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DC Field Emission Studies on Nb

Description: The DC field emission studies in TJNAF aim to further explore the causes of field emission from Niobium surfaces and enhance our understanding of various preparation techniques for the purpose of improving field emission suppression. Field emitters on Nb samples are located by a DC field emission scanning apparatus in ultra high vacuum, then individually studied under SEM with EDS for characterization. Results at above 100 MV/m from samples prepared by BCP, and by electropolishing are presented and compared.
Date: September 1, 2001
Creator: Wang, T.; Reece, C. & Sundelin, R.
Partner: UNT Libraries Government Documents Department

Extension of the Southern Hemisphere Atmospheric Radiocarbon Curve, 2120-850 years BP: Results from Tasmanian Huon Pine

Description: Decadal samples of dendrochronologically-dated pine (Lagorostrobos franklinii) from the Stanley River basin, Tasmania have been radiocarbon dated between 2120-850 yr BP. This data set overlaps and extends the current Southern Hemisphere record, which currently covers the period 110-995 yr BP. There is good agreement between the two records between 995-850 yr BP, between sample replicates and with consensus values for standards. As in the younger dataset, we find evidence for a distinct but variable offset between the southern hemisphere data and IntCal04; although this is likely due to real temporal variability in the interhemispheric offset, further work is planned to rule out possible laboratory or sample preparation differences.
Date: February 12, 2010
Creator: Zimmerman, S R; P.Guilderson, T; Buckley, B M & Cook, E
Partner: UNT Libraries Government Documents Department

Loss of Radioactivity from Barium Carbonate Samples

Description: The exchange loss of radioactivity from solid samplos of barium carbonate through the agency of carbonic acid and its ions has been investigated under a variety of conditions. It is concluded that the losses observed are greatly dependent upon the method of sample preparation, in particular the nature or any heat treatment which the sample materials undergo.
Date: January 9, 1948
Creator: Yankwich, Peter E.
Partner: UNT Libraries Government Documents Department

Laser: a Tool for Optimization and Enhancement of Analytical Methods

Description: In this work, we use lasers to enhance possibilities of laser desorption methods and to optimize coating procedure for capillary electrophoresis (CE). We use several different instrumental arrangements to characterize matrix-assisted laser desorption (MALD) at atmospheric pressure and in vacuum. In imaging mode, 488-nm argon-ion laser beam is deflected by two acousto-optic deflectors to scan plumes desorbed at atmospheric pressure via absorption. All absorbing species, including neutral molecules, are monitored. Interesting features, e.g. differences between the initial plume and subsequent plumes desorbed from the same spot, or the formation of two plumes from one laser shot are observed. Total plume absorbance can be correlated with the acoustic signal generated by the desorption event. A model equation for the plume velocity as a function of time is proposed. Alternatively, the use of a static laser beam for observation enables reliable determination of plume velocities even when they are very high. Static scattering detection reveals negative influence of particle spallation on MS signal. Ion formation during MALD was monitored using 193-nm light to photodissociate a portion of insulin ion plume. These results define the optimal conditions for desorbing analytes from matrices, as opposed to achieving a compromise between efficient desorption and efficient ionization as is practiced in mass spectrometry. In CE experiment, we examined changes in a poly(ethylene oxide) (PEO) coating by continuously monitoring the electroosmotic flow (EOF) in a fused-silica capillary during electrophoresis. An imaging CCD camera was used to follow the motion of a fluorescent neutral marker zone along the length of the capillary excited by 488-nm Ar-ion laser. The PEO coating was shown to reduce the velocity of EOF by more than an order of magnitude compared to a bare capillary at pH 7.0. The coating protocol was important, especially at an intermediate pH of 7.7. The increase of ...
Date: January 1, 1997
Creator: Preisler, Jan
Partner: UNT Libraries Government Documents Department

