Comparison of measurements of the outer scale of turbulence by three different techniques

We have made simultaneous and nearly simultaneous measurements of L0, the outer scale of turbulence, at the Palomar Observatory by using three techniques: angle-of-arrival covariance measurements with the Generalized Seeing Monitor (GSM), differential-image-motion measurements with the adaptive-optics system on the Hale 5-m telescope, and fringe speed measurements with the Palomar Testbed Interferometer (PTI). The three techniques give consistent results, an outer scale of approximately 10-20 m, despite the fact that the spatial scales of the three instruments vary from 1 m for the GSM to 100 m for the PTI.     

Nonlinear inversion techniques in combustion flame temperature measurements

Abstract

Combustion flame temperature profiles can be obtained from a single‐line‐of‐sight multi‐frequency set of radiance measurements. Nonlinear inversion techniques, developed mostly for satellite meterology, are used and compared in this highly nonlinear application. It is found that accuracy and rapid convergence depend critically on the availability of transmittance kernels featuring sharp and well spaced maxima. A systematic use of pivotal techniques is also necessary. Several typical flame configurations are tested, including the practical case where the unknown concentration profile is also to be retrieved.     

Method for the analysis of delta18O in water

A new method has been developed for the oxygen isotopic analysis of water utilizing the exchange of oxygen atoms with nitrite followed by conversion of nitrite to nitrous oxide by hydrazoic acid. This method is analogous to that employing carbon dioxide equilibration in that the analyte is added as a reagent to the water sample and exchanges oxygen isotopes with the water. In this procedure, however, the equilibration is more rapid and less sensitive to changes in ambient temperature, as the exchange is terminated by conversion of nitrite to nitrous oxide prior to analysis. The nitrous oxide is then analyzed using an on-line purge and trap system coupled to an isotope ratio mass spectrometer. This method makes use of previously established methods for nitrite isotopic analysis and commercially available equipment. It has high throughput, relatively low standard deviation (0.1 per thousand or better), and small sample size (down to 100 microL), is simple, and is applicable to both fresh- and seawater samples.     

Scattering properties of sands. 1. Comparison between different techniques of measurements

Measuring linear polarization of light scattered by a cloud of particles can help retrieve their physical properties. We present an extensive study of polarimetric measurements of sand grains that can be found on the surface and in the atmosphere of the Earth. Different techniques of measurements are compared using the Laboratoire de Météorologie Physique nephelometer on the ground and the Propriétés Optiques des Grains Astronomiques et Atmosphériques on the ground and in microgravity during parabolic flights. The techniques used on the ground bias the measurements. When the grains are lifted by an air draft, differentiation is produced in the size distribution and the nature of the floating particles. When the grains are carried along with the airflow, some grains become oriented along the flow direction at air speeds greater than a few meters per second, producing abnormal negative polarization. On the other hand, measurements conducted under microgravity permit the retrieval of the representative optical properties of the lifted sand grains with sizes greater than tens of micrometers.     

Isotope 18O/16O ratio measurements of water vapor by use of the 950-nm wavelength region with cavity ring-down and photoacoustic spectroscopic techniques

Two optical methods, cavity ring-down spectroscopy and photoacoustic spectroscopy, are applied to the measurement of the isotope ratio 18O/16O in water-vapor samples with a Nd3+:YAG pumped-dye laser. The combination band of (2v1 + v3) in the 960-nm region of water molecules is investigated for two standard water samples, the Vienna Standard Mean Ocean Water and the Standard Light Antarctic Precipitation. The results demonstrate that the two methods have the potential of compact systems for in-situ measurements of H2O isotope ratio in the environment.     

