Femtosecond Terahertz Pulse Propagation Measurements and Simulations of Dewetting Kinetics in Real Time.

We report a terahertz time-domain study of dewetting kinetics on two time scales: femtoseconds and in real time (on the order of minutes). We recorded full electric field terahertz time domain signals with femtosecond time resolution during dewetting of water in cellulose. The femtosecond time-domain signals were analyzed with respect to the amplitude and signal emission times and how these two quantities changed over the course of dewetting kinetics.

Near-infrared spectra of liquid and gas samples by diffuse reflectance employing benchtop and handheld spectrophotometers.

This paper describes a new method to obtain NIR spectra of liquid and gas samples by diffuse reflectance, which is especially suitable for handheld spectrophotometers, since most of these instruments are designed to acquire spectrum using this geometry. The core of the method is a diffuse reflectance cell, which consists of a vial containing a mixture of the liquid or gas sample (rare medium) and a powder (dense medium). Using this strategy, no adaptation is required to measure spectra with most portable NIR spectrometers.

Understanding the Metastability of Theophylline FIII by Means of Low-Frequency Vibrational Spectroscopy.

While theophylline has been extensively studied with multiple polymorphs discovered, there is still currently no conclusive structure for the metastable theophylline form III. In this present work, by combining more widely used techniques such as X-ray diffraction and thermogravimetric analysis with more emerging techniques like low-frequency Raman and terahertz time-domain spectroscopy, to analyze the structure and dynamics of a crystalline system, it was possible to provide further evidence that the form III structure has a theophylline monohydrate structure with the water molecules removed. Solid-state density functional theory simulations were paramount in proving that this proposed structure is correct and explain how vibrational modes within the crystal structures feature and govern polymorphic transitions and the metastable form III.

Low-frequency Raman spectrophotometer with wide laser illumination on the sample: A tool for pharmaceutical analytical analysis.

This work describes an optical configuration for a Raman spectrophotometer, which permits variation of the laser spot size from 3 to 3000 μm, maintaining a high Raman photons throughput and allowing acquisitions with a short integration time. In addition, the instrument can acquire spectra from the low to middle frequency vibrational range (10 to 2000 cm), on the Stokes and anti-Stokes sides. One of the features of this new optical configuration is the non-use of beam splitters to redirect the scattered light to the detector, which would sacrifice the laser power.

Near infrared emission spectroscopy for rapid compositional analysis of Portland cements.

Near infrared emission spectroscopy (NIRES) has been investigated to yield a new analytical method for determination of CaO, SiO, AlO, FeO, MgO, and SO in Portland cement samples. The analyses were accomplished by correlation of the second derivative NIRES spectra with reference elemental analyses made by X-ray Fluorescence (XRF), using Partial Least Square (PLS) regression models. Four different types of cements (type II, III, IV and V) were included in the models.

Electric field-assisted solid phase extraction and cleanup of ionic compounds in complex food matrices: Fluoroquinolones in eggs.

The use of electric fields as additional driving forces in sample preparation techniques is an innovative approach that is environmentally friendly, straightforward, and able to overcome several limitations of conventional sample preparation procedures. In this work, the advantages of electric field-assisted solid phase extraction (E-SPE) using syringe-type cartridges were demonstrated for the extraction of four fluoroquinolones (FQs) in their anionic forms. The FQs were extracted from eggs and subsequently determined by UHPLC-MS/MS.

A new approach to polarimetric measurements based on birefringent crystals and diode lasers.

A new polarimetric instrument and measurement method is described based on the use of diode lasers as radiation source (532, 650 and 1064nm) and birefringent prisms, such as Glan-Laser and Wollaston, as analyzers. The laser radiation is passed through a dichroic polarizer film for further orientation of its polarization plane at 45° in relation to the polarization plane of the analyzer. The polarized beam, oriented in that way, passes the sample cell, impinges the prism surface, and the intensities of the two emerged beams are detected by two twin silicon detectors.

Determination of pentavalent antimony in antileishmaniotic drugs using an automated system for liquid-liquid extraction with on-line detection.

An automated system for liquid-liquid extraction flow analysis (LLE-FA) for the determination of Sb(V) in antileishmanial drugs is presented. The method is based on extraction in a 5mL glass extraction chamber of an ion pair formed between hexachloroantimoniate anion and rhodamine B cation into toluene. The detection system consists of a green light emitting diode (LED) and a photodiode.

Effect of ethanol in the organic phase on liquid-liquid extraction in monosegmented flow analysis. Determination of zinc in drugs.

In liquid-liquid extraction performed by monosegmented flow analysis (MSFA), the aqueous sample is introduced between two air bubbles and flows, under restricted dispersion, through a glass extraction tube where the analyte is retained, usually at pH higher than 8. The retained analyte is removed to a small volume of an organic phase containing a ligand which is introduced after the second air bubble. In this work, the effect of the organic phase composition on the extraction of Cu(II), Zn(II) and Cd(II) in MSFA systems was investigated by changing the ethanol content (0.

A monosegmented-flow Karl Fischer titrator.

A monosegmented volumetric Karl Fischer titrator is described to mechanize the determination of water content in organic solvents. The system is based on the flow-batch characteristics of the monosegmented analysis concept and employs biamperometry to monitor the progress of the titration. The system shows accuracy and precision that are highly independent of the flow rate, does not require calibration, and is carried out in a closed system capable of minimizing contact of the sample and reagents with ambient moisture.

A new approach to flow-batch titration. A monosegmented flow titrator with coulometric reagent generation and potentiometric or biamperometric detection.

Monosegmented flow analysis (MSFA) has been used as a flow-batch system to produce a simple, robust, and mechanized titrator that enables true titrations to be performed without the use of standards. This paper also introduces the use of coulometry with monosegmented titration by proposing a versatile flow cell. Coulometric generation of the titrand is attractive for titrations performed in monosegmented systems, because the reagent can be added without increasing the volume of sample injected.