Thermal analysis of lithium peroxide prepared by various methods

Behavior of lithium peroxide samples at heating in air was studied by the methods of thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the temperature range from 32 to 82°C all the studied samples we found to react with water vapor forming lithium peroxide monohydrate as confirmed by the methods of chemical analysis and of qualitative X-ray phase analysis. It was found experimentally that in the temperature range from 340 to 348°C lithium peroxide began to decompose into lithium oxide and oxygen, the starting temperature depended on the method of preparation of lithium peroxide. For all the studied samples polymorphism in the temperature range from 25 to 340°C was not detected.     

Extraction and analysis of different Cannabis samples by headspace solid-phase microextraction combined with gas chromatography-mass spectrometry

A headspace solid-phase microextraction combined with GC-MS method was developed for the extraction and analysis of cannabinoids from Cannabis samples. Different commercially available fibres were evaluated; polydimethylsiloxane 100 microm was selected as the most efficient one. In order to enhance sensitivity and reduce analysis time, the sampling temperature was studied and it showed that extraction should be performed at a high temperature (150 degrees C). In relation with the high lipophilicity of cannabinoids, a relatively long desorption time (3 min) was necessary to ensure a total transfer from the fibre into the injection port of the gas chromatograph. The method was finally applied to the extraction of Swiss marijuana samples from different regions. Data treatment by principal component analysis and hierarchical cluster analysis allowed a discrimination of the different batches.     

Ionic liquid for high temperature headspace liquid-phase microextraction of chlorinated anilines in environmental water samples

Based on the non-volatility of room temperature ionic liquids (IL), 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) IL was employed as an advantageous extraction solvent for high temperature headspace liquid-phase microextraction (LPME) of chloroanilines in environmental water samples. At high temperature of 90 degrees C, 4-chloroaniline, 2-chloroaniline, 3,4-dichloroaniline, and 2,4-dichloroaniline were extracted into a 10 microl drop of [C4MIM][PF6] suspended on the needle of a high-performance liquid chromatography (HPLC) microsyringe held at the headspace of the samples. Then, the IL was injected directly into the HPLC system for determination. Parameters related to LPME were optimized, and high selectivity and low detection limits of the four chlorinated anilines were obtained because the extraction was performed at high temperature in headspace mode and the very high affinity between IL and chlorinated anilines. The proposed procedure was applied for the analysis of the real samples including tap water, river water and wastewater samples from a petrochemical plant and a printworks, and only 3,4-dichloroaniline was detected in the printworks wastewater at 88.2 microg l(-1) level. The recoveries for the four chlorinated anilines in the four samples were all in the range of 81.9-99.6% at 25 microg l(-1) spiked level.     

DSC study of the combustion properties of turkish coals

In this research, differential scanning calorimetry (DSC) was used to determine the combustion behavior and kinetic analysis of raw and cleaned coal samples of different size fractions. DSC curves of the three coal samples (Soma, Tuncbilek and Afsin Elbistan) showed two reaction regions. The first reaction region was due to moisture loss (endothermic) and observed in the temperature range of ambient to 150°C. The second region was the exothermic region due to the combustion and observed in the temperature range of 150 to 600°C. Kinetic parameters of the samples were determined using Roger and Morris kinetic model and the results are discussed. This revised version was published online in July 2006 with corrections to the Cover Date.     

The effect of sterilization methods on the thermo-gelation properties of xyloglucan hydrogels

In this study, the influence of different sterilization methods on the thermo-gelation and structural properties of xyloglucan hydrogels was investigated. Xyloglucan samples were treated by either 70% ethanol, 70% isopropanol, γ-irradiation (10 kGy) at room temperature, γ-irradiation (10 kGy) in dry ice or autoclaving. These samples were tested for sterility by incubation with sterile Lysogeny Broth (LB) at room temperature, 30 °C and 37 °C for 30 days. According to the results obtained, xyloglucan hydrogels were only effectively sterilized by autoclaving or by γ-irradiation either at room temperature or in dry ice. These samples were analyzed by rheology measurements and dynamic and static light scattering analysis. Gamma-irradiation at room temperature markedly changed the polymer structure, preventing thermo-gelation. Only autoclaving and γ-irradiation in dry ice preserved the rheological properties of the polymer. The sol-gel transition as a function of the temperature was similar for these samples and the control sample.     

