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NASA NTRS1985

Collection and analysis of NASA clean room air samples

The environment of the HALOE assembly clean room at NASA Langley Research Center is analyzed to determine the background levels of airborne organic compounds. Sampling is accomplished by pumping the clean room air through absorbing cartridges. For volatile organics, cartridges are thermally desorbed and then analyzed by gas chromatography and mass spectrometry, compounds are identified by searching the EPA/NIH data base using an interactive operator INCOS computer search algorithm. For semivolatile organics, cartridges are solvent entracted and concentrated extracts are analyzed by gas chromatography-electron capture detection, compound identification is made by matching gas chromatogram retention times with known standards. The detection limits for the semivolatile organics are; 0.89 ng cu m for dioctylphlhalate (DOP) and 1.6 ng cu m for polychlorinated biphenyls (PCB). The detection limit for volatile organics ranges from 1 to 50 parts per trillion. Only trace quantities of organics are detected, the DOP levels do not exceed 2.5 ng cu m and the PCB levels do not exceed 454 ng cu m.

Sheldon, L. S.↗

DOE OSTI2022

Developments and Challenges in the Design of the ITER DRGA

We report the ITER Diagnostic Residual Gas Analyzer (DRGA) will measure the distribution of gas species, i.e., deuterium (D), tritium (T), and impurities, in the divertor exhaust stream and in the plasma periphery, with time resolution relevant to fusion plasma–wall particle dynamics. The uniqueness of the DRGA, over previous implementations of plasma dynamics residual gas analysis, is an integrated approach, combining mass and low-temperature plasma-activated optical spectroscopy, in a differentially pumped analysis station. A further unique feature of the ITER divertor-specific DRGA is an ~8-m separation of the analysis station from the sampled pumping duct, while still maintaining a ~1-s response time for hydrogen isotopic concentrations. ITER DRGA final design activities are strongly benefiting from testing of prototypical DRGA components and methods on present fusion devices, most currently on JET and W7-X. DRGA systems are implemented on both these devices and include sensors (and pumping methods) that are directly relevant to the ITER DRGA design. The recent JET-DTE2 campaign has provided the first experience on operating the combined ITER DRGA sensors with D-T plasmas. While enhancing system design for ITER, this experience on operating devices has also revealed additional engineering challenges, which further guide the continuing final design project. Meanwhile, the recent determination that the ITER DRGA, with slight optimization, will resolve the helium isotopes well enough to support an ITER pre-DT, He-3-based heating scheme, has greatly increased ITER Research Program interest in the DRGA and its implementation well ahead of the DT phase.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry

Detection of surface contamination on niobium materials used in superconducting radio frequency (SRF) applications is difficult due to quantitative sensitivity and near-atomic depth resolution needed. Inspection of samples known to have experienced surface contamination was found to have inconsistent nitride coverage after high-temperature nitrogen gas exposure (“doping”). Here we compare contaminating species found on samples treated in several different vacuum furnaces, both “exposed” directly in the chamber and “protected” by containment shielding from evaporative sources with “furnace caps.” Typically, furnace caps are used to impede contamination from reaching the interior surface of cavities during the high-temperature vacuum bake that immediately precedes exposure to nitrogen gas. Although, to date, little is known about the effectiveness of these caps, SIMS results showed that they were effective in limiting contamination arising from the furnace environment. Inspection of sample surfaces by SEM showed a lack of nitrides present on contaminated specimens. TEM with energy dispersive spectroscopy performed on these samples revealed that a carbon-rich layer now existed, indicating that a relatively high contaminant load prevents the nucleation and growth of surface nitrides, while thus inhibiting interstitial nitrogen uptake. Except in extreme cases, subsequent removal of the top several micrometers of the surface via electropolishing appears to effectively eliminate any strong influence on the subsequent SRF cavity performance. With the absence of furnace cleaning, carbon contamination was found to be nearly 10× higher for protected nitrogen-doped and electropolished samples, with minimal metallic contamination detected for both processes. SIMS analysis was also performed to compare the cleanliness of samples fully prepared by such nitrogen “doping” with those prepared by a related process, involving the dissolution of niobium surface oxide and diffusion of oxygen into the surface. This oxygen doping or alloying process offers attractive advantages.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1986

Analysis and composition of a model trace gaseous mixture for a spacecraft

Growing concern over trace gaseous contaminant accumulations in the enclosed atmospheres of long duration spacecraft missions has prompted the development of a trace contaminant data base on the basis of gas, lithium hydroxide, and charcoal samples collected on Space Shuttle missions. A model trace contaminant gas mixture containing 14 compounds was chosen with the aid of a FORTRAN program, on the strength of contaminant chemical and toxicological categories, frequency of occurrence, and worst-case concentration. The model gas mixture can be used to test trace contaminant control hardware for a manned spacecraft environment.

