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This paper aims to set up viable units of thermal processing of numerous agricultural wastes in a sustainable development and eco-friendly approach that could create new economic profitable circuits in an increasingly competitive context. One of the most problematic food wastes are tomato processing by-products; concentrating and canning industrial activities generate important amounts of them, particularly in the Tunisian context. As no reference was found in literature dealing with these last residues, this work intended to explore their potential as biomass fuels. Pyrolysis is then applied in thermogravimetric conditions for different heating rates (5, 10, 20, and 30 °C/min) in order to recover energy on one hand and to extract the corresponding kinetic parameters for an accurate design of reactors on the other hand. Main results include suitability of the tomato residues to a thermal valorization thanks to high contents of volatiles and fixed carbon and low ash percentage as well as an interesting heating value comparable to lignocellulosic biomass. Mass loss profiles indicate consecutive and overlapping stages of drying, active pyrolysis, and passive pyrolysis. The experimental profiles of conversion rate were well fitted by the three isoconversional methods; the best fitting is recorded by the Flynn-Wall-Ozawa associated with a first-order model for the intermediate pyrolysis and with a contracted sphere (n = 1/3) for the slowest studied pyrolysis.

Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, 1 , with formula Cd 3 (ox)F 2 (Ina) 2 (Ina = isonicotinate) and 2 , Cd(NO 3 ) 2 (4,4'-Bpy) (4,4'-Bpy = 4,4'-Bipyridine). The modification of the reaction conditions has allowed to obtain 2 as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound 1 is isostructural to the previously reported Cd 2 Zn(ox)(OH) 2 (Ina) 2 . It crystallizes in the monoclinic space group P 2 1 /n and present a three-dimensional (3D) network, built-up from [Cd 3 (ox)F 2 ] n 2n+ layers, linked by isonicotinate ligands. Crystals of 2 are formed by twins of two components which are rotated ca. 180° to each other. This compound crystallizes in the triclinic P -1 space group and its structure can be describe as a two-dimensional (2D) 4 connected 'sql' net. The layers are composed by [Cd(NO 3 ) 2 ] n chains linked through 4,4'-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of 2 was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 °C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.

As a global pollutant, microplastics have attracted attention from the public and researchers. However, the lack of standard and time-saving methods for analysis has become one of the bottlenecks in microplastics research. Here, we demonstrate TGA coupled to FTIR to identify and quantify certain microplastics in environment. Samples were pyrolyzed in TGA and the pyrolysis gases were analyzed by FTIR. Combining TGA and FTIR data adds discriminatory power as temperature profiles and absorption spectra differ among several common plastics. To quantify on a mass basis, we calibrated on characteristic IR peaks at temperatures of maximum weight loss for individual polymers. The method can distinguish PVC, PS and was validated by spiking samples with known quantities of microplastics. The result of field sample experiments showed that TGA-FTIR can be used to identify and quantify PVC and PS in bivalves, seawater and soil. And the method may be applicable to environmental samples., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Morphology-controlled nanomaterials such as silica play a critical role in the development of technologies for use in the fields of energy, environment (water and air pollution) and health. Since the discovery of Stöber's silica, followed by the discovery of mesoporous silica materials (MSNs) such as MCM-41 and SBA-15, a surge in the design and synthesis of nanosilica with various sizes, shapes, morphologies and textural properties (surface area, pore size and pore volume) has occurred. Dendritic fibrous nanosilica (DFNS; also known as KCC-1) is one of the recent discoveries in morphology-controlled nanomaterials. DFNS shows exceptional performance in large numbers of fields, including catalysis, gas capture, solar energy harvest, energy storage, sensors and biomedical applications. This material possesses a unique fibrous morphology, unlike the tubular porous structure of various conventional silica materials. It has a high surface area to volume ratio, with improved accessibility to the internal surface, tunable pore size and pore volume, controllable particle size and, importantly, improved stability. However, synthesis of DFNS with controllable size, textural properties and fiber density is still tricky because of several of the steps involved. This protocol provides a comprehensive step-wise description of DFNS synthesis and advice regarding how to control size, surface area, pore size, pore volume and fiber density. We also provide details of how to apply DFNS in catalysis and CO 2 capture. Detailed characterization protocols for these materials using scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption and thermal gravimetric analysis (TGA) studies are also provided.

Thermal decomposition of solids often includes simultaneous occurrence of the overlapping processes with unequal contributions in a specific physical quantity variation during the overall reaction (e.g., the opposite effects of decomposition and evaporation on the caloric signal). Kinetic analysis for such reactions is not a straightforward, while the applicability of common kinetic calculation methods to the particular complex processes has to be justified. This study focused on the critical analysis of the available kinetic calculation methods applied to the mathematically simulated thermogravimetry (TG) and differential scanning calorimetry (DSC) data. Comparing the calculated kinetic parameters with true kinetic parameters (used to simulate the thermoanalytical curves), some caveats in the application of the Kissinger, isoconversional Friedman, Vyazovkin and Flynn-Wall-Ozawa methods, mathematical and kinetic deconvolution approaches and formal kinetic description were highlighted. The model-fitting approach using simultaneously TG and DSC data was found to be the most useful for the complex processes assumed in the study.

The study reports on the effect of anaerobic digestate derived composts on the metabolite composition and thermal behaviour of rosemary (Rosmarinus officinalis L.). Plants were cultivated in semiarid soil under four different fertiliser treatments (composts of anaerobic digested cattle (C) or pig slurry (P) at 30t/ha and 60 t/ha, and two control treatments (inorganic fertiliser and no fertiliser application). Samples of leaves and stems were analysed to investigate the effect of treatment on chemical composition and thermochemical properties. Three orthogonal analytical approaches were used, namely: Fourier transform mid infrared spectroscopy (FTIR), gas chromatography/mass spectrometry (GC/MS) and thermochemical gravimetric analysis (TGA). FTIR and GC/MS showed fertiliser treatment resulted in tissue specific changes in sample metabolite composition. Fertiliser treatment was detected to change the thermogravimetric properties of the leaf samples and from inorganic and composted pig slurry digestate treatments had greater ash content and lower proportions of fixed carbon compared with samples from the unfertilised control treatment. This study provides information on how the composition of rosemary might be altered by fertiliser application in regions of poor soil, and has implications for biomass quality when rosemary is grown on semi-wild sites for the purpose of soil improvement.

Non-isothermal sublimation kinetics of low-volatile materials is more favorable over isothermal data when time is a crucial factor to be considered, especially in the subject of detecting explosives. In this article, we report on the in-situ measurements of the sublimation activation energy for 2,4,6-trinitrotoluene (TNT) continuous nanofilms in air using rising-temperature UV-Vis absorbance spectroscopy at different heating rates. The TNT films were prepared by the spin coating deposition technique. For the first time, the most widely used procedure to determine sublimation rates using thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) was followed in this work using UV-Vis absorbance spectroscopy. The sublimation kinetics were analyzed using three well-established calculating techniques. The non-isothermal based activation energy values using the Ozawa, Flynn⁻Wall, and Kissinger models were 105.9 ± 1.4 kJ mol -1 , 102.1 ± 2.7 kJ mol -1 , and 105.8 ± 1.6 kJ mol -1 , respectively. The calculated activation energy agreed well with our previously reported isothermally-measured value for TNT nanofilms using UV-Vis absorbance spectroscopy. The results show that the well-established non-isothermal analytical techniques can be successfully applied at a nanoscale to determine sublimation kinetics using absorbance spectroscopy.