Saponin Stabilization via Progressive Freeze Concentration and Sterilization Treatment

Saponin is a biopesticide used to suppress the growth of the golden apple snail population. This study aims to determine the stabilized conditions for saponin storage. The maceration process was used for saponin extraction, and for saponin concentration, progressive freeze concentration (PFC) was used. Afterwards, stability analysis was performed by storing the sample for 21 days in two conditions: Room temperature (26 °C) and cold room (10 °C). The samples kept in a cold room were sterilized samples that undergo thermal treatment by placing the sample in the water bath. The non-sterilized samples were kept in room temperature condition for 21 days. The results showed that saponin stored in the cold room (sterilized sample) has low degradation with higher concentration than those stored at room temperature in stability analysis with the highest saponin concentration (0.730 mg/mL) at a concentration temperature of −6 °C and concentration time of 15 min. The lowest saponin concentration obtained by saponin stored at room temperature (non-sterilized sample) is 0.025 mg/mL at a concentration temperature of −6 °C and concentration time of 10 min. Thus, the finding concluded that saponin is sensitive to temperature. Hence, the best storage condition to store saponin after thermal treatment is to keep it in a cold room at 10 °C.     

Catalytic pyrolysis of atmospheric residue on a fluid catalytic cracking catalyst for the production of light olefins

Catalytic pyrolysis of Chinese Daqing atmospheric residue on a commercial fluid catalytic cracking (FCC) catalyst was investigated in a confined fluidized bed reactor. The results show that the commercial FCC catalyst has good capability of cracking atmospheric residue to light olefins. The analysis of gas samples shows that the content of total light olefins in cracked gas is above 80%. The analysis of liquid samples shows that the content of aromatics in liquid samples ranges from 60% to 80%, and it increases with the enhancement of reaction temperature. The yield of total light olefins shows a maximum with the increase of reaction temperature, the weight ratios of catalyst-to-oil and steam-to-oil, respectively. The optimal reaction temperature, the weight ratios of catalyst-to-oil and steam-to-oil are about 650℃, 15 and 0.75, respectively.     

Accelerated solid-phase dynamic extraction for the analysis of biogenic volatile organic compounds in air

In this study, accelerated solid phase dynamic extraction (ASPDE) technique was used to identify biogenic volatile organic compounds (BVOCs) emitted from Norway spruce (Picea abies). Compounds that were determined in tree samples are: tricycylene, α-pinene, camphene, β-pinene, myrcene, 3-carene, p-cymene, limonene, cineole, α-phellandrene, α-terpinene, γ-terpinene and terpinolene. ASPDE showed a potential for the analysis of environmental samples as well as for field applications. This technique was further studied by using a gaseous mixture of BVOCs (sabinene, α-pinene, β-pinene, limonene, linalool, and (Z)-hexenyl acetate) and exhibited a good repeatability during all the experiments in the range of 2.5% (α-pinene) and 14.6% (linalool). However, during the analysis of samples it was observed that desorption at high temperature (230°C) can lead to the formation of artifacts, which were not observed at the desorption temperature of 100°C. Further experimental investigations revealed that monoterpenes appeared as unanticipated compounds during desorption of ASPDE samples; these compounds were degradation products of linalool.     

The effect of microwave radiation on some thermal,rheological and structural properties of cassava starch

Three samples of native or untreated cassava starch were exposed to microwave radiation for periods of 5, 10 or 15 min. The temperature of each sample was measured immediately after each exposure time and the temperature of the samples was around 135 °C. The samples were cooled to room temperature and maintained in a desiccator with anhydrous calcium chloride. All the samples were analysed by thermogravimetry-derivative thermogravimetry, differential scanning calorimetry (DSC), rapid viscoamylographic analysis (RVA), X-ray diffraction powder patterns, non-contact atomic force microscopy and colour characteristics by reflectance spectrophotometry. The thermal behaviour, gelatinisation temperatures, enthalpy and pasting properties were determined. Relative to the time of microwave exposure, the peak viscosity and gelatinisation (RVA and DSC) increased slightly after 5 min, and, after 10 and 15 min, it decreased considerably. The degree of relative crystallinity (%) decreased, while the average roughness increased. The reflectance spectrophotometry showed that microwave action occured quickly and progressively, causing colour changes (mainly with trends to yellow) and very small differences to the starch samples that were heated at controlled temperature in a conventional oven.     