Platinum Catalyzed Decomposition of Activated Carbon: 1. Initial Studies

Description: Carbon is an important support for heterogeneous catalysts, such as platinum supported on activated carbon (AC). An important property of these catalysts is that they decompose upon heating in air. Consequently, Pt/AC catalysts can be used in applications requiring rapid decomposition of a material, leaving little residue. This report describes the catalytic effects of platinum on carbon decomposition in an attempt to maximize decomposition rates. Catalysts were prepared by impregnating the AC with two different Pt precursors, Pt(NH{sub 3}){sub 4}(NO{sub 3}){sub 2} and H{sub 2}PtCl{sub 6}. Some catalysts were treated in flowing N{sub 2} or H{sub 2} at elevated temperatures to decompose the Pt precursor. The catalysts were analyzed for weight loss in air at temperatures ranging from 375 to 450 C, using thermogravimetric analysis (TGA). The following results were obtained: (1) Pt/AC decomposes much faster than pure carbon; (2) treatment of the as-prepared 1% Pt/AC samples in N{sub 2} or H{sub 2} enhances decomposition; (3) autocatalytic behavior is observed for 1% Pt/AC samples at temperatures {ge} 425 C; (4) oxygen is needed for decomposition to occur. Overall, the Pt/AC catalyst with the highest activity was impregnated with H{sub 2}PtCl{sub 6} dissolved in acetone, and then treated in H{sub 2}. However, further research and development should produce a more active Pt/AC material.
Date: December 1, 2001
Partner: UNT Libraries Government Documents Department

Evaluation of kinetic phosphorescence analysis for the determination of uranium

Description: In the past, New Brunswick Laboratory (NBL) has used a fluorometric method for the determination of sub-microgram quantities of uranium. In its continuing effort to upgrade and improve measurement technology, NBL has evaluated the commercially-available KPA-11 kinetic phosphorescence analyzer (Chemchek, Richland, WA). The Chemchek KPA-11 is a bench-top instrument which performs single-measurement, quench-corrected analyses for trace uranium. It incorporates patented kinetic phosphorimetry techniques to measure and analyze sample phosphorescence as a function of time. With laser excitation and time-corrected photon counting, the KPA-11 has a lower detection limit than conventional fluorometric methods. Operated with a personal computer, the state-of-the-art KPA-11 offers extensive time resolution and phosphorescence lifetime capabilities for additional specificity. Interferences are thereby avoided while obtaining precise measurements. Routine analyses can be easily and effectively accomplished, with the accuracy and precision equivalent to the pulsed-laser fluorometric method presently performed at NBL, without the need for internal standards. Applications of kinetic phosphorimetry at NBL include the measurement of trace level uranium in retention tank, waste samples, and low-level samples. It has also been used to support other experimental activities at NBL by the measuring of nanogram amounts of uranium contamination (in blanks) in isotopic sample preparations, and the determining of elution curves of different ion exchange resins used for uranium purification. In many cases, no pretreatment of samples was necessary except to fume them with nitric acid, and then to redissolve and dilute them to an appropriate concentration with 1 M HNO{sub 3} before measurement. Concentrations were determined on a mass basis ({micro}g U/g of solution), but no density corrections were needed since all the samples (including the samples used for calibration) were in the same density matrix (1 M HNO{sub 3}). A statistical evaluation of the determination of uranium using kinetic phosphorimetry is described in this report, along with ...
Date: December 1, 1997
Creator: Croatto, P.V.; Frank, I.W.; Johnson, K.D.; Mason, P.B. & Smith, M.M.
Partner: UNT Libraries Government Documents Department

Calibration of laser ablation inductively coupled plasma mass spectrometry using dried solution aerosols for the quantitative analysis of solid samples

Description: Inductively coupled plasma mass spectrometry (ICP-MS) has become the method of choice for elemental and isotopic analysis. Several factors contribute to its success. Modern instruments are capable of routine analysis at part per trillion levels with relative detection limits in part per quadrillion levels. Sensitivities in these instruments can be as high as 200 million counts per second per part per million with linear dynamic ranges up to eight orders of magnitude. With standards for only a few elements, rapid semiquantitative analysis of over 70 elements in an individual sample can be performed. Less than 20 years after its inception ICP-MS has shown to be applicable to several areas of science. These include geochemistry, the nuclear industry, environmental chemistry, clinical chemistry, the semiconductor industry, and forensic chemistry. In this introduction, the general attributes of ICP-MS will be discussed in terms of instrumentation and sample introduction. The advantages and disadvantages of current systems are presented. A detailed description of one method of sample introduction, laser ablation, is given. The paper also gives conclusions and suggestions for future work. Chapter 2, Quantitative analysis of solids by laser ablation inductively coupled plasma mass spectrometry using dried solution aerosols for calibration, has been removed for separate processing.
Date: February 12, 1999
Creator: Leach, J.
Partner: UNT Libraries Government Documents Department

