Development of a simple analytical method for determining trihalomethanes in beer using a headspace solid-phase microextraction technique

We developed a simple, rapid, and solventless method for analyzing trihalomethanes in beer samples using headspace solid-phase microextraction. The effects of varying experimental parameters, such as extraction temperature and time, addition of sodium chloride, and agitation speed, on extraction yield were studied using a univariate experimental design. Limits of detection between 0.22 and 0.46 µg L- 1 and wide linear ranges were achieved for trihalomethanes. We measured the trihalomethane recoveries and precision (as the standard deviation of repeat measurements) and demonstrated the applicability of the proposed method by analyzing 32 beer samples.

KINETIC STUDY OF SELECTIVE GAS-PHASE OXIDATION OF ISOPROPANOL TO ACETONE USING MONOCLINIC ZRO2 AS A CATALYST

Zirconia was prepared by a precipitation method and calcined at 723 K, 1023 K, and 1253 K in order to obtain monoclinic zirconia. The prepared zirconia was characterized by XRD, SEM, EDX, surface area and pore size analyzer, and particle size analyzer. Monoclinic ZrO2 as a catalyst was used for the gas-phase oxidation of isopropanol to acetone in a Pyrex-glass-flow-type reactor with a temperature range of 443 K - 473 K. It was found that monoclinic ZrO2 shows remarkable catalytic activity (68%) and selectivity (100%) for the oxidation of isopropanol to acetone. This kinetic study reveals that the oxidation of isopropanol to acetone follows the L-H mechanism.

Influence of the Al content on the phase transformations in Cu-Al-Ag alloys

The influence of the Al content on the phase transformations in Cu-Al-Ag alloys was studied by classical differential thermal analysis (DTA), optical microscopy (OM) and X-ray diffractometry (XRD). The results indicated that the increase in the Al content and the presence of Ag decrease the rate of the b1 phase decomposition reaction and contribute for the raise of this transition temperature, thus decreasing the stability range of the perlitic phase resulted from the b1 decomposition reaction.

Current-phase relation in graphene Josephson junction

In this thesis, we present the results of high-frequency measurements on superconductor-graphene-superconductor junctions. We obtained the relation between the supercurrent through the junction and the superconducting phase. The relation allowed us to extract true critical current and to determine the transport regime of graphene in our SGS-junction samples at the Dirac point and away from it. An experimental temperature dependence of the current-phase relation is presented. We have calculated theoretical supercurrent-phase relation in the case of ballistic and diffusive junction. For the diffusive case, we have considered short and long limits where the coherence length is larger or smaller than the sample length, respectively.

Benefits of automated acclimatization during the pre-milking phase of lactating girolando cows

The aim of this paper was to evaluate the automated acclimatization effects during pre-milking of cows on thermal conditioning, physiology, milk production and cost-benefit of the automated adiabatic evaporative cooling system (AECS). The treatments 20; 30; 40 min and control consisted of exposure time of pre-milking cows to the automated AECS. Sixteen cows were used with an average daily milk yield of 19 kg, distributed in a 4 x 4 Latin square design. The Tukey's test (P<0.05) was used to compare the means. The environmental variables, dry bulb temperature (DBT, ºC) and relative humidity (RH, %), were recorded every minute, which allowed the determination of the system efficiency through the Temperature and Humidity Index (THI). The respiratory rate (RR), rectal temperature (RT) and temperature of the coat (TC) were measured before and after the acclimatization. The 40 min treatment kept the environmental variables and the comfort indexes within recommended limits. The physiological variables (RR, RT and TC) were lower in the 40 min treatment and reflected positively on milk production, which increased 3.66% compared to the control treatment. The system was profitable, having a 43 days return on investment and a monthly revenue increase of R$ 1,992.67.

Impact of elevated temperature scenarios on potato leaf development

The objective of this study was to simulate the impact of elevated temperature scenarios on leaf development of potato in Santa Maria, RS, Brazil. Leaf appearance was estimated using a multiplicative model that has a non-linear temperature response function which calculates the daily leaf appearance rate (LAR, leaves day-1) and the accumulated number of leaves (LN) from crop emergence to the appearance of the upper last leaf. Leaf appearance was estimated during 100 years in the following scenarios: current climate, +1 °C, +2 °C, +3 °C, +4 °C e +5 °C. The LAR model was estimated with coefficients of the Asterix cultivar in five emergence dates and in two growing seasons (Fall and Spring). Variable of interest was the duration (days) of the crop emergence to the appearance of the final leaf number (EM-FLN) phase. Statistical analysis was performed assuming a three-factorial experiment, with main effects being climate scenarios, growing seasons, and emergence dates in a completely randomized design using years (one hundred) as replications. The results showed that warmer scenarios lead to an increase, in the fall, and a decrease, in the spring growing season, in the duration of the leaf appearance phase, indicating high vulnerability and complexity of the response of potato crop grown in a Subtropical environment to climate change.

Determination of piglets’ rectal temperature and respiratory rate through skin surface temperature under climatic chamber conditions

ABSTRACT In animal farming, an automatic and precise control of environmental conditions needs information from variables derived from the animals themselves, i.e. they act as biosensors. Rectal temperature (RT) and respiratory rate (RR) are good indicators of thermoregulation in pigs. Since there is a growing concern on animal welfare, the search for alternatives to measure RT has become even more necessary. This research aimed to identify the most adequate body surface areas, on nursery-phase pigs, to take temperature measurements that best represent the correlation of RT and RR. The main experiment was carried out in a climate chamber with five 30-day-old littermate female Landrace x Large White piglets. Temperature conditions inside chamber were varied from 14 °C up to 35.5 °C. The measurements were taken each 30 minutes, over six different skin regions, using a temperature data logger Thermochron iButton® - DS1921G (Tb) and an infrared thermometer (Ti). As shown by the results, the tympanic region is the best one for RT and RR monitoring using an infrared thermometer (TiF). In contrast, when using temperature sensors, the ear (TbE) is preferred to be used for RT predictions and the loin region (TbC) for RR.

Analysis of emergency braking performance with particular consideration of temperature effects on brakes

During vehicle deceleration due to braking there is friction between the lining surface and the brake drum or disc. In this process the kinetic energy of vehicle is turned into thermal energy that raises temperature of the components. The heating of the brake system in the course of braking is a great problem, because besides damaging the system, it may also affect the wheel and tire, which can cause accidents. In search of the best configuration that considers the true conditions of use, without passing the safety limits, models and formulations are presented with respect to the brake system, considering different braking conditions and kinds of brakes. Some modeling was analyzed using well-known methods. The flat plate model considering energy conservation was applied to a bus, using for this a computer program. The vehicle is simulated to undergo an emergency braking, considering the change of temperature on the lining-drum. The results include deceleration, braking efficiency, wheel resistance, normal reaction on the tires and the coefficient of adhesion. Some of the results were compared with dynamometer tests made by FRAS-LE and others were compared with track tests made by Mercedes-Benz. The convergence between the results and the tests is sufficient to validate the mathematical model. The computer program makes it possible to simulate the brake system performance in the vehicle. It assists the designer during the development phase and reduces track tests.

Luteal phase of the menstrual cycle increases sweating rate during exercise

The present study evaluated whether the luteal phase elevation of body temperature would be offset during exercise by increased sweating, when women are normally hydrated. Eleven women performed 60 min of cycling exercise at 60% of their maximal work load at 32ºC and 80% relative air humidity. Each subject participated in two identical experimental sessions: one during the follicular phase (between days 5 and 8) and the other during the luteal phase (between days 22 and 25). Women with serum progesterone >3 ng/mL, in the luteal phase were classified as group 1 (N = 4), whereas the others were classified as group 2 (N = 7). Post-exercise urine volume (213 ± 80 vs 309 ± 113 mL) and specific urine gravity (1.008 ± 0.003 vs 1.006 ± 0.002) changed (P < 0.05) during the luteal phase compared to the follicular phase in group 1. No menstrual cycle dependence was observed for these parameters in group 2. Sweat rate was higher (P < 0.05) in the luteal (3.10 ± 0.81 g m-2 min-1) than in the follicular phase (2.80 ± 0.64 g m-2 min-1) only in group 1. During exercise, no differences related to menstrual cycle phases were seen in rectal temperature, heart rate, rate of perceived exertion, mean skin temperature, and pre- and post-exercise body weight. Women exercising in a warm and humid environment with water intake seem to be able to adapt to the luteal phase increase of basal body temperature through reduced urinary volume and increased sweating rate.

Head Space Solid Phase Micro-Extraction (HS - SPME) of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636)

The aim of the present study was the assessment of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636) using methyl and ethyl ricinoleate, ricinoleic acid and castor oil as precursors. The analysis of the volatile organic compounds was carried out using Head Space Solid Phase Micro-Extraction (HS - SPME). Factorial experimental design was used for investigating extraction conditions, verifying stirring rate (0-400 rpm), temperature (25-60 ºC), extraction time (10-30 minutes), and sample volume (2-3 mL). The identification of volatile organic compounds was carried out by Gas Chromatography with Mass Spectrum Detector (GC/MSD). The conditions that resulted in maximum extraction were: 60 ºC, 10 minutes extraction, no stirring, sample volume of 2.0 mL, and addition of saturated KCl (1:10 v/v). In the bio-production of volatile organic compounds the effect of stirring rate (120-200 rpm), temperature (23-33 ºC), pH (4.0-8.0), precursor concentration (0.02-0.1%), mannitol (0-6%), and asparagine concentration (0-0.2%) was investigated. The bio-production at 28 ºC, 160 rpm, pH 6,0 and with the addition of 0.02% ricinoleic acid to the medium yielded the highest production of VOCs, identified as 1,4-butanediol, 1,2,2-trimethylciclopropilamine, beta-ionone; 2,3-butanodione, pentanal, tetradecane, 2-isononenal, 4-octen-3-one, propanoic acid, and octadecane.

Phase transitions in biodegradable films based on blends of gelatin and poly (vinyl alcohol)

The aim of this work was to study the effect of the hydrolysis degree (HD) and the concentration (C PVA) of two types of poly (vinyl alcohol) (PVA) and the effect of the type and the concentration of plasticizers on the phase properties of biodegradable films based on blends of gelatin and PVA, using a response-surface methodology. The films were made by casting and the studied properties were their glass (Tg) and melting (Tm) transition temperatures, which were determined by diferential scanning calorimetry (DSC). For the data obtained on the first scan, the fitting of the linear model was statistically significant and predictive only for the second melting temperature. In this case, the most important effect on the second Tm of the first scan was due to the HD of the PVA. In relation to the second scan, the linear model could be fit to Tg data with only two statistically significant parameters. Both the PVA and plasticizer concentrations had an important effect on Tg. Concerning the second Tm of the second scan, the linear model was fit to data with two statistically significant parameters, namely the HD and the plasticizer concentration. But, the most important effect was provoked by the HD of the PVA.

Evaluation of the Efficiency of Line-Start Permanent-Magnet Machines as a Function of the Operating Temperature

The standard squirrel-cage induction machine has nearly reached its maximum efficiency. In order to further increase the energy efficiency of electrical machines, the use of permanent magnets in combination with the robust design and the line start capability of the induction machine is extensively investigated. Many experimental designs have been suggested in literature, but recently, these line-start permanent-magnet machines (LSPMMs) have become off-the-shelf products available in a power range up to 7.5 kW. The permanent magnet flux density is a function of the operating temperature. Consequently, the temperature will affect almost every electrical quantity of the machine, including current, torque, and efficiency. In this paper, the efficiency of an off-the-shelf 4-kW three-phase LSPMM is evaluated as a function of the temperature by both finite-element modeling and by practical measurements. In order to obtain stator, rotor, and permanent magnet temperatures, lumped thermal modeling is used.

La1-xSrxMnO3 as a candidate for a room temperature pressure sensor /

Perovskite manganite compounds, Lai-xDxMnOs (D-divalent alkaline earth Ca, Sr or Ba), whose electrical and magnetic properties were first investigated nearly a half century ago, have attracted a great deal of attention due to their rich phase diagram. From the point of view of designing a future application, the strong pressure dependence of the resistivity and the accompanying effects in thin films have potential for application in pressure sensing and electronic devices. In this study we report our experimental investigations of pressure dependence of the resistivity of Lao.siSvo^iQMnOs and Lai-xSvxMnOs (LSMO) epitaxial films with x= 0.15, 0.20, 0.25, 0.30, 0.35, on SrTiOs substrates.

Investigations into the extraction and the determination of polycyclic aromatic hydrocarbons (PAHs) from water by solid-phase extraction and capillary gas chromatography/ mass spectrometry

Factors affecting the detennination of PAHs by capillary GC/MS were studied. The effect of the initial column temperature and the injection solvent on the peak areas and heights of sixteen PAHs, considered as priority pollutants, USillg crosslinked methyl silicone (DB!) and 5% diphenyl, 94% dimethyl, 1% vinyl polysiloxane (DBS) columns was examined. The possibility of using high boiling point alcohols especially butanol, pentanol, cyclopentanol, and hexanol as injection solvents was investigated. Studies were carried out to optimize the initial column temperature for each of the alcohols. It was found that the optimum initial column temperature is dependent on the solvent employed. The peak areas and heights of the PAHs are enhanced when the initial column temperature is 10-20 c above the boiling point of the solvent using DB5 column, and the same or 10 C above the boiling point of the solvent using DB1 column. Comparing the peak signals of the PAHs using the alcohols, p-xylene, n-octane, and nonane as injection solvents, hexanol gave the greatest peak areas and heights of the PAHs particularly the late-eluted peaks. The detection limits were at low pg levels, ranging from 6.0 pg for fluorene t9 83.6 pg for benzo(a)pyrene. The effect of the initial column temperature on the peak shape and the separation efficiency of the PARs was also studied using DB1 and DB5 columns. Fronting or splitting of the peaks was obseIVed at very low initial column temperature. When high initial column temperature was used, tailing of the peaks appeared. Great difference between DB! and.DB5 columns in the range of the initial column temperature in which symmetrical.peaks of PAHs can be obtained is observed. Wider ranges were shown using DB5 column. Resolution of the closely-eluted PAHs was also affected by the initial column temperature depending on the stationary phase employed. In the case of DB5, only the earlyeluted PAHs were affected; whereas, with DB1, all PAHs were affected. An analytical procedure utilizing solid phase extraction with bonded phase silica (C8) cartridges combined with GC/MS was developed to analyze PAHs in water as an alternative method to those based on the extraction with organic solvent. This simple procedure involved passing a 50 ml of spiked water sample through C8 bonded phase silica cartridges at 10 ml/min, dried by passing a gentle flow of nitrogen at 20 ml/min for 30 sec, and eluting the trapped PAHs with 500 Jll of p-xylene at 0.3 ml/min. The recoveries of PAHs were greater than 80%, with less than 10% relative standard deviations of nine determinations. No major contaminants were present that could interfere with the recognition of PAHs. It was also found that these bonded phase silica cartridges can be re-used for the extraction of PAHs from water.

The versatility and utilization of phosphorus based compounds in classic carbon-carbon bond forming and esterification reactions

The phosphonium salt room temperature ionic liquid tetradecyltrihexylphosphonium chloride (THPC) has been employed as an efficient reusable media for the palladium catalyzed Suzuki cross-coupling reaction of aryl halides, including aryl chlorides, under mild conditions. The cross-coupling reactions were found to proceed in THPC containing small amounts ofwater and toluene (single phase) using potassium phosphate and 1% Pd2(dba)3'CHCI3. Variously substituted iodobenzenes, including electron rich derivatives, reacted efficiently in THPC with a variety of arylboronic acids and were all complete within 1 hour at 50°C. The corresponding aryl bromides also reacted under these conditions with the addition of a catalytic amount of triphenylphosphine that allowed for complete conversion and high isolated yields. The reactions involving aryl chlorides were considerably slower, although the addition of triphenylphosphine and heating at 70°C allowed high conversion of electron deficient derivatives. Addition of water and hexane to the reaction products results in a triphasic system, from which the catalyst was then recycled by removing the top (hexanes) and bottom (aqueous) layers and adding the reagents to the ionic liquid which was heated again at 50°C; resulting in complete turnover of iodobenzene. Repetition of this procedure gave the biphenyl product in 82-97% yield (repeated five times) for both the initial and recycled reaction sequences. IL ESTERIFICATIONREACTION A new class oftrialkylphosphorane has been prepared through reaction of a trialkylphosphine with 2-chlorodimethylmalonate in the presence oftriethylamine. These new reagents promote the condensation reaction of carboxylic acids with alcohols to provide esters along with trialkylphosphine oxide and dimethylmalonate. The condensation reaction of chiral secondary alcohols can be controlled to give either high levels of inversion or retention through a subtle interplay involving basicity of the reaction media, solvent, and tuning the electronic and steric nature of the carboxylic acid and stenc nature of the phosphorane employed. A coherent mechanism is postulated to explain these observations involving reaction via an initial acyloxyphosphonium ion.