Enantiomeric separation of four methylenedioxylated amphetamines on β-cyclodextrin chiral stationary phases

Summary Native and derivatized β-cyclodextrins such as chiral stationary phases (CSP) were used for the simultaneous enantiomeric separation of four methylenedioxylated amphetamines (MDA, MDMA, MDEA and MBDB) by liquid chromatography. Fluorimetric detection was used in order to enhance sensitivity and selectivity. The mobile phase was, optimised by studying the influence of pH, triethylamine concentration, organic solvent type, column temperature and flow rate of the mobile phase. This method was validated by determining linearity, precision, accuracy, limits of detection and quantification, and was applied to the stereoselective analysis of illicit tablets (23 samples) and of human whole blood samples (spiked samples and two post-mortem cases). Whereas no significant deviation from a racemic ratio was observed in the tablets contents, the analysis of blood samples showed an enantioselective metabolism of MDMA.     

Analysis of ice water by the thermally stimulated depolarized current (TSDC) method.

The thermally stimulated depolarized current and temperature profiles (TSDC analysis) on iced water was proved to be an effective tool for the qualitative evaluation of various water samples, each having an independent relaxation process, brought about by a pure dipolar orientation. The method proved to be applicable to different kinds of water samples used in the experiment and tap-water samples from different suppliers. Five main peaks (A to E, in the order of increasing temperature) were observed, of which two peaks (B and D) were found for the first time. The appearance of multiple peaks suggested the existence of multi-states of the hydrogen bond, cleaved by the TSDC process. The TSDC profiles were quite reproducible when the water samples contained practically no cations. A separate addition of each cation at a low concentration level revealed that a cation with a smaller ionic radius shifted peak A to a higher temperature. For ice of tap water, which contained relatively higher amount of cations, the TSDC profiles were quite different in shape compared with the standard ice-water samples (shift of peaks A - D to higher temperature, and a strong increase in the current strength of peaks B - E). However, it was still possible to tell from which districts the water samples were supplied.     

Improved accuracy for Raman spectroscopic determination of polyethylene property by optimization of measurement temperature and elucidation of its origin by multiple perturbation two-dimensional correlation spectroscopy

A novel strategy is demonstrated to improve the accuracy for determination of polyethylene (PE) density using Raman spectroscopy by optimizing the temperature of sample measurement. Spectral features associated with the conformation change of the polymer induced by temperature may provide valuable information to quantify important polymer properties such as density. To evaluate possible existence of an optimal temperature providing improved quantitative accuracy, Raman spectra of PE pellets with different densities were collected at eight different temperatures from 30 to 100 °C at 10 °C intervals. Using the spectral datasets collected at each temperature, partial least squares (PLS) models were developed using the reference PE density values determined by a standard density gradient method at 23 °C. Interestingly, the most accurate determination of density was realized at 70 °C. Multiple perturbation two-dimensional (MP2D) correlation analysis and differential scanning calorimetry (DSC) were used to examine the origin of improved accuracy at 70 °C. From these analyses, the pre-melt behavior of the PE samples was identified below their melting temperatures. Structural variations induced at the pre-melt stages enhance Raman spectral selectivity among the samples, thereby providing more accurate determination of PE density. The MP2D correlation analysis revealed the unforeseen thermal behavior of PE samples and successfully explained the improved accuracy at 70 °C.     

Gasoline and crude oil fingerprinting using constant energy synchronous luminescence spectrometry

Constant energy synchronous luminescence spectrometry (CESLS) is applied to environmental analysis involving gasoline and crude oil samples containing polyaromatic hydrocarbons (PAHs). Sample identification at low temperature (77 °K) with quartz tubes and room temperature on filter paper is performed. The ability to identify individual PAHs in samples as well as fingerprint different samples based on total PAH content with CESLS is demonstrated.     