Ion Chromatography Analysis of Dibutyl Phosphoric Acid

Description: Analysis of dibutyl phosphate (DBP), a degradation product of tributyl phosphate (TBP), has long been a problem analysis by Ion Chromatography at the Savannah River Site. Due to the presence of UO{sub 2}{sup +2} and high NO{sub 3}{sup {minus}1} concentrations, inadequate recovery and separation of DBP on the chromatographic column had rendered the analysis undependable and very inconsistent, thus causing high uncertainties in the data. The method presented here by the Savannah River Technology Center (SRTC)/Analytical Development Section (ADS) addresses the sample preparation problems encountered when analyzing for DBP in the presence of uranium and nitrate. The data presented reflects the improvements made to decrease data uncertainty and increase data accuracy and precision.
Date: December 4, 1998
Creator: Ray, R.J.
Partner: UNT Libraries Government Documents Department

Laboratory analysis of soil hydraulic properties of CDBM 2 and CDBM 3 samples

Description: Daniel B. Stephens & Associates, Inc. (DBS&A) was requested by Dr. Alan Stoker of Los Alamos National Laboratory to perform laboratory analysis for properties of CDBM 2 and CDBM 3 samples, as outlined in Subcontract No. 9-XTI-027EE-1. The scope of work included conducting tests for the following properties: Initial moisture content, dry bulk density, and calculated porosity; Saturated hydraulic conductivity; Moisture characteristics; Unsaturated hydraulic properties (calculated); and Transient outflow.
Date: December 1, 1992
Partner: UNT Libraries Government Documents Department

Advanced biomolecular materials based on membrane-protein/polymer complexation

Description: This is the final report of a three-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). The goal of this project was to apply neutron reflectometry and atomic force microscopy to the study of lipid membranes containing proteins. Standard sample preparation techniques were used to produce thin films of these materials appropriate for these techniques. However, these films were not stable, and a new sample preparation technique was required. Toward this goal, the authors have developed a new capability to produce large, freely suspended films of lipid multi-bilayers appropriate for these studies. This system includes a controlled temperature/humidity oven in which the films 5-cm x 5-cm are remotely drawn. The first neutron scattering experiments were then performed using this oven.
Date: December 1, 1998
Creator: Smith, G.S.; Nowak, A. & Safinya, C.
Partner: UNT Libraries Government Documents Department

Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

Description: The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.
Date: March 31, 1999
Creator: Tan, H.
Partner: UNT Libraries Government Documents Department

A new procedure for making TEM specimens of superconductor devices

Description: A new procedure is developed for making TEM specimens of thin film devices. In this procedure the sample is flatly polished to an overall ion-mill-ready thickness so that any point in the 2-D sample pane can be thinned to an electron-transparent thickness by subsequent ion-milling. Using this procedure, small regions of interest can be easily reached in both cross-section and plan-view samples. This is especially useful in device studies. Applications of this procedure to the study of superconductor devices yield good results. This procedure, using commercially available equipment and relatively cheap materials, is simple and easy to realize.
Date: April 1, 1997
Creator: Huang, Y. & Merkle, K.L.
Partner: UNT Libraries Government Documents Department

Small angle neutron and X-ray scattering studies of carbons prepared using inorganic templates

Description: Small angle neutron (SANS) and X-ray (SAXS) scattering analyses of carbons derived from organic-loaded inorganic template materials, used as anodes in lithium ion cells, have been performed. Two clays were used as templates to load the organic precursors, pillared montmorrillonite (PILC), a layered silicate clay whose sheets have been permanently propped open by sets of thermally stable molecular props, and sepiolite, a natural channeled clay. Five different organic precursors were used to load the PILC: pyrene, styrene, pyrene/trioxane copolymer, ethylene and propylene, whereas only propylene and ethylene were used to load sepiolite. Pyrolysis took place at 700{degrees}C under nitrogen. Values such as hole radius, fractal dimension, cutoff length and density of the final carbons will be compared as a function of the clay and carbon precursors.
Date: September 1, 1997
Creator: Sandi, G.; Thiyagarajan, P.; Winans, R.E. & Carrado, K.A.
Partner: UNT Libraries Government Documents Department