Schwartz, M. R.↗

DOE OSTI2023

Equilibrated Gas and Carbonate Standard‐Derived Dual (Δ 47 and Δ 48 ) Clumped Isotope Values

Abstract Carbonate clumped isotope geochemistry has primarily focused on mass spectrometric determination of m/z 47 CO 2 for geothermometry, but theoretical calculations and recent experiments indicate paired analysis of the m/z 47 ( 13 C 18 O 16 O) and m/z 48 ( 12 C 18 O 18 O) isotopologues (referred to as Δ 47 and Δ 48 ) can be used to study non‐equilibrium isotope fractionations and refine temperature estimates. We utilize 5,448 Δ 47 and 3,400 Δ 48 replicate measurements of carbonate samples and standards, and 183 Δ 47 and 195 Δ 48 replicate measurements of gas standards from 2015 to 2021 from a multi‐year and multi‐instrument data set to constrain Δ 47 and Δ 48 values for 27 samples and standards, including Devils Hole cave calcite, and study equilibrium Δ 47 ‐Δ 48 , Δ 47 ‐temperature, and Δ 48 ‐temperature relationships. We compare results to previously published findings and calculate equilibrium regressions based on data from multiple laboratories. We report acid digestion fractionation factors, Δ* 63‐47 and Δ* 64‐48 , and account for their dependence on the initial clumped isotope values of the mineral.

58 GEOSCIENCES↗

DOE OSTI2022

Comparative Evaluation of Microwave and Conventional Gasification of Different Coal Types: Experimental Reaction Studies

Here, effects of gasifier conditions (microwave or conventional) on the gasification characteristics of four different types of coal are evaluated by analysis of gaseous species generated during pyrolysis and gasification reactions. Four different coal samples are tested: a lignite (Mississippi), a low-ash subbituminous (Wyodak), a high-ash subbituminous (Usibelli), and a low volatile bituminous (Pocahontas #3). Gas composition, overall yields, carbon conversion efficiency, and cold gas efficiency are evaluated to compare gasification reactivity of the different coal types under microwave and conventional heating. During microwave pyrolysis (Ar atmosphere), greater selectivity of syngas species (H2 + CO) and greater overall non-condensable gas yields are observed, compared to conventional pyrolysis for all coals tested. The high yield of syngas during microwave pyrolysis is attributed to primary pyrolysis gases subsequently gasifying the char of the same sample to produce greater amounts of H2 and CO. During microwave gasification (CO2 atmosphere), selective heating and formation of hotspots within the coal enable the reverse Boudouard reaction to occur at a low bulk gasification temperature of 700 °C, which is less favorable under thermal gasification at this temperature. Yields of syngas are much higher under microwave gasification of all coals. Carbon conversion is found to have a linear correlation with volatile matter of the parent coal. Carbon conversion and cold gas efficiency are highest for coals gasified under microwave irradiation, and gasification reactivity of the four coals was determined to be dependent on the coal type.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

Standardized multi-omics of Earth’s microbiomes reveals microbial and metabolite diversity

Despite advances in sequencing, lack of standardization makes comparisons across studies challenging and hampers insights into the structure and function of microbial communities across multiple habitats on a planetary scale. Here we present a multi-omics analysis of a diverse set of 880 microbial community samples collected for the Earth Microbiome Project. We include amplicon (16S, 18S, ITS) and shotgun metagenomic sequence data, and untargeted metabolomics data (liquid chromatography-tandem mass spectrometry and gas chromatography mass spectrometry). We used standardized protocols and analytical methods to characterize microbial communities, focusing on relationships and co-occurrences of microbially related metabolites and microbial taxa across environments, thus allowing us to explore diversity at extraordinary scale. In addition to a reference database for metagenomic and metabolomic data, we provide a framework for incorporating additional studies, enabling the expansion of existing knowledge in the form of an evolving community resource. We demonstrate the utility of this database by testing the hypothesis that every microbe and metabolite is everywhere but the environment selects. Our results show that metabolite diversity exhibits turnover and nestedness related to both microbial communities and the environment, whereas the relative abundances of microbially related metabolites vary and co-occur with specific microbial consortia in a habitat-specific manner. We additionally show the power of certain chemistry, in particular terpenoids, in distinguishing Earth’s environments (for example, terrestrial plant surfaces and soils, freshwater and marine animal stool), as well as that of certain microbes including Conexibacter woesei (terrestrial soils), Haloquadratum walsbyi (marine deposits) and Pantoea dispersa (terrestrial plant detritus). This Resource provides insight into the taxa and metabolites within microbial communities from diverse habitats across Earth, informing both microbial and chemical ecology, and provides a foundation and methods for multi-omics microbiome studies of hosts and the environment.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2018