Surface modification may lead activated carbon (AC) to take on different properties. This study aimed to promote surface modification of activated carbons using corona treatment (electrical discharge). In this study, powdered commercial activated carbon was used. Activated carbons were subjected to corona treatment at different exposure times (2, 5, 8 and 10 min) at 4.5 cm height from the source. To observe differences promoted by treatment, activated carbons were analyzed by acidity, surface functional groups, Fourier Transform Infrared Spectroscopy (FTIR), elemental analysis (CHN), proximate analysis and thermogravimetry. Corona treatment impacted surface chemistry of activated carbons. There was a trend of increasing surface acidity according to exposure time. There were changes in functional groups, increasing carboxyl acid and decreasing lactone and phenol groups. FTIR analysis showed peaks in the bands at 3500, 1650 and 1300 cm-1. Increase of oxygen content and decrease of carbon content were also found. Immediate analysis followed similar tendency for volatile and fixed carbon content. There were also differences in thermogravimetry analysis. Treated activated carbons were different compared to virgin activated carbon. This difference was performed by surface oxidation. Thus, this study showed that corona treatment caused surface modifications and might impact adsorption process.

As a renewable, Miscanthus offers numerous advantages such as high photosynthesis activity (as a C₄ plant) and an exceptional CO₂ fixation rate. These properties make Miscanthus very attractive for industrial exploitation, such as lignin generation. In this paper, we present a systematic study analyzing the correlation of the lignin structure with the Miscanthus genotype and plant portion (stem versus leaf). Specifically, the ratio of the three monolignols and corresponding building blocks as well as the linkages formed between the units have been studied. The lignin amount has been determined for M . x giganteus (Gig17, Gig34, Gig35), M . nagara (NagG10), M . sinensis (Sin2), and M . robustus (Rob4) harvested at different time points (September, December, and April). The influence of the Miscanthus genotype and plant component (leaf vs. stem) has been studied to develop corresponding structure-property relationships (i.e., correlations in molecular weight, polydispersity, and decomposition temperature). Lignin isolation was performed using non-catalyzed organosolv pulping and the structure analysis includes compositional analysis, Fourier transform infradred (FTIR), ultraviolet/visible (UV-Vis), hetero-nuclear single quantum correlation nuclear magnetic resonsnce (HSQC-NMR), thermogravimetric analysis (TGA), and pyrolysis gaschromatography/mass spectrometry (GC/MS). Structural differences were found for stem and leaf-derived lignins. Compared to beech wood lignins, Miscanthus lignins possess lower molecular weight and narrow polydispersities (<1.5 Miscanthus vs. >2.5 beech) corresponding to improved homogeneity. In addition to conventional univariate analysis of FTIR spectra, multivariate chemometrics revealed distinct differences for aromatic in-plane deformations of stem versus leaf-derived lignins. These results emphasize the potential of Miscanthus as a low-input resource and a Miscanthus -derived lignin as promising agricultural feedstock.

As the most significant solid residue generated in the oil production industry, upstream oily sludge was regarded as hazardous waste in China due to its toxicity and ignitability, and to date, the incineration process has been considered the most efficient method in practice. Due to the complicated components of oily sludge, a kinetic model of the incineration process was difficult to build, and is still absent in engineering use. In this study, multiple non-isothermal thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis were applied for the kinetic analysis of upstream oily sludge in air conditions. A viewpoint regarding the rules to sectionalize the reaction stages was raised, and a differential integral method to obtain the incineration kinetic model was provided. The results showed that four stages that were divided based on the weight-loss regions in the TGA curves and the endothermic/exothermic sections in the DSC curves were suitable to obtain an incineration kinetic model of oily sludge. The integral method was beneficial for obtaining the average activation energy of each stage, and the differential method was suitable for gaining the nth-order reaction rate equation and the pre-exponential factor before the operating temperature became lower than 635.968 °C. The average activation energies of stages one, two, three, and four were 60.87 KJ/mol, 78.11 KJ/mol, 98.82 KJ/mol, and 15.96 KJ/mol, respectively. The nth-order reaction rate equations and pre-exponential factors of stages one, two, and three were 0.82, 3.50, and 2.50, and e 13.32 min - 1 , e 19.69 min - 1 , and e 21.00 min - 1 , respectively.

Laboratory analytical techniques employed for triglyceride quantification in oleaginous biomass (e.g., microalgae and oilseeds) involve multiple steps and typically require use of volatile organic solvents. Here we describe a single-step approach for measurement of triglycerides using thermogravimetry (TG). We have observed that triglycerides undergo complete volatilization over a narrow temperature interval of 370-450 °C, with negligible solid residue under inert atmosphere, whereas other constituents of oleaginous biomass (such as proteins and carbohydrates) primarily degrade below 350 °C. As a result, triglyceride content of biomass can be estimated using TG by determining the mass loss of the sample in the temperature interval of 370-450 °C.

The measurement of lignin content in ruminant diet and fecal samples is important for digestibility studies, but it is typically time-consuming and costly. The work reported involves correlation of traditional wet chemistry data with those from three rapid instrumental techniques, Fourier transform infrared spectroscopy (FTIR), conventional thermogravimteric analysis (TGA), and high-resolution TGA (MaxRes TGA) to predict the lignin content of diets and feces from digestibility trials. Calibration and performance data indicate that the FTIR model is acceptable for screening, while the conventional and MaxRes TGA predictions are high accuracy for quantitative analysis. Cross validation and model performance data reveal that MaxRes TGA provides the best-performing predictive model. This work shows that MaxRes TGA can accurately predict lignin content in ruminant diet and fecal samples with distinct advantages over traditional wet chemistry: namely, the requirement of small sample size, ease of sample preparation, speed of analysis, and high sample throughput at considerably lower cost.

In this work, the effect of sodium citrate mixed with tobacco, in the presence and absence of SBA-15 material, was studied by thermogravimetric analysis coupled to Fourier-transform infrared spectrometry under N 2 and air atmospheres. Depending on the atmosphere used, the decomposition of sodium citrate changes considerably at high temperatures, mainly due to the oxidation of the residue. The analysis of the experimental and calculated derivative thermogravimetric data of the sodium citrate/SBA-15 mixtures allows the observation of marked widening of the peaks appearing at lower temperatures, due to the presence of SBA-15, while the expected peak at high temperatures in air completely disappears. The presence of sodium citrate in tobacco and tobacco/SBA-15 mixtures produces changes, especially in air atmosphere, where the main peaks increase their intensity, whereas decreasing that of the oxidation of the residue at around 450 °C and an important peak appears at 630 °C. In N 2 atmosphere, all decomposition processes of tobacco proceed at lower temperatures and with higher intensities. The peak due to the citrate at temperatures around 200 °C completely disappears in all samples. © 2018 Society of Chemical Industry., (© 2018 Society of Chemical Industry.)