Procedure for the permeabilization and cryobiological preservation of Drosophila embryos

Description: The authors describe the detailed protocol developed in their laboratory at Oak Ridge for the permeabilization and cryobiological preservation of embryos of Drosophila melanogaster, Oregon R strain. The protocol is supplemented by notes containing two sorts of information. One category includes references to the appropriate portions of their published papers giving the scientific rationale and experimental basis for important steps. The other category is concerned with the criticality of certain steps and the precision with which they need to be performed. As an aid to investigators, the authors list even ordinary pieces of equipment. Brand names and model numbers are given where it is either important or convenient for readers to know precisely what is used.
Date: May 6, 1993
Creator: Cole, K.W.; Schreuders, P.D.; Mahowald, A.P. & Mazur, P.
Partner: UNT Libraries Government Documents Department

Testing of explosives mixed with clay to determine maximum explosive content of non-reactive mixtures

Description: This report contains a detailed description of the experiments conducted to demonstrate that debris from explosives testing in a shot tank that contains 4 weight percent or less of explosive is non-reactive under the specified testing protocol in the Code of Federal Regulations. As such it is a companion report to UCRL-ID-128999, "Program for Certification of Waste from Contained Firing Facility - Establishment of Waste as Non-Reactive and Discussion of Potential Waste Generation Problems."
Date: July 21, 1998
Creator: Garza, R; Green, L; Maienschein, J & Pruneda, C
Partner: UNT Libraries Government Documents Department

Sample preparation of tank 241-C-106 grab samples and testing For compatibility with tank 241-AY-102 supernate

Description: This test plan describes a sample separation method which will be used to obtain physical measurements and separated 241-C-106 solids and supernate fractions. In addition compatibility of tank 241-C-106 sludge with tank 241-AY-102 supernate will be determined.
Date: February 23, 1996
Creator: Crawford, B.A.
Partner: UNT Libraries Government Documents Department

Reactive gas plasma specimen processing for use in microanalysis and imaging in analytical electron microscopy

Description: It has long been the bane of analytical electron microscopy (AEM) that the use of focused probes during microanalysis of specimens increases the local rate of hydrocarbon contamination. This is most succinctly observed by the formation of contamination deposits during focused probe work typical of AEM studies. While serving to indicate the location of the electron probe, the contamination obliterates the area of the specimen being analyzed and adversely affects all quantitative microanalysis methodologies. A variety of methods including: UV, electron beam flooding, heating and/or cooling can decrease the rate of contamination, however, none of these methods directly attack the source of specimen borne contamination. Research has shown that reactive gas plasmas may be used to clean both the specimen and stage for AEM, in this study the authors report on quantitative measurements of the reduction in contamination rates in an AEM as a function of operating conditions and plasma gases.
Date: January 1997
Creator: Zaluzec, N. J.; Kestel, B. J. & Henriks, D.
Partner: UNT Libraries Government Documents Department

Capillary electrophoresis separation of neutral organic compounds, pharmaceutical drugs, proteins and peptides, enantiomers, and anions

Description: Addition of a novel anionic surfactant, namely lauryl polyoxyethylene sulfate, to an aqueous-acetonitrile electrolyte makes it possible to separate nonionic organic compounds by capillary electrophoresis. Separation is based on differences in the association between analytes and the surfactant. Highly hydrophobic compounds such as polyaromatic hydrocarbons are well separated by this new surfactant. Migration times of analytes can be readily changed over an unusually large range by varying the additive concentration and the proportion of acetonitrile in the electrolyte. Several examples are given, including the separation of four methylbenz[a]anthracene isomers and the separation of normal and deuterated acetophenone. The effect of adding this new surfactant to the acidic electrolyte was also investigated. Incorporation of cetyltrimethylammonium bromide in the electrolyte is shown to dynamically coat the capillary and reverse electroosmotic flow. Chiral recognition mechanism is studied using novel synthetic surfactants as chiral selectors, which are made from amino acids reacting with alkyl chloroformates. A satisfactory separation of both inorganic and organic anions is obtained using electrolyte solutions as high as 5 M sodium chloride using direct photometric detection. The effect of various salts on electrophoretic and electroosmotic mobility is further discussed. Several examples are given under high-salt conditions.
Date: February 12, 1999
Creator: Ding, W.L.
Partner: UNT Libraries Government Documents Department