Abstract for CRADA between Solar Turbines Incorporated and NETL

The National Energy Technology Laboratory is developing the Raman Gas Analyzer (RGA) to be a fast, non-destructive instrument for on-line measurement of gas composition. The RGA has been demonstrated to have an extremely fast response (<1 second) multi-gas analysis capability. All but the noble gases are Raman active, but Raman interaction is weak with gas phase substances. The RGA uses a reflectively lined capillary as the optical cell in a patented configuration, providing both a small sample volume for fast gas exchange, and a much greater Raman signal collection than traditional instrument configurations. This allows very fast measurement of fuel gases (hydrogen, methane, ethane, propane) as well as other common industrial gases (including CO, CO2, N2, O2, H2O). The RGA provides a new enabling technology for faster, smarter process control based on the chemical composition of the gases in the process, such as improving fuel flexibility and efficiency for power generation systems. NETL has constructed a field prototype of the RGA to test the instrument performance in various applications in fossil energy. The objective of this CRADA is to field test the Raman Gas Analyzer in a commercial or near-commercial gas turbine application, to advance its Technology Readiness Level and support technology transfer to the commercial marketplace.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

Long term monitoring of methane in the atmosphere by multiplex gas chromatography

Methane is of interest in the study of the Earth's atmosphere because of its implication in the future global warming of the surface. This warming is produced by the absorption of infrared energy by trace gases. It has been estimated that in the next 40 to 50 years, methane could contribute 20 to 25 pct. as much atmospheric warming as that expected from carbon dioxide increases. Studies to examine sources, sinks, and cycles of methane will require analytical methods capable of continuous unattended measurement with temporal resolution of an hour or less for weeks at a time. Gas chromatography (GC) is one of the most practical methods available to conduct the analysis of air, but limitations in this technique still exist which can be alleviated with multiplex GC (MGC). MGC is a technique where many samples are pseudo-randomly introduced to the chromatograph without regard to the length of time required for an analysis. The resulting data must then be reduced using computational methods such as cross correlation. In the technique reported, a tube packed with silver oxide was used at the inlet of the GC column to create concentration pulses of methane in a sample stream of air. By using only one carrier, i.e., ambient air, an effective and accurate method to monitor the variations in concentration of methane in the atmosphere over long periods of time was developed. Methane in ambient air was monitored for an eight day period and an interesting temporal variability was found. This work has shown the utility of a relatively simple MGC for the analysis of a real environmental sample.

Valentin, Jose R.↗

NASA NTRS2011

Search for Chemical Biomarkers on Mars Using the Sample Analysis at Mars Instrument Suite on the Mars Science Laboratory

One key goal for the future exploration of Mars is the search for chemical biomarkers including complex organic compounds important in life on Earth. The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) will provide the most sensitive measurements of the organic composition of rocks and regolith samples ever carried out in situ on Mars. SAM consists of a gas chromatograph (GC), quadrupole mass spectrometer (QMS), and tunable laser spectrometer to measure volatiles in the atmosphere and released from rock powders heated up to 1000 C. The measurement of organics in solid samples will be accomplished by three experiments: (1) pyrolysis QMS to identify alkane fragments and simple aromatic compounds; pyrolysis GCMS to separate and identify complex mixtures of larger hydrocarbons; and (3) chemical derivatization and GCMS extract less volatile compounds including amino and carboxylic acids that are not detectable by the other two experiments.