Generation of O2 from BaSO4 using a CO2-laser fluorination system for simultaneous analysis of delta18O and delta17O

With the observation of mass-independent isotopic anomalies in numerous atmospheric molecules, the ability to measure both delta17O and delta18O in a range of samples is needed. Sulfate oxygen isotopic studies conventionally report only delta18O values. Recent findings indicate that sulfate delta17O and delta18O values, particularly the delta17O value (= delta17O - (0.52)(delta18O)), can provide independent information on the origin, mixing, and transformation of sulfate in the atmospheric and surface environments, which is not resolvable by only delta18O measurements. Existing methods for analyzing sulfate delta17O and delta18O are extremely laborious and demand high-purity BrF5. Here we report a novel method of generating O2 directly from Barite (BaSO4) for simultaneous analysis of delta18O and delta17O by isotope ratio mass spectrometry (IRMS). The method utilizes a CO2-laser fluorination system that can also be used to quantitatively generate O2 from silicates and oxides. Partial but consistent oxygen yields from BaSO4 are obtained for samples >4 mg. Correction factors of +9.4% for delta18O and 4.89% for delta17O are obtained, and there is no deviation in the delta17O value due to the nonquantitative O2 generation. The system may process more than a dozen samples per working day, with analytical error of +/-0.05% and +/-0.8% for delta17O and delta18O, respectively. This new method is ideal for studies emphasizing an accurate sulfate delta17O value.     

Determination of the total oxygen isotopic composition of nitrate and the calibration of a delta 17O nitrate reference material

A thermal decomposition method was developed and tested for the simultaneous determination of delta 18O and delta 17O in nitrate. The thermal decomposition of AgNO3 allows for the rapid and accurate determination of 18O/ 16O and 17O/16O isotopic ratios with a precision of +/- 1.5 per thousand for delta 18O and +/- 0.11 per thousand for delta 17O (delta 17O = delta 17O - 0.52 x delta 18O). The international nitrate isotope reference material IAEA-NO3 yielded a delta 18O value of +23.6 per thousand and delta 17O of -0.2 per thousand, consistent with normal terrestrial mass-dependent isotopic ratios. In contrast, a large sample of NaNO3 from the Atacama Desert, Chile, was found to have delta 17O = 21.56 +/- 0.11 per thousand and delta 18O = 54.9 +/- 1.5 per thousand, demonstrating a substantial mass-independent isotopic composition consistent with the proposed atmospheric origin of the desert nitrate. It is suggested that this sample (designated USGS-35) can be used to generate other gases (CO2, CO, N2O, O2) with the same delta 17O to serve as measurement references for a variety of applications involving mass-independent isotopic compositions in environmental studies.     

Comparative analysis of cellulose preparation techniques for use with 13C, 14C, AND 18O isotopic measurements

A number of operationally defined methods exist for pretreating plant tissues in order to measure C, N, and O isotopes. Because these isotope measurements are used to infer information about environmental conditions that existed at the time of tissue growth, it is important that these pretreatments remove compounds that may have exchanged isotopes or have been synthesized after the original formation of these tissues. In stable isotope studies, many pretreatment methods focus on isolating "cellulose" from the bulk tissue sample because cellulose does not exchange C and O isotopes after original synthesis. We investigated the efficacy of three commonly applied pretreatment methods, the Brendel method and two variants of the Brendel method, the Jayme-Wise method and successive acid/base/acid washes, for use on three tissue types (wood, leaves, roots). We then compared the effect of each method on C and O isotope composition (13C, 14C, 18O), C and N content, and chemical composition of the residue produced (using 13C nuclear magnetic resonance (NMR)). Our results raised concerns over use of the Brendel method as published, as it both added C and N to the sample and left a residue that contains remnant lipids and waxes. Furthermore, this method resulted in 18O values that are enriched relative to the other methods. Modifying the Brendel method by adding a NaOH step (wash) solved many of these problems. We also found that processed residues vary by tissue type. For wood and root tissues, the 13C NMR spectra and the 18O and 13C data showed only small differences between residues for the Jayme-Wise and modified Brendel methods. However, for leaf tissue, 13C NMR data showed that Jayme-Wise pretreatments produced residues that are more chemically similar to cellulose than the other methods. The acid/base/acid washing method generated 13C NMR spectra with incomplete removal of lignin for all tissues tested and both isotopic, and 13C NMR results confirmed that this method should not be used if purified cellulose is desired.     