The crystal structure of indinavir sulfate, a pharmaceutical administered as an ethanol solvate, is presented, revealing a unique channel/ionic solvate structure to be characteristic of the compound. The properties of the material with regard to thermal treatment and water adsorption follow closely from the structure. The in situ amorphization of the pharmaceutical upon contacting liquid water is observed and highlights the unique dissolution enhancement of marketing the crystalline solvate dosage. Through survey of published crystal structures, an ambiguous sulfate/bisulfate ionization state is also observed in the crystal, which challenges the general understanding of the pharmaceutical. This study provides a solid-state insight into the function of a special multicomponent crystalline pharmaceutical form., (Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.)

A controlled release fertilizer system based on phosphate bound-carboxymethyl starch-graft-polyacrylamide (P-CMS-g-PAM) has been prepared in order to deliver the phosphate fertilizer to the plant at a constant rate thereby. This system aims to increase fertilizer phosphorus use efficiency (FPUE) and maintain a hydration level for the plant at the same time. Two types of starch phosphate monoesters were prepared using mono-ammonium (MAP) and di-ammonium phosphate (DAP). First, starch was converted to carboxymethyl starch and then was phosphorylated with mono-ammonium dihydrogen phosphate and di-ammonium dihydrogen phosphate. After phosphorylation, the samples were grafted with acrylamide in the presence of methylene bisacrylamide as a crosslinking agent. The prepared systems of P-CMS-g-PAM were differently characterized by Fourier transformer infrared (FT-IR), thermogravimetric analysis (TGA), scanning electron microscope (SEM) and phosphorous analysis. The swelling behavior was investigated. The kinetics of grafting reaction were also studied. The release behavior of phosphate bound was studied at pH 7 and 25 °C. The mechanism of the phosphate release from P-CMS-g-PAM was examined using the Korsmeyer-Peppas model., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Novel bioactive edible films based on sodium alginate (A) and chitosan biguanidine hydrochloride (CG) with different weight percents were successfully prepared. 13 C NMR and 1 H NMR confirmed the successful guanidylation of chitosan. Fourier transform infrared confirmed the successful reaction between CG and A. The interaction between CG and A was confirmed through the reduction of the crystalline peaks of both CG and A as detected from their wide-angle X-ray diffraction. Thermogravimetric analysis confirmed that CG enhanced the thermal stability of films as detected from the calculated integral procedure decomposition temperature (IPDT) values. CG incorporation improved the mechanical properties of dry and wet samples. A/CG films exhibited a reduced water vapor permeability and good color properties. The antibacterial study proved that the prepared films showed a remarkable antibacterial killing ability. These results revealed that A/CG films could be an alternative candidate to be used as antibacterial edible films in food industries., (Copyright © 2018. Published by Elsevier B.V.)

In this study, a novel magnetic guanidinylated chitosan nanobiocomposite was synthesized and characterized by Fourier transform infrared (FT-IR) spectroscopy, elemental analysis (CHN), thermogravimetric analysis (TGA), X-ray diffraction (XRD) pattern, energy dispersive X-ray (EDX) analysis, vibrating sample magnetometer (VSM) curves, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images. SEM and TEM images of the nanobiocomposite showed its nearly spherical shape and uniform size distribution with an average size of about 42 nm. In the current protocol, the amino functional groups on the surface of chitosan were increased due to successfully modification of chitosan via simply conversion of amino groups to guanidine. Therefore, due to the highly amount of amino functional groups and magnetic properties of the synthesized nanobiocomposite, it was successfully utilized as a heterogeneous catalyst for the one-pot multicomponent synthesis of 1,4-dihydropyridines. These products are important class of N-heterocyclic and biologically-active compounds. Many of these reported synthesis methods for these nucleuses require expensive reagents, organic solvents, long reaction time and tedious work-up methods. Noteworthy, the advantages of this method are easy separation and reusability of catalyst, high-to-excellent yields of products, use of a green solvent, mild reaction conditions and simple and chromatography free work-up procedure., (Copyright © 2018 Elsevier B.V. All rights reserved.)

In this study, the formation of caffeine/dapsone (CAF/DAP) cocrystals by scalable production methods, such as liquid-assisted grinding (LAG) and spray drying, was investigated in the context of the potential use of processed cocrystal powder for pulmonary delivery. A CAF/DAP cocrystal (1:1 M ratio) was successfully prepared by slow evaporation from both acetone and ethyl acetate. Acetone, ethyl acetate, and ethanol were all successfully used to prepare cocrystals by LAG and spray drying. The powders obtained were characterized by X-ray diffractometry (XRD), differential scanning calorimetry (DSC), thermogravimetry (TGA), and Fourier transform infrared spectroscopy (FTIR). Laser diffraction analysis indicated a median particle size (D 50 ) for spray-dried powders prepared from acetone, ethanol, and ethyl acetate of 5.4 ± 0.7, 5.2 ± 0.1, and 5.1 ± 0.0 μm respectively, which are appropriate sizes for pulmonary delivery by means of a dry powder inhaler. The solubility of the CAF/DAP cocrystal in phosphate buffer pH 7.4, prepared by spray drying using acetone, was 506.5 ± 31.5 μg/mL, while pure crystalline DAP had a measured solubility of 217.1 ± 7.8 μg/mL. In vitro cytotoxicity studies using Calu-3 cells indicated that the cocrystals were not toxic at concentrations of 0.1 and of 1 mM of DAP, while an in vitro permeability study suggested caffeine may contribute to the permeation of DAP by hindering the efflux effect. The results obtained indicate that the CAF/DAP cocrystal, particularly when prepared by the spray drying method, represents a possible suitable approach for inhalation formulations with applications in pulmonary pathologies.

