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At least 127 records · Page 7

Organic Evaporation and Oxidation Testing in Support of Hanford Sample-and-Send

The Hanford site has approximately 56 million gallons of radioactive mixed waste stored in 177 underground storage tanks. The Hanford Waste Treatment and Immobilization Plant (WTP) is being built to treat and immobilize the tank waste. The baseline method for immobilization of Low Activity Waste (LAW) through the WTP is vitrification, but additional immobilization capacity is needed to supplement the initial LAW melters. An alternative cementitious waste form is being investigated for that future immobilization method to supplement vitrification. However, one impediment to a cementitious waste form is the presence of Land Disposal Restricted (LDR) organic chemicals in tank waste. This work evaluates potential avenues to eliminate that impediment to permit possible use of a cementitious waste form and work towards a decision whether additional LDR organic pretreatment would be required. Savannah River National Laboratory (SRNL) performed testing using simulants to examine evaporation as a method to remove some prevalent organics from LAW. Spiking the caustic LAW simulant with selected regulated organic chemicals found one that clearly decomposes because of caustic instability. Oxidation testing of other organic chemicals found some LDR organics degrade as desired and others are stable in the presence of peroxide and permanganate. In addition to studies with simulants, a literature review was performed to evaluate radiological stability of LDR organics. Descriptions of the experimental details, equipment, and results are included in this report. Evaporation testing consisted of preparing the LAW simulant, spiking that simulant with organic chemicals, and evaporating the mixture via differential distillation. The apparatus was a laboratory-scale vacuum evaporator operated at 60 ±5 torr absolute (vacuum evaporation) and also at atmospheric pressure. The LAW simulant represented the liquid expected to be retrieved from the Hanford tank farms at approximately 4.0 M [Na + ] total sodium ion concentration. The concentration of the organic chemicals added was significantly higher than typically found in the tank waste samples since the higher levels were necessary to assist in analytical measurement and tracking of the spiked species. Organic chemicals were chosen for the work with a consideration of how their volatility compares with that of methanol. This was done by comparing the ratio of the pure water Henry’s law coefficient (K h ) of methanol to that of the compound in question (hereafter termed the K h ratio), where ratios above unity indicated less volatility than methanol. Methanol was chosen because it is a common regulated chemical with relatively low volatility but which has been removed by evaporation in previous laboratory work. While organic separation results depend on evaporator design, laboratory experiments verified that organic partitioning to the overhead condensate stream by evaporation is a practical process. The work reported here found difficulties in quantitative analysis of the organic chemicals in aqueous samples. Most of the time there was insufficient analysis to close a mass balance for evaporator runs, but qualitative evidence of carryover was obtained. The methods were also able to show whether organic chemicals were susceptible or resistant to solution oxidation in permanganate or hydrogen peroxide tests.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

The Varestraint test for refractory metals, task 2

The principles of the Varestraint test were applied to the evaluation of refractory metal alloys. This required development of a special test apparatus employing a modest specimen size for improved economy and compatible with the high purity inert atmosphere required for welding these alloys. Minimum specimen size is desirable because of the high cost of these alloys and also to permit timely testing of limited production developmental alloys. The Varestraint apparatus satisfies these requirements by providing a timely and economic test for hot crack sensitivity. This test can be used both for alloy development and production surveillance. The test apparatus was designed for use in vacuum purged dry boxes and is completely compatible with high purity inert atmosphere. Augmented strain can be varied continuously from 1/4% thru 4%. In addition to varying the augmented strain, the primary Varestraint variable, the effect on hot cracking of varying other weld parameters such as unit weld length heat input have also been studied. Test reproducibility, in terms of bending or strain rate, was demonstrated using high speed photography.

Lessmann, G. G.↗

Diffusion in liquid state and solidification of binary system (M-7)

Diffusion is one of the most fundamental physical phenomena. It relates to the manufacturing of almost all materials. Therefore, the precise knowledge of diffusivities of relevant materials is necessary for the optimization of these processes. On the other hand, such knowledge is indispensable to understanding the diffusion mechanism and structure of liquid metal in the field of physical metallurgy. Many diffusion experiments on solid metal were undertaken and a lot of data were accumulated. But on liquid metals there are few measurements because of experimental difficulties, such as thermal convection, induced by very slight temperature gradients in the specimen. Under microgravity conditions, the movement of liquid metal due to density differences and thermal convection must be suppressed markedly. Therefore, the transportation process will be controlled only by the diffusion of constituent atoms. These conditions offer the optimum environments for the diffusion experiment. The experiments are briefly described. Diffusion couples are prepared by attaching end to end two rods of different pure metals using hot press equipment. These couples are inserted into a graphite crucible and then doubly enclosed by two silica ampoules, respectively. The specimen is inserted into a tantalum cartridge, which is welded in a vacuum using an electron-beam apparatus. These cartridges are charged in the continuous heating furnace in space and held at a given temperature for a predetermined time and then solidified. The concentration distribution of elements in these specimens will be measured along the rod axis by means of an electron probe microanalyzer. The counterdiffusivity of the liquid metal binary system is determined on the basis of the compensated concentration distribution profile for thermal contraction.

