracting time and increase the content of the active ingredients in product. As to the operation in MAE, the continuous radiation process is more convenient for the extraction for traditional Chinese medicine than the intermittent radiation process. Optimized by uniform design, MAE was proved to be an effective and novel process for extracting active ingredients in Ciwujia. The optimized MAE conditions are as follows: the microwave power is 510W, the radiation time 30min, the alcohol concentration at 80%, the ratio of solvent to solid material being 5:1, the soaking time 0.5h, and the herbal particle size is (520±19)μm.

Microwave-assisted Extraction of Rutin and Quercetin from Flos Sophorae

Three microwave-assisted extraction(MAE) procedures were studied. The first procedure was household microwave oven dynamic extraction(HMODE). The second procedure was special microwave oven bath extraction(SMOBE). The third procedure was microwave resonant cavity dynamic extraction(MRCDE). The results obtained by the three microwave-assisted extraction procedures were compared with those obtained by using traditional Soxhlet extraction. The results indicate that the MAE not only took a shorter time, but also simplified the procedure, and made the extraction a higher yield. At the same time the results obtained by the three MAE procedures were also compared with each other.

Optimization of microwave-assisted extraction of bioactive alkaloids from lotus plumule using response surface methodology

In this work,a fast and efficient microwave-assisted extraction(MAE) method was developed to extract main bioactive alkaloids from lotus plumue.To optimize MAE conditions,three main factors were selected using univariate approach experiments,and then central composite design(CCD).The optimal extraction conditions were as follows:methanol concentration of 65%,microwave power of 200 W,and extraction time of 260 s.A high performance liquid chromatography–diode array detector(HPLC–DAD) method was established to quantitatively analyze these phytochemicals in different lotus plumule samples and in different part of lotus.Chromatographic separation was carried out on an Agilent Zorbax Extend-C_(18) column(4.6 mm×150 mm,3.5 μm).Gradient elution was applied with the mobile phase constituted with 0.1% triethylamine in water(A)and acetonitrile(B):40%-70% B at 0-8 min,70%-100% B at 8–9 min,100% B for 2 min,and then equilibrated with 40% B for 2 min.

Microwave-assisted Micellar Extraction and Determination of Glycyrrhizic Acid and Liquiritin in Licorice Root by HPLC

The feasibility of emploving non-ionic surfactant （Triton X-100） as an alternative and effective solventfor the microwave-assisted extraction of glycyrrhizic acid （GA） and liquiritin （LQ） from licorice root was studied.The optimal extraction parameters based on the microwave-assisted micellar extraction technique were determined.Under the optimal conditions, i.e. 5% （by volume） Triton X-100, microwave-assisted extraction for 3--5min at 373K, the percentage extraction of active ingredients reached the highest value. The preconcentration tactor for GA and L＇Q （about 13.5） and the extraction efficiency for these two ingredients approached 100% showed the coupling of microwave-assisted extraction and cloud-point extraction could be employed as a new and. effective techniquefor the rapid extraction and preconcentration of pharrnacologically active ingredients from medicinal plants SUCh aslicorice root without disturbing chromatographic analysis.

Microwave-assisted solvent extraction of castor oil from castor seeds

This study was aimed at evaluating the physicochemical properties and oxidation stability of castor oil using microwave-assisted solvent extraction(MAE). MAE was performed using 5% ethanol in hexane as solvent at different extraction times, power intensities and solvent-to-feed(S/F, ml of solvent to gram of feed) ratios.The process parameters were optimized by statistical approach using historical data design of response surface method(RSM). The oils were characterized for yield, physicochemical properties, dielectric properties and oxidation stability, and comparison was also made with oil extracted using Soxhlet method. Results show that the maximum oil yield of 37% was obtained at 20 min with microwave power intensity of 330 W and S/F ratio of 20. The main fatty acid composition of castor oil is ricinoleic acid. The density, refractive index, dielectric properties and oxidation stability of oils are not affected by the extraction methods and extraction parameters of MAE. However, the MAE-extracted oil is more viscous compared to that by Soxhlet method. With extra caution on oil oxidation, MAE could be a promising solvent extraction method with an 86% less in processing time and a higher yield.

Dynamic microwave-assisted extraction combined with liquid phase microextraction based on the solidification of a floating drop for the analysis of organochlorine pesticides in grains followed by GC

A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides in grains including rice,maize and millet.Twelve samples can be processed simultaneously in the method.During the extraction process,10%acetonitrile-water solutions containing 110μL of n-hexadecane were used to extract organochlorine pesticides.Subsequently,1.0 g sodium chloride was placed in the extract,and then centrifuged and cooled.The n-hexadecane drops containing the analytes were solidifi ed and transferred for determination by gas chromatography-electron capture detector without any further filtration or cleaning process.Limits of detection for organochlorine pesticides were 0.97–1.01μg/kg and the RSDs were in the range of 2.6%–8.5%.The developed technology has succeeded in analyzing six real grains samples and the recoveries of the organochlorine pesticides were 72.2%–94.3%.Compared with the published extraction methods,the developed method was used to analyze organochlorine pesticides in grains,being more environmentally friendly,which is suitable for the daily determination of organochlorine pesticides.

Green evaluation of microwave-assisted leaching process of high titanium slag on life cycle assessment

A greenness evaluation index and system of microwave-assisted leaching method were established.The effects of the life cycle assessment variables,such as the resource consumption,environment impact,cost,time and quality,were investigated,and the concept of green degree was applied in the production of synthetic rutile.An analytic hierarchy process was utilized to assess matrix of greenness evaluation.The Gauss-Seidel iterative matrix method was employed to solve the assessment matrix and obtain the weights and membership functions of all evaluation indexes.A fuzzy decision-making method was applied to build the greenness evaluation model,and then the scores of green degree in microwave-assisted leaching process was obtained.The greenness evaluation model was applied to the life cycle assessment of the microwave-assisted leaching process.The results show that the microwave-assisted leaching process has advantages over the conventional ones,with respect to energy-consumption,processing time and environmental protection.