Efficiency of methods for Karl Fischer determination of water in oils based on oven evaporation and azeotropic distillation

The efficiency of azeotropic distillation and oven evaporation techniques for trace determination of water in oils has recently been questioned by the National Institute of Standards and Technology (NIST), on the basis of measurements of the residual water found after the extraction step. The results were obtained by volumetric Karl Fischer (KF) titration in a medium containing a large excess of chloroform (> or = 65%), a proposed prerequisite to ensure complete release of water from the oil matrix. In this work, the extent of this residual water was studied by means of a direct zero-current potentiometric technique using a KF medium containing more than 80% chloroform, which is well above the concentration recommended by NIST. A procedure is described that makes it possible to correct the results for dilution errors as well as for chemical interference effects caused by the oil matrix. The corrected values were found to be in the range of 0.6-1.5 ppm, which should be compared with the 12-34 ppm (uncorrected values) reported by NIST for the same oils. From this, it is concluded that the volumetric KF method used by NIST gives results that are much too high.     

A dry process for production of microfluidic devices based on the lamination of laser-printed polyester films

A new microfabrication process based on a xerographic process is described. A laser printer is used to selectively deposit toner on a polyester film, which is subsequently laminated against another polyester film. The toner layer binds the two polyester films and allows the blank regions to become channels for microfluidics. These software-outlined channels are approximately 6 microm deep. Approximately twice this depth is obtained by laminating two printed films. The resulting devices were not significantly damaged after 24 h of exposure to aqueous solutions of H3PO4, NaOH, methanol, acetonitrile, or sodium dodecyl sulfate. Electric tests with an impedance analyzer and microchannels filled with KCl solution demonstrated that (1) wide channels suffer from deformation of the top and bottom walls due to the lamination of the polyester films and (2) the toner walls are somewhat porous. Although these drawbacks limit the maximum width of a channel and the minimum distance between two channels, the process is an attractive option to other expensive, laborious, and time-consuming methods for microchannels fabrication. The process has been used to implement devices for electrospray tip and capillary electrophoresis with contactless conductivity detection.     

Highly efficient transmission gratings in fused silica for chirped-pulse amplification systems

We report on highly efficient transmission gratings in fused silica with a grating period of 800 nm generated by electron-beam lithography. At a wavelength of 1060 nm, 95% diffraction efficiency is achieved under Littrow conditions. The damage threshold, extremely enhanced compared with conventional gold-coated diffraction gratings, makes these gratings the key elements in high average power (>100 W) femtosecond fiber chirped-pulse amplification systems.     

Self-compression and Raman soliton generation in a photonic crystal fiber of 100-fs pulses produced by a diode-pumped Yb-doped oscillator

We present the use of a photonic crystal fiber to straightforwardly compress ultrashort pulses from a diode-pumped ytterbium laser emitting around 1 microm. 75-fs pulse generation and a large 1-1.3-microm tunability for sub-100-fs pulses is reported.     

Snow metamorphism as revealed by scanning electron microscopy

Current theories of snow metamorphism indicate that sublimating snow crystals have rounded shapes, while growing crystals have shapes that depend on growth rates. At slow growth rates, crystals are rounded. At moderate rates, they have flat faces with rounded edges. At fast growth rates, crystals have flat faces with sharp edges, and they have hollow faces at very fast growth rates. The main growth/sublimation mechanism is thought to be by the homogeneous nucleation of new layers at or near crystal edges. It was also suggested that the equilibrium shape of snow crystals would be temperature dependent: rounded above -10.5 degrees C, and faceted below. To test these paradigms, we have performed SEM investigations of snow samples having undergone metamorphism under natural conditions, and of snow samples subjected to isothermal metamorphism at -4 degrees and -15 degrees C in the laboratory. In general, current theories predicting crystal shapes as a function of growth rates, and of whether crystals are growing or sublimating, are verified. However, the transition in equilibrium shapes from rounded to faceted at -10.5 degrees C is not observed in our isothermal experiments that reveal a predominance of rounded shapes after more than a month of metamorphism at -4 and -15 degrees C. Some small crystals with flat faces that also have sharp angles at -15 degrees C, are observed in our isothermal experiments. These faces are newly formed, and contradict current theory. Several hypotheses are proposed to explain their occurrence. One is that they are due to sublimation at emerging dislocations.     