Dan, T.↗

Apparatus for performing high-temperature fiber push-out testing

The apparatus disclosed in the present invention measures the force at which a fiber resist the motion of an indenter driven at constant speed. This apparatus conducts these test in a vacuum of about 10(exp -6) tort and at temperatures up to 1100 C. Temperature and vacuum environment are maintained while controlling indenter motion, sample position, and providing magnified visual inspection during the test.

Eldridge, Jeffrey I.↗

Apparatus and method for gelling liquefied gasses

The present invention is a method and apparatus for gelling liquid propane and other liquefied gasses. The apparatus includes a temperature controlled churn mixer, vacuum pump, liquefied gas transfer tank, and means for measuring amount of material entering the mixer. The method uses gelling agents such as silicon dioxide, clay, carbon, or organic or inorganic polymers, as well as dopants such as titanium, aluminum, and boron powders. The apparatus and method are particularly useful for the production of high quality rocket fuels and propellants.

Elliott, Adam↗

Insulation-Testing Cryostat With Lifting Mechanism

The figure depicts selected aspects of an apparatus for testing thermal-insulation materials for cryogenic systems at temperatures and under vacuum or atmospheric conditions representative of those encountered in use. This apparatus, called "Cryostat-100," is based on the established cryogen-boil-off calorimeter method, according to which the amount of heat that passes through an insulation specimen to a cryogenic fluid in a container, and thus the effective thermal conductance of the specimen, is taken to be proportional to the amount of the cryogenic fluid that boils off from the container. The design of Cryostat-100 is based partly on, and incorporates improvements over, the design of a similar prior apparatus called "Cryostat-1" described in "Improved Methods of Testing Cryogenic Insulation Materials" (KSC-12107 & KSC- 12108), NASA Tech Briefs, Vol. 24, No. 12 (December 2000), page 46. The design of Cryostat-100 also incorporates the best features of two other similar prior apparatuses called "Cryostat-2" (also described in the cited prior article) and "Cryostat- 4." Notable among the improvements in Cryostat-100 is the addition of a lifting mechanism that enables safe, rapid, reliable insertion and removal of insulation specimens and facilitates maintenance operations that involve lifting. As in Cryostat-1, the cold mass is a vertical stainless-steel cylindrical vessel subdivided into a larger measurement vessel with smaller thermal-guard vessels at both ends. During operation, all three vessels are kept filled with liquid nitrogen near saturation at ambient pressure (temperature .77.4 K). The cold mass of Cryostat-100 has a length of 1 m and diameter of 168 mm. Each specimen has a corresponding nominal length and inner diameter and a nominal thickness of 25.4 mm. Specimens that are shorter and have thicknesses between 0 and 50 mm are also acceptable. Bulk-fill, foam, clam-shell, multilayer insulation, and layered materials can be tested over a very wide range of thermal transmission: apparent thermal conductivity from 0.01 to 60 mW/m-K and heat flux from 0.1 to 500 W/sq m. A test in Cryostat-100 can be conducted at any desired gas pressure between ambient atmospheric pressure at one extreme and a vacuum with residual pressure <10(exp -5) torr (<1.33 10(exp -3) Pa) at the other extreme. The residual gas (and purge gas) is typically nitrogen, but can be any suitable purge gas (e.g., helium, argon, or carbon dioxide). Usually, the temperature on the warm boundary of the insulation specimen is maintained near the ambient value (approximately 293 K), while the boiling of liquid nitrogen at atmospheric pressure in the cold mass maintains the temperature on the cold boundary of the specimen at approximately 77 K.

Fesmire, James↗

Apparatus for producing diamond-like carbon flakes

A vacuum arc from a spot at the face of a graphite cathode to a graphite anode produces a beam of carbon ions and atoms. A carbon coating from this beam is deposited on an ion beam sputtered target to produce diamond-like carbon flakes. A graphite tube encloses the cathode, and electrical isolation is provided by an insulating sleeve. The tube forces the vacuum arc spot to be confined to the surface on the outermost end of the cathode. Without the tube the arc spot will wander to the side of the cathode. This spot movement results in low rates of carbon deposition, and the properties of the deposited flakes are more graphite-like than diamond-like.