In this study, a novel ionic liquid-type surfactant modified attapulgite named as 1-dodecyl-3-methylimidazolium bromide-attapulgite (C 12 MIM-ATP) is successfully prepared and applied in dispersive solid phase extraction (dSPE) for the fast determination of pyrethroid residues in tea drinks. The primary factors that influenced the extraction efficiency, including sorbent type, amount of sorbent, extraction time, desorption conditions, pH and ionic strength, are investigated. The optimized results reveal that the extraction and desorption equilibria are rapidly obtained within 1 min. Under the optimized conditions, good linearity (2-500 μg/L) is observed for four pyrethroids in tea drinks with determination coefficients (r 2 ) ranged from 0.9992 to 1.0000. The limits of detection (LODs) are 0.6 μg/L for all pesticides. Acceptable extraction recoveries of target analytes are found from 90.28 to 107.56% with relative standard deviations (RSDs) less than 8.30% in real tea drink samples. The batch-to-bath repeatability is evaluated by recovery test on five independent synthesized C 12 MIM-ATP sorbents. Satisfactory batch-to-batch repeatability is obtained with the recovery factors varied in 15%. A small matrix effect is observed using C 12 MIM-ATP as the sorbent for detection pyrethroids in tea drinks., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Liquid crystalline molecularly imprinted polymers (LC-MIPs) were low cross-linking MIPs (5-20 mol%) by introducing a LC monomer into the MIP polymerization system to keep the shape of the imprinted cavities due to additional interactions between the mesogenic groups. The multiwalled carbon nanotubes (MWCNTs) coated LC-MIP (MWCNT@LC-MIP) was the first fabricated as a novel floating interaction-controlled DDS. The synthesis was achieved by adding 9-vinylanthracene to obtain the high-density vinyl group functionalized MWCNTs firstly, and then polymerization of LC MIPs was performed on the surface of MWCNTs using a mixture of methacrylic acid, ethylene glycol dimethacrylate, and 4-methyl phenyl dicyclohexyl ethylene (LC monomer) with levofloxacin (LVF) as model template drug. Both template/functional monomer ratio and levels of crosslinker were optimized to obtain the best imprinting factor. Characterizations of polymer were investigated by the transmission electron microscope, nitrogen adsorption, thermogravimetric analysis, Fourier transform infrared spectra and floating behavior studies. The imprinting effect was confirmed by the adsorption isotherms, adsorption kinetics and effect of selectivity. In vitro release studies were examined by the LVF-loaded MWCNT@LC-MIP and the control samples, MWCNT@LC-NIP, MWCNT@MIP, MWCNT@NIP and the bare MWCNT using acetonitrile as the dissolute medium. The release profiles showed an obvious zero-order release of LVF from MWCNT@LC-MIP, which exhibited 3.8 μg/h of the release rate with duration of about 20 h. In vivo pharmacokinetic study displayed the relative bioavailability of the gastro-floating MWCNT@LC-MIP was 578.9%, whereas only 58.0% of MWCNT@MIP and 11.7% of the bared MWCNT. As a conclusion, MWCNT@LC-MIP showed potentials for oral administration by the innovative combination of floating and controlled release properties., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Objectives: To determine the effect of applied power settings, coil wetness conditions, and e-liquid compositions on the coil heating temperature for e-cigarettes with a "top-coil" clearomizer, and to make associations of coil conditions with emission of toxic carbonyl compounds by combining results herein with the literature., Methods: The coil temperature of a second generation e-cigarette was measured at various applied power levels, coil conditions, and e-liquid compositions, including (1) measurements by thermocouple at three e-liquid fill levels (dry, wet-through-wick, and full-wet), three coil resistances (low, standard, and high), and four voltage settings (3-6 V) for multiple coils using propylene glycol (PG) as a test liquid; (2) measurements by thermocouple at additional degrees of coil wetness for a high resistance coil using PG; and (3) measurements by both thermocouple and infrared (IR) camera for high resistance coils using PG alone and a 1:1 (wt/wt) mixture of PG and glycerol (PG/GL)., Results: For single point thermocouple measurements with PG, coil temperatures ranged from 322 ‒ 1008°C, 145 ‒ 334°C, and 110 ‒ 185°C under dry, wet-through-wick, and full-wet conditions, respectively, for the total of 13 replaceable coil heads. For conditions measured with both a thermocouple and an IR camera, all thermocouple measurements were between the minimum and maximum across-coil IR camera measurements and equal to 74% ‒ 115% of the across-coil mean, depending on test conditions. The IR camera showed details of the non-uniform temperature distribution across heating coils. The large temperature variations under wet-through-wick conditions may explain the large variations in formaldehyde formation rate reported in the literature for such "top-coil" clearomizers., Conclusions: This study established a simple and straight-forward protocol to systematically measure e-cigarette coil heating temperature under dry, wet-through-wick, and full-wet conditions. In addition to applied power, the composition of e-liquid, and the devices' ability to efficiently deliver e-liquid to the heating coil are important product design factors effecting coil operating temperature. Precautionary temperature checks on e-cigarettes under manufacturer-recommended normal use conditions may help to reduce the health risks from exposure to toxic carbonyl emissions associated with coil overheating.

Rufinamide (R) is a triazole derivative approved for the management of partial seizures and seizures associated with Lennox-Gastaut Syndrome, in November 2007. Crystal structure, solid state characterization, drug-excipient compatibility and solubility play a pivotal role in formulation development. This work deals with the crystal structure elucidation of R by single crystal X-ray diffraction and solid state characterization by thermal, spectroscopic and crystallographic techniques. Drug- excipient compatibility was assessed by differential scanning calorimetry (DSC). New RP-HPLC method for quantification of R was developed with improved retention time. Solubility and dissolution of drug in different media was determined. Additionally, the flow behavior of the drug was evaluated by measuring Carr's index and Hausner's ratio, while the compressibility behavior was studied using Well's protocol. R crystallized from dimethylformamide (R-DMF) was utilized for single crystal analysis. The drug crystallized in triclinic crystal system with P-1 space group. Asymmetric unit cell consists of two molecules of R held by intermolecular hydrogen bond (connected by NH⋯O, which forms the catemeric chain). Analytical outcomes from DSC, thermogravimetric analysis (TGA) and powder X-ray diffraction (PXRD) revealed that the drug was present in pure crystalline form and was devoid of any polymorphic or pseudopolymorphic impurities. Influence of pH on the solubility and dissolution of R-DMF was found to be insignificant. The drug exhibited poor aqueous solubility, which was improved nearly 4.6 fold with the addition of 2% sodium lauryl sulphate (SLS). The drug exhibits poor flow and elastic compression nature. Excipients such as poly ethylene glycol (PEG) 8000, SLS, lactose monohydrate, starch and Hydroxypropyl methylcellulose (HPMC) E15 were incompatible with R-DMF as identified by thermal analysis. It is envisaged that these information regarding solid state properties of R-DMF would aid in identifying a logical path for formulation development., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Furosemide is the most commonly prescribed diuretic drug in spite of its suboptimal biopharmaceutical properties. In this work, the addition of different amino-acids was studied with the aim of selecting an enhancer of the furosemide solubility. The best results were obtained with arginine. Also, binary (furosemide:arginine) and ternary (furosemide:arginine:β-cyclodextrin and furosemide:arginine:maltodextrin) systems were prepared by the kneading method and they were compared with their corresponding physical mixtures. These new systems were characterized by Fourier transform infrared and Raman spectroscopy, X-ray powder diffractometry, scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry. In addition, dissolution studies were performed in simulated gastric fluid. The best results in relation to improving biopharmaceutical properties were obtained with a binary combination of furosemide and arginine, demonstrating that this system could result in a suitable candidate for the development of a promising pharmaceutical formulation of the drug., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Two crystalline forms of tasimelteon, a drug approved by the U.S. Food and Drug Administration for the treatment of non-24-h sleep-wake disorder, have been studied by single crystal and powder diffraction analyses, thermogravimetric analysis, differential scanning calorimetry, spectroscopic, and optical methods. The synthetic method forming tasimelteon is described in detail, with its full analytical, spectroscopic, and enantiopurity characterization. Solid tasimelteon hemihydrate, C 15 H 19 NO 2 ·0.5H 2 O, is tetragonal with a = b = 7.3573(2) Å, c = 52.062(2) Å, V = 2818.1(2) Å 3 ; Z = 8. Its crystal structure has been solved and refined in the P4 3 2 1 2 space group, showing the occurrence of polymeric (H-bonded) slabs, thanks to the presence of water molecule (O W ) tetrahedrally linked to 4 distinct tasimelteon molecules in a N 2 (O W )O 2 fashion. The anhydrous form of tasimelteon, C 15 H 19 NO 2 , crystallizes in the monoclinic P2 1 space group, with a = 11.130(4), b = 4.907(2), c = 12.230(6) Å, β = 91.03(3)°, V = 667.8(5) Å 3 ; Z = 2. Thanks to the availability of good-quality specimens, the structure of the latter phase was solved by conventional single-crystal diffraction analysis, showing short intermolecular C=O … H-N interactions between (translationally related) tasimelteon molecules, forming, in the crystal, well-defined chains running along the b axis. The morphology of the 2 crystal forms has been analyzed by the means of optical microscopy and particle size distribution analysis. Worthy of note, the newly determined crystal structures enable the successful usage of full-pattern matching X-ray-based quantitative analyses of batches of industrial interest, in search for contamination or phase stability issues., (Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.)