Addition of trace metals increases denitrification rate in closed marine systems

We investigated the effect of trace metals (Fe, Mn, Cu, Zn and Mo) on the denitrification unit at the Montreal Biodome. Two dosages of the five trace metals were tested on a denitrifying bacterial population which was extracted from the denitrification unit and cultured in 250 mL chemostats with artificial seawater. The low dosage showed a 20% increase in the denitrification rate whereas the high dosage had a more pronounced effect with a 250% increase. No increase in bacterial growth was observed, suggesting that the trace metals had an effect on the denitrification activity. When the trace metals were tested separately, only iron had a significant effect similar to the increase in the denitrification rate observed when the five trace metals were added. The combination of Fe and Mn caused a small but significant increase compared to the five trace metals. We then tested the effect of adding Fe, Mn and Cu to the denitrification unit at the Montreal Biodome. A high dosage of these trace metals showed a 250% increase in the denitrification rate, which went from 200 to 700 g NO(x)-N/d. Our results showed that the addition of trace metals is crucial for denitrification activities.     

Synthesis and enzymatic degradation of epichlorohydrin cross-linked pectins

The water solubility of pectin was successfully decreased by cross-linking with increasing amounts of epichlorohydrin in the reaction media. The initial molar ratios of epichlorohydrin/ galacturonic acid monomer in the reaction mixtures were 0, 0.37, 0.56, 0.74, 1.00, 1.47, and 2.44. The resulting epichlorohydrin cross-linked pectins were thus referred to as C-LP0, C-LP37, C-LP56, C-LP75, C-LP100, C-LP150, and C-LP250, respectively. Methoxylation degrees ranged from 60.5 ± 0.9% to 68.0 ± 0.6%, and the effective cross-linking degrees, determined by quantification of the hydroxyl anions consumed during the reaction, were 0, 17.8, 26.0, 38.3, 46.5, 53.5, and 58.7%, respectively. After incubating the different cross-linked pectins (0.5% w/v) in 25 mL of 0.05 M acetate-phosphate buffer (pH 4.5), containing 50 µL of Pectinex® Ultra SP-L (pectinolytic enzymes), between 60 and 80% of the pectin osidic bounds were broken in less than 1 hr. Moreover, increasing the cross-linking degree only resulted in a weak slowing on the enzymatic degradation velocity.     

High resolution processing techniques for ultrasound doppler velocimetry in the presence of colored noise. Part I: Nonstationary methods

Real-time flow velocity measurement is a practical issue in industrial and biomedical applications. Because their good frequency resolution, parametric methods such as autoregressive (AR) modeling and time-frequency distributions (TFD) are generally preferred to Fourier analysis. However, these methods become highly inaccurate in the presence of colored noise. We review here the principal parametric and nonparametric techniques and show their limitations in the estimation of Doppler frequency in the presence of strong colored noise. Different solutions to overcome these limitations are then proposed and compared using synthetic Doppler signals with colored noise.     

High resolution processing techniques for ultrasound doppler velocimetry in the presence of colored noise. Part II: Multiplephase pipe-flow velocity measurement

For pt.I see ibid., vol.50, no.3, p.267-78 (2003). This paper presents an application of continuous wave ultrasound Doppler velocity measurements to two-phase flow in pipes. In many petroleum wells, the multiphase flow is separated into two phases: the first is a liquid phase and the second is a gas phase with small scatterers. The problem of multiphase velocity profile measurements has not been satisfactorily solved by classical approaches due to the multiphase nature of the fluid and the presence of colored noise, which introduces a significant bias in classical frequency estimators. We propose the use of resolution frequency techniques to overcome the classical limitations. Direct estimation of Doppler frequency then obtained using either time frequency maximum frequency or arguments of poles of the parametric model that identifies the Doppler part of the signal is discussed. The tests made with synthetic Doppler signals and two-phase flow have demonstrated the excellent performance of the high resolution techniques based on reassignment and parametric techniques.     

Novel modeling technique for the stator of traveling wave ultrasonic motors

Traveling wave ultrasonic motors (TWUM) are a promising type of piezoelectric transducers, which are based on the friction transmission of mechanical propagating waves. These waves are excited on the stator by using high Q piezoelectric ceramics. This article presents a modeling strategy, which allows for a quick and precise modal and forced analysis of the stator of TWUM. First-order shear deformation laminated plate theory is applied to annular subdomains (super-elements) of the stator. In addition to shear deformations, the model takes into account the effect of rotary inertia, the stiffness contribution of the teeth, and the linear varying thickness of the stator. Moreover, the formulation considers a more realistic function for the electric field inside the piezoelectric ceramic, i.e., a linear function, instead of the generally assumed constant electric field. The Ritz method is used to find an approximated solution for the dynamic equations. Finally, the modal response is obtained and compared against the results from classical simplified models and the finite element method. Thus, the high accuracy and short computation times of the novel strategy were demonstrated.