Non-destructive microstructural analysis by electrical conductivity: Comparison with hardness measurements in different materials

The use of non-destructive evaluation (NDE) techniques for assessing microstructural changes in processed materials is of particular importance as it can be used to assess, qualitatively, the integrity of any material/structure. Among the several NDE techniques available, electrical conductivity measurements using eddy currents attract great attention owing to its simplicity and reliability. In this work, the electrical conductivity profiles of friction stir processed Ti6Al4V, Cu, Pb, S355 steel and gas tungsten arc welded AISI 304 stainless steel were determined through eddy currents and four-point probe. In parallel, hardness measurements were also performed. The profiles matched well with the optical macrographs of the materials: while entering in the processed region a variation in both profiles was always observed. One particular advantage of electrical conductivity profiles over hardness was evident: it provides a better resolution of the microstructural alterations in the processed materials. Moreover, when thermomechanical processing induces microstructural changes that modify the magnetic properties of a material, eddy currents testing can be used to qualitatively determine the phase fraction in a given region of the material. A qualitative relation between electrical conductivity measurements and hardness is observed.     

Observations of infrared bands of asymmetrical ozone isotopologues 16O16O18O and 16O18O18O

Infrared spectra (0.003 cm(-1) resolution) of 16O16O18O and 16O18O18O ozone isotopologues have been recorded and analyzed in the range 600-5000 cm(-1). Several thousand rovibrational lines belonging to 32 absorption bands have been measured and assigned. An accurate determination of band centers through the rovibrational analysis has been done, 12 bands being observed for the first time to our knowledge. In addition to atmospheric retrieval applications, these results are also useful for a validation of potential energy surfaces and for the study of isotope effects in dynamic processes of ozone.     

Photocatalytic reduction of nitrate in wastewater using ZnO nanopowder synthesized by solution combustion method

ZnO nanopowder was synthesized by a unique method which is called solution combustion method (SCM). This nanopowder was used for a photocatalyst to decompose nitrate that is a toxic pollutant in wastewater. It has been known that TiO2, the most popular photocatalyst, does not decompose the nitrate. In this paper, however, the SCM ZnO nanopowder decomposed about 13% of nitrate. Furthermore, adding methanol as a hole scavenger, the decomposition rate was enhanced by about 5 times. On the other hand, it has been reported that the photocatalytic reduction reaction of nitrate produces ammonia as a final product. The present results, however, suggest that the final product is non-toxic nitrogen gas rather than the toxic ammonia. These results would be very valuable for drinking water purification.     

High-precision laser spectroscopy D/H and 18O/16O measurements of microliter natural water samples

Newly available gas analyzers based on off-axis integrated cavity output spectroscopy (OA-ICOS) lasers have been advocated as an alternative to conventional isotope-ratio mass spectrometers (IRMS) for the stable isotopic analysis of water samples. In the case of H2O, OA-ICOS is attractive because it has comparatively low capital and maintenance costs, the instrument is small and field laboratory portable, and provides simultaneous D/H and 16O/18O ratio measurements directly on H2O molecules with no conversion of H2O to H2, CO, or H2/CO2-water equilibration required. Here we present a detailed assessment of the performance of a liquid-water isotope analyzer, including instrument precision, estimates of sample memory and sample mass effects, and instrumental drift. We provide a recommended analysis procedure to achieve optimum results using OA-ICOS. Our results show that, by using a systematic sample analysis and data normalization procedure routine, measurement accuracies of +/-0.8 per thousand for deltaD and +/-0.1 per thousand delta18O are achievable on nanoliter water samples. This is equivalent or better than current IRMS-based methods and at a comparable sample throughput rate.     

An automated technique for measuring deltaD and delta18O values of porewater by direct CO2 and H2 equilibration

The stable-oxygen and -hydrogen isotopic values (deltaD, delta18O) of porewater in geologic media are commonly determined on water obtained by extraction techniques such as centrifugation, mechanical squeezing, vacuum heating and cryogenic microdistillation, and azeotropic distillation. Each of these techniques may cause isotopic fractionation as part the extraction process and each is laborious. Here we demonstrate a new approach to obtain automated, high-precision deltaD and delta18O measurements of porewater in geologic sediments by direct H2- and CO2-porewater equilibration using a modified commercial CO2-water equilibrator. This technique provides an important and cost-effective improvement over current extraction methods, because many samples can be rapidly analyzed with minimal handling, thereby reducing errors and potential for isotopic fractionation. The precision and accuracy of direct H2- and CO2-porewater equilibration is comparable to or better than current porewater extraction methods. Finally, the direct equilibration technique allows investigators to obtain high-resolution (cm scale) porewater deltaD and delta18O profiles using cores from individual boreholes, eliminating the need for costly piezometers or conventional porewater extractions.     