Thermal characterization and electrical properties of Fe-modified cellulose long fibers and micro crystalline cellulose

Thermal properties of polylactic acid (PLA) filled with Fe-modified cellulose long fibers (CLF) and microcrystalline cellulose (MCC) were studied using thermo gravimetric analysis (TG), differential scanning calorimetry, and dynamic mechanical analysis (DMA). The Fe-modified CLFs and MCCs were compared with unmodified samples to study the effect of modification with Fe on electrical conductivity. Results from TG showed that the degradation temperature was higher for all composites when compared to the pure PLA and that the PLA composites filled with unmodified celluloses resulted in the best thermal stability. No comparable difference was found in glass transition temperature (T _g) and melting temperature (T _m) between pure PLA and Fe-modified and unmodified CLF- and MCC-based PLA biocomposites. DMA results showed that the storage modulus in glassy state was increased for the biocomposites when compared to pure PLA. The results obtained from a femtostat showed that electrical conductivity of Fe-modified CLF and MCC samples were higher than that of unmodified samples, thus indicating that the prepared biocomposites have potential uses where conductive biopolymers are needed. These modified fibers can also be tailored for fiber orientation in a matrix when subjected to a magnetic field.     

(1-x)La_(0.67)Ca_(0.33)MnO_3/xCuO复合体系与La_(0.67)Ca_(0.33)Mn_(1-x)Cu_xO_3电输运行为比较

用不同实验方法制备了名义组分为(1-x)La_(0.67)Ca_(0.33)MnO_3/xCuO(LCMO/CuO)和La_(0.67)Ca_(0.33)Mn_(1-x)Cu_xO_3(LCMCO)两组样品,在宽的温度范围内研究了样品的电输运行为随Cu含量x的变化关系,发现这两组样品表现出不同的行为.对于LCMCO,随x的增加,金属-绝缘体转变温度T_p迅速降低,当x=5.5%,样品表现出绝缘体导电行为;而LCMO/CuO复合样品,当x≤6%时,随x增加,Tp逐渐下降,x≥6%时,T_p不再继续降低,所有样品几乎表现出相同的电输运行为.另外,这两组样品均表现出较好的低场磁电阻效应(LFMR),在0.3 T下样品的最大磁电阻分别达到了～76%和88%.基于样品结构以及制备过程的分析,我们认为LFMR效应的增强主要是因为颗粒边界上形成的Cu相关自旋无序层引起的.     

Direct loading of ethanol solution into high-power nitrogen–oxygen mixed gas microwave-induced plasma and the emission characteristics

A nitrogen–oxygen mixed gas microwave-induced plasma (MIP) with an Okamoto cavity was utilized as an atomization and excitation source for emission analysis when organic solvent samples are directly aspirated. Compared with the pure nitrogen plasma (excitation temperature of 5650 K), the excitation temperature in the nitrogen–oxygen mixed gas plasma (5100 K) was reduced, and thus, the detection sensitivity of ionic emission lines requiring higher excitation energy was degraded. However, nitrogen–oxygen mixed gases could produce the very stable microwave-induced plasma with a high robustness against the loading of ethanol solution. This effect might be because the organic solvent was completely burned in the oxygen-containing plasma. The excitation temperature was almost independent of the ethanol content in sample solutions, implying that the analytical performance was less effected by introducing organic solvent samples.     

Study of the influence of NaOH treatment on the pyrolysis of different leather tanned using thermogravimetric analysis and Py/GC-MS system

This paper presents a study of the influence of a NaOH treatment on leather samples tanned using different tanning agents. Thermogravimetric analysis (TG/DTG) and flash pyrolysis (Py/GC-MS) was carried out on treated samples, and the results were compared with those obtained with the untreated samples. Treatment with sodium hydroxide seemed to decrease the temperature of maximum leather decomposition rate between 4 and 27 °C, depending on the tanning agent, and increased the range of temperatures where leather degradation occurs. From flash pyrolysis experiments, it was found that the volatile products obtained from NaOH-treated samples contain higher amounts of nitrogen compounds than those obtained from untreated samples. The results of a multivariate analysis applied to pyrolytic products obtained in the flash pyrolysis of samples showed greater similarity between the results obtained in all treated samples than between treated and untreated samples produced with the same tanning process.     

