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At least 55 records · Page 3

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Finally, looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standard

47 OTHER INSTRUMENTATION↗

Altering the sulfur content in the propanethiol plasma polymers using the capacitive-to-inductive mode transition in inductively coupled plasma discharge

The effect of the transition from capacitive (E) to inductive (H) mode on propanethiol plasma polymer films properties was investigated by optical emission as well as by x-ray photoelectron spectroscopy. The E mode is characterized by low deposition rate and by high sulfur content in the films ({approx}40% vs {approx}20% in H mode). After aging, a strong decrease of sulfur to carbon content (from {approx}0.75 to 0.13), attributed to desorption of unbounded sulfur-based molecules (e.g., H{sub 2}S), is detected at low power in E mode. The importance of the E-H transition for altering the film properties is highlighted.

36 MATERIALS SCIENCE↗

External control of electron energy distributions in a dual tandem inductively coupled plasma

The control of electron energy probability functions (EEPFs) in low pressure partially ionized plasmas is typically accomplished through the format of the applied power. For example, through the use of pulse power, the EEPF can be modulated to produce shapes not possible under continuous wave excitation. This technique uses internal control. In this paper, we discuss a method for external control of EEPFs by transport of electrons between separately powered inductively coupled plasmas (ICPs). The reactor incorporates dual ICP sources (main and auxiliary) in a tandem geometry whose plasma volumes are separated by a grid. The auxiliary ICP is continuously powered while the main ICP is pulsed. Langmuir probe measurements of the EEPFs during the afterglow of the main ICP suggests that transport of hot electrons from the auxiliary plasma provided what is effectively an external source of energetic electrons. The tail of the EEPF and bulk electron temperature were then elevated in the afterglow of the main ICP by this external source of power. Results from a computer simulation for the evolution of the EEPFs concur with measured trends.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Transients using low-high pulsed power in inductively coupled plasmas

Pulsed inductively coupled plasmas (ICPs) are widely deployed in the fabrication of semi-conductor devices. Pulse repetition frequencies (PRFs) of up to tens of kHz are commonly used during plasma etching for the high power densities they generate during the pulse-on period, and for their unique chemistries during the pulse-off period. The use of highly attaching halogen gases produces low electron densities during the pulse-off period, and these low density can result in instabilities, E-H transitions and ignition delays when applying power on the next pulse. To mitigate these possibilities, a low-level power environment could be maintained during “pulse-off” to moderate the minimum plasma density, therefore reducing ignition delays and enhancing plasma stability. In this work, ICPs sustained by 5 kHz pulsed power using Ar/Cl 2 mixtures at 20 mTorr were computationally investigated. For these conditions, the computed electron temperature (T e ) reaches a quasi-steady state during both the high- and low-power excitation. The model predicts that within the electromagnetic skin-depth, T e spikes to a high value during a low-to-high power modulation, and to a low value during a high-to-low power modulation. At the same time, a few cm above the substrate, there is little modulation in T e , as electron power convected from the skin depth disperses in traversing the reactor. Finally, the positive and negative spikes, and convection of transients across the reactors, are functions of power ramping time and gas mixtures.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Optical emission spectroscopic studies and comparisons of CH{sub 3}F/CO{sub 2} and CH{sub 3}F/O{sub 2} inductively coupled plasmas

A CH{sub 3}F/CO{sub 2} inductively coupled plasma (ICP), sustained in a compact plasma reactor, was investigated as a function of power (5–400 W) and feed gas composition, at a pressure of 10 mTorr, using optical emission spectroscopy and rare gas actinometry. Number densities of H, F, and O increased rapidly between 74% and 80% CO{sub 2}, ascribed to the transition from polymer-covered to polymer-free reactor walls, similar to that found previously in CH{sub 3}F/O{sub 2} ICPs at 48% O{sub 2}. Below 40% O{sub 2} or CO{sub 2}, relative emission intensity ratios were almost identical for most key species in CH{sub 3}F/O{sub 2} and CH{sub 3}F/CO{sub 2} ICPs except for higher OH/Xe (a qualitative measure of OH and H{sub 2}O densities) over the full range of CH{sub 3}F/O{sub 2} composition. The number density of H, F, and O increased with power in CH{sub 3}F/CO{sub 2} (20%/80%) plasmas (polymer-free walls), reaching 4.0, 0.34, and 1.6 × 10{sup 13}/cm{sup 3}, respectively, at 300 W. The CO number density increased with power and was estimated, based on self-actinometry, to be 8.8 × 10{sup 13}/cm{sup 3} at 300 W. The CO{sub 2} number density was independent of power below 40 W (where very little decomposition occurred), and then decreased rapidly with increasing power, reaching 2.8 × 10{sup 13}/cm{sup 3} at 300 W, corresponding to 83% dissociation. Films deposited on p-Si, 10 cm from the open, downstream end of the plasma reactor, were analyzed by x-ray photoelectron spectroscopy. Between 10% and 40% CO{sub 2} or O{sub 2} addition to CH{sub 3}F, film deposition rates fell and O content in the films increased. Faster deposition rates in CH{sub 3}F/CO{sub 2} plasmas were ascribed mainly to a larger thermodynamic driving force to form solid carbon, compared with CH{sub 3}F/O{sub 2} plasmas. Oxygen content in the films increased with increasing CO{sub 2} or O{sub 2} addition, but for the same deposition rate, no substantial differences were observed in the composition of the films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Induction of genomic instability in TK6 human lymphoblasts exposed to 137Cs gamma radiation: comparison to the induction by exposure to accelerated 56Fe particles