Structural and electrochemical properties of LiNi0.3Co0.7O2 synthesized by different low-temperature techniques

Single phase LiNi_1−yCo_yO₂ (y=0.7) with fine particles were prepared by two different low-temperature methods, namely sol–gel and combustion techniques. It was found that bulk quantities of submicron-sized particles of layered LiNi_0.3Co_0.7O₂ can be obtained at temperatures below 400°C by these solution techniques. The methods involved the mixing of either acetates or nitrates of the metals, Ni and Co, with a chelating agent, carboxylic acid (sol–gel method) or a complexing agent, glycine (combustion method) in an aqueous medium. Both carboxylic acid and glycine acted as fuels, decomposed the homogeneous precipitate of metal complexes at low temperature, and yielded the free impurity LiNi_0.3Co_0.7O₂ compound. The synthesized products were characterized by structural (XRD, SEM), spectroscopic (FTIR) and thermal (DTA-TG) analyses. The electrochemical performance of the synthesized products in rechargeable Lithium cells were evaluated using a non-aqueous organic electrolyte mixture of 1M LiPF₆ in EC+DMC. The electrochemical behavior of synthesized LiNi_0.7Co_0.3O₂ is discussed in relation with its synthesis procedures.     

Flowability measurements of pharmaceutical powder mixtures with poor flow using five different techniques

Four different tablet formulations for direct compression with poor flow properties were tested regarding flowability using five different techniques: Hausner ratio, avalanching behavior, powder rheometer, uniaxial tester, and Jenike tester. In addition, the behavior of three of the formulations during emptying of the mixer and tableting was observed and compared to the results of the flowability measurements. The rank order correlation of the formulations was generally the same with all techniques. The flow properties measured by the different techniques reflected the behavior during processing of the powder mixtures.     

Comparison of CdS thin films prepared by different techniques for applications in solar cells as window materials

CdS thin films as window materials for solar cells have been prepared by three procedures; chemical bath deposition, electrodeposition in an aqueous medium at 80 °C and electrodeposition in a non-aqueous medium at 170 °C. As deposited films along with those obtained after annealing in air at 400 °C for 15 min were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), glow discharge optical emission spectroscopy (GDOES), scanning electron microscopy (SEM), optical absorption spectra and photoelectrochemical spectroscopy (PEC) techniques under identical experimental conditions. X-ray diffraction data indicate the formation of hexagonal CdS as the predominent phase, but the SEM studies show that their textures are widely dependent on the conditions employed. GDOES profiling indicates the incorporation of Na and Si into CdS films prepared by all three techniques. Annealing of chemical bath deposited films causes a red shift of the absorbance edge and also a shift in the maxima of the photocurrent action spectra towards the low energy side. However, this effect was comparatively negligible for the samples prepared by the other two techniques. PEC studies indicate that CdS materials grown by all three techniques are all n-type. All studies indicate that the films grown at 170 °C using non-aqueous solutions are of better crystallinity and of improved electrical properties. © 1998 Kluwer Academic Publishers     

Emission characteristics of coal combustion in different O2/N2, O2/CO2 and O2/RFG atmosphere