The thermal characteristics and the thermal degradation of crystalline and amorphous nilotinib hydrochloride (NH) were studied. The spray drying technique was successfully utilized for the amorphization of NH and was evaluated by spectroscopic techniques and differential scanning calorimetry (DSC). The ethanolic spray drying process yielded amorphous NH with a glass transition temperature (T g ) of 147°C. Thermal characterization of the amorphous phase was performed by heat capacity measurements using modulated DSC (mDSC). Thermal degradation was studied by thermogravimetric analysis (TGA). The derived thermodynamic properties of the amorphous NH indicate fragile behaviour and a low crystallization tendency. NH was found to be molecularly stable up to 193°C. After which, the thermal degradation displayed two phases. The values of the thermal degradation parameters were estimated using the Ozawa-Flynn-Wall and Friedman non-isothermal, model-free, isoconversional methods The results indicate the two phases to be single-step reactions. The examination of the physical stability of amorphous NH during storage and at elevated temperatures showed stability at 180°C for at least 5h and at 20-25°C/60% RH for at least 6 months. During these periods, no crystallization was observed. This study is the first to report the thermal characteristics of NH. Additionally, it is also the first to describe the full thermal analysis of a spray-dried amorphous drug. The thermal data may be used in the projection of future production processes and storage conditions of amorphous NH., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Nanoparticles are critical components in nanomedicine and nanotherapeutic applications. Some nanoparticles, such as metallic nanoparticles, consist of a surface coating or surface modification to aid in its dispersion and stability. This surface coating may affect the behavior of nanoparticles in a biological environment, thus it is important to measure. Thermogravimetric analysis (TGA) can be used to determine the amount of coating on the surface of the nanoparticle. TGA experiments run under inert atmosphere can also be used to determine residual metal content present in the sample. In this chapter, the TGA technique and experimental method are described.

The combustion characteristics of textile dyeing sludge (TDS) in N2/O2, CO2/O2, and N2/CO2 atmospheres, and blends of TDS with coal were analyzed using TGA (thermogravimetric analysis). Results showed that the replacement of N2 by CO2 resulted in negative effects on the combustion and pyrolysis of TDS. Comparing N2/O2 and CO2/O2 atmospheres, combustion of TDS was easier in a N2/O2 atmosphere, but the residual mass after TDS pyrolysis in pure CO2 was less than that in N2 by approximately 4.51%. When the proportion of TDS was 30-50% in the blends of coal with TDS, a synergistic interaction clearly occurred, and it significantly promoted combustion. In considering different combustion parameters, the optimal proportion of TDS may be between 20-30%. The activation energy Ea value decreased from 155.6 kJ/mol to 53.35 kJ/mol with an increasing TDS proportion from 0% to 50%, and it rapidly decreased when the TDS proportion was below 20%.

In this article, the solution-mediated polymorphic transformation of rifampicin was investigated and simulated in 3 solvents at 30°C. The solid-state form I and form II of rifampicin was characterized by powder X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, Raman spectroscopy, and Fourier transform infrared spectroscopy (FTIR). To explore the relative stability, solubility data of form I and form II of rifampicin in butan-1-ol were determined using a dynamical method. In addition, Raman spectroscopy and focused beam reflectance measurement were used to in situ monitor the transformation of rifampicin from form II to form I. The liquid state concentration of rifampicin was measured by UV spectroscopic method. To investigate the effect of solvent on transformation, the transformation experiments were carried out in 3 solvents. Furthermore, a mathematical model was built to describe the kinetics of dissolution, nucleation, and growth processes during transformation by using experimental data. By combination of experimental and simulation results, it was found that the transformation process of rifampicin is controlled by dissolution of form II in heptane, whereas the transformation in hexane and octane was firstly controlled by dissolution of solid-state form and then controlled by growth of form I., (Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.)

Thermal properties of powders are critical material attributes that control temperature rise during tableting and roll compaction. In this study, various analytical methods were used to measure the thermal properties of widely used pharmaceutical excipients including microcrystalline cellulose (MCC) of three different grades (Avicel PH 101; Avicel PH 102 and Avicel DG), lactose and mannitol. The effect of relative density on the measured thermal properties was investigated by compressing the powders into specimen of different relative densities. Differential thermal analysis (DTA) was employed to explore endothermic or exothermic events in the temperature range endured during typical pharmaceutical manufacturing processes, such as tabletting and roll compaction. Thermogravimetric analysis (TGA) was performed to analyse the water/solvent content, either in the form as solvates or as loosely bound molecules on the particle surface. Thermal conductivity analysis (TCA) was conducted to measure thermal conductivity and volumetric heat capacity. It is shown that, for the MCC powders, almost no changes in morphology or structural changes were observed during heating to temperatures up to 200°C. An increase in relative density or temperature leads to a high thermal conductivity and the volumetric heat capacity. Among all MCC powders considered, Avicel DG showed the highest increase in thermal conductivity and the volumetric heat capacity, but this heat capacity was not sensitive to the measurement temperature. For lactose and mannitol, some endothermic events occurred during heating. The thermal conductivity increased with the increase in temperature and relative density. A model was also developed to describe the variation of the thermal conductivity and the volumetric heat capacity with the relative density and the temperature. It was shown that the empirical model can well predict the dependency of the thermal conductivity and the volumetric heat capacity on the relative density and the temperature., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Thermogravimetry-coupled with differential scanning calorimetry, quadrupole mass spectrometry, and Fourier-transform infrared spectroscopy (TG-DSC-QMS-FTIR)-was applied to monitor the thermal stability (in an N2 pyrolytic atmosphere) and chemical properties of natural polymers, fulvic (FA) and humic acids (HA), isolated from chemically different soils. Three temperature ranges, R1, 40-220°C; R2, 220-430°C; and R3, 430-650°C, were distinguished from the DSC data, related to the main thermal processes of different structures (including transformations without weight loss). Weight loss (ΔM) estimated from TG curves at the above temperature intervals revealed distinct differences within the samples in the content of physically adsorbed water (at R1), volatile and labile functional groups (at R2) as well as recalcitrant and refractory structures (at R3). QMS and FTIR modules enabled the chemical identification (by masses and by functional groups, respectively) of gaseous species evolved during thermal decomposition at R1, R2 and R3. Variability in shape, area and temperature of TG, DSC, QMS and FTIR peaks revealed differences in thermal stability and chemical structure of the samples between the FAs and HAs fractions of different origin. The statistical analysis showed that the parameters calculated from QMS (areas of m/z = 16, 17, 18, 44), DSC (MaxDSC) and TG (ΔM) at R1, R2 and R3 correlated with selected chemical properties of the samples, such as N, O and COOH content as well as E2/E6 and E2/E4 indexes. This indicated a high potential for the coupled method to monitor the chemical changes of humic substances. A new humification parameter, HTD, based on simple calculations of weight loss at specific temperature intervals proved to be a good alternative to indexes obtained from other methods. The above findings showed that the TG-DSC-QMS-FTIR coupled technique can represent a useful tool for the comprehensive assessment of FAs and HAs properties related to their various origin.