Glavin, D. P.↗

NASA NTRSDate not supplied

Real Time Nitrogen Monitoring and Quality Control System for NASA Astromaterials Collection

The Nitrogen system is a vital utility supporting the curation office within NASA's Astromaterials Re-search and Exploration Science (ARES) Division at the Johnson Space center (JSC). Since the Apollo samples were returned in 1969. It has played an essential role in preserving NASA’s astromaterial collections (now nine collections) by maintaining contamination-free, controlled environments required for long term curation and advanced scientific research. To meet the stringent purity requirements for contamination control, high purity modified Grade C Liquid Nitrogen (LN2) is delivered weekly by an industrial gas vendor to a 15,000-gallon tank located outside at NASA JSC near the ARES facility. This nitrogen is vital for creating an inert atmosphere to store the collection in, ensuring they are continuously shielded from contaminants and alterations through a constant N2purge. For most of the past 65 years deliveries of LN2 have required a CoA (Certificate of Analysis) prior to delivery. If those were not available, then LN2 deliver were sent to third-party laboratories for verification, creating an operational bottleneck and quality gap. To address this challenge and maintain rigorous quality control, NASA JSC Infrastructure and Astromaterials Acquisition & Curation Office initiated the development of an on-site Analytical Gas Sampling (AGS) Laboratory. Designed to streamline quality verification if a CoA unavailable, the AGS lab was constructed by a subcontractor in Newton, NJ. After a successful factory acceptance test conducted by the NASA ARES Infrastructure team, the lab was trans-ported to NASA JSC, where it was anchored and integrated into the site’s nitrogen pressure system using stainless steel, oxygen-cleaned tubing. The ARES nitrogen system was modified to provide parallel flows to the AGS lab for quality control and to the astromaterials collection labs for maintaining an inert environment. The AGS lab features two operational modes: (1)Primary: Gaseous Nitrogen (GN2) Quality Monitoring –The AGS system continuously samples the site’s GN2 supply every 15 minutes to ensure compliance with required purity levels. (2) Secondary: LN2 Quality Verification when a comprehensive CoA is not available, a cryogenic vaporizer converts LN2 to GN2, which is then analyzed for impurities: H₂, Ar, O₂, CO, CO₂, H₂O, and total hydrocarbons (THC). By significantly enhancing on-site analytical capabilities, the AGS lab eliminates reliance on external testing, ensures uninterrupted quality monitoring of the nitrogen pressure system, and reinforces NASA’s commitment to preserving pristine astromaterials under the highest standards of curation and research integrity.

glove box↗

NASA NTRS1993

The effects of flaring in H1 on the observed velocity field of spirals

This work is part of a larger project in which we want to determine the shapes of dark halos around spiral galaxies. Rotation curves 'probe' the halos in the radial direction. The derived halo mass distributions are badly constrained. The local halo densities fully determine the width of the gas distribution once the gaseous velocity dispersion is known. There where the dark halo dominates, the Full Width at Half Maximum (FWHM) of the gas layer is proportional to (rho(sub halo))(exp -0.5). Therefore, measuring the width of the gas layer probes the halo density directly. In a dark halo dominated potential, the FWHM of the gas layer increases linearly with radius. This increase of the thickness of the gas layer is known as 'flaring'. Flaring has been found inside the stellar disk. Beyond the edge of the stellar disk, the analysis is hampered by the onset of the warp. Since the galaxy we are studying, NGC 4244, has no significant warp we hope to extend Rupen's analysis into the halo dominated regime. The usual method to derive a rotation curve from an observed 2-dimensional velocity field is to assume that the hydrogen is distributed in infinitely thin rings. For a flaring disk, any line of sight samples many different parts of the galaxy, all having different densities and projected velocities. In order to fully exploit the information contained in the gas distribution, we have to understand the effects of flaring on the observables (the spectrum for each point of the galaxy). We have investigated the effects of a flaring disk on the observed velocity field. It is obvious that the largest (kinematical) effects are to be expected for low density dark halos at large inclinations. For low mass galaxies we expect that the flaring of the H1 layer will have a major effect on the observed kinematics. For galaxy with intermediate V(sub max,halo) seen at intermediate inclinations, one overestimates Vsin(i) typically by a few percent. For more massive galaxies, any effects arising from the flaring H1 layer are minuscule unless the inclination is not too far from 90 deg.