Banks, Bruce A.↗

Moisture content and gas sampling device

An apparatus is described for measuring minute quantities of moisture and other contaminants within sealed enclosures such as electronic assemblies which may be subject to large external atmospheric pressure variations. An array of vacuum quality valves is arranged to permit cleansing of the test apparatus of residual atmospheric components from a vacuum source. This purging operation evacuates a gas sample bottle, which is then connected by valve settings to provide the drive for withdrawing a gas sample from the sealed enclosure under test into the sample bottle through a colometric detector tube (Drager tube) which indicates moisture content. The sample bottle may be disconnected and its contents (drawn from the test enclosure) separately subjected to mass spectrograph analysis.

Krieg, H. C., Jr.↗

Insulation Test Cryostat with Lift Mechanism

A multi-purpose, cylindrical thermal insulation test apparatus is used for testing insulation materials and systems of materials using a liquid boil-off calorimeter system for absolute measurement of the effective thermal conductivity (k-value) and heat flux of a specimen material at a fixed environmental condition (cold-side temperature, warm-side temperature, vacuum pressure level, and residual gas composition). The apparatus includes an inner vessel for receiving a liquid with a normal boiling point below ambient temperature, such as liquid nitrogen, enclosed within a vacuum chamber. A cold mass assembly, including the upper and lower guard chambers and a middle test vessel, is suspended from a lid of the vacuum canister. Each of the three chambers is filled and vented through a single feedthrough. All fluid and instrumentation feedthroughs are mounted and suspended from a top domed lid to allow easy removal of the cold mass. A lift mechanism allows manipulation of the cold mass assembly and insulation test article.

Fesmire, James E.↗

Resistively Heated SiC Nozzle for Generating Molecular Beams

An improved nozzle has been developed to replace nozzles used previously in an apparatus that generates a substantially unidirectional beam of molecules passing through a vacuum at speeds of several kilometers per second. The basic principle of operation of the apparatus is the same for both the previous and the present nozzle designs. The main working part of the nozzle is essentially a cylinder that is closed except that there is an inlet for a pressurized gas and, at one end, the cylinder is closed by a disk that contains a narrow central hole that serves as an outlet. The cylinder is heated to increase the thermal speeds of the gas molecules into the desired high-speed range. Heated, pressurized gas escapes through the outlet into a portion of the vacuum chamber that is separated, by a wall, from the rest of the vacuum chamber. In this portion of the vacuum chamber, the gas undergoes a free jet expansion. Most of the expanded gas is evacuated and thus does not become part of the molecular beam. A small fraction of the expanded beam passes through a narrow central orifice in the wall and thereby becomes a needle- thin molecular beam in the portion of the vacuum on the downstream side of the wall.

Cagiano, Steven↗

High-temperature compressive creep tests of U 3 Si 2 with spark plasma sintering: Experiments and finite element modeling

This paper reports a systematic high-temperature creep behavior of dense U 3 Si 2 pellets using a spark plasma sintering (SPS) apparatus at elevated temperatures and pressures under vacuum conditions. The stress exponent was subsequently derived to be 3.21 at 1173 K and 2.17 at 1223 K, respectively, indicating a grain boundary sliding creep mechanism. The creep activation energy was determined to be 203.6 ± 19.0 kJ/mol, which agrees well with the literature. Finite element modeling was performed using the creep parameters fitted from the strain-time plot. Additionally, the results suggest an excellent match with the experimental data, confirming the validity of the experiments. Microstructure characterizations indicate that the main phase of the specimens after creep tests remains to be U 3 Si 2 , with a 4 μm thick layer of nano-sized particles induced from the diffusion between U 3 Si 2 and alumina disc used to avoid electric current passing through the sample. The successful conduct of creep experiments demonstrates the great potential of SPS to perform high-temperature mechanical testing of nuclear fuels under vacuum conditions. The subsequent finite element modeling exhibits excellent capabilities for accurately predicting material performance in the creep tests and provides a practical tool in evaluating nuclear fuels’ performance for a much-extended time scale.

36 MATERIALS SCIENCE↗

Experimental studies of high-temperature thermal dissociation of iso-propanol

iso-Propanol is an important biofuel for transportation and industrial applications, as well as a canonical compound for understanding alcohol reaction chemistry. There are few studies of the thermal decomposition of iso-propanol, hence the objective of this work was to investigate the mechanism of iso-propanol pyrolysis at high-temperature conditions. Shock tube studies were used to investigate the thermal decomposition of iso-propanol and identify the dominant reaction pathways and the intermediate species present in the temperature range of 1395–2053 K and at pressures of 0.3–4 bar. Time-resolved mass spectra were obtained from pyrolysis experiments in shock tube/mass spectrometer apparatuses using electron impact ionization or synchrotron vacuum ultraviolet photoionization. The relative concentrations of the intermediate species were used to identify the dominant reaction channels. iso-Propanol dissociated by water loss to propene and by elimination of a methyl radical yielding a 1-hydroxyethyl radical at the conditions studied. The time-dependent mass spectra allowed secondary products to be identified along with the orders of appearance. Notably, peaks at m/z = 50 and 52 were observed providing insight into secondary reactions. These features have not been previously reported in propanol-pyrolysis literature.