For the preparation of fully biobased unsaturated polyester resins (UPRs), the replacement of styrene with alternate nonpetroleum-based monomers turned out to be one of the most challenging tasks. Its complexity lies in the fact that reactive diluents (RD) have to have low viscosity and volatility, good compatibility with prepolymer, and capability to homopolymerize and copolymerize with its unsaturations. In this context, we directed our efforts to develop fully biobased UPRs using the dialkyl itaconates as an alternative to styrene. Therefore, a series of 100% biobased UPRs were prepared from itaconic acid and 1,2-propandiol and diluted by dialkyl itaconates. The resins were characterized by Fourier transform infrared spectroscopy, NMR, volatility, and viscosity measurements, while the cured samples were characterized by dynamic mechanical properties, thermomechanical analysis, thermogravimetric analysis data, and tensile tests. The influence of RD structure on the properties of cured samples was discussed in detail. It was shown that the prepared resins had evaporation rates of dialkyl itaconates of several orders of magnitude less compared to styrene. The cured resins with dimethyl itaconate showed comparable or even better thermal and mechanical properties compared to the one with styrene. This investigation showed that itaconic acid and dialkyl itaconates are promising bioresources for the preparation of fully biobased UPRs for mass consumption.

Pyrolysis is an eco-friendly process to achieve valuable products like bio-oil, char and gases. In the last decades, biochar production from pyrolysis of a wide variety of industrial and agricultural wastes become popular, which can be utilized as adsorbent instead of the expensive activated carbons. In this study, cherry pulp was pyrolyzed in a fixed bed tubular reactor at five different temperatures (400, 500,550, 600 and 700 °C) and three different heating rates (10, 100 and 200 °C/min) to obtain biochar. Proximate, ultimate, nitrogen adsorption/desorption isotherms, scanning electron microscopy, thermogravimetric analysis, x-ray fluorescence, x-ray diffraction, and Fourier transform infrared spectroscopy were performed on cherry pulp and its chars to examine the chemical alterations after the pyrolysis process. Biochar yields were decreased with increasing pyrolysis temperature and heating rate, based on experimental results. Porous biochars are carbon rich and includes high potassium content. The aromaticity of biochars increased and O/C mass ratio reduced with an increase in the pyrolysis temperature as a result of the development of compact aromatic structure in char. Pyrolysis provides a promising conversion procedure for the production of high energy density char which has promising applications in existing coal-fired boilers without any upgrading., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

In this study, a new polymorph of ciprofloxacin saccharinate has been thoroughly evaluated with respect to structural as well as biopharmaceutical properties. Preliminary characterization of the new polymorph was performed by differential scanning calorimetry and thermogravimetric analysis, later confirmed by Fourier transform infra-red spectroscopy. The crystal structure was determined from the powder X-ray diffraction pattern using the direct-space algorithm. It lies in the triclinic P-1 space group. It is having lattice parameters different from previously reported forms. The solid-state 13 C NMR data calculated from the crystal structure by exploiting density functional theory were found to be in excellent agreement with corresponding experimental 13 C NMR data, thus providing a robust validation of the authenticity of the structure. The prepared polymorph shows enhanced aqueous solubility and dissolution rate in contrast to previously reported polymorph. The new form demonstrated improved oral bioavailability and inhibition of bacterial species. The enhanced biopharmaceutical properties are attributed to the higher extent of its absorption and distribution with respect to the individual components. The new form is a potential candidate for the pharmaceutical industry., (Copyright © 2017 Elsevier B.V. All rights reserved.)

The formation of molecularly dispersed amorphous solid dispersions by the hot-melt extrusion technique relies on the thermal and mechanical energy inputs, which can cause chemical degradation of drugs and polymeric carriers. Additionally, drug degradation may be exacerbated as drugs convert from a more stable crystalline form to a higher energy amorphous form. Therefore, it is imperative to study how drug degrades and evaluate methods to minimize drug degradation during the extrusion process. In this work, gliclazide was used as a model thermally labile drug for the degradation kinetics and process optimization studies. Preformulation studies were conducted using thermal analyses, and liquid chromatography-mass spectroscopy to identify drug degradation pathways and to determine initial extrusion conditions. Formulations containing 10% drug and 90% AFFINISOL™ HPMC HME 100LV were then extruded using a twin screw extruder, and the extrudates were characterized using X-ray powder diffraction, modulated dynamic scanning calorimetry, and potency testing to evaluate physicochemical properties. The energies of activation for both amorphous gliclazide, crystalline gliclazide, and gliclazide solution were calculated using the Arrhenius equation to further guide the extrusion optimization process. Preformulation studies identify two hydrolysis degradation pathways of gliclazide at elevated temperatures. The activation energy study indicates a significantly higher degradation rate for the amorphous gliclazide compared to the crystalline form. After optimization of the hot-melt extrusion process, including improved screw designs, machine setup, and processing conditions, gliclazide amorphous solid dispersion with ∼95% drug recovery was achieved. The ability to process thermally labile drugs and polymers using hot-melt extrusion will significantly expand the possible applications of this manufacturing process., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Two novel heteropolyoxomolybdate [XMo₈O 31 ] n- (X = Ge( 1 ) or P( 2 )) manganese carbonyl derivatives [(CH₃)₄N]₆H₆{Mn II (GeMo₈O 31 )[Mn I (CO)₃]₂}₂·12H₂O ( 1 ) and [(CH₃)₄N]₄H₆{Mn II (PMo₈O 31 )[Mn I (CO)₃]₂}₂·14H₂O ( 2 ), have been successfully synthesized and characterized in the solid state by single crystal X-ray diffraction, IR and thermogravimetric analysis, and in solution by UV-Vis spectroscopy and electrochemistry. The two polyoxomolybdate-based organometallic compounds 1 and 2 represent rare examples of transition metal sandwich-based polyoxometalate metal carbonyl derivatives (PMCDs), in which the organic-inorganic hybrids are composed of four Mn(CO)₃⁺ groups symmetrically occupied the tetravacant sites of dimeric heteropolyoxomolybdate {Mn₂(XMo₈O 31 )₂} n- through Mn I -O-Mo bonds. The carbonyl functionalized Mn atoms are octahedrally coordinated via three μ₂-oxygens of the [XMo₈O 31 ] n- unit and three carbonyl carbon atoms. Interestingly, 1 and 2 form a psedocuboidal ring Mn(CO)₃Mo₃O 12 with {Mn(CO)₃}⁺ occupying the three fold axis of the Mo₃O 12 octahedral triad. Beside this, the two centrally placed adjacent Mn II atoms show intramolecular Mn∙∙∙Mn interactions of 3.11 and 3.16 Å in 1 and 2 , respectively. Significant n→π* and O···O intermolecular interactions between the orthogonally aligned adjacent carbonyl groups through the overlap of lone-pair electrons on oxygen atoms with the antibonding orbital (π*) of the adjacent carbony carbon atom of the subsequent units in 1 and 2 were observed. The electrochemical properties of the two compounds were also been investigated.