Olling, Rob↗

NASA NTRS1993

Verification of thermal analysis codes for modeling solid rocket nozzles

One of the objectives of the Solid Propulsion Integrity Program (SPIP) at Marshall Space Flight Center (MSFC) is development of thermal analysis codes capable of accurately predicting the temperature field, pore pressure field and the surface recession experienced by decomposing polymers which are used as thermal barriers in solid rocket nozzles. The objective of this study is to provide means for verifications of thermal analysis codes developed for modeling of flow and heat transfer in solid rocket nozzles. In order to meet the stated objective, a test facility was designed and constructed for measurement of the transient temperature field in a sample composite subjected to a constant heat flux boundary condition. The heating was provided via a steel thin-foil with a thickness of 0.025 mm. The designed electrical circuit can provide a heating rate of 1800 W. The heater was sandwiched between two identical samples, and thus ensure equal power distribution between them. The samples were fitted with Type K thermocouples, and the exact location of the thermocouples were determined via X-rays. The experiments were modeled via a one-dimensional code (UT1D) as a conduction and phase change heat transfer process. Since the pyrolysis gas flow was in the direction normal to the heat flow, the numerical model could not account for the convection cooling effect of the pyrolysis gas flow. Therefore, the predicted values in the decomposition zone are considered to be an upper estimate of the temperature. From the analysis of the experimental and the numerical results the following are concluded: (1) The virgin and char specific heat data for FM 5055 as reported by SoRI can not be used to obtain any reasonable agreement between the measured temperatures and the predictions. However, use of virgin and char specific heat data given in Acurex report produced good agreement for most of the measured temperatures. (2) Constant heat flux heating process can produce a much higher heating rate than the radiative heating process. The results show that heating rates of 125 C/s (225 F/s) can be achieved. (3) The electrical resistance of the FM 5055 samples were about 150 Omega in the virgin state, and decreased to about 35 Omega when charred. A reliable scheme must be developed to electrically insulate the composite from the heater foil in order to prevent any current leakage into the sample which can result in volumetric heating of the char zone of the composite.

Keyhani, M.↗

NASA NTRS1972

Analysis of organogenic compounds in Apollo 11, 12, and 14 lunar samples.

DCl was used to distinguish hydrocarbons produced by acid treatment from hydrocarbons originally present in the samples when volatiles released by acid and thermal treatments from Apollo 11, 12, and 14 lunar samples were studied by quadrupole mass spectrometry and gas chromatography mass spectrometry. Multiple ion plotting permitted separation of deuterated from nondeuterated hydrocarbons in the DCl products. Stepwise thermal treatment was used to distinguish the source of the volatile compounds. The presence of LM rocket exhaust products was traced in two samples, and the presence of high-temperature stable nitrides in some samples is indicated.

Flory, D. A.↗

NASA NTRS1990

Analysis of pressure-broadened ozone spectra in the 3 micron region

The Molecular Spectroscopy Lab at NASA-Langley has been involved in a long term effort to carefully characterize the infrared spectra of small molecules of atmospheric interest, including methane, water vapor, ozone, and their isotopic counterparts. High resolution gas phase infrared spectra are obtained using both a tunable diode laser system, and the McMath Fourier transform spectrometer at the Kitt Peak Solar Observatory. Spectra are obtained at various pressures and temperatures for pure gas samples, and for samples containing mixtures of the species of interest in nitrogen, oxygen, or air. From these spectra, using a nonlinear least squares fitting technique, spectral parameters of position, intensity, and half-width were determined for varying laboratory conditions that approximate atmospheric conditions experienced in remote sensing situations. These parameters are of interest in theoretical studies of these species, as well as in allowing more accurate interpretation of remote sensing data. The current work involves the analysis of a series of McMath FTIR spectra of ozone broadened by mixing with air, nitrogen, or oxygen. Each spectrum covers the region from 2396 to 4057/cm. Each vibrational band is analyzed by first diving its region into small intervals containing a few well isolated absorption lines of reasonable intensity. Each of these small intervals is fit by multiple iterations of the nonlinear least square program until residuals are minimized to a reasonable value which corresponds to the noise level of the measured spectrum. Intervals for the 3 nu(sub 3) ozone band in the region from 3000 to 3060 wavenumbers are being examined.