Analysis of furan in foods by headspace solid-phase microextraction-gas chromatography-ion trap mass spectrometry

A headspace-solid-phase microextraction (HS-SPME) coupled to gas chromatography-ion trap mass spectrometry (GC-IT-MS) method is proposed for the analysis of furan in different heat-treated carbohydrate-rich food samples. The extraction efficiency of six commercially available fibres was evaluated and it was found that a 75mum carboxen/polydimethylsiloxane coating was the most suitable for the extraction of the furan. Parameters affecting the efficiency of HS-SPME procedure such as extraction temperature and time, ionic strength, headspace and aqueous volume ratio (V(h)/V(w)), desorption temperature and time, were optimized. Quality parameters were established using spiked water and food samples. Linearity ranged between 0.02 and 0.5ngg(-1) and run-to-run and day-to-day precisions for food samples were lower than 6% and 10%, respectively. The limit of detection (LOD) of the method is sample dependent and ranged from 8 to 70pgg(-1), while the limit of quantification is from 30 to 250pgg(-1). Isotope dilution using furan-d(4) is proposed for furan determination providing similar results to those obtained by standard addition with internal standard (US Food and Drug Administration method). The developed HS-SPME-GC-IT-MS method was applied to the analysis of furan in different Spanish food samples from a local market, and concentrations ranging from 0.17 to 2279ngg(-1) were found.     

Effect of water release on thermal properties of polyaniline

Conducting polyaniline (PANI) was studied by thermal expansion measurement, thermogravimetric analysis and by electrical conductivity measurement. Relative elongation and coefficient of thermal expansion (CTE) were determined from room temperature to 60 °C. Various temperature profiles were used. During heating, the treatment of samples at a constant temperature higher than the room temperature, or evacuation, water was released from the samples. Water release was detected by mass and thermogravimetric analysis. Water release was connected with shrinkage of the PANI samples and apparent negative CTE in the first thermal cycle. In the following thermal cycles, it increased and reached a positive value. CTE of PANI attained values in the range of ?30 × 10^?6 K^?1 up to 20 × 10^?6 K^?1 in dependence on water content in the sample before measurement and on experimental conditions of measurement. Irreversible shrinkage of the polymer was the largest in the first thermal cycle. Water release exhibited a strong time and temperature dependence, and it was only partially reversible. The electrical conductivity was measured by a four-point van der Pauw method. Relative electrical conductivity decreased with amounts of water release. Relative decrease of electrical conductivity reached as far as 20% after evacuation 7 h at the room temperature.     

In situ temperature-time effect on MetA-S-SIMS

Metal-assisted (MetA) static secondary ion mass spectrometry (S-SIMS) is one of several ion yield enhancing methods developed for S-SIMS in the last decades. MetA-S-SIMS uses a very thin coating of gold or silver on the sample. Earlier experiments revealed dependence of the ion yield enhancement on the applied metal, the nature of the studied sample, the time after metallization, and the heating temperature (ex situ, i.e., under atmospheric pressure). This paper reports on the effects of time and temperature when samples are heated to temperatures between 30 and 80 degrees C inside the S-SIMS vacuum chamber (in situ). Thick layers of poly(vinylbutyral-co-vinylalcohol-co-vinylacetate) (PVB) containing dihydroxybenzophenone (DHBPh) were coated with a nm-thin-layer of gold. The S-SIMS analysis was performed over a period of several hours while samples were kept at a constant elevated temperature. Compared to ex situ heating in an oven, heating in the analysis chamber provided more rapid signal enhancement, but the magnitude of the enhancement was less (by a factor of two). Furthermore, additional experiments on ex situ heated samples revealed that storage of samples with enhanced ion yields at -8 degrees C is not sufficient to "stabilize" the enhancement. A steep decrease of the ion yields was observed as a function of time after 2.5 h.