The induction of genomic instability in TK6 human lymphoblasts by exposure to (137)Cs gamma radiation was investigated by measuring the frequency and characteristics of unstable clones isolated approximately 36 generations after exposure. Clones surviving irradiation and control clones were analyzed for 17 characteristics including chromosomal aberrations, growth defects, alterations in response to a second irradiation, and mutant frequencies at the thymidine kinase and Na(+)/K(+) ATPase loci. Putative unstable clones were defined as those that exhibited a significant alteration in one or more characteristics compared to the controls. The frequency and characteristics of the unstable clones were compared in clones exposed to (137)Cs gamma rays or (56)Fe particles. The majority of the unstable clones isolated after exposure to either gamma rays or (56)Fe particles exhibited chromosomal instability. Alterations in growth characteristics, radiation response and mutant frequencies occurred much less often than cytogenetic alterations in these unstable clones. The frequency and complexity of the unstable clones were greater after exposure to (56)Fe particles than to gamma rays. Unstable clones that survived 36 generations after exposure to gamma rays exhibited increases in the incidence of dicentric chromosomes but not of chromatid breaks, whereas unstable clones that survived 36 generations after exposure to (56)Fe particles exhibited increases in both chromatid and chromosome aberrations.

Non-NASA Center↗

New measurement of the 238 U decay constant with inductively coupled plasma mass spectrometry [New Measurement of the U-238 Decay Constant with Inductively Coupled Plasma Mass Spectrometry]

The 238 U decay constant (λ U-238 ) is fundamental to radioisotope-based chronometry in the Earth and planetary sciences, yet only a single published λ U-238 value (Jaffey et al. in Phys Rev C 4(5):1889–1906, 1971) is widely applied. We have determined λ U-238 via the novel approach of measuring of 234 Th ingrowth in high-purity 238U solutions, using isotope dilution mass spectrometry (ID-MS). The 234 Th decay constant (λ Th-234 ) was measured via decay counting with high-purity Ge (HPGe) $\gamma$ detectors. Preliminary results for λ U-238 agree with the value determined by $a$-counting [1] within the elevated uncertainty of 0.462% (k = 2). Ongoing efforts to reproduce λ U-238 with reduced experimental uncertainties will inform future conclusions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Uncertainty Measurement for Trace Element Analysis of Uranium and Plutonium Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

The measurement uncertainty estimation associated with trace element analysis of impurities in U and Pu was evaluated using the Guide to the Expression of Uncertainty Measurement (GUM). I this evaluation the uncertainty sources were identified and standard uncertainties for the components were categorized as either Type A or B. The combined standard uncertainty was calculated and a coverage factor k = 2 was applied to obtain the expanded uncertainty, U. The ICP-AES and ICP-MS methods used were developed for the multi-element analysis of U and Pu samples. A typical analytical run consists of standards, process blanks, samples, matrix spiked samples, post digestion spiked samples and independent calibration verification standards. The uncertainty estimation was performed on U and Pu samples that have been analyzed previously as part of the U and Pu Sample Exchange Programs. Control chart results and data from the U and Pu metal exchange programs were combined with the GUM into a concentration dependent estimate of the expanded uncertainty. Comparison of trace element uncertainties obtained using this model was compared to those obtained for trace element results as part of the Exchange programs. This process was completed for all trace elements that were determined to be above the detection limit for the U and Pu samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Heating system with induction power supply and electromagnetic acoustic transducer with induction power supply

A system for heating a fluid and an electromagnetic acoustic transducer EMAT system is provided. Both systems have a drive circuit. The amount of heat and the amplitude (and acceleration) of the vibrations is respectively controllable by controlling an input to a terminal of a switch. The heating system comprises a porous graphite foam conductor which is exposed to an electromagnetic field generated by an oscillating circuit. When exposed, the foam conductor conducts induced electric current which heats the same and a fluid in contact with the conductor. The EMAT system comprises at least one magnet configured to generate a static magnetic field, an oscillating circuit and a working element. The working element, when exposed to the static magnetic field and the electromagnetic field produced by the oscillating circuit, vibrates against a load. The vibrations dry the load.

Kisner, Roger A.↗

Introduction of a Variable Inductance Transformer for the Design of Resonant Power Converters

Magnetic integration is a hot topic in power electronics that concerns the use of a transformer’s leakage and magnetizing inductances purposefully in isolated power electronic converters, thereby giving the opportunity to save the cost and footprint of any additional inductor. This is of prime interest, especially in CLLLC resonant converters which require up to three inductors. For a complete integration of these inductances, the concept of a variable inductance transformer (VIT) is introduced in this thesis. A VIT is an adaptive magnetic structure that facilitates an easy adjustment of both magnetizing and leakage inductances to meet their desired values. However, for a more promising design, an accurate estimation of these inductances is necessary. While the evaluation of magnetizing inductance is quite straightforward, the calculation of leakage inductance is rather convoluted, because the leakage inductance is influenced by both the winding layout and the operating frequency. In this thesis, three new semi-analytical methods for calculating the frequency-independent leakage inductance, and a novel semi-analytical method for evaluating the frequency-dependent leakage inductance are proposed. These methods can calculate the respective leakage inductances of a VIT within an outstanding ±5% uncertainty. Finally, a bidirectional CLLLC resonant dc-dc converter is investigated for the constant current constant voltage (CCCV) charging of the next-generation 900 V traction battery of an electric vehicle. A new voltage gain equation is derived for designing the CLLLC resonant tank, and a small-signal model is presented for designing the variable-frequency feedback controller. Furthermore, a new methodology to design a VIT is developed to overcome the challenges associated with small coupling coefficients and guarantee a complete magnetic integration of the tank inductances. All theoretical results presented herein are verified through simulations and experiments performed on hardware prototypes designed in the lab.

24 POWER TRANSMISSION AND DISTRIBUTION↗