Prochaska, Eleanor S.↗

DOE OSTI2017

Molecular Outflows in Local ULIRGs: Energetics from Multitransition OH Analysis

We report on the energetics of molecular outflows in 14 local ultraluminous infrared galaxies (ULIRGs) that show unambiguous outflow signatures (P Cygni profiles or high-velocity absorption wings) in the far-infrared lines of OH measured with the Herschel/PACS spectrometer. All sample galaxies are gas-rich mergers at various stages of the merging process. Detection of both ground-state (at 119 and 79 μm) and one or more radiatively excited (at 65 and 84 μm) lines allows us to model the nuclear gas (≲300 pc) and the more extended components using spherically symmetric radiative transfer models. Reliable models and the corresponding energetics are found in 12 of the 14 sources. The highest molecular outflow velocities are found in buried sources, in which slower but massive expansion of the nuclear gas is also observed. With the exception of a few outliers, the outflows have momentum fluxes of (2–5) × L {sub IR}/c and mechanical luminosities of (0.1–0.3)% of L {sub IR}. The moderate momentum boosts in these sources (≲3) suggest that the outflows are mostly momentum driven by the combined effects of active galactic nuclei (AGNs) and nuclear starbursts, as a result of radiation pressure, winds, and supernova remnants. In some sources (∼20%), however, powerful (10{sup 10.5–11} L {sub ⊙}) AGN feedback and (partially) energy-conserving phases are required, with momentum boosts in the range of 3–20. These outflows appear to be stochastic, strong AGN feedback events that occur throughout the merging process. In a few sources, the outflow activity in the innermost regions has subsided in the past ∼1 Myr. While OH traces the molecular outflows at subkiloparsec scales, comparison of the masses traced by OH with those previously inferred from tracers of more extended outflowing gas suggests that most mass is loaded (with loading factors of M-dot /SFR=1--10) from the central galactic cores (a few × 100 pc), qualitatively consistent with an ongoing inside-out quenching of star formation. Outflow depletion timescales are <10{sup 8} yr, shorter than the gas consumption timescales by factors of 1.1–15, and are anticorrelated with the AGN luminosity.

79 ASTRONOMY AND ASTROPHYSICS↗

NASA NTRS1973

Monte-Carlo analysis of rarefied-gas diffusion including variance reduction using the theory of Markov random walks

Molecular diffusion through a rarefied gas is analyzed by using the theory of Markov random walks. The Markov walk is simulated on the computer by using random numbers to find the new states from the appropriate transition probabilities. As the sample molecule during its random walk passes a scoring position, which is a location at which the macroscopic diffusing flow variables such as molecular flux and molecular density are desired, an appropriate payoff is scored. The payoff is a function of the sample molecule velocity. For example, in obtaining the molecular flux across a scoring position, the random walk payoff is the net number of times the scoring position has been crossed in the positive direction. Similarly, when the molecular density is required, the payoff is the sum of the inverse velocity of the sample molecule passing the scoring position. The macroscopic diffusing flow variables are then found from the expected payoff of the random walks.

Perlmutter, M.↗

DOE OSTI2019

3013 Inner Can Lid Leak Test System Development

Contained in this report is a description of the 3013 inner container lid leak detection system, a listing of the data collected to validate the system and a statistical analysis of collected data. The 3013 Container Surveillance Program provides assessment criteria and evaluates 3013 containers selected from the storage inventory for potential degradation mechanisms. The 3013 outer container is the boundary credited to prevent release of material to the environment. The integrity of the outer container is only at risk if the inner container loses its seal and allows corrosive gases to diffuse into the outer container. To date, the determination of potential outer container exposure to corrosive gases has been through comparison of the gas analysis of the annular space and the inner container. If the two volumes have the same gas composition and pressure, then the inner container may have leaked. The leak detection system described in this report will provide a direct measurement of the integrity of the inner container, and if approved, will provide for the elimination of gas analysis. The inner container lid leak testing system consists of two basic parts: the Agilent leak testing instrument and the leak test fixture. The test fixture base provides the connection between the leak test instrument and the test sample. This connection allows helium to flow into the leak detector when a leak path exists in the test sample allowing leak measurement to be performed. The tests reported here were conducted in a cold lab using a configuration very similar, but not identical to, the configuration anticipated when installed in a glove box. A total of sixty-five leak rate measurements were made on 10 containers and the data is included in the report. The data analysis shows that the leak detection system can identify leaks in the lid, including the weld and heat affected zone of 3013 inner containers, during destructive examination. The measurements taken support that a 3013 IC lid with a leak rate value greater than 2.0 x 10 -7 atm cc/sec will be identified using the leak test system prior to introduction into a glove box. These results from the baseline for future tests of the leak test system after it is installed in the glove box for use as part of surveillance DE.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