Kim, John H. [Univ. of Michigan, Ann Arbor, MI (Un↗

A superconducting gyroscope to test Einstein's general theory of relativity

Schiff (1960) proposed a new test of general relativity based on measuring the precessions of the spin axes of gyroscopes in earth orbit. Since 1963 a Stanford research team has been developing an experiment to measure the two effects calculated by Schiff. The gyroscope consists of a uniform sphere of fused quartz 38 mm in diameter, coated with superconductor, electrically suspended and spinning at about 170 Hz in vacuum. The paper describes the proposed flight apparatus and the current state of development of the gyroscope, including techniques for manufacturing and measuring the gyro rotor and housing, generating ultralow magnetic fields, and mechanizing the readout.

Everitt, C. W. F.↗

Concentrating Gaseous Contaminants For Monitoring

Apparatus concentrates contaminants outgassing from specimens in vacuum and passes concentrated contaminants to gas-chromatography/mass-spectrometry system for analysis. Cold wall of collection chamber adsorbs gases from specimen in isothermal cell. When wall heated, plate desorbs gases so they can be analyzed. Collection chamber maintained at low pressure throughout adsorption and desorption process. Determines whether candidate materials for use in vacuum environments generate harmful substances.

Mahone, William C.↗

Outgassing Data for Selecting Spacecraft Materials

This tenth compilation of outgassing data of materials intended for spacecraft use supersedes Reference Publication 1124, Revision 2, November 1990. The data were obtained at the Goddard Space Flight Center (GSFC), utilizing equipment developed at Stanford Research Institute (SRI) under contract to the Jet Propulsion Laboratory (JPL). SRI personnel developed an apparatus for determining the mass loss in vacuum and for collecting the outgassed products. The outgassing data have been presented in three different ways in order to facilitate material selection. In Section A, the materials are divided by category into the 18 probable uses, such as adhesives, greases, paints, potting compounds, and so forth. In Section B, all the materials contained in Section A are listed in alphabetical order by the manufacturer's identification. In Section C, the only materials listed are those having 'Total Mass Loss' (TML) and Collected Volatile Condensable Materials (CVCM) equal to or lower than a maximum 1.0 percent TML and a maximum 0.10 percent CVCM. These are grouped by use, as in Section A.

Campbell, William A., Jr.↗

Improved Apparatus for Testing Monoball Bearings

A desk-sized apparatus for testing monoball bearings and their lubricants offers advantages, relative to prior such apparatuses, of (1) a greater degree of automation and (2) capability of operation under wider and more realistic ranges of test conditions. The ranges of attainable test conditions include load from 100 to greater h than 50,000 lb (445 to greater than 2.22 x 10(exp 5) N), resisting torque up to 30,000 lb-in. (approximately equal to 3,390 N-m), oscillating rotation through an angle as large as 280 degrees, and oscillation frequency from 0 to 6 Hz. With addition of some components and without major modification of the apparatus, it is also possible to perform tests under environmental conditions that include temperature from -320 to 1,000 F (-196 to +538 C), relative humidity from 0 to 100 percent, and either air at ambient pressure, high vacuum, or an atmosphere of monatomic oxygen. In the apparatus (see Figure 1), a monoball bearing specimen is driven in oscillating rotation by a hydraulic rotary actuator through a series of shafts, one of which incorporates a torque meter and one of which is a flexible coupling. The torque meter measures the resisting torque; the flexible coupling accommodates misalignment, wear, and compression of the specimen and ensures equal loading on opposite sides of the monoball. Not shown in the figure is an angular-position sensor that is used for measuring the angle of rotation of the shafts.

Hall, Phillip B.↗

Optical multiple sample vacuum integrating sphere

An integrating sphere comprised of a uniform difusely reflecting spherical cavity, having mutually transverse input and output ports, and a linear sample transport mechanism is described. The sample transport mechanism is secured so that the multiple samples can be brought into registration with the input port, one at a time, without having to open or disassemble the apparatus when a change of sample is desired. A vacuum tight seal is provided between the cavity and the transport mechanism. This maintains the integrity of a vacuum generated with the sphere when attached to the source of optical energy. The device is utilized to test emissive characteristics such as the relative fluorescence quantum efficiency of a dye sample placed in the path of a monochromatic optical energy source coupled to the input port while having a light detector coupled to the output port.

Butner, C. L.↗