Unique applications of solvent removal in inductively coupled plasma mass spectrometry

Description: Inductively coupled plasma mass spectrometry (ICP-MS) is the technique of choice for rapid, high precision, semiquantitative elemental and isotopic analysis for over 70 elements. Less than 20 years after the first mass spectrum was obtained by ICP-MS, this technique has applications in clinical chemistry, geochemistry, the semiconductor industry, the nuclear industry, environmental chemistry, and forensic chemistry. The determination of many elements, though, by ICP-MS is complicated by spectral interferences from background species, interelement spectral overlaps, and polyatomic ions of matrix elements. The emphasis of this thesis is the unique applications of solvent removal using cryogenic and membrane desolvation. Chapter 1 is a general introduction providing background information concerning the need for these methods and some information about the methods themselves. Chapter 5 discusses general conclusions and general observations pertaining to this work. Chapters 2, 3, and 4 have been processed separately for inclusion on the database. Chapter 2 describes a method to screen urine samples for vanadium using cryogenic desolvation. Chapter 3 compares solvent removal by cryogenic and membrane desolvation. Chapter 4 describes the use of cool plasma conditions for the determination of potassium in the presence of excess sodium by ICP-MS.
Date: January 10, 1997
Creator: Minnich, M.
Partner: UNT Libraries Government Documents Department

A Novel Method for the Determination of Gross Transuranic Activity in Uranium Compounds

Description: A Method is described to determine gross transuranic activity present in Uranium compounds and HP smears. From one count and one spectrum, three or more isotopes can be quantified. The method involves a simple digestion prep, sample extraction and precipitation. Results are obtained quickly with a very small expenditure on the part of the analytical lab.
Date: November 16, 1998
Creator: Mann, D.K. & Tucker, M.C.
Partner: UNT Libraries Government Documents Department

Mechanics of Metals with Phase Changes

Description: New experimental data is presented on some exotic metals that exhibit phase changes at cryogenic temperatures. The types of phase changes that were detected in the specific heat data range from martensitic (diffusion less) transitions to superconducting transitions. In addition, the charge density wave (CDW) state in uranium metal was detected in the specific heat. Specific-heat measurements were made in zero-magnetic field using an apparatus capable of obtaining temperatures as low as 0.4 K. Calibration performed on this apparatus, using a single-crystal copper sample, show its accuracy to be 0.50%, while the resolution was better than 0.1%. Our measurements demonstrate that similar high precision and accurate specific-heat measurements can be obtained on milligram-scale samples. In Chapters 2 and 3, specific-heat measurements are presented for the B2 (CsCl structure) alloy AuZn and for {alpha}-uranium (orthorhombic symmetry). The AuZn alloy exhibits a continuous transition at 64.75 K and an entropy of transition of ({Delta}S{sub tr}) 2.02 J K{sup {minus}1} mol{sup {minus}1}. Calculation of the Debye temperature, by extrapolating of the high temperature phase elastic constants to T = 0 K yields a value of 207 K ({+-}2 K), in favorable agreement with the calorimetric value of 219 K ({+-}0.50 K), despite the intervening martensitic transition. Reported results for single-crystal {alpha}-U show a low-temperature limiting {Theta}{sub D} of 256 K ({+-}0.50 K) and four low-temperature anomalies: a superconducting transition below 1 K, an electronic transition at 22 K, and two anomalies at 38 K and at 42 K indicative of the CDW state. In order to continue the study of the actinide series of elements, a program was initiated to first purify and then grow single crystals of plutonium. Accordingly, the focus of Chapters 4 through 6 will be a description of plutonium sample preparation. In this program plutonium metal was purified via ...
Date: January 1, 2001
Creator: Lashley, J.C.
Partner: UNT Libraries Government Documents Department