We have engineered streptavidin labelled Europium doped fluorescent silica nanoparticles which significantly increased sensitivity without compromising the specificity of the immunoassay. As a proof of concept, a time resolved fluorescence based sandwich immunoassay was developed to detect HIV-1 p24 antigen in clinical specimens. The detection range of the silica nanoparticle based immunoassay (SNIA) was found to be between 0.02 to 500 pg/mL in a linear dose dependent manner. SNIA offers 1000 fold enhancement over conventional colorimetric ELISA. Testing of plasma samples that were HIV negative showed no false positive results in the detection of HIV-1 p24 antigen. This highly sensitive p24 assay can help improve blood safety by reducing the antibody negative window period in blood donors in resource limited settings where nucleic acid testing is not practical or feasible. This technology can also be easily transferred to a lab-on-a-chip platform for use in resource limited settings and can also be easily adopted for the detection of other antigens.

Herein, a promising carrier, graphene oxide (GO) decorated with ZnO nanoparticles, denoted as GO/ZnO composite, has been designed and constructed. This carrier was characterized by X-ray powder diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy and thermogravimetry. Then, Candida rugosa lipase (CRL) was immobilized onto the GO-based materials via physical adsorption. Our results indicated that the lipase loading amount on the GO/ZnO composites was about 73.52 mg of protein per g. In the activity assay, the novel immobilized lipase GO/ZnO@CRL, exhibited particularly excellent performance in terms of thermostability and reusability. Within 30 min at 50 °C, the free lipase, GO@CRL and ZnO@CRL had respectively lost 64%, 62% and 41% of their initial activity. However, GO/ZnO@CRL still retained its activity of 63% after 180 min at 50 °C. After reuse of the GO/ZnO@CRL 14 times, 90% of the initial activity can be recovered. Meanwhile, the relative activity of GO@CRL and ZnO@CRL was 28% and 23% under uniform conditions. Hence, GO-decorated ZnO nanoparticles may possess great potential as carriers for immobilizing lipase in a wide range of applications., Competing Interests: The authors declare no conflict of interest.

Objectives: The aim of this study was to investigate the influence of process parameters during dry coating on particle and dosage form properties upon varying the surface adsorbed moisture of microcrystalline cellulose (MCC), a model filler/binder for orally disintegrating tablets (ODTs)., Methods: The moisture content of MCC was optimised using the spray water method and analysed using thermogravimetric analysis. Microproperty/macroproperty assessment was investigated using atomic force microscopy, nano-indentation, scanning electron microscopy, tablet hardness and disintegration testing., Key Findings: The results showed that MCC demonstrated its best flowability at a moisture content of 11.2% w/w when compared to control, comprising of 3.9% w/w moisture. The use of the composite powder coating process (without air) resulted in up to 80% increase in tablet hardness, when compared to the control. The study also demonstrated that surface adsorbed moisture can be displaced upon addition of excipients during dry processing circumventing the need for particle drying before tabletting., Conclusions: It was concluded that MCC with a moisture content of 11% w/w provides a good balance between powder flowability and favourable ODT characteristics., (© 2016 Royal Pharmaceutical Society.)

Carboxymethyl chitosan (CMCS) microparticles are a potential candidate for hemostatic wound dressing. However, its low swelling property limits its hemostatic performance. Poly(γ-glutamic acid) (PGA) is a natural polymer with excellent hydrophilicity. In the current study, a novel CMCS/PGA composite microparticles with a dual-network structure was prepared by the emulsification/internal gelation method. The structure and thermal stability of the composite were determined by Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis (TGA). The effects of preparation conditions on the swelling behavior of the composite were investigated. The results indicate that the swelling property of CMCS/PGA composite microparticles is pH sensitive. Levofloxacin (LFX) was immobilized in the composite microparticles as a model drug to evaluate the drug delivery performance of the composite. The release kinetics of LFX from the composite microparticles with different structures was determined. The results suggest that the CMCS/PGA composite microparticles are an excellent candidate carrier for drug delivery.

This two-part study firstly investigated Tetraselmis suecica grown in different CO 2 (0.04-15%v/v) concentration through indoor and outdoor cultivation systems. A high CO 2 concentration led to a high lipid content, and low nitrogen and oxygen content, which are desirable for transport fuel production. Pyrolysis characteristics were investigated by TG-IR and synchrotron IR microscopy. The results show Tetraselmis suecica grown in 10%CO 2 had the highest decomposition rate corresponding to more volatile products produced during the main thermal cracking stage and derived from protein-and lipid-corresponding functional groups. Moreover, a high reaction temperature and CO 2 concentration resulted in a low retention of surface functional groups. The nitrogen functional groups initially decomposed at a temperature range of 250-300°C and still remained at 550°C, while the lipid-corresponding functional groups completely disappeared at a temperature range of 400-500°C. Besides, the decomposition of chemical components followed the order of carbohydrate, protein and lipid., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The templated synthesis of hydroxyapatite (HAP) nanowires@metal-organic framework (MOF) core/shell nanofibers (named HAP@MIL-100(Fe) nanofibers) is demonstrated. The ultralong hydroxyapatite nanowires are adopted as a hard template for the nucleation and growth of MIL-100(Fe) (a typical MOF) through the layer-by-layer method. The Coulombic and chelation interactions between Ca 2+ ions on the surface of the HAP nanowires and the COO - organic linkers of MIL-100(Fe) play key roles in the formation process. The as-prepared, water-stable HAP@MIL-100(Fe) nanofibers exhibit peroxidase-like activity toward the oxidation of different peroxidase substrates in the presence of H 2 O 2 , accompanied by a clear color change of the solution. Furthermore, a flexible, recyclable HAP@MIL-100(Fe) test paper is prepared successfully by using HAP@MIL-100(Fe) nanofibers as building blocks. A simple, low-cost, and sensitive colorimetric method for the detection of H 2 O 2 and glucose is established based on the as-prepared, flexible, recyclable HAP@MIL-100(Fe) test paper. More importantly, the HAP@MIL-100(Fe) test paper can be recovered easily for reuse by simply dipping in absolute ethanol for just 30 min, thus showing excellent recyclability. With its combination of advantages such as easy transportation, easy storage and use, rapid recyclability, light weight, and high flexibility, this HAP@MIL-100(Fe) test paper is promising for wide applications in various fields., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Thermogravimetric analysis, Gaussian-fit-peak model (GFPM), and distributed activation energy model (DAEM) were firstly used to explore the effect of anaerobic digestion on sequential pyrolysis kinetic of four organic solid wastes (OSW). Results showed that the OSW weight loss mainly occurred in the second pyrolysis stage relating to organic matter decomposition. Compared with raw substrate, the weight loss of corresponding digestate was lower in the range of 180-550°C, but was higher in 550-900°C. GFPM analysis revealed that organic components volatized at peak temperatures of 188-263, 373-401 and 420-462°C had a faster degradation rate than those at 274-327°C during anaerobic digestion. DAEM analysis showed that anaerobic digestion had discrepant effects on activation energy for four OSW pyrolysis, possibly because of their different organic composition. It requires further investigation for the special organic matter, i.e., protein-like and carbohydrate-like groups, to confirm the assumption., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Four new solvatomorphs of betulin were reported and characterized by X-ray diffractometry as well as thermal and vibrational spectroscopic analyses. Single-crystal X-ray diffraction was used to analyze the X-ray structures of the compounds and confirmed the stoichiometric ratio between the host and guest molecules from thermal data. Results indicated that solvatomorphism occurred in several betulin solvates. Changes in intermolecular arrangements, stoichiometry, and hydrogen-bonding interactions of solvatomorphs were due to solvent incorporation to solvates. Hirshfeld surface analyses, especially d norm surface and fingerprint plots, were used to determine intermolecular interactions in the crystal network. Solvent molecules played an important role in the construction of a 3D architecture. The stabilities of these solvates were evaluated by thermal analyses. Nonisothermal kinetic analysis was used to explain the kinetics of solid-solid phase transition (desolvation) of betulin solvates. The apparent activation energies were evaluated using Kissinger and Ozawa methods. Moreover, phase transitions were visually investigated by hot-stage microscopic analysis., (Copyright © 2017. Published by Elsevier Inc.)

The pyrolytic characteristics of tyre powder treated under different microwave powers (300, 500, and 700 W) were studied via microwave thermogravimetric analysis. The product yields at different power levels were studied, along with comparative analysis of microwave pyrolysis and conventional pyrolysis. The feedstock underwent preheating, intense pyrolysis, and final pyrolysis in sequence. The main and secondary weight loss peaks observed during the intense pyrolysis stage were attributed to the decomposition of natural rubbers and synthetic rubbers, respectively. The total mass loss rates, bulk temperatures, and maximum temperatures were distinctively higher at higher powers. However, the maximum mass loss rate (0.005 s -1 ), the highest yields of liquid product (53%), and the minimum yields of residual solid samples (43.83%) were obtained at 500 W. Compared with conventional pyrolysis, microwave pyrolysis exhibited significantly different behaviour with faster reaction rates, which can decrease the decomposition temperatures of both natural and synthetic rubber by approximately 110 °C-140 °C.

Thermogravimetric kinetic of bamboo waste (BW) pyrolysis has been studied using Asymmetric Double Sigmoidal (Asym2sig) function deconvolution. Through deconvolution, BW pyrolytic profiles could be separated into three reactions well, each of which corresponded to pseudo hemicelluloses (P-HC), pseudo cellulose (P-CL), and pseudo lignin (P-LG) decomposition. Based on Friedman method, apparent activation energy of P-HC, P-CL, P-LG was found to be 175.6kJ/mol, 199.7kJ/mol, and 158.4kJ/mol, respectively. Energy compensation effects (lnk 0, z vs. E z ) of pseudo components were in well linearity, from which pre-exponential factors (k 0 ) were determined as 6.22E+11s -1 (P-HC), 4.50E+14s -1 (P-CL) and 1.3E+10s -1 (P-LG). Integral master-plots results showed pyrolytic mechanism of P-HC, P-CL, and P-LG was reaction order of f(α)=(1-α) 2 , f(α)=1-α and f(α)=(1-α) n (n=6-8), respectively. Mechanism of P-HC and P-CL could be further reconstructed to n-th order Avrami-Erofeyev model of f(α)=0.62(1-α)[-ln(1-α)] -0.61 (n=0.62) and f(α)=1.08(1-α)[-ln(1-α)] 0.074 (n=1.08). Two-steps reaction was more suitable for P-LG pyrolysis., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

This study evaluated three different methods for the formation of an inclusion complex between alpha- and beta-cyclodextrin (α- and β-CD) and limonene (LIM) with the goal of improving the physicochemical properties of limonene. The study samples were prepared through physical mixing (PM), paste complexation (PC), and slurry complexation (SC) methods in the molar ratio of 1:1 (cyclodextrin:limonene). The complexes prepared were evaluated with thermogravimetry/derivate thermogravimetry, infrared spectroscopy, X-ray diffraction, complexation efficiency through gas chromatography/mass spectrometry analyses, molecular modeling, and nuclear magnetic resonance. The results showed that the physical mixing procedure did not produce complexation, but the paste and slurry methods produced inclusion complexes, which demonstrated interactions outside of the cavity of the CDs. However, the paste obtained with β-cyclodextrin did not demonstrate complexation in the gas chromatographic technique because, after extraction, most of the limonene was either surface-adsorbed by β-cyclodextrin or volatilized during the procedure. We conclude that paste complexation and slurry complexation are effective and economic methods to improve the physicochemical character of limonene and could have important applications in pharmacological activities in terms of an increase in solubility.

Microplastics are increasingly detected in the environment and the consequences on water resources and ecosystems are not clear to date. The present study provides a cost-effective and straightforward method to determine the mass concentrations of polymer types using thermal analysis. Characteristic endothermic phase transition temperatures were determined for seven plastic polymer types using TGA-DSC. Based on that, extracts from wastewater samples were analyzed. Results showed that among the studied polymers, only PE and PP could be clearly identified, while the phase transition signals of the other polymers largely overlap each other. Subsequently, calibration curves were run for PE and PP for qualitative measurements. 240 and 1540mg/m(3) of solid material (12µm to 1mm) was extracted from two wastewater effluent samples of a municipal WWTP of which 34% (81mg/m(3)) and 17% (257mg/m(3)) could be assigned to PE, while PP was not detected in any of the samples. The presented application of TGA-DSC provides a complementary or alternative method to FT-IR analyses for the determination of PE and PP in environmental samples., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Co-combustion of lignite with distillation residue derived from rice straw pyrolysis oil was investigated by non-isothermal thermogravimetric analysis (TGA). The addition of distillation residue improved the reactivity and combustion efficiency of lignite, such as increasing the weight loss rate at peak temperature and decreasing the burnout temperature and the total burnout. With increasing distillation residue content in the blended fuels, the synergistic interactions between distillation residue and lignite firstly increased and then decreased during co-combustion stage. Results of XRF, FTIR, (13)C NMR and SEM analysis indicated that chemical structure, mineral components and morphology of samples have great influence on the synergistic interactions. The combustion mechanisms and kinetic parameters were calculated by the Coats Redfern model, suggesting that the lowest apparent activation energy (120.19kJ/mol) for the blended fuels was obtained by blending 60wt.% distillation residue during main co-combustion stage., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The thermal decomposition and kinetic parameters of synthetized imatinib mesylate α form α form were determined by thermogravimetry (TGA/DTG) under non-isothermal conditions. The experiments were performed at a 25-940°C temperature range at five different heating rates: 2.5Kmin(-1), 5Kmin(-1), 10Kmin(-1), 15Kmin(-1) and 20Kmin(-1) per minute in a nitrogen atmosphere. Imatinib mesylate α form presents one-step mass loss during the degradation process. The thermal stability of the examined material, the melting temperature (Tonset=220.6°C) and ΔH fusion=-95.74Jg(-1) at a heating rate of 10°Cmin(-1) was established. The values of activation energies have been estimated using Kissinger, Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS) methods., (Copyright © 2016 Elsevier B.V. All rights reserved.)

The aim of this work is to provide a wide database of kinetic data for the most common biomass by thermogravimetric analysis (TGA) and differential thermogravimetry (DTG). Due to the characteristic parameters of DTG curves, a two-stage reaction model is proposed and the kinetic parameters obtained from model-based methods with energy activation values for first and second stages in the range 1.75·10(4)-1.55·10(5)J/mol and 1.62·10(4)-2.37·10(5)J/mol, respectively. However, it has been found that Flynn-Wall-Ozawa and Kissinger-Akahira-Sunose model-free methods are not suitable to determine the kinetic parameters of biomass combustion since the assumptions of these two methods were not accomplished in the full range of the combustion process., (Copyright © 2016 Elsevier Ltd. All rights reserved.)