This study investigates the emission characteristics of CO(2), SO(2) and NOx in the flue gas of coal combustion by varying the compositions and concentrations of feed gas (O(2)/CO(2)/N(2)) and the ratios of recycled flue gas. The differences between O(2)/recycled flue gas (O(2)/RFG) combustion and general air combustion are also discussed. Experimental results indicate that the maximum concentration of CO(2) in O(2)/CO(2) combustion system is 95% as the feed gas is 30% O(2)/70% CO(2). The average concentration of CO(2) in the flue gas of O(2)/CO(2) coal combustion system is higher than 90% and much higher than that of O(2)/N(2) coal combustion system. This high concentration of CO(2) is beneficial for the separation of CO(2) from the flue gas by adsorption or absorption technologies. The maximum concentration of CO(2) in O(2)/N(2) combustion system is only 34% at the feed gas 50% O(2)/50% N(2), the concentration of CO(2) is increased with the concentration of O(2) in feed gas. By O(2)/CO(2) combustion technology, higher concentration of SO(2) is produced as the feed gas is 30% O(2)/70% CO(2) or 40% O(2)/60% CO(2), while higher concentration of NOx is produced as the feed gas is 20% O(2)/80% CO(2) or 50% O(2)/50% CO(2). The mass flow rates of CO(2), SO(2) and NOx in the flue gas are all increased with the ratio of recycled flue gas except for the feed gas 20% O(2)/80% CO(2). The enhanced mass flow rates of air pollutants in such O(2)/RFG combustion system are also beneficial for improving the control efficiencies of air pollution control devices. By O(2)/N(2) combustion technology, higher concentrations of SO(2) and NOx are produced as the feed gas is 21% O(2)/79% N(2). The results also indicate that the formation of NOx in general air combustion system is higher than that in O(2)/RFG or O(2)/CO(2) combustion system.     

Preparation of nanostructured NiFe2O4 catalysts by combustion reaction

Nanosize nickel ferrite powders (NiFe₂O₄) have been prepared by combustion reaction using nitrates and urea as fuel. The resulting powders were characterized by X-ray diffraction (XRD), nitrogen physical adsorption (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and catalytic activity. The results showed nanosize nickel ferrite powders with high specific surface area (55.21 m²/g). The powders showed extensive XRD line broadening and the crystallite size calculated from the XRD line broadening was 18.0 nm. The nickel ferrite powder presented significant activity as catalyst for the water gas shift reaction, over the temperature range of 250–450 °C.     

High resolution spectral measurements of Raman shifts in barium nitrate

High resolution spectral measurements of the first, second, and third Stokes shifts in barium nitrate are reported. The laser source for the experiment is a frequency-doubled, injection-seeded Nd:YAG laser. Spectra for both single-pass conversion and for a Raman oscillator are compared. Significant gain narrowing of the spectrum is observed.     

Wood cellulose preparation methods and mass spectrometric analyses of delta13C, delta18O, and nonexchangeable delta2H values in cellulose, sugar, and starch: an interlaboratory comparison

Interlaboratory comparisons involving nine European stable isotope laboratories have shown that the routine methods of cellulose preparation resulted in data that generally agreed within the precision of the isotope ratio mass spectrometry (IRMS) method used: +/-0.2 per thousand for carbon and +/-0.3 per thousand for oxygen. For carbon, the results suggest that holocellulose is enriched up to 0.39 per thousand in 13C relative to the purified alpha-cellulose. The comparisons of IRMS measurements of carbon on cellulose, sugars, and starches showed low deviations from -0.23 to +0.23 per thousand between laboratories. For oxygen, IRMS measurements varied between means from -0.39 to 0.58 per thousand, -0.89 to 0.42 per thousand, and -1.30 to 1.16 per thousand for celluloses, sugars, and starches, respectively. This can be explained by different effects arising from the use of low- or high-temperature pyrolysis and by the variation between laboratories in the procedures used for drying and storage of samples. The results of analyses of nonexchangeable hydrogen are very similar in means with standard deviations between individual methods from +/-2.7 to +/-4.9 per thousand. The use of a one-point calibration (IAEA-CH7) gave significant positive offsets in delta2H values up to 6 per thousand. Detailed analysis of the results allows us to make the following recommendations in order to increase quality and compatibility of the common data bank: (1) removal of a pretreatment with organic solvents, (2) a purification step with 17% sodium hydroxide solution during cellulose preparation procedure, (3) measurements of oxygen isotopes under an argon hood, (4) use of calibration standard materials, which are of similar nature to that of the measured samples, and (5) using a two-point calibration method for reliable result calculation.