Franklinmacdonald4417

This work proposes a simple device for thermometric titration using a contactless sensor. A low-cost infrared sensor (around $5) was adapted in a disposable, polystyrene vessel for monitoring the temperature to determine the endpoint of neutralization, redox, and complexation titrations, using a homemade syringe pump to titration control. Open-source software was developed to control the device using the Raspberry Pi platform and to perform automatic endpoint determination. The influence of sample volume, the flow rate of titrant, and sensor distance from the solution were evaluated to lower the variation among measurements. The parameters chosen in this regard were 10 mL of sample, 0.8 mL min-1 of titrant solution flow rate, and 3 cm of distance from the sensor to the solution. Results for the determination of the acidity of sauces and the ascorbic acid and calcium content of pharmaceutical products were compared with those from official compendia. The performance of the sensor also was compared with an infrared camera. The proposed method agreed with conventional ones to an extent ranging from 93% to 106%. The robust analytical performance and low cost of the system are essential features that could broaden the use of enthalpimetric analysis in several laboratories.A phenomenon of supramolecular solvents formation in aqueous solutions containing primary amine and monoterpenoid compound is presented for the first time. A novel supramolecular solvent-based liquid phase microextraction was developed. In an aqueous phase primary amine formed isotropic solution due to formation of amphiphile supramolecular assembly. The phase separation was achieved by a coacervation process. The monoterpenoid phenol (thymol) acted as a coacervation agent and induced spontaneous in situ formation of tiny supramolecular solvent droplets. The applicability of the proposed microextraction procedure was demonstrated for the separation of sulfonamides from biological fluids (human plasma and serum). An obtained composition of supramolecular solvent (1-decylamine, thymol, water) promoted satisfactory extraction of polar analytes from aqueous phase. The calibration graphs were linear over the concentration ranges of 0.06-50 mg L-1 for sulfamethoxazole, sulfamethazine and sulfapyridine. The limit of detection calculated from the blank tests based on 3σ was 0.02 mg L-1 for all analytes. The total analysis time was 15 min.We describe a novel polymer-based zwitterionic stationary phase for hydrophilic interaction chromatography (HILIC). It is prepared by chemical modification of poly (glycidyl methacrylate-divinylbenzene) (GMA-DVB) by converting epoxide groups of microsphere surface to diol groups via hydrolysis, then clicking cysteine onto the microsphere with pendant double bonds of microsphere surface via "thiol-ene" click chemistry. The phase has been characterized by scanning electron micrograph, elemental analysis and zeta potential measurement. Diol and zwitterionic group (carboxylate and amine group associated with cysteine) onto the surface of GMA-DVB microspheres make them possess good hydrophilicity, as supported by effective separation towards common polar analytes. It shows good stability at alkaline solution (e.g. pH 10) and negligible bleed (e.g. only 1.7-fold blank and ~55-fold lower than a commercial silica-based polar phase tested with the minimal bleed level). Such phase exhibits specific separation selectivity to ionic analytes and simultaneous separation of anions and cations is achieved in the retention order of I- less then NO3- less then Choline less then Br- less then Cl- less then K+ less then Na+.Solvents with both low density and viscosity have the advantage of higher extraction efficiency due to lower diffusivity and consequently higher mass transfer. In this study, a mixture design was performed for the synthesis of three different natural deep eutectic solvents (NADES) using citric acid, malic acid, and xylitol. The optimized proportion for each of the three solvents synthesized was selected based on density and viscosity values. The NADES were characterized by infrared spectroscopy analysis, that showed characteristic bands of the initial reagents and the presence of hydrogen bonds confirming the formation of each deep eutectic solvent. Then, the NADES were used as solvents in ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) of biological tissue and plant material samples for the determination of As, Cd, Hg, Pb, Se, and V by inductively coupled plasma mass spectrometry (ICP-MS). The results for the proposed methods were compared to microwave-assisted acid digestion (MW-AD). The extraction recoveries ranged from 80 to 120% for most of the elements determined. The use of NADES as carbon sources improved the sensitivity of the As and Cd analyses, due to charge transfer reactions between the analyte and C+ and/or other carbon species. BMS-986158 mw In addition, the Analytical Eco-Scale was used to assess the greenness of the proposed analytical procedures (UAE and MAE). It showed that the UAE and MAE methods provided excellent green analyses, while the MW-AD method was rated as an acceptable green procedure.Herein we propose, for the first time, a rapid method based on flow injection analysis, electrospray ionization-tandem mass spectrometry (FIA-ESI-MS/MS) and multivariate calibration for the determination of l-leucine, l-isoleucine and L-allo-isoleucine in saliva. As far as we know, multivariate calibration has never been applied to the data from this non-separative approach. The possibilities of its use were explored and the results obtained were compared with the corresponding ones when using univariate calibration. Partial least square regression (PLS1) multivariate calibration models were built for each analyte by analyzing different saliva samples, and were subsequently applied to the analysis of another set of samples which had not been used in any calibration step. For Leu, the model worked satisfactorily with root mean square errors in the prediction step of 17%. This error can be considered acceptable and is common in methodologies that do not include a separation step. Results were compared with those obtained when univariate calibration was used, using the m